[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 2018 Edition]
[From the U.S. Government Publishing Office]



[[Page i]]

          
          
          Title 40

Protection of Environment


________________________

Parts 136 to 149

                         Revised as of July 1, 2018

          Containing a codification of documents of general 
          applicability and future effect

          As of July 1, 2018
                    Published by the Office of the Federal Register 
                    National Archives and Records Administration as a 
                    Special Edition of the Federal Register

[[Page ii]]

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[[Page iii]]




                            Table of Contents



                                                                    Page
  Explanation.................................................       v

  Title 40:
          Chapter I--Environmental Protection Agency 
          (Continued)                                                3
  Finding Aids:
      Table of CFR Titles and Chapters........................    1059
      Alphabetical List of Agencies Appearing in the CFR......    1079
      List of CFR Sections Affected...........................    1089

[[Page iv]]





                     ----------------------------

                     Cite this Code: CFR
                     To cite the regulations in 
                       this volume use title, 
                       part and section number. 
                       Thus, 40 CFR 136.1 refers 
                       to title 40, part 136, 
                       section 1.

                     ----------------------------

[[Page v]]



                               EXPLANATION

    The Code of Federal Regulations is a codification of the general and 
permanent rules published in the Federal Register by the Executive 
departments and agencies of the Federal Government. The Code is divided 
into 50 titles which represent broad areas subject to Federal 
regulation. Each title is divided into chapters which usually bear the 
name of the issuing agency. Each chapter is further subdivided into 
parts covering specific regulatory areas.
    Each volume of the Code is revised at least once each calendar year 
and issued on a quarterly basis approximately as follows:

Title 1 through Title 16.................................as of January 1
Title 17 through Title 27..................................as of April 1
Title 28 through Title 41...................................as of July 1
Title 42 through Title 50................................as of October 1

    The appropriate revision date is printed on the cover of each 
volume.

LEGAL STATUS

    The contents of the Federal Register are required to be judicially 
noticed (44 U.S.C. 1507). The Code of Federal Regulations is prima facie 
evidence of the text of the original documents (44 U.S.C. 1510).

HOW TO USE THE CODE OF FEDERAL REGULATIONS

    The Code of Federal Regulations is kept up to date by the individual 
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    To determine whether a Code volume has been amended since its 
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OMB CONTROL NUMBERS

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Federal agencies to display an OMB control number with their information 
collection request.

[[Page vi]]

Many agencies have begun publishing numerous OMB control numbers as 
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PAST PROVISIONS OF THE CODE

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this volume.

[[Page vii]]

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    Oliver A. Potts,
    Director,
    Office of the Federal Register
    July 1, 2018







[[Page ix]]



                               THIS TITLE

    Title 40--Protection of Environment is composed of thirty-seven 
volumes. The parts in these volumes are arranged in the following order: 
Parts 1-49, parts 50-51, part 52 (52.01-52.1018), part 52 (52.1019-
52.2019), part 52 (52.2020-end of part 52), parts 53-59, part 60 (60.1-
60.499) , part 60 (60.500-end of part 60, sections), part 60 
(Appendices), parts 61-62, part 63 (63.1-63.599), part 63 (63.600-
63.1199), part 63 (63.1200-63.1439), part 63 (63.1440-63.6175), part 63 
(63.6580-63.8830), part 63 (63.8980-end of part 63), parts 64-71, parts 
72-79, part 80, part 81, parts 82-86, parts 87-95, parts 96-99, parts 
100-135, parts 136-149, parts 150-189, parts 190-259, parts 260-265, 
parts 266-299, parts 300-399, parts 400-424, parts 425-699, parts 700-
722, parts 723-789, parts 790-999, parts 1000-1059, and part 1060 to 
end. The contents of these volumes represent all current regulations 
codified under this title of the CFR as of July 1, 2018.

    Chapter I--Environmental Protection Agency appears in all thirty-
seven volumes. Regulations issued by the Council on Environmental 
Quality, including an Index to Parts 1500 through 1508, appear in the 
volume containing parts 1060 to end. The OMB control numbers for title 
40 appear in Sec.  9.1 of this chapter.

    For this volume, Cheryl E. Sirofchuck was Chief Editor. The Code of 
Federal Regulations publication program is under the direction of John 
Hyrum Martinez, assisted by Stephen J. Frattini.

[[Page 1]]



                   TITLE 40--PROTECTION OF ENVIRONMENT




                  (This book contains parts 136 to 149)

  --------------------------------------------------------------------
                                                                    Part

chapter i--Environmental Protection Agency (Continued)......         136

[[Page 3]]



         CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)




  --------------------------------------------------------------------


  Editorial Note: Nomenclature changes to chapter I appear at 65 FR 
47324, 47325, Aug. 2, 2000, and at 66 FR 34375, 34376, June 28, 2001.

                SUBCHAPTER D--WATER PROGRAMS (CONTINUED)
Part                                                                Page
136             Guidelines establishing test procedures for 
                    the analysis of pollutants..............           5
140             Marine sanitation device standard...........         420
141             National primary drinking water regulations.         424
142             National primary drinking water regulations 
                    implementation..........................         735
143             National secondary drinking water 
                    regulations.............................         795
144             Underground injection control program.......         800
145             State UIC program requirements..............         869
146             Underground injection control program: 
                    Criteria and standards..................         882
147             State, tribal, and EPA-administered 
                    underground injection control programs..         935
148             Hazardous waste injection restrictions......        1042
149             Sole source aquifers........................        1051

[[Page 5]]



                 SUBCHAPTER D_WATER PROGRAMS (CONTINUED)





PART 136_GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS 
OF POLLUTANTS--Table of Contents



Sec.
136.1 Applicability.
136.2 Definitions.
136.3 Identification of test procedures.
136.4 Application for and approval of alternate test procedures for 
          nationwide use.
136.5 Approval of alternate test procedures for limited use.
136.6 Method modifications and analytical requirements.
136.7 Quality assurance and quality control.

Appendix A to Part 136--Methods for Organic Chemical Analysis of 
          Municipal and Industrial Wastewater
Appendix B to Part 136--Definition and Procedure for the Determination 
          of the Method Detection Limit--Revision 1.11
Appendix C to Part 136--Determination of Metals and Trace Elements in 
          Water and Wastes by Inductively Coupled Plasma-Atomic Emission 
          Spectrometry Method 200.7
Appendix D to Part 136--Precision and Recovery Statements for Methods 
          for Measuring Metals

    Authority: Secs. 301, 304(h), 307 and 501(a), Pub. L. 95-217, 91 
Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (the Federal Water 
Pollution Control Act Amendments of 1972 as amended by the Clean Water 
Act of 1977).



Sec.  136.1  Applicability.

    (a) The procedures prescribed herein shall, except as noted in 
Sec. Sec.  136.4, 136.5, and 136.6, be used to perform the measurements 
indicated whenever the waste constituent specified is required to be 
measured for:
    (1) An application submitted to the Director and/or reports required 
to be submitted under NPDES permits or other requests for quantitative 
or qualitative effluent data under parts 122 through 125 of this 
chapter; and
    (2) Reports required to be submitted by dischargers under the NPDES 
established by parts 124 and 125 of this chapter; and
    (3) Certifications issued by States pursuant to section 401 of the 
Clean Water Act (CWA), as amended.
    (b) The procedure prescribed herein and in part 503 of title 40 
shall be used to perform the measurements required for an application 
submitted to the Administrator or to a State for a sewage sludge permit 
under section 405(f) of the Clean Water Act and for recordkeeping and 
reporting requirements under part 503 of title 40.
    (c) For the purposes of the NPDES program, when more than one test 
procedure is approved under this part for the analysis of a pollutant or 
pollutant parameter, the test procedure must be sufficiently sensitive 
as defined at 40 CFR 122.21(e)(3) and 122.44(i)(1)(iv).

[72 FR 14224, Mar. 26, 2007, as amended at 77 FR 29771, May 18, 2012; 79 
FR 49013, Aug. 19, 2014; 82 FR 40846, Aug. 28, 2017]



Sec.  136.2  Definitions.

    As used in this part, the term:
    (a) Act means the Clean Water Act of 1977, Pub. L. 95-217, 91 Stat. 
1566, et seq. (33 U.S.C. 1251 et seq.) (The Federal Water Pollution 
Control Act Amendments of 1972 as amended by the Clean Water Act of 
1977).
    (b) Administrator means the Administrator of the U.S. Environmental 
Protection Agency.
    (c) Regional Administrator means one of the EPA Regional 
Administrators.
    (d) Director means the director as defined in 40 CFR 122.2.
    (e) National Pollutant Discharge Elimination System (NPDES) means 
the national system for the issuance of permits under section 402 of the 
Act and includes any State or interstate program which has been approved 
by the Administrator, in whole or in part, pursuant to section 402 of 
the Act.
    (f) Detection limit means the minimum concentration of an analyte 
(substance) that can be measured and reported with a 99% confidence that 
the analyte concentration is distinguishable from the method blank 
results as determined by the procedure set forth at appendix B of this 
part.

[38 FR 28758, Oct. 16, 1973, as amended at 49 FR 43250, Oct. 26, 1984; 
82 FR 40846, Aug. 28, 2017]

[[Page 6]]



Sec.  136.3  Identification of test procedures.

    (a) Parameters or pollutants, for which methods are approved, are 
listed together with test procedure descriptions and references in 
Tables IA, IB, IC, ID, IE, IF, IG, and IH of this section. The methods 
listed in Tables IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by 
reference, see paragraph (b) of this section, with the exception of EPA 
Methods 200.7, 601-613, 624.1, 625.1, 1613, 1624, and 1625. The full 
texts of Methods 601-613, 624.1, 625.1, 1613, 1624, and 1625 are printed 
in appendix A of this part, and the full text of Method 200.7 is printed 
in appendix C of this part. The full text for determining the method 
detection limit when using the test procedures is given in appendix B of 
this part. In the event of a conflict between the reporting requirements 
of 40 CFR parts 122 and 125 and any reporting requirements associated 
with the methods listed in these tables, the provisions of 40 CFR parts 
122 and 125 are controlling and will determine a permittee's reporting 
requirements. The full texts of the referenced test procedures are 
incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and 
IH. The year after the method number indicates the latest editorial 
change of the method. The discharge parameter values for which reports 
are required must be determined by one of the standard analytical test 
procedures incorporated by reference and described in Tables IA, IB, IC, 
ID, IE, IF, IG, and IH or by any alternate test procedure which has been 
approved by the Administrator under the provisions of paragraph (d) of 
this section and Sec. Sec.  136.4 and 136.5. Under certain circumstances 
(paragraph (c) of this section, in Sec.  136.5(a) through (d) or 40 CFR 
401.13) other additional or alternate test procedures may be used.

[[Page 7]]



                                     Table IA--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                Method \1\                  EPA              Standard methods       AOAC, ASTM, USGS            Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Bacteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Coliform (fecal), number per 100  Most Probable Number    p. 132,\3\ 1680,11 15   9221 C E-2006........
 mL or number per gram dry weight.    (MPN), 5 tube, 3        1681 11 20.
                                      dilution, or.
                                     Multiple tube/multiple  ......................  .....................  .....................  Colilert-18[supreg]13
                                      well, or.                                                                                     18 21 29.
                                     Membrane filter (MF)    p. 124 \3\............  9222 D-2006 \30\.....  B-0050-85 \4\........
                                      \2\, single step.
2. Coliform (fecal) in presence of   MPN, 5 tube, 3          p. 132 \3\............  9221 C E-2006........
 chlorine, number per 100 mL.         dilution, or.
                                     MF \2\, single step     p. 124 \3\............  9222 D-2006 \30\.....
                                      \5\.
3. Coliform (total), number per 100  MPN, 5 tube, 3          p. 114 \3\............  9221 B-2006..........
 mL.                                  dilution, or.
                                     MF \2\, single step or  p. 108 \3\............  9222 B-2006..........  B-0025-85 \4\........
                                      two step.
4. Coliform (total), in presence of  MPN, 5 tube, 3          p. 114 \3\............  9221 B-2006..........
 chlorine, number per 100 mL.         dilution, or.
                                     MF \2\ with enrichment  p. 111 \3\............  9222 B-2006..........
                                      \5\.
5. E. coli, number per 100 mL \21\.  MPN 6 8 16 multiple     ......................  9221B.2-2006/9221F-
                                      tube, or.                                       2006 12 14.
                                     multiple tube/multiple  ......................  9223 B-2004 \13\.....  991.15 \10\..........  Colilert[supreg] 13
                                      well, or.                                                                                     18.
                                                                                                                                   Colilert-18[supreg]
                                                                                                                                    13 17 18
                                     MF 2 6 7 8 single step  1603 \22\.............  .....................  .....................  mColiBlue-
                                                                                                                                    24[supreg]\19\.
6. Fecal streptococci, number per    MPN, 5 tube, 3          p. 139 \3\............  9230 B-2007..........
 100 mL.                              dilution, or.
                                     MF \2\, or............  p. 136 \3\............  9230 C-2007..........  B-0055-85 \4\........
                                     Plate count...........  p. 143 \3\............
7. Enterococci, number per 100 mL    MPN, 5 tube, 3          p. 139 \3\............  9230 B-2007..........
 \21\.                                dilution, or.
                                     MPN 6 8, multiple tube/ ......................  9230 D-2007..........  D6503-99 \9\.........  Enterolert[supreg] 13
                                      multiple well, or.                                                                            24.
                                     MF 2 6 7 8 single step  1600 \25\.............  9230 C-2007..........
                                      or.
                                     Plate count...........  p. 143 \3\............

[[Page 8]]

 
8.Salmonella number per gram dry     MPN multiple tube.....  1682 \23\.............
 weight \11\.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                    Aquatic Toxicity
--------------------------------------------------------------------------------------------------------------------------------------------------------
9. Toxicity, acute, fresh water      Ceriodaphnia dubia      2002.0 \26\...........
 organisms, LC50, percent effluent.   acute.
                                     Daphnia puplex and      2021.0 \26\...........
                                      Daphnia magna acute.
                                     Fathead Minnow,         2000.0 \26\...........
                                      Pimephales promelas,
                                      and Bannerfin shiner,
                                      Cyprinella leedsi,
                                      acute.
                                     Rainbow Trout,          2019.0 \26\...........
                                      Oncorhynchus mykiss,
                                      and brook trout,
                                      Salvelinus
                                      fontinalis, acute.
10. Toxicity, acute, estuarine and   Mysid, Mysidopsis       2007.0 \26\...........
 marine organisms of the Atlantic     bahia, acute.
 Ocean and Gulf of Mexico, LC50,
 percent effluent.
                                     Sheepshead Minnow,      2004.0 \26\...........
                                      Cyprinodon
                                      variegatus, acute.
                                     Silverside, Menidia     2006.0 \26\...........
                                      beryllina, Menidia
                                      menidia, and Menidia
                                      peninsulae, acute.
11. Toxicity, chronic, fresh water   Fathead minnow,         1000.0 \27\...........
 organisms, NOEC or IC25, percent     Pimephales promelas,
 effluent.                            larval survival and
                                      growth.

[[Page 9]]

 
                                     Fathead minnow,         1001.0 \27\...........
                                      Pimephales promelas,
                                      embryo-larval
                                      survival and
                                      teratogenicity.
                                     Daphnia, Ceriodaphnia   1002.0 \27\...........
                                      dubia, survival and
                                      reproduction.
                                     Green alga,             1003.0 \27\...........
                                      Selenastrum
                                      capricornutum, growth.
12. Toxicity, chronic, estuarine     Sheepshead minnow,      1004.0 \28\...........
 and marine organisms of the          Cyprinodon
 Atlantic Ocean and Gulf of Mexico,   variegatus, larval
 NOEC or IC25, percent effluent.      survival and growth.
                                     Sheepshead minnow,      1005.0 \28\...........
                                      Cyprinodon
                                      variegatus, embryo-
                                      larval survival and
                                      teratogenicity.
                                     Inland silverside,      1006.0 \28\...........
                                      Menidia beryllina,
                                      larval survival and
                                      growth.
                                     Mysid, Mysidopsis       1007.0 \28\...........
                                      bahia, survival,
                                      growth, and fecundity.
                                     Sea urchin, Arbacia     1008.0 \28\...........
                                      punctulata,
                                      fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. U.S. EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.

[[Page 10]]

 
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
  organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
  results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
\11\ Approved for enumeration of target organism in sewage sludge.
\12\ The multiple-tube fermentation test is used in 9221B.2-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
  glucuronidase produced by E. coli.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.2-2006, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC
  media supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\15\ Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-
  14-009. September 2014. U.S. EPA.
\16\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] and the MPN calculated from the table provided by the manufacturer.
\17\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\18\ Descriptions of the Colilert[supreg], Colilert-18[supreg], and Quanti-Tray[supreg] may be obtained from IDEXX Laboratories, Inc.
\19\ A description of the mColiBlue24[supreg] test, is available from Hach Company.
\20\ Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
\21\ Approved for enumeration of target organism in wastewater effluent.
\22\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (modified
  mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.
\23\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014.
  U.S. EPA.
\24\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\25\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-14-011.
  September 2014. U.S. EPA.
\26\ Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA-821-R-02-012. Fifth Edition,
  October 2002. U.S. EPA.
\27\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA-821-R-02-013. Fourth Edition,
  October 2002. U.S. EPA.
\28\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA-821-R-02-014. Third
  Edition, October 2002. U.S. EPA.
\29\ To use Colilert-18[supreg] to assay for fecal coliforms, the incubation temperature is 44.5  0.2 [deg]C, and a water bath
  incubator is used.
\30\ On a monthly basis, at least ten blue colonies from the medium must be verified using Lauryl Tryptose Broth and EC broth, followed by count
  adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications
  should be done from randomized sample sources.


[[Page 11]]


                                                  Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                  Methodology \58\            EPA \52\            Standard methods             ASTM             USGS/AOAC/other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L.........  Electrometric endpoint  ......................  2310 B-2011..........  D1067-11.............  I-1020-85.\2\
                                      or phenolphthalein
                                      endpoint.
2. Alkalinity, as CaCO3, mg/L......  Electrometric or        ......................  2320 B-2011..........  D1067-11.............  973.43,\3\ I-1030-
                                      Colorimetric                                                                                  85.\2\
                                      titration to pH 4.5,
                                      Manual.
                                     Automatic.............  310.2 (Rev. 1974) \1\.  .....................  .....................  I-2030-85.\2\
3. Aluminum--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 D-2011 or 3111 E- .....................  I-3051-85.\2\
                                      \36\.                                           2011.
                                     AA furnace............  ......................  3113 B-2010.
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     Direct Current Plasma   ......................  .....................  D4190-08.............  See footnote.\34\
                                      (DCP) \36\.
                                     Colorimetric            ......................  3500-Al B-2011.......
                                      (Eriochrome cyanine
                                      R).
4. Ammonia (as N), mg/L............  Manual distillation     350.1, Rev. 2.0 (1993)  4500-NH3 B-2011......  .....................  973.49.\3\
                                      \6\ or gas diffusion
                                      (pH  11),
                                      followed by any of
                                      the following:.
                                     Nesslerization........  ......................  .....................  D1426-08 (A).........  973.49,\3\ I-3520-
                                                                                                                                    85.\2\
                                     Titration.............  ......................  4500-NH3 C-2011......
                                     Electrode.............  ......................  4500-NH3 D-2011 or E-  D1426-08 (B).........
                                                                                      2011.
                                     Manual phenate,         ......................  4500-NH3 F-2011......  .....................  See footnote.\60\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods.

[[Page 12]]

 
                                     Automated phenate,      350.1,\30\ Rev. 2.0     4500-NH3 G-2011, 4500- .....................  I-4523-85.\2\
                                      salicylate, or other    (1993).                 NH3 H-2011.
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods.
                                     Automated electrode...  ......................  .....................  .....................  See footnote.\7\
                                     Ion Chromatography....  ......................  .....................  D6919-09.............
                                     Automated gas           ......................  .....................  .....................  Timberline Ammonia-
                                      diffusion, followed                                                                           001.\74\
                                      by conductivity cell
                                      analysis.
5. Antimony--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011..........
                                      \36\.
                                     AA furnace............  ......................  3113 B-2010..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
6. Arsenic-Total,\4\ mg/L..........  Digestion,\4\ followed  206.5 (Issued 1978)
                                      by any of the           \1\.
                                      following:.
                                     AA gaseous hydride....  ......................  3114 B-2011 or 3114 C- D2972-08 (B).........  I-3062-85.\2\
                                                                                      2011.
                                     AA furnace............  ......................  3113 B-2010..........  D2972-08 (C).........  I-4063-98.\49\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     Colorimetric (SDDC)...  ......................  3500-As B-2011.......  D2972-08 (A).........  I-3060-85.\2\
7. Barium--Total,\4\ mg/L..........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 D-2011..........  .....................  I-3084-85.\2\
                                      \36\.
                                     AA furnace............  ......................  3113 B-2010..........  D4382-12.............
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  .....................  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).

[[Page 13]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP \36\..............  ......................  .....................  .....................  See footnote.\34\
8. Beryllium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:.
                                     AA direct aspiration..  ......................  3111 D-2011 or 3111 E- D3645-08 (A).........  I-3095-85.\2\
                                                                                      2011.
                                     AA furnace............  ......................  3113 B-2010..........  D3645-08 (B).........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP...................  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric            ......................  See footnote.\61\
                                      (aluminon).
9. Biochemical oxygen demand         Dissolved Oxygen        ......................  5210 B-2011..........  .....................  973.44,\3\ p. 17,\9\
 (BOD5), mg/L.                        Depletion.                                                                                    I-1578-78,\8\ See
                                                                                                                                    footnote.10 63
10. Boron--Total,\37\ mg/L.........  Colorimetric            ......................  4500-B B-2011........  .....................  I-3112-85.\2\
                                      (curcumin).
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP...................  ......................  .....................  D4190-08.............  See footnote.\34\
11. Bromide, mg/L..................  Electrode.............  ......................  .....................  D1246-10.............  I-1125-85.\2\
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2011, C-2011,   D4327-03.............  993.30.\3\
                                                              and 300.1, Rev 1.0      D-2011.
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
12. Cadmium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D3557-12 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2011.                                         I-3135-85\2\ or I-
                                                                                                                                    3136-85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D3557-12 (D).........  I-4138-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-1472-85 \2\ or I-
                                                              \68\ 200.7, Rev. 4.4                                                  4471-97.\50\
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Voltametry \11\.......  ......................  .....................  D3557-12 (C).........

[[Page 14]]

 
                                     Colorimetric            ......................  3500-Cd-D-1990.......
                                      (Dithizone).
13. Calcium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........  D511-09(B)...........  I-3152-85.\2\
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2011..........  .....................  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Titrimetric (EDTA)....  ......................  3500-Ca B-2011.......  D511-09 (A)..........
                                     Ion Chromatography....  ......................  .....................  D6919-09.............
14. Carbonaceous biochemical oxygen  Dissolved Oxygen        ......................  5210 B-2011..........  .....................  See footnote.35 63
 demand (CBOD5), mg/L \12\.           Depletion with
                                      nitrification
                                      inhibitor.
15. Chemical oxygen demand (COD),    Titrimetric...........  410.3 (Rev. 1978) \1\.  5220 B-2011 or C-2011  D1252-06 (A).........  973.46,\3\ p. 17,\9\
 mg/L.                                                                                                                              I-3560-85.\2\
                                     Spectrophotometric,     410.4, Rev. 2.0 (1993)  5220 D-2011..........  D1252-06 (B).........  See footnotes.13 14,
                                      manual or automatic.                                                                          I-3561-85.\2\
16. Chloride, mg/L.................  Titrimetric: (silver    ......................  4500-Cl- B-2011......  D512-04 (B)..........  I-1183-85.\2\
                                      nitrate).
                                     (Mercuric nitrate)....  ......................  4500-Cl- C-2011......  D512-04 (A)..........  973.51,\3\ I-1184-
                                                                                                                                    85.\2\
                                     Colorimetric: Manual..  ......................  .....................  .....................  I-1187-85.\2\
                                     Automated               ......................  4500-Cl- E-2011......  .....................  I-2187-85.\2\
                                      (ferricyanide).
                                     Potentiometric          ......................  4500-Cl- D-2011......
                                      Titration.
                                     Ion Selective           ......................  .....................  D512-04 (C)..........
                                      Electrode.
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2011 or 4110 C- D4327-03.............  993.30,\3\ I-2057-
                                                              and 300.1, Rev 1.0      2011.                                         90.\51\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
17. Chlorine-Total residual, mg/L..  Amperometric direct...  ......................  4500-Cl D-2011.......  D1253-08.............
                                     Amperometric direct     ......................  4500-Cl E-2011.......
                                      (low level).
                                     Iodometric direct.....  ......................  4500-Cl B-2011.......
                                     Back titration ether    ......................  4500-Cl C-2011.......
                                      end-point \15\.
                                     DPD-FAS...............  ......................  4500-Cl F-2011.......

[[Page 15]]

 
                                     Spectrophotometric,     ......................  4500-Cl G-2011.......
                                      DPD.
                                     Electrode.............  ......................  .....................  .....................  See footnote.\16\
17A. Chlorine-Free Available, mg/L.  Amperometric direct...  ......................  4500-Cl D-2011.......  D1253-08.............
                                     Amperometric direct     ......................  4500-Cl E-2011.......
                                      (low level).
                                     DPD-FAS...............  ......................  4500-Cl F-2011.......
                                     Spectrophotometric,     ......................  4500-Cl G-2011.......
                                      DPD.
18. Chromium VI dissolved, mg/L....  0.45-micron filtration
                                      followed by any of
                                      the following:
                                     AA chelation-           ......................  3111 C-2011..........  .....................  I-1232-85.\2\
                                      extraction.
                                     Ion Chromatography....  218.6, Rev. 3.3 (1994)  3500-Cr C-2011.......  D5257-11.............  993.23.\3\
                                     Colorimetric (diphenyl- ......................  3500-Cr B-2011.......  D1687-12 (A).........  I-1230-85.\2\
                                      carbazide).
19. Chromium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011..........  D1687-12 (B).........  974.27,\3\ I-3236-
                                      \36\.                                                                                         85.\2\
                                     AA chelation-           ......................  3111 C-2011..........
                                      extraction.
                                     AA furnace............  ......................  3113 B-2010..........  D1687-12 (C).........  I-3233-93.\46\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2          3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003),\68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric (diphenyl- ......................  3500-Cr B-2011.......
                                      carbazide).
20. Cobalt--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011 or 3111 C- D3558-08 (A or B)....  p. 37,\9\ I-3239-
                                                                                      2011.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D3558-08 (C).........  I-4243-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.7, Rev. 4.4 (1994)  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP...................  ......................  .....................  D4190-08.............  See footnote.\34\

[[Page 16]]

 
21. Color, platinum cobalt units or  Colorimetric (ADMI)...  ......................  2120 F-2011 \78\.....
 dominant wavelength, hue,
 luminance purity.
                                     Platinum cobalt visual  ......................  2120 B-2011..........  .....................  I-1250-85.\2\
                                      comparison.
                                     Spectrophotometric....  ......................  .....................  .....................  See footnote.\18\
22. Copper--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D1688-12 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2011.                                         I-3270-85\2\ or I-
                                                                                                                                    3271-85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D1688-12 (C).........  I-4274-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Cu B-2011.......
                                      (Neocuproine).
                                     Colorimetric            ......................  3500-Cu C-2011.......  .....................  See footnote.\19\
                                      (Bathocuproine).
23. Cyanide--Total, mg/L...........  Automated UV digestion/ ......................  .....................  .....................  Kelada-01.\55\
                                      distillation and
                                      Colorimetry.
                                     Segmented Flow          ......................  .....................  D7511-12.............
                                      Injection, In-Line
                                      Ultraviolet
                                      Digestion, followed
                                      by gas diffusion
                                      amperometry.
                                     Manual distillation     335.4, Rev. 1.0 (1993)  4500-CN- B-2011 and C- D2036-09(A), D7284-13  10-204-00-1-X.\56\
                                      with MgCl2, followed    \57\.                   2011.
                                      by any of the
                                      following:.
                                     Flow Injection, gas     ......................  .....................  D2036-09(A) D7284-13.
                                      diffusion amperometry.
                                     Titrimetric...........  ......................  4500-CN- D-2011......  D2036-09(A)..........  p. 22.\9\
                                     Spectrophotometric,     ......................  4500-CN- E-2011......  D2036-09(A)..........  I-3300-85.\2\
                                      manual.

[[Page 17]]

 
                                     Semi-Automated \20\...  335.4, Rev. 1.0 (1993)  .....................  .....................  10-204-00-1-X,\56\ I-
                                                              \57\.                                                                 4302-85.\2\
                                     Ion Chromatography....  ......................  .....................  D2036-09(A)..........
                                     Ion Selective           ......................  4500-CN- F-2011......  D2036-09(A)..........
                                      Electrode.
24. Cyanide--Available, mg/L.......  Cyanide Amenable to     ......................  4500-CN- G-2011......  D2036-09(B)..........
                                      Chlorination (CATC);
                                      Manual distillation
                                      with MgCl2, followed
                                      by Titrimetric or
                                      Spectrophotometric.
                                     Flow injection and      ......................  .....................  D6888-09.............  OIA-1677-09.\44\
                                      ligand exchange,
                                      followed by gas
                                      diffusion amperometry
                                      \59\.
                                     Automated Distillation  ......................  .....................  .....................  Kelada-01.\55\
                                      and Colorimetry (no
                                      UV digestion).
24.A Cyanide--Free, mg/L...........  Flow Injection,         ......................  .....................  D7237-10.............  OIA-1677-09.\44\
                                      followed by gas
                                      diffusion amperometry.
                                     Manual micro-diffusion  ......................  .....................  D4282-02.............
                                      and colorimetry.
25. Fluoride--Total, mg/L..........  Manual                  ......................  4500-F- B-2011.......
                                      distillation,\6\
                                      followed by any of
                                      the following:
                                     Electrode, manual.....  ......................  4500-F- C-2011.......  D1179-10 (B).........
                                     Electrode, automated..  ......................  .....................  .....................  I-4327-85.\2\
                                     Colorimetric, (SPADNS)  ......................  4500-F- D-2011.......  D1179-10 (A).........
                                     Automated complexone..  ......................  4500-F- E-2011.......
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2011 or C-2011  D4327-03.............  993.30.\3\
                                                              and 300.1, Rev 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
26. Gold--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........
                                     AA furnace............  231.2 (Issued 1978)     3113 B-2010..........
                                                              \1\.

[[Page 18]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
27. Hardness--Total, as CaCO3, mg/L  Automated colorimetric  130.1 (Issued 1971)
                                                              \1\.
                                     Titrimetric (EDTA)....  ......................  2340 C-2011..........  D1126-12.............  973.52B,\3\ I-1338-
                                                                                                                                    85.\2\
                                     Ca plus Mg as their     ......................  2340 B-2011..........
                                      carbonates, by any
                                      approved method for
                                      Ca and Mg (See
                                      Parameters 13 and
                                      33), provided that
                                      the sum of the lowest
                                      point of quantitation
                                      for Ca and Mg is
                                      below the NPDES
                                      permit requirement
                                      for Hardness..
28. Hydrogen ion (pH), pH units....  Electrometric           ......................  4500-H+ B-2011.......  D1293-99 (A or B)....  973.41,\3\ I-1586-
                                      measurement.                                                                                  85.\2\
                                     Automated electrode...  150.2 (Dec. 1982) \1\.  .....................  .....................  See footnote,\21\ I-
                                                                                                                                    2587-85.\2\
29. Iridium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........
                                     AA furnace............  235.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2011..........
30. Iron--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D1068-10 (A).........  974.27,\3\ I-3381-
                                      \36\.                                           2011.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D1068-10 (B).........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Fe B-2011.......  D1068-10 (C).........  See footnote.\22\
                                      (Phenanthroline).

[[Page 19]]

 
31. Kjeldahl Nitrogen \5\--Total,    Manual digestion \20\   ......................  4500-Norg B-2011 or C- D3590-11 (A).........  I-4515-91.\45\
 (as N), mg/L.                        and distillation or                             2011 and 4500-NH3 B-
                                      gas diffusion,                                  2011.
                                      followed by any of
                                      the following:.
                                     Titration.............  ......................  4500-NH3 C-2011......  .....................  973.48.\3\
                                     Nesslerization........  ......................  .....................  D1426-08 (A).........
                                     Electrode.............  ......................  4500-NH3 D-2011 or E-  D1426-08 (B).........
                                                                                      2011.
                                     Semi-automated phenate  350.1, Rev. 2.0 (1993)  4500-NH3 G-2011 4500-
                                                                                      NH3 H-2011.
                                     Manual phenate,         ......................  4500-NH3 F-2011......  .....................  See footnote.\60\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods.
                                     Automated gas           ......................  .....................  .....................  Timberline Ammonia-
                                      diffusion, followed                                                                           001.\74\
                                      by conductivity cell
                                      analysis.
                                    --------------------------------------------------------------------------------------------------------------------
                                                              Automated Methods for TKN that do not require manual distillation.
                                    --------------------------------------------------------------------------------------------------------------------
                                     Automated phenate,      351.1 (Rev. 1978) \1\.  .....................  .....................  I-4551-78.\8\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods
                                      colorimetric (auto
                                      digestion and
                                      distillation).
                                     Semi-automated block    351.2, Rev. 2.0 (1993)  4500-Norg D-2011.....  D3590-11 (B).........  I-4515-91.\45\
                                      digestor colorimetric
                                      (distillation not
                                      required).
                                     Block digester,         ......................  .....................  .....................  See footnote.\39\
                                      followed by Auto
                                      distillation and
                                      Titration.
                                     Block digester,         ......................  .....................  .....................  See footnote.\40\
                                      followed by Auto
                                      distillation and
                                      Nesslerization.

[[Page 20]]

 
                                     Block Digester,         ......................  .....................  .....................  See footnote.\41\
                                      followed by Flow
                                      injection gas
                                      diffusion
                                      (distillation not
                                      required).
                                     Digestion with          ......................  .....................  .....................  Hach 10242.\76\
                                      peroxdisulfate,
                                      followed by
                                      Spectrophotometric
                                      (2,6-dimethyl phenol).
                                     Digestion with          ......................  .....................  .....................  NCASI TNTP
                                      persulfate, followed                                                                          W10900.\77\
                                      by Colorimetric.
32. Lead--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D3559-08 (A or B)....  974.27,\3\ I-3399-
                                      \36\.                                           2011.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D3559-08 (D).........  I-4403-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Voltametry \11\.......  ......................  .....................  D3559-08 (C).........
                                     Colorimetric            ......................  3500-Pb B-2011.......
                                      (Dithizone).
33. Magnesium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........  D511-09 (B)..........  974.27,\3\ I-3447-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Ion Chromatography....  ......................  .....................  D6919-09.............
34. Manganese--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011..........  D858-12 (A or B).....  974.27,\3\ I-3454-
                                      \36\.                                                                                         85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  D858-12 (C)..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)

[[Page 21]]

 
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Mn B-2011.......  .....................  920.203.\3\
                                      (Persulfate).
                                     Colorimetric            ......................  .....................  .....................  See footnote.\23\
                                      (Periodate).
35. Mercury--Total,\4\ mg/L........  Cold vapor, Manual....  245.1, Rev. 3.0 (1994)  3112 B-2011..........  D3223-12.............  977.22,\3\ I-3462-
                                                                                                                                    85.\2\
                                     Cold vapor, Automated.  245.2 (Issued 1974)
                                                              \1\.
                                     Cold vapor atomic       245.7 Rev. 2.0 (2005)   .....................  .....................  I-4464-01.\71\
                                      fluorescence            \17\.
                                      spectrometry (CVAFS).
                                     Purge and Trap CVAFS..  1631E \43\............
36. Molybdenum--Total,\4\ mg/L.....  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2011..........  .....................  I-3490-85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  .....................  I-3492-96.\47\
                                     ICP/AES \36\..........  200.7, Rev. 4.4 (1994)  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
37. Nickel--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D1886-08 (A or B)....  I-3499-85.\2\
                                      \36\.                                           2011.
                                     AA furnace............  ......................  3113 B-2010..........  D1886-08 (C).........  I-4503-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
38. Nitrate (as N), mg/L...........  Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2011 or C-2011  D4327-03.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
                                     Ion Selective           ......................  4500-NO3- D-2011.....
                                      Electrode.
                                     Colorimetric (Brucine   352.1 (Issued 1971)     .....................  .....................  973.50,\3\ 419D1 7 p.
                                      sulfate).               \1\.                                                                  28.\9\

[[Page 22]]

 
                                     Spectrophotometric      ......................  .....................  .....................  Hach 10206.\75\
                                      (2,6-dimethylphenol).
                                     Nitrate-nitrite N
                                      minus Nitrite N (See
                                      parameters 39 and 40).
39. Nitrate-nitrite (as N), mg/L...  Cadmium reduction,      ......................  4500-NO3- E-2011.....  D3867-04 (B).........
                                      Manual.
                                     Cadmium reduction,      353.2, Rev. 2.0 (1993)  4500-NO3- F-2011.....  D3867-04 (A).........  I-2545-90.\51\
                                      Automated.
                                     Automated hydrazine...  ......................  4500-NO3- H-2011.....
                                     Reduction/Colorimetric  ......................  .....................  .....................  See footnote.\62\
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2011 or C-2011  D4327-03.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
                                     Enzymatic reduction,    ......................  .....................  .....................  I-2547-11,\72\ I-2548-
                                      followed by automated                                                                         11,\72\ N07-
                                      colorimetric                                                                                  0003.\73\
                                      determination.
                                     Spectrophotometric      ......................  .....................  .....................  Hach 10206.\75\
                                      (2,6-dimethylphenol).
40. Nitrite (as N), mg/L...........  Spectrophotometric:     ......................  4500-NO2- B-2011.....  .....................  See footnote.\25\
                                      Manual.
                                     Automated               ......................  .....................  .....................  I-4540-85,\2\ See
                                      (Diazotization).                                                                              footnote.\62\
                                     Automated (*bypass      353.2, Rev. 2.0 (1993)  4500-NO3- F-2011.....  D3867-04 (A).........  I-4545-85.\2\
                                      cadmium reduction).
                                     Manual (*bypass         ......................  4500-NO3- E-2011.....  D3867-04 (B).........
                                      cadmium reduction).
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2011 or C-2011  D4327-03.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
                                     Automated (*bypass      ......................  .....................  .....................  I-2547-11,\72\ I-2548-
                                      Enzymatic reduction).                                                                         11,\72\ N07-
                                                                                                                                    0003.\73\

[[Page 23]]

 
41. Oil and grease--Total            Hexane extractable      1664 Rev. A; 1664 Rev.  5520 B-2011 \38\.....
 recoverable, mg/L.                   material (HEM): n-      B \42\.
                                      Hexane extraction and
                                      gravimetry.
                                     Silica gel treated HEM  1664 Rev. A; 1664 Rev.  5520 B-2011 \38\ and
                                      (SGT-HEM): Silica gel   B \42\.                 5520 F-2011\38\.
                                      treatment and
                                      gravimetry.
42. Organic carbon--Total (TOC), mg/ Combustion............  ......................  5310 B-2011..........  D7573-09.............  973.47,\3\ p. 14.\24\
 L.
                                     Heated persulfate or    ......................  5310 C-2011, 5310 D-   D4839-03.............  973.47,\3\ p. 14.\24\
                                      UV persulfate                                   2011.
                                      oxidation.
43. Organic nitrogen (as N), mg/L..  Total Kjeldahl N
                                      (Parameter 31) minus
                                      ammonia N (Parameter
                                      4).
44. Ortho-phosphate (as P), mg/L...  Ascorbic acid method:
                                     Automated.............  365.1, Rev. 2.0 (1993)  4500-P F-2011 or G-    .....................  973.56,\3\ I-4601-
                                                                                      2011.                                         85.\2\
                                     Manual single reagent.  ......................  4500-P E-2011........  D515-88 (A)..........  973.55.\3\
                                     Manual two reagent....  365.3 (Issued 1978)
                                                              \1\.
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2011 or C-2011  D4327-03.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-10.............  D6508, Rev. 2.\54\
45. Osmium--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2011..........
                                     AA furnace............  252.2 (Issued 1978)
                                                              \1\.
46. Oxygen, dissolved, mg/L........  Winkler (Azide          ......................  4500-O (B-F)-2011....  D888-09 (A)..........  973.45B,\3\ I-1575-
                                      modification).                                                                                78.\8\
                                     Electrode.............  ......................  4500-O G-2011........  D888-09 (B)..........  I-1576-78.\8\
                                     Luminescence Based      ......................  .....................  D888-09 (C)..........  See footnote.\63\ See
                                      Sensor.                                                                                       footnote.\64\
47. Palladium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........

[[Page 24]]

 
                                     AA furnace............  253.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2011..........
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
48. Phenols, mg/L..................  Manual                  420.1 (Rev. 1978) \1\.  5530 B-2010..........  D1783-01.............
                                      distillation,\26\
                                      followed by any of
                                      the following:
                                     Colorimetric (4AAP)     420.1 (Rev. 1978) \1\.  5530 D-2010 \27\.....  D1783-01 (A or B)....
                                      manual.
                                     Automated colorimetric  420.4 Rev. 1.0 (1993).
                                      (4AAP).
49. Phosphorus (elemental), mg/L...  Gas-liquid              ......................  .....................  .....................  See footnote.\28\
                                      chromatography.
50. Phosphorus--Total, mg/L........  Digestion,\20\          ......................  4500-P B(5)-2011.....  .....................  973.55.\3\
                                      followed by any of
                                      the following:
                                     Manual................  365.3 (Issued 1978)     4500-P E-2011........  D515-88 (A)..........
                                                              \1\.
                                     Automated ascorbic      365.1 Rev. 2.0 (1993).  4500-P (F-H)-2011....  .....................  973.56,\3\ I-4600-
                                      acid reduction.                                                                               85.\2\
                                     ICP/AES 4 36..........  200.7, Rev. 4.4 (1994)  3120 B-2011..........  .....................  I-4471-97.\50\
                                     Semi-automated block    365.4 (Issued 1974)     .....................  D515-88 (B)..........  I-4610-91.\48\
                                      digestor (TKP           \1\.
                                      digestion).
                                     Digestion with          ......................  .....................  .....................  NCASI TNTP
                                      persulfate, followed                                                                          W10900.\77\
                                      by Colorimetric.
51. Platinum--Total \4\, mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........
                                     AA furnace............  255.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2011..........
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
52. Potassium--Total \4\, mg/L.....  Digestion,\4\ followed
                                      by any of the
                                      following:.
                                     AA direct aspiration..  ......................  3111 B-2011..........  .....................  973.53,\3\ I-3630-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2011..........
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     Flame photometric.....  ......................  3500-K B-2011........
                                     Electrode.............  ......................  3500-K C-2011........
                                     Ion Chromatography....  ......................  .....................  D6919-09.............

[[Page 25]]

 
53. Residue--Total, mg/L...........  Gravimetric, 103-       ......................  2540 B-2011..........  .....................  I-3750-85.\2\
                                      105[deg].
54. Residue--filterable, mg/L......  Gravimetric, 180[deg].  ......................  2540 C-2011..........  D5907-13.............  I-1750-85.\2\
55. Residue--non-filterable (TSS),   Gravimetric, 103-       ......................  2540 D-2011..........  D5907-13.............  I-3765-85.\2\
 mg/L.                                105[deg] post washing
                                      of residue.
56. Residue--settleable, mg/L......  Volumetric, (Imhoff     ......................  2540 F-2011..........
                                      cone), or gravimetric.
57. Residue--Volatile, mg/L........  Gravimetric, 550[deg].  160.4 (Issued 1971)     2540-E-2011..........  .....................  I-3753-85.\2\
                                                              \1\.
58. Rhodium--Total \4\, mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration,   ......................  3111 B-2011..........
                                      or.
                                     AA furnace............  265.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2011..........
59. Ruthenium--Total \4\, mg/L.....  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration,   ......................  3111 B-2011..........
                                      or.
                                     AA furnace............  267.2 \1\.............
                                     ICP/MS................  ......................  3125 B-2011..........
60. Selenium--Total \4\, mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA furnace............  ......................  3113 B-2010..........  D3859-08 (B).........  I-4668-98.\49\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003)   3120 B-2011..........  D1976-12.............
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     AA gaseous hydride....  ......................  3114 B-2011, or 3114   D3859-08 (A).........  I-3667-85.\2\
                                                                                      C-2011.
61. Silica--Dissolved,\37\ mg/L....  0.45-micron filtration
                                      followed by any of
                                      the following:
                                     Colorimetric, Manual..  ......................  4500-SiO2 C-2011.....  D859-10..............  I-1700-85.\2\
                                     Automated               ......................  4500-SiO2 E-2011 or F- .....................  I-2700-85.\2\
                                      (Molybdosilicate).                              2011.
                                     ICP/AES...............  200.5, Rev. 4.2 (2003)  3120 B-2011..........  .....................  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).

[[Page 26]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
62. Silver--Total,4 31 mg/L........  Digestion,4 29
                                      followed by any of
                                      the following:
                                     AA direct aspiration..  ......................  3111 B-2011 or 3111 C- .....................  974.27,\3\ p. 37,\9\
                                                                                      2011.                                         I-3720-85.\2\
                                     AA furnace............  ......................  3113 B-2010..........  .....................  I-4724-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.5, Rev. 4.2 (2003)  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
63. Sodium--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........  .....................  973.54,\3\ I-3735-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.5, Rev. 4.2 (2003)  3120 B-2011..........  .....................  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Flame photometric.....  ......................  3500-Na B-2011.......
                                     Ion Chromatography....  ......................  .....................  D6919-09.............
64. Specific conductance, micromhos/ Wheatstone bridge.....  120.1 (Rev. 1982) \1\.  2510 B-2011..........  D1125-95(99) (A).....  973.40,\3\ I-2781-
 cm at 25 [deg]C.                                                                                                                   85.\2\
65. Sulfate (as SO4), mg/L.........  Automated colorimetric  375.2, Rev. 2.0 (1993)  4500-SO42- F-2011 or
                                                                                      G-2011.
                                     Gravimetric...........  ......................  4500-SO42- C-2011 or   .....................  925.54.\3\
                                                                                      D-2011.
                                     Turbidimetric.........  ......................  4500-SO42- E-2011....  D516-11..............
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2011 or C-2011  D4327-03.............  993.30,\3\ I-4020-
                                                              and 300.1, Rev. 1.0                                                   05.\70\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2011..........  D6508-1010...........  D6508, Rev. 2.\54\
66. Sulfide (as S), mg/L...........  Sample Pretreatment...  ......................  4500-S2- B, C-2011...
                                     Titrimetric (iodine)..  ......................  4500-S2- F-2011......  .....................  I-3840-85.\2\
                                     Colorimetric            ......................  4500-S2- D-2011......
                                      (methylene blue).
                                     Ion Selective           ......................  4500-S2- G-2011......  D4658-09.............
                                      Electrode.

[[Page 27]]

 
67. Sulfite (as SO3), mg/L.........  Titrimetric (iodine-    ......................  4500-SO32- B-2011....
                                      iodate).
68. Surfactants, mg/L..............  Colorimetric            ......................  5540 C-2011..........  D2330-02.............
                                      (methylene blue).
69. Temperature, [deg]C............  Thermometric..........  ......................  2550 B-2010..........  .....................  See footnote.\32\
70. Thallium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........
                                     AA furnace............  279.2 (Issued 1978)     3113 B-2010..........
                                                              \1\.
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2011..........  D1976-12.............
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
71. Tin--Total,\4\ mg/L............  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2011..........  .....................  I-3850-78.\8\
                                     AA furnace............  ......................  3113 B-2010..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.5, Rev. 4.2 (2003)
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
72. Titanium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2011..........
                                     AA furnace............  283.2 (Issued 1978)
                                                              \1\.
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
73. Turbidity, NTU \53\............  Nephelometric.........  180.1, Rev. 2.0 (1993)  2130 B-2011..........  D1889-00.............  I-3860-85.\2\ See
                                                                                                                                    footnote.\65\ See
                                                                                                                                    footnote.\66\ See
                                                                                                                                    footnote.\67\
74. Vanadium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2011..........
                                     AA furnace............  ......................  3113 B-2010..........  D3373-12.............

[[Page 28]]

 
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP...................  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric (Gallic    ......................  3500-V B-2011........
                                      Acid).
75. Zinc--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2011 or 3111 C- D1691-12 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2011.                                         I-3900-85.\2\
                                     AA furnace............  289.2 (Issued 1978)
                                                              \1\.
                                     ICP/AES \36\..........  200.5, Rev. 4.2 (2003)  3120 B-2011..........  D1976-12.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2011..........  D5673-10.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP \36\..............  ......................  .....................  D4190-08.............  See footnote.\34\
                                     Colorimetric (Zincon).  ......................  3500 Zn B-2011.......  .....................  See footnote.\33\
76. Acid Mine Drainage.............  ......................  1627 \69\.............
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB Notes:
\1\ Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.
\2\ Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological
  Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.
\3\ Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC
  International.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion
  procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable
  form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations, a digestion using nitric acid (as specified in
  Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to
  gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a
  combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as
  Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in
  EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain
  elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic
  absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced
  method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission
  spectrometry (ICP-AES), the direct current plasma (DCP) technique or EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA
  Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB); the
  total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion
  procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.

[[Page 29]]

 
\6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation
  step is not necessary: However, manual distillation will be required to resolve any controversies. In general, the analytical method should be
  consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to
  evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation
  step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future
  analysis. Comparable is defined as <20% RPD for all tested matrices). Alternatively the two populations of spike recovery percentages may be compared
  using a recognized statistical test.
\7\ Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Bran & Luebbe Analyzing
  Technologies Inc.
\8\ The approved method is that cited in Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources
  Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. USGS.
\9\ American National Standard on Photographic Processing Effluents. April 2, 1975. American National Standards Institute.
\10\ In-Situ Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\ Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ``total 5-day BOD.'' The
  addition of the nitrification inhibitor is not a procedural option, but must be included to report the CBOD5 parameter. A discharger whose permit
  requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's
  permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation.
\14\ Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company.
\15\ The back titration method will be used to resolve controversy.
\16\ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research Incorporated. The calibration graph for the Orion
  residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium
  iodate/100 mL solution, respectively.
\17\ Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA.
\18\ National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253 (1971) and Technical Bulletin 803, May 2000.
\19\ Method 8506, Bicinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company.
\20\ When using a method with block digestion, this treatment is not required.
\21\ Industrial Method Number 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Autoanalyzer II. October 1976. Bran &
  Luebbe Analyzing Technologies.
\22\ Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company.
\23\ Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company.
\24\ Methods for Analysis of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological
  Survey, Book 5, Chapter A3, (1972 Revised 1987). 1987. USGS.
\25\ Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The colorimetric reaction must be conducted at a pH of 10.0  0.2.
\28\ Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography, Journal of Chromatography,
  47(3):421-426.
\29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as
  an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble
  in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be
  diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
  approved method is satisfactory.
\30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method
  specified quality control acceptance criteria are met.
\31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in
  solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2
  to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent
  the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with
  reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as
  well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the
  cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ ``Water Temperature-Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 1, Chapter D1. 1975. USGS.
\33\ Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.
\34\ Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised
  1991. Thermo Jarrell Ash Corporation.

[[Page 30]]

 
\35\ In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\36\ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater
  Samples for Determination of Metals. April 16, 1992. CEM Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use n-hexane (n-Hexane--85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil
  and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of
  other extraction solvents is prohibited.
\39\ Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical.
\40\ Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.
\41\ Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical.
\42\ Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable
  Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-
  821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane
  Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001.
\43\ Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision
  E. August 2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA Water
  Quality Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations.
\44\ Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.
\45\ Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonium Plus
  Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS.
\46\ Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by
  Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.
\47\ Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by
  Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS.
\48\ Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by
  Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS.
\49\ Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium
  in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS.
\50\ Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-
  water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS.
\51\ Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and
  Organic Constituents in Water and Fluvial Sediments. 1993. USGS.
\52\ Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in U.S. EPA. May 1994. Methods for the Determination of
  Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in
  Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of
  Inorganic Ions in Drinking Water by Ion Chromatography.
\53\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCal\TM\ or equivalent) are acceptable
  substitutes for formazin.
\54\ Method D6508-10, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate
  Electrolyte. 2010. ASTM.
\55\ Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001.
  US EPA. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control
  (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the
  method, provided that the QC acceptance criteria are met.
\56\ QuikChem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of
  Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Lachat Instruments.
\57\ When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to
  distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method,
  approved digestion and/or distillation are required prior to analysis.

[[Page 31]]

 
\59\ Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-09 that contain particulate matter may be
  filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing
  available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the
  ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.
\60\ Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color
  reagent in Berthelot Reaction (``phenol-hypochlorite reaction'') colorimetric ammonium determination methods. For example when phenol is used as the
  color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively--see, Patton, C.J. and S.R. Crouch. March 1977.
  Anal. Chem. 49:464-469. These reaction parameters increase to pH  12.6 and 665 nm when salicylate is used as the color reagent--see, Krom,
  M.D. April 1980. The Analyst 105:305-316.
\61\ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may
  be used. This method has poorer precision and bias than the methods of choice.
\62\ Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.
\63\ Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5.
  Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for
  measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).
\64\ In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\65\ Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\66\ Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\67\ Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.
\68\ EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/
  600/R-06/115. Revision 4.2, October 2003. US EPA.
\69\ Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. US EPA.
\70\ Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell
  Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis,
  2006. USGS.
\71\ Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.
\72\ USGS Techniques and Methods 5-B8, Chapter 8, Section B, Methods of the National Water Quality Laboratory Book 5, Laboratory Analysis, 2011 USGS.
\73\ NECi Method N07-0003, ''Nitrate Reductase Nitrate-Nitrogen Analysis,'' Revision 9.0, March 2014, The Nitrate Elimination Co., Inc.
\74\ Timberline Instruments, LLC Method Ammonia-001, ``Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell
  Analysis,'' June 2011, Timberline Instruments, LLC.
\75\ Hach Company Method 10206, ``Spectrophotometric Measurement of Nitrate in Water and Wastewater,'' Revision 2.1, January 2013, Hach Company.
\76\ Hach Company Method 10242, ``Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater,'' Revision 1.1, January
  2013, Hach Company.
\77\ National Council for Air and Stream Improvement (NCASI) Method TNTP-W10900, ``Total (Kjeldahl) Nitrogen and Total Phosphorus in Pulp and Paper
  Biologically Treated Effluent by Alkaline Persulfate Digestion,'' June 2011, National Council for Air and Stream Improvement, Inc.
\78\ The pH adjusted sample is to be adjusted to 7.6 for NPDES reporting purposes.


[[Page 32]]


                                                         Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
           Parameter \1\                     Method                    EPA 2 7                 Standard methods                       ASTM                                  Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene....................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
2. Acenaphthylene..................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
3. Acrolein........................  GC....................  603........................  ..........................
                                     GC/MS.................  624.1,\4\ 1624B............  ..........................
4. Acrylonitrile...................  GC....................  603........................  ..........................
                                     GC/MS.................  624.1,\4\ 1624B............  ..........................
5. Anthracene......................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
6. Benzene.........................  GC....................  602........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
7. Benzidine.......................  Spectro-photometric...  ...........................  ..........................  ....................................  See footnote,\3\ p.1.
                                     GC/MS.................  625.1\5\, 1625B............  6410 B-2000...............
                                     HPLC..................  605........................  ..........................
8. Benzo(a)anthracene..............  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
9. Benzo(a)pyrene..................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
10. Benzo(b)fluoranthene...........  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
11. Benzo(g,h,i)perylene...........  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
12. Benzo(k)fluoranthene...........  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
13. Benzyl chloride................  GC....................  ...........................  ..........................  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  ...........................  ..........................  ....................................  See footnote,\6\ p. S102.
14. Butyl benzyl phthalate.........  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
15. bis(2-Chloroethoxy) methane....  GC....................  611........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
16. bis(2-Chloroethyl) ether.......  GC....................  611........................  ..........................

[[Page 33]]

 
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
17. bis(2-Ethylhexyl) phthalate....  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
18. Bromodichloromethane...........  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
19. Bromoform......................  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
20. Bromomethane...................  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
21. 4-Bromophenyl phenyl ether.....  GC....................  611........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
22. Carbon tetrachloride...........  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
23. 4-Chloro-3-methyl phenol.......  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
24. Chlorobenzene..................  GC....................  601, 602...................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
25. Chloroethane...................  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
26. 2-Chloroethylvinyl ether.......  GC....................  601........................  ..........................
                                     GC/MS.................  624.1, 1624B...............  ..........................
27. Chloroform.....................  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
28. Chloromethane..................  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
29. 2-Chloronaphthalene............  GC....................  612........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
30. 2-Chlorophenol.................  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
31. 4-Chlorophenyl phenyl ether....  GC....................  611........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
32. Chrysene.......................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
33. Dibenzo(a,h)anthracene.........  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
34. Dibromochloromethane...........  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
35. 1,2-Dichlorobenzene............  GC....................  601, 602...................  6200 C-2011...............
                                     GC/MS.................  624.1, 1625B...............  6200 B-2011...............  ....................................  See footnote,\9\ p. 27.
36. 1,3-Dichlorobenzene............  GC....................  601, 602...................  6200 C-2011...............
                                     GC/MS.................  624.1, 1625B...............  6200 B-2011...............  ....................................  See footnote,\9\ p. 27.
37. 1,4-Dichlorobenzene............  GC....................  601, 602...................  6200 C-2011...............

[[Page 34]]

 
                                     GC/MS.................  624.1, 1625B...............  6200 B-2011...............  ....................................  See footnote,\9\ p. 27.
38. 3,3'-Dichlorobenzidine.........  GC/MS.................  625.1, 1625B...............  6410 B-2000...............
                                     HPLC..................  605........................  ..........................
39. Dichlorodifluoromethane........  GC....................  601........................  ..........................
                                     GC/MS.................  ...........................  6200 C-2011...............
40. 1,1-Dichloroethane.............  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
41. 1,2-Dichloroethane.............  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
42. 1,1-Dichloroethene.............  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
43. trans-1,2-Dichloroethene.......  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
44. 2,4-Dichlorophenol.............  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
45. 1,2-Dichloropropane............  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
46. cis-1,3-Dichloropropene........  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
47. trans-1,3-Dichloropropene......  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
48. Diethyl phthalate..............  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
49. 2,4-Dimethylphenol.............  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
50. Dimethyl phthalate.............  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
51. Di-n-butyl phthalate...........  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
52. Di-n-octyl phthalate...........  GC....................  606........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
53. 2, 4-Dinitrophenol.............  GC....................  604........................  6420 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............
54. 2,4-Dinitrotoluene.............  GC....................  609........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
55. 2,6-Dinitrotoluene.............  GC....................  609........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
56. Epichlorohydrin................  GC....................  ...........................  ..........................  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  ...........................  ..........................  ....................................  See footnote,\6\ p. S102.
57. Ethylbenzene...................  GC....................  602........................  6200 C-2011...............

[[Page 35]]

 
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
58. Fluoranthene...................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
59. Fluorene.......................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
60. 1,2,3,4,6,7,8-Heptachloro-       GC/MS.................  1613B......................  ..........................
 dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro-       GC/MS.................  1613B......................  ..........................
 dibenzofuran.
62. 1,2,3,4,6,7,8- Heptachloro-      GC/MS.................  1613B......................  ..........................
 dibenzo-p-dioxin.
63. Hexachlorobenzene..............  GC....................  612........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
64. Hexachlorobutadiene............  GC....................  612........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
65. Hexachlorocyclopentadiene......  GC....................  612........................  ..........................
                                     GC/MS.................  625.1,\5\ 1625B............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
66. 1,2,3,4,7,8-Hexachloro-          GC/MS.................  1613B......................  ..........................
 dibenzofuran.
67. 1,2,3,6,7,8-Hexachloro-          GC/MS.................  1613B......................  ..........................
 dibenzofuran.
68. 1,2,3,7,8,9-Hexachloro-          GC/MS.................  1613B......................  ..........................
 dibenzofuran.
69. 2,3,4,6,7,8-Hexachloro-          GC/MS.................  1613B......................  ..........................
 dibenzofuran.
70. 1,2,3,4,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B......................  ..........................
 p-dioxin.
71. 1,2,3,6,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B......................  ..........................
 p-dioxin.
72. 1,2,3,7,8,9-Hexachloro-dibenzo-  GC/MS.................  1613B......................  ..........................
 p-dioxin.
73. Hexachloroethane...............  GC....................  612........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
74. Indeno(1,2,3-c,d) pyrene.......  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
75. Isophorone.....................  GC....................  609........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
76. Methylene chloride.............  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
77. 2-Methyl-4,6-dinitrophenol.....  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.

[[Page 36]]

 
78. Naphthalene....................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............
79. Nitrobenzene...................  GC....................  609........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  ...........................  ..........................  D4657-92 (98).......................
80. 2-Nitrophenol..................  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
81. 4-Nitrophenol..................  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
82. N-Nitrosodimethylamine.........  GC....................  607........................  ..........................
                                     GC/MS.................  625.1,\5\ 1625B............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
83. N-Nitrosodi-n-propylamine......  GC....................  607........................  ..........................
                                     GC/MS.................  625.1,\5\ 1625B............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
84. N-Nitrosodiphenylamine.........  GC....................  607........................  ..........................
                                     GC/MS.................  625.1,\5\ 1625B............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
85. Octachlorodibenzofuran.........  GC/MS.................  1613B \10\.................  ..........................
86. Octachlorodibenzo-p-dioxin.....  GC/MS.................  1613B \10\.................  ..........................
87. 2,2'-oxybis(1-chloropropane)     GC....................  611........................  ..........................
 \12\ [also known as bis(2-Chloro-1-
 methylethyl) ether].
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
88. PCB-1016.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
89. PCB-1221.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
90. PCB-1232.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
91. PCB-1242.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
92. PCB-1248.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
93. PCB-1254.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\

[[Page 37]]

 
                                     GC/MS.................  625.1......................  6410 B-2000...............
94. PCB-1260.......................  GC....................  608.3......................  ..........................  ....................................  See footnote,\3\ p. 43; See
                                                                                                                                                             footnote.\8\
                                     GC/MS.................  625.1......................  6410 B-2000...............
95. 1,2,3,7,8-Pentachloro-           GC/MS.................  1613B......................  ..........................
 dibenzofuran.
96. 2,3,4,7,8-Pentachloro-           GC/MS.................  1613B......................  ..........................
 dibenzofuran.
97. 1,2,3,7,8,-Pentachloro-dibenzo-  GC/MS.................  1613B......................  ..........................
 p-dioxin.
98. Pentachlorophenol..............  GC....................  604........................  6420 B-2000...............  ....................................  See footnote,\3\ p. 140.
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
99. Phenanthrene...................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
100. Phenol........................  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
101. Pyrene........................  GC....................  610........................  ..........................
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
                                     HPLC..................  610........................  6440 B-2005...............  D4657-92 (98).......................
102. 2,3,7,8-Tetrachloro-            GC/MS.................  1613B \10\.................  ..........................
 dibenzofuran.
103. 2,3,7,8-Tetrachloro-dibenzo-p-  GC/MS.................  613, 625.1,\5a\ 1613B......  ..........................
 dioxin.
104. 1,1,2,2-Tetrachloroethane.....  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
105. Tetrachloroethene.............  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
106. Toluene.......................  GC....................  602........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
107. 1,2,4-Trichlorobenzene........  GC....................  612........................  ..........................  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
108. 1,1,1-Trichloroethane.........  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
109. 1,1,2-Trichloroethane.........  GC....................  601........................  6200 C-2011...............  ....................................  See footnote,\3\ p. 130.
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
110. Trichloroethene...............  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............
111. Trichlorofluoromethane........  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1......................  6200 B-2011...............
112. 2,4,6-Trichlorophenol.........  GC....................  604........................  6420 B-2000...............
                                     GC/MS.................  625.1, 1625B...............  6410 B-2000...............  ....................................  See footnote,\9\ p. 27.
113. Vinyl chloride................  GC....................  601........................  6200 C-2011...............
                                     GC/MS.................  624.1, 1624B...............  6200 B-2011...............

[[Page 38]]

 
114. Nonylphenol...................  GC/MS.................  ...........................  ..........................  D7065-11............................
115. Bisphenol A (BPA).............  GC/MS.................  ...........................  ..........................  D7065-11............................
116. p-tert-Octylphenol (OP).......  GC/MS.................  ...........................  ..........................  D7065-11............................
117. Nonylphenol Monoethoxylate      GC/MS.................  ...........................  ..........................  D7065-11............................
 (NP1EO).
118. Nonylphenol Diethoxylate        GC/MS.................  ...........................  ..........................  D7065-11............................
 (NP2EO).
119. Adsorbable Organic Halides      Adsorption and          1650 \11\..................  ..........................
 (AOX).                               Coulometric Titration.
120. Chlorinated Phenolics.........  In Situ Acetylation     1653 \11\..................  ..........................  ....................................
                                      and GC/MS.
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([micro]g/L) except for Method 1613B, in which the parameters are expressed in picograms per liter (pg/L).
\2\ The full text of Methods 601-613, 1613B, 1624B, and 1625B are provided at appendix A, Test Procedures for Analysis of Organic Pollutants. The standardized test procedure to be used to
  determine the method detection limit (MDL) for these test procedures is given at appendix B of this part, Definition and Procedure for the Determination of the Method Detection Limit. These
  methods are available at: https://www.epa.gov/cwa-methods as individual PDF files.
\3\ Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA.
\4\ Method 624.1 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate the ability to detect and quantify
  these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample introduction techniques other than simple purge-and-trap may be required. QC
  acceptance criteria from Method 603 should be used when analyzing samples for acrolein and acrylonitrile in the absence of such criteria in Method 624.1.
\5\ Method 625.1 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi-n-propylamine, and N-nitrosodiphenylamine. However, when they are known to
  be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.
\5a\ Method 625.1 screening only.
\6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and
  Wastewater. 1981. American Public Health Association (APHA).
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 1624B, and 1625B in accordance with
  procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624.1 and 625.1 and 100% for methods
  1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the
  quality control (QC) acceptance criteria in the pertinent method, analytical results for that parameter in the unspiked sample are suspect. The results should be reported but cannot be used
  to demonstrate regulatory compliance. If the method does not contain QC acceptance criteria, control limits of  three standard deviations around the mean of a minimum
  of five replicate measurements must be used. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ Organochlorine Pesticides and PCBs in Wastewater Using Empore\TM\ Disk. Revised October 28, 1994. 3M Corporation.
\9\ Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in
  Water and Fluvial Sediments. 1993. USGS.
\10\ Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the
  method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of
  this method is provided in appendix A to this part and at https://www.epa.gov/cwa-methods/approved-cwa-methods-organic-compounds.

[[Page 39]]

 
\11\ Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997 U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and
  GCMS. Revision A, 1997 U.S. EPA. The full text for both of these methods is provided at appendix A in part 430 of this chapter, The Pulp, Paper, and Paperboard Point Source Category.
\12\ The compound was formerly inaccurately labeled as 2,2'-oxybis(2-chloropropane) and bis(2-chloroisopropyl) ether. Some versions of Methods 611, and 1625 inaccurately list the analyte as
  ``bis(2-chloroisopropyl)ether,'' but use the correct CAS number of 108-60-1.


                                              Table ID--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                        Method                EPA 2 7 10          Standard methods             ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin..........................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-96     See footnote,\3\ p.
                                                                                                             (02).                  7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
2. Ametryn.........................  GC.....................  507, 619.............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\9\
                                                                                                                                    O-3106-93; See
                                                                                                                                    footnote,\6\ p. S68.
                                     GC/MS..................  525.2, 625.1.........  .....................  .....................  See footnote,\14\ O-
                                                                                                                                    1121-91.
3. Aminocarb.......................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC...................  632..................
4. Atraton.........................  GC.....................  619..................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.
                                     GC/MS..................  625.1................
5. Atrazine........................  GC.....................  507, 619, 608.3......  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS..................  525.1, 525.2, 625.1..  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
6. Azinphos methyl.................  GC.....................  614, 622, 1657.......  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS..................  625.1................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
7. Barban..........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     GC/MS..................  625.1................
8. [alpha]-BHC.....................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS..................  625.1 \5\............  6410 B-2000..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
9. [beta]-BHC......................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\8\
                                                                                                             96(02).                3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
10. [delta]-BHC....................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\8\
                                                                                                             96(02).                3M0222.

[[Page 40]]

 
                                     GC/MS..................  625.1................  6410 B-2000..........
11. [gamma]-BHC (Lindane)..........  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1 \5\............  6410 B-2000..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
12. Captan.........................  GC.....................  617, 608.3...........  6630 B-2007..........  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7.
13. Carbaryl.......................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94, See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC...................  531.1, 632...........
                                     HPLC/MS................  553..................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS..................  625.1................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
14. Carbophenothion................  GC.....................  617, 608.3...........  6630 B-2007..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
                                     GC/MS..................  625.1................
15. Chlordane......................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
16. Chloropropham..................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     GC/MS..................  625.1................
17. 2,4-D..........................  GC.....................  615..................  6640 B-2006..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
18. 4,4[min]-DDD...................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3105-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
19. 4,4[min]-DDE...................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
20. 4,4[min]-DDT...................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
21. Demeton-O......................  GC.....................  614, 622.............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.

[[Page 41]]

 
                                     GC/MS..................  625.1................
22. Demeton-S......................  GC.....................  614, 622.............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS..................  625.1................
23. Diazinon.......................  GC.....................  507, 614, 622, 1657..  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\6\ p. S51.
                                     GC/MS..................  525.2, 625.1.........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
24. Dicamba........................  GC.....................  615..................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    115.
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
25. Dichlofenthion.................  GC.....................  622.1................  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
26. Dichloran......................  GC.....................  608.2, 617, 608.3....  6630 B-2007..........  .....................  See footnote,\3\ p.
                                                                                                                                    7.
27. Dicofol........................  GC.....................  617, 608.3...........  .....................  .....................  See footnote,\4\ O-
                                                                                                                                    3104-83.
28. Dieldrin.......................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
29. Dioxathion.....................  GC.....................  614.1, 1657..........  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
30. Disulfoton.....................  GC.....................  507, 614, 622, 1657..  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS..................  525.2, 625.1.........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
31. Diuron.........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  553..................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
32. Endosulfan I...................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\
                                                                                                                                    3M0222).
                                     GC/MS..................  625.1 \5\............  6410 B-2000..........  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
33. Endosulfan II..................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS..................  625.1 \5\............  6410 B-2000..........  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
34. Endosulfan Sulfate.............  GC.....................  617, 608.3...........  6630 C-2007..........  .....................  See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
35. Endrin.........................  GC.....................  505, 508, 617, 1656,   6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                               608.3.                                        96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  525.1, 525.2,          6410 B-2000..........
                                                               625.1\5\.
36. Endrin aldehyde................  GC.....................  617, 608.3...........  6630 C-2007..........  .....................  See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS..................  625.1................
37. Ethion.........................  GC.....................  614, 614.1, 1657.....  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.

[[Page 42]]

 
                                     GC/MS..................  625.1................  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
38. Fenuron........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
39. Fenuron-TCA....................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
40. Heptachlor.....................  GC.....................  505, 508, 617, 1656,   6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                               608.3.                                        96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  525.1, 525.2, 625.1..  6410 B-2000..........
41. Heptachlor epoxide.............  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\6\ p. S73;
                                                                                                                                    See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS..................  625.1................  6410 B-2000..........
42. Isodrin........................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  .....................  See footnote,\4\ O-
                                                                                                                                    3104-83; See
                                                                                                                                    footnote,\6\ p. S73.
                                     GC/MS..................  625.1................
43. Linuron........................  GC.....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  553..................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS..................  .....................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
44. Malathion......................  GC.....................  614, 1657............  6630 B-2007..........  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS..................  625.1................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
45. Methiocarb.....................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC...................  632..................
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
46. Methoxychlor...................  GC.....................  505, 508, 608.2, 617,  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                               1656, 608.3.                                  96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS..................  525.1, 525.2, 625.1..  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
47. Mexacarbate....................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC...................  632..................
                                     GC/MS..................  625.1................

[[Page 43]]

 
48. Mirex..........................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83.
                                     GC/MS..................  625.1................
49. Monuron........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
50. Monuron-TCA....................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
51. Neburon........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
52. Parathion methyl...............  GC.....................  614, 622, 1657.......  6630 B-2007..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\3\
                                                                                                                                    p. 25.
                                     GC/MS..................  625.1................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
53. Parathion ethyl................  GC.....................  614..................  6630 B-2007..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\3\
                                                                                                                                    p. 25.
                                     GC/MS..................  .....................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
54. PCNB...........................  GC.....................  608.1, 617, 608.3....  6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7.
55. Perthane.......................  GC.....................  617, 608.3...........  .....................  D3086-90, D5812-       See footnote,\4\ O-
                                                                                                             96(02).                3104-83.
56. Prometon.......................  GC.....................  507, 619.............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS..................  525.2, 625.1.........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
57. Prometryn......................  GC.....................  507, 619.............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS..................  525.1, 525.2, 625.1..  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
58. Propazine......................  GC.....................  507, 619, 1656, 608.3  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS..................  525.1, 525.2, 625.1..
59. Propham........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
60. Propoxur.......................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC...................  632..................
61. Secbumeton.....................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.

[[Page 44]]

 
                                     GC.....................  619..................
62. Siduron........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
                                     HPLC/MS................  .....................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
63. Simazine.......................  GC.....................  505, 507, 619, 1656,   .....................  .....................  See footnote,\3\ p.
                                                               608.3.                                                               83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS..................  525.1, 525.2, 625.1..  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
64. Strobane.......................  GC.....................  617, 608.3...........  6630 B-2007 & C-2007.  .....................  See footnote,\3\ p.
                                                                                                                                    7.
65. Swep...........................  TLC....................  .....................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC...................  632..................
66. 2,4,5-T........................  GC.....................  615..................  6640 B-2006..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
67. 2,4,5-TP (Silvex)..............  GC.....................  615..................  6640 B-2006..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
68. Terbuthylazine.................  GC.....................  619, 1656, 608.3.....  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.
                                     GC/MS..................  .....................  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
69. Toxaphene......................  GC.....................  505, 508, 617, 1656,   6630 B-2007 & C-2007.  D3086-90, D5812-       See footnote,\3\ p.
                                                               608.3.                                        96(02).                7; See footnote; \8\
                                                                                                                                    See footnote,\4\ O-
                                                                                                                                    3105-83.
                                     GC/MS..................  525.1, 525.2, 625.1..  6410 B-2000..........
70. Trifluralin....................  GC.....................  508, 617, 627, 1656,   6630 B-2007..........  .....................  See footnote,\3\ p.
                                                               608.3.                                                               7; See footnote,\9\
                                                                                                                                    O-3106-93.
                                     GC/MS..................  525.2, 625.1.........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC of this
  section, where entries are listed by chemical name.
\2\ The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at appendix B of this
  part, Definition and Procedure for the Determination of the Method Detection Limit.
\3\ Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA
  publication includes thin-layer chromatography (TLC) methods.
\4\ Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 5, Chapter A3. 1987. USGS.
\5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
  Method 608.3 is the preferred method.
\6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard
  Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).

[[Page 45]]

 
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608.3 and
  625.1 in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and
  analyze 5% of all samples analyzed with Method 608.3 or 5% of all samples analyzed with Method 625.1 to monitor and evaluate laboratory data quality
  in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results
  for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These
  quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ Organochlorine Pesticides and PCBs in Wastewater Using Empore\TM\ Disk. Revised October 28, 1994. 3M Corporation.
\9\ Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of
  Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography With Nitrogen Phosphorus Detectors. 1994. USGS.
\10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional
  Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in
  Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA
  Method 525.2 is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass
  Spectrometry, Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods for the Determination of Nonconventional Pesticides in Municipal
  and Industrial Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA. Methods 608.3 and 625.1 are available at https://www.epa.gov/cwa-methods/
  approved-cwa-test-methods-organic-compounds.
\11\ Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995.
  USGS.
\12\ Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass
  Spectrometry. 2001. USGS.
\13\ Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass
  spectrometry. 2001. USGS.
\14\ Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion
  monitoring. 1992. USGS.


                                                                   Table IE--List of Approved Radiologic Test Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                             Reference (method number or page)
                                                          --------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                 Method                                  Standard Methods 18th,
                                                                  EPA \1\               19th, 20th Ed.          Standard Methods Online              ASTM                      USGS \2\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter.....  Proportional or        900.0................  7110 B....................  7110 B-00.................  D1943-90, 96..............  pp. 75 and 78 \3\
                                     scintillation
                                     counter.
2. Alpha-Counting error, pCi per    Proportional or        Appendix B...........  7110 B....................  7110 B-00.................  D1943-90, 96..............  p. 79
 liter.                              scintillation
                                     counter.
3. Beta-Total, pCi per liter......  Proportional counter.  900.0................  7110 B....................  7110 B-00.................  D1890-90, 96..............  pp. 75 and 78 \3\
4. Beta-Counting error, pCi.......  Proportional counter.  Appendix B...........  7110 B....................  7110 B-00.................  D1890-90, 96..............  p. 79
5. (a) Radium Total pCi per liter.  Proportional counter.  903.0................  7500-Ra B.................  7500-Ra B-01..............  D2460-90, 97..............
(b) Ra, pCi per liter.............
                                    Scintillation counter  903.1................  7500-Ra C.................  7500-Ra C-01..............  D3454-91, 97..............  p. 81
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.
\2\ Fishman, M. J. and Brown, Eugene, ``Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters,'' U.S. Geological Survey, Open-File Report 76-177 (1976).
\3\ The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, the two results must be added to obtain the
  ``total.''


[[Page 46]]


                        Table IF--List of Approved Methods for Pharmaceutical Pollutants
----------------------------------------------------------------------------------------------------------------
                                      CAS registry
     Pharmaceuticals pollutants            No.                         Analytical method number
----------------------------------------------------------------------------------------------------------------
Acetonitrile.......................         75-05-8  1666/1671/D3371/D3695/624.1
n-Amyl acetate.....................        628-63-7  1666/D3695
n-Amyl alcohol.....................         71-41-0  1666/D3695
Benzene............................         71-43-2  D4763/D3695/502.2/524.2/624.1
n-Butyl-acetate....................        123-86-4  1666/D3695
tert-Butyl alcohol.................         75-65-0  1666/624.1
Chlorobenzene......................        108-90-7  502.2/524.2/624.1
Chloroform.........................         67-66-3  502.2/524.2/551/624.1
o-Dichlorobenzene..................         95-50-1  1625C/502.2/524.2/624.1
1,2-Dichloroethane.................        107-06-2  D3695/502.2/524.2/624.1
Diethylamine.......................        109-89-7  1666/1671
Dimethyl sulfoxide.................         67-68-5  1666/1671
Ethanol............................         64-17-5  1666/1671/D3695/624.1
Ethyl acetate......................        141-78-6  1666/D3695/624.1
n-Heptane..........................        142-82-5  1666/D3695
n-Hexane...........................        110-54-3  1666/D3695
Isobutyraldehyde...................         78-84-2  1666/1667
Isopropanol........................         67-63-0  1666/D3695
Isopropyl acetate..................        108-21-4  1666/D3695
Isopropyl ether....................        108-20-3  1666/D3695
Methanol...........................         67-56-1  1666/1671/D3695/624.1
Methyl Cellosolve[supreg] (2-              109-86-4  1666/1671
 Methoxy ethanol).
Methylene chloride.................         75-09-2  502.2/524.2/624.1
Methyl formate.....................        107-31-3  1666
4-Methyl-2-pentanone (MIBK)........        108-10-1  1624C/1666/D3695/D4763/524.2/624.1
Phenol.............................        108-95-2  D4763
n-Propanol.........................         71-23-8  1666/1671/D3695/624.1
2-Propanone (Acetone)..............         67-64-1  D3695/D4763/524.2/624.1
Tetrahydrofuran....................        109-99-9  1666/524.2/624.1
Toluene............................        108-88-3  D3695/D4763/502.2/524.2/624.1
Triethlyamine......................        121-44-8  1666/1671
Xylenes............................        (Note 1)  1624C/1666/624.1
----------------------------------------------------------------------------------------------------------------
Table IF note:
\1\ 1624C: m-xylene 108-38-3, o,p-xylene, E-14095 (Not a CAS number; this is the number provided in the
  Environmental Monitoring Methods Index [EMMI] database.); 1666: m,p-xylene 136777-61-2, o-xylene 95-47-6.


         Table IG--Test Methods for Pesticide Active Ingredients
                            [40 CFR part 455]
------------------------------------------------------------------------
                                                         EPA analytical
   EPA survey code     Pesticide name       CAS No.       method No.(s)
                                                               \3\
------------------------------------------------------------------------
8...................  Triadimefon.....      43121-43-3  507/633/525.1/
                                                         525.2/1656/
                                                         625.1.
12..................  Dichlorvos......         62-73-7  1657/507/622/
                                                         525.1/525.2/
                                                         625.1.
16..................  2,4-D; 2,4-D             94-75-7  1658/515.1/615/
                       Salts and                         515.2/555.
                       Esters [2,4-
                       Dichloro-
                       phenoxyacetic
                       acid].
17..................  2,4-DB; 2,4-DB           94-82-6  1658/515.1/615/
                       Salts and                         515.2/555.
                       Esters [2,4-
                       Dichlorophenoxy
                       butyric acid].
22..................  Mevinphos.......       7786-34-7  1657/507/622/
                                                         525.1/525.2/
                                                         625.1.
25..................  Cyanazine.......      21725-46-2  629/507/608.3/
                                                         625.1.
26..................  Propachlor......       1918-16-7  1656/508/608.1/
                                                         525.1/525.2/
                                                         608.3/625.1.
27..................  MCPA; MCPA Salts         94-74-6  1658/615/555.
                       and Esters.
                      [2-Methyl-4-
                       chlorophenoxyac
                       etic acid].
30..................  Dichlorprop;            120-36-5  1658/515.1/615/
                       Dichlorprop                       515.2/555.
                       Salts and
                       Esters [2-(2,4-
                       Dichlorophenoxy
                       ) propionic
                       acid].
31..................  MCPP; MCPP Salts         93-65-2  1658/615/555.
                       and Esters [2-
                       (2-Methyl-4-
                       chlorophenoxy)
                       propionic acid].
35..................  TCMTB [2-             21564-17-0  637.
                       (Thiocyanomethy
                       lthio) benzo-
                       thiazole].
39..................  Pronamide.......      23950-58-5  525.1/525.2/507/
                                                         633.1/625.1.
41..................  Propanil........        709-98-8  632.1/1656/
                                                         608.3.
45..................  Metribuzin......      21087-64-9  507/633/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
52..................  Acephate........      30560-19-1  1656/1657/608.3.
53..................  Acifluorfen.....      50594-66-6  515.1/515.2/555.
54..................  Alachlor........      15972-60-8  505/507/645/
                                                         525.1/525.2/
                                                         1656/608.3/
                                                         625.1.
55..................  Aldicarb........        116-06-3  531.1.
58..................  Ametryn.........        834-12-8  507/619/525.2/
                                                         625.1.
60..................  Atrazine........       1912-24-9  505/507/619/
                                                         525.1/525.2/
                                                         1656/ 608.3/
                                                         625.1.
62..................  Benomyl.........      17804-35-2  631.

[[Page 47]]

 
68..................  Bromacil;               314-40-9  507/633/525.1/
                       Bromacil Salts                    525.2/1656/
                       and Esters.                       608.3/625.1.
69..................  Bromoxynil......       1689-84-5  1625/1661/625.1.
69..................  Bromoxynil             1689-99-2  1656/608.3.
                       Octanoate.
70..................  Butachlor.......      23184-66-9  507/645/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
73..................  Captafol........       2425-06-1  1656/608.3/
                                                         625.1.
75..................  Carbaryl [Sevin]         63-25-2  531.1/632/553/
                                                         625.1.
76..................  Carbofuran......       1563-66-2  531.1/632/625.1.
80..................  Chloroneb.......       2675-77-6  1656/508/608.1/
                                                         525.1/525.2/
                                                         608.3/625.1.
82..................  Chlorothalonil..       1897-45-6  508/608.2/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
84..................  Stirofos........        961-11-5  1657/507/622/
                                                         525.1/525.2/
                                                         625.1.
86..................  Chlorpyrifos....       2921-88-2  1657/508/622/
                                                         625.1.
90..................  Fenvalerate.....      51630-58-1  1660.
103.................  Diazinon........        333-41-5  1657/507/614/622/
                                                         525.2/625.1.
107.................  Parathion methyl        298-00-0  1657/614/622/
                                                         625.1.
110.................  DCPA [Dimethyl         1861-32-1  508/608.2/525.1/
                       2,3,5,6-                          525.2/515.1 \2\/
                       tetrachloro-                      515.2 \2\/1656/
                       terephthalate].                   608.3/625.1.
112.................  Dinoseb.........         88-85-7  1658/515.1/615/
                                                         515.2/555/
                                                         625.1.
113.................  Dioxathion......         78-34-2  1657/614.1.
118.................  Nabonate                138-93-2  630.1.
                       [Disodium
                       cyanodithio-
                       imidocarbonate].
119.................  Diuron..........        330-54-1  632/553.
123.................  Endothall.......        145-73-3  548/548.1.
124.................  Endrin..........         72-20-8  1656/505/508/617/
                                                         525.1/525.2/
                                                         608.3/625.1.
125.................  Ethalfluralin...      55283-68-6  1656/627/608.3
                                                         See footnote 1.
126.................  Ethion..........        563-12-2  1657/614/614.1/
                                                         625.1.
127.................  Ethoprop........      13194-48-4  1657/507/622/
                                                         525.1/525.2/
                                                         625.1.
132.................  Fenarimol.......      60168-88-9  507/633.1/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
133.................  Fenthion........         55-38-9  1657/622/625.1.
138.................  Glyphosate [N-         1071-83-6  547.
                       (Phosphonomethy
                       l) glycine].
140.................  Heptachlor......         76-44-8  1656/505/508/617/
                                                         525.1/525.2/
                                                         608.3/625.1.
144.................  Isopropalin.....      33820-53-0  1656/627/608.3.
148.................  Linuron.........        330-55-2  553/632.
150.................  Malathion.......        121-75-5  1657/614/625.1.
154.................  Methamidophos...      10265-92-6  1657.
156.................  Methomyl........      16752-77-5  531.1/632.
158.................  Methoxychlor....         72-43-5  1656/505/508/
                                                         608.2/617/525.1/
                                                         525.2/608.3/
                                                         625.1.
172.................  Nabam...........        142-59-6  630/630.1.
173.................  Naled...........        300-76-5  1657/622/625.1.
175.................  Norflurazon.....      27314-13-2  507/645/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
178.................  Benfluralin.....       1861-40-1  1656/627/608.3
                                                         See footnote 1.
182.................  Fensulfothion...        115-90-2  1657/622/625.1.
183.................  Disulfoton......        298-04-4  1657/507/614/622/
                                                         525.2/625.1.
185.................  Phosmet.........        732-11-6  1657/622.1/
                                                         625.1.
186.................  Azinphos Methyl.         86-50-0  1657/614/622/
                                                         625.1.
192.................  Organo-tin            12379-54-3  Ind-01/200.7/
                       pesticides.                       200.9.
197.................  Bolstar.........      35400-43-2  1657/622.
203.................  Parathion.......         56-38-2  1657/614/625.1.
204.................  Pendimethalin...      40487-42-1  1656.
205.................  Pentachloronitro         82-68-8  1656/608.1/617/
                       benzene.                          608.3/625.1.
206.................  Pentachloropheno         87-86-5  1625/515.2/555/
                       l.                                515.1/525.1/
                                                         525.2/625.1.
208.................  Permethrin......      52645-53-1  608.2/508/525.1/
                                                         525.2/1656/1660/
                                                         608.3 \4\/625.1
                                                         \4\.
212.................  Phorate.........        298-02-2  1657/622/625.1.
218.................  Busan 85                128-03-0  630/630.1.
                       [Potassium
                       dimethyldithioc
                       arbamate].
219.................  Busan 40              51026-28-9  630/630.1.
                       [Potassium N-
                       hydroxymethyl-N-
                       methyldithiocar
                       bamate].
220.................  KN Methyl               137-41-7  630/630.1.
                       [Potassium N-
                       methyl-
                       dithiocarbamate
                       ].
223.................  Prometon........       1610-18-0  507/619/525.2/
                                                         625.1.
224.................  Prometryn.......       7287-19-6  507/619/525.1/
                                                         525.2/625.1.
226.................  Propazine.......        139-40-2  507/619/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
230.................  Pyrethrin I.....        121-21-1  1660.
232.................  Pyrethrin II....        121-29-9  1660.
236.................  DEF [S,S,S-              78-48-8  1657.
                       Tributyl
                       phosphorotrithi
                       oate].
239.................  Simazine........        122-34-9  505/507/619/
                                                         525.1/525.2/
                                                         1656/608.3/
                                                         625.1.
241.................  Carbam-S [Sodium        128-04-1  630/630.1.
                       dimethyldithio-
                       carbamate].

[[Page 48]]

 
243.................  Vapam [Sodium           137-42-8  630/630.1.
                       methyldithiocar
                       bamate].
252.................  Tebuthiuron.....      34014-18-1  507/525.1/525.2/
                                                         625.1.
254.................  Terbacil........       5902-51-2  507/633/525.1/
                                                         525.2/1656/
                                                         608.3/625.1.
255.................  Terbufos........      13071-79-9  1657/507/614.1/
                                                         525.1/525.2/
                                                         625.1.
256.................  Terbuthylazine..       5915-41-3  619/1656/608.3.
257.................  Terbutryn.......        886-50-0  507/619/525.1/
                                                         525.2/625.1.
259.................  Dazomet.........        533-74-4  630/630.1/1659.
262.................  Toxaphene.......       8001-35-2  1656/505/508/617/
                                                         525.1/525.2/
                                                         608.3/625.1.
263.................  Merphos                 150-50-5  1657/507/525.1/
                       [Tributyl                         525.2/622/
                       phosphorotrithi                   625.1.
                       oate].
264.................  Trifluralin \1\.       1582-09-8  1656/508/617/627/
                                                         525.2/608.3/
                                                         625.1.
268.................  Ziram [Zinc             137-30-4  630/630.1.
                       dimethyldithioc
                       arbamate].
------------------------------------------------------------------------
Table IG notes:
\1\ Monitor and report as total Trifluralin.
\2\ Applicable to the analysis of DCPA degradates.
\3\ EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are
  available in Methods for the Determination of Nonconventional
  Pesticides in Municipal and Industrial Wastewater, Volume I, EPA 821-R-
  93-010A, Revision I, August 1993, U.S. EPA. EPA Methods 200.9 and 505
  through 555 are available in Methods for the Determination of
  Nonconventional Pesticides in Municipal and Industrial Wastewater,
  Volume II, EPA 821-R-93-010B, August 1993, U.S. EPA. The full text of
  Methods 608.3, 625.1, and 1625 are provided at appendix A of this
  part. The full text of Method 200.7 is provided at appendix C of this
  part. Methods 608.3 and 625.1 are available at https://www.epa.gov/cwa-
  methods/approved-cwa-test-methods-organic-compounds.
\4\ Permethrin is not listed within methods 608.3 and 625.1; however,
  cis-permethrin and trans-permethrin are listed. Permethrin can be
  calculated by adding the results of cis- and trans-permethrin.


[[Page 49]]


                                          Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units              Method \1\                    EPA                Standard methods      AOAC, ASTM, USGS            Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Bacteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Coliform (fecal), number per     Most Probable Number  p. 132 \3\..................  9221 C E-2006.
 100 mL or number per gram dry       (MPN), 5 tube, 3
 weight.                             dilution, or.
                                    Membrane filter       p. 124 \3\..................  9222 D-2006 \ 27\...  B-0050-85. \4\
                                     (MF),\2\ single
                                     step.
2. Coliform (fecal) in presence of  MPN, 5 tube, 3        p. 132 \3\..................  9221 C E-2006.
 chlorine, number per 100 mL.        dilution, or.
                                    MF,\2\ single step    p. 124 \3\..................  9222 D-2006. \ 27\
                                     \5\.
3. Coliform (total), number per     MPN, 5 tube, 3        p. 114 \3\..................  9221 B-2006.
 100 mL.                             dilution, or.
                                    MF,\2\ single step    p. 108 \3\..................  9222 B-2006.........  B-0025-85. \4\
                                     or two step.
4. Coliform (total), in presence    MPN, 5 tube, 3        p. 114 \3\..................  9221 B-2006.
 of chlorine, number per 100 mL.     dilution, or.
                                    MF \2\ with           p. 111 \3\..................  9222 B-2006.
                                     enrichment.
5. E. coli, number per 100 mL.....  MPN,6 8 14 multiple   ............................  9221 B.2-2006/9221 F-
                                     tube, or.                                           2006 11 13.
                                    Multiple tube/        ............................  9223 B-2004 \12\....  991.15 \10\.........  Colilert[supreg],12
                                     multiple well, or.                                                                              16 Colilert-
                                                                                                                                     18[supreg].12 15 16
                                    MF,2 5 6 7 8 two      1103.1 \19\.................  9222 B-2006/9222 G-   D-5392-93. \9\
                                     step, or.                                           2006,\18\ 9213 D-
                                                                                         2007.
                                    Single step.........  1603,\20\ 1604 \21\.........  ....................  ....................  mColiBlue-
                                                                                                                                     24[supreg].\17\
6. Fecal streptococci, number per   MPN, 5 tube, 3        p. 139 \3\..................  9230 B-2007.
 100 mL.                             dilution, or.
                                    MF \2\, or..........  p. 136 \3\..................  9230 C-2007.........  B-0055-85 \4\.......
                                    Plate count.........  p. 143. \3\
7. Enterococci, number per 100 mL.  MPN,6 8 multiple      ............................  9230 D-2007.........  D6503-99 \9\........  Enterolert[supreg].1
                                     tube/multiple well,                                                                             2 22
                                     or.
                                    MF 2 5 6 7 8 two      1106.1 \23\.................  9230 C-2007.........  D5259-92. \9\
                                     step, or.
                                    Single step, or.....  1600 \24\...................  9230 C-2007.
                                    Plate count.........  p. 143. \3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Protozoa
--------------------------------------------------------------------------------------------------------------------------------------------------------
8. Cryptosporidium................  Filtration/IMS/FA...  1622, \25\ 1623. \26\

[[Page 50]]

 
9. Giardia........................  Filtration/IMS/FA...  1623. \26\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IH notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water, and Wastes. EPA/600/8-78/017. 1978. U.S. EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may
  contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
  comparability of results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.
\11\ The multiple-tube fermentation test is used in 9221B.2-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.
\12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
  glucuronidase produced by E. coli.
\13\ After prior enrichment in a presumptive medium for total coliform using 9221B.2-2006, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC
  media supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C, rather than the 24 h required for the Colilert[supreg] test, and is recommended for marine water samples.
\16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], and Quanti-Tray[supreg] may be obtained from IDEXX Laboratories Inc.
\17\ A description of the mColiBlue24[supreg] test may be obtained from Hach Company.
\18\ Subject total coliform positive samples determined by 9222B-2006 or other membrane filter procedure to 9222G-2006 using NA-MUG media.
\19\ Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-10-
  002. March 2010. U.S. EPA.
\20\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified
  mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.
\21\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. New Medium for the
  Simultaneous Detection of Total Coliform and Escherichia coli in Water. Appl. Environ. Microbiol. 59:3534-3544 and in Method 1604: Total Coliforms and
  Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium), EPA 821-R-02-024, September 2002,
  U.S. EPA.
\22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.

[[Page 51]]

 
\23\ Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), EPA-821-R-09-015. December 2009.
  U.S. EPA.
\24\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-14-011.
  September 2014. U.S. EPA.
\25\ Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
  concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
  Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. U.S. EPA.
\26\ Method 1623 uses a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
  determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
  of Cryptosporidium and Giardia oocysts and cysts. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002. December
  2005. U.S. EPA.
\27\ On a monthly basis, at least ten blue colonies from the medium must be verified using Lauryl Tryptose Broth and EC broth, followed by count
  adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications
  should be done from randomized sample sources.


[[Page 52]]

    (b) Certain material is incorporated by reference into this part 
with the approval of the Director of the Federal Register under 5 U.S.C. 
552(a) and 1 CFR part 51. All approved material is available for 
inspection at EPA's Water Docket, EPA West, 1301 Constitution Avenue 
NW., Room 3334, Washington, DC 20004, Telephone: 202-566-2426, and is 
available from the sources listed below. It is also available for 
inspection at the National Archives and Records Administration (NARA). 
For information on the availability of this material at NARA, call 202-
741-6030, or go to: https://www.archives.gov/federal-register/cfr/ibr-
locations.html.
    (1) Environmental Monitoring and Support Laboratory, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm or from: National 
Technical Information Service, 5285 Port Royal Road, Springfield, 
Virginia 22161
    (i) Microbiological Methods for Monitoring the Environment, Water, 
and Wastes. 1978. EPA/600/8-78/017, Pub. No. PB-290329/A.S.
    (A) Part III Analytical Methodology, Section B Total Coliform 
Methods, page 108. Table IA, Note 3; Table IH, Note 3.
    (B) Part III Analytical Methodology, Section B Total Coliform 
Methods, 2.6.2 Two-Step Enrichment Procedure, page 111. Table IA, Note 
3; Table IH, Note 3.
    (C) Part III Analytical Methodology, Section B Total Coliform 
Methods, 4 Most Probable Number (MPN) Method, page 114. Table IA, Note 
3; Table IH, Note 3.
    (D) Part III Analytical Methodology, Section C Fecal Coliform 
Methods, 2 Direct Membrane Filter (MF) Method, page 124. Table IA, Note 
3; Table IH, Note 3.
    (E) Part III, Analytical Methodology, Section C Fecal Coliform 
Methods, 5 Most Probable Number (MPN) Method, page 132. Table IA, Note 
3; Table IH, Note 3.
    (F) Part III Analytical Methodology, Section D Fecal Streptococci, 2 
Membrane Filter (MF) Method, page 136. Table IA, Note 3; Table IH, Note 
3.
    (G) Part III Analytical Methodology, Section D Fecal Streptococci, 4 
Most Probable Number Method, page 139. Table IA, Note 3; Table IH, Note 
3.
    (H) Part III Analytical Methodology, Section D Fecal Streptococci, 5 
Pour Plate Method, page 143. Table IA, Note 3; Table IH, Note 3.
    (ii) [Reserved]
    (2) Environmental Monitoring and Support Laboratory, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) Method 300.1 (including Errata Cover Sheet, April 27, 1999), 
Determination of Inorganic Ions in Drinking Water by Ion Chromatography, 
Revision 1.0, 1997. Table IB, Note 52.
    (ii) Method 551, Determination of Chlorination Disinfection 
Byproducts and Chlorinated Solvents in Drinking Water by Liquid-Liquid 
Extraction and Gas Chromatography With Electron-Capture Detection. 1990. 
Table IF.
    (3) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental 
Protection Agency, Cincinnati OH (US EPA). Available from http://
water.epa.gov/scitech/methods/cwa/index.cfm or from the National 
Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, 
VA 22161. Telephone: 800-553-6847.
    (i) Methods for the Determination of Inorganic Substances in 
Environmental Samples. August 1993. EPA/600/R-93/100, Pub. No. PB 
94120821. Table IB, Note 52.
    (A) Method 180.1, Determination of Turbidity by Nephelometry. 
Revision 2.0. Table IB, Note 52.
    (B) Method 300.0, Determination of Inorganic Anions by Ion 
Chromatography. Revision 2.1. Table IB, Note 52.
    (C) Method 335.4, Determination of Total Cyanide by Semi-Automated 
Colorimetry. Revision 1.0. Table IB, Notes 52 and 57.
    (D) Method 350.1, Determination of Ammonium Nitrogen by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Notes 30 and 52.
    (E) Method 351.2, Determination of Total Kjeldahl Nitrogen by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Note 52.

[[Page 53]]

    (F) Method 353.2, Determination of Nitrate-Nitrite Automated 
Colorimetry. Revision 2.0. Table IB, Note 52.
    (G) Method 365.1, Determination of Phosphorus by Automated 
Colorimetry. Revision 2.0. Table IB, Note 52.
    (H) Method 375.2, Determination of Sulfate by Automated Colorimetry. 
Revision 2.0. Table IB, Note 52.
    (I) Method 410.4, Determination of Chemical Oxygen Demand by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Note 52.
    (ii) Methods for the Determination of Metals in Environmental 
Samples, Supplement I. May 1994. EPA/600/R-94/111, Pub. No. PB 95125472. 
Table IB, Note 52.
    (A) Method 200.7, Determination of Metals and Trace Elements in 
Water and Wastes by Inductively Coupled Plasma-Atomic Emission 
Spectrometry. Revision 4.4. Table IB, Note 52.
    (B) Method 200.8, Determination of Trace Elements in Water and 
Wastes by Inductively Coupled Plasma Mass Spectrometry. Revision 5.3. 
Table IB, Note 52.
    (C) Method 200.9, Determination of Trace Elements by Stabilized 
Temperature Graphite Furnace Atomic Absorption Spectrometry. Revision 
2.2. Table IB, Note 52.
    (D) Method 218.6, Determination of Dissolved Hexavalent Chromium in 
Drinking Water, Groundwater, and Industrial Wastewater Effluents by Ion 
Chromatography. Revision 3.3. Table IB, Note 52.
    (E) Method 245.1, Determination of Mercury in Water by Cold Vapor 
Atomic Absorption Spectrometry. Revision 3.0. Table IB, Note 52.
    (4) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental 
Protection Agency, Cincinnati OH (US EPA). Available at http://
water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) EPA Method 200.5, Determination of Trace Elements in Drinking 
Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission 
Spectrometry. Revision 4.2, October 2003. EPA/600/R-06/115. Table IB, 
Note 68.
    (ii) EPA Method 525.2, Determination of Organic Compounds in 
Drinking Water by Liquid-Solid Extraction and Capillary Column Gas 
Chromatography/Mass Spectrometry. Revision 2.0, 1995. Table ID, Note 10.
    (5) Office of Research and Development, Cincinnati OH. U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm or from ORD 
Publications, CERI, U.S. Environmental Protection Agency, Cincinnati OH 
45268.
    (i) Methods for Benzidine, Chlorinated Organic Compounds, 
Pentachlorophenol, and Pesticides in Water and Wastewater. 1978. Table 
IC, Note 3; Table ID, Note 3.
    (ii) Methods for Chemical Analysis of Water and Wastes. March 1979. 
EPA-600/4-79-020. Table IB, Note 1.
    (iii) Methods for Chemical Analysis of Water and Wastes. Revised 
March 1983. EPA-600/4-79-020. Table IB, Note 1.
    (A) Method 120.1, Conductance, Specific Conductance, [micro]mhos at 
25 [deg]C. Revision 1982. Table IB, Note 1.
    (B) Method 130.1, Hardness, Total (mg/L as CaCO3), 
Colorimetric, Automated EDTA. Issued 1971. Table IB, Note 1.
    (C) Method 150.2, pH, Continuous Monitoring (Electrometric). 
December 1982. Table IB, Note 1.
    (D) Method 160.4, Residue, Volatile, Gravimetric, Ignition at 550 
[deg]C. Issued 1971. Table IB, Note 1.
    (E) Method 206.5, Arsenic, Sample Digestion Prior to Total Arsenic 
Analysis by Silver Diethyldithiocarbamate or Hydride Procedures. Issued 
1978. Table IB, Note 1.
    (F) Method 231.2, Gold, Atomic Absorption, Furnace Technique. Issued 
1978. Table IB, Note 1.
    (G) Method 245.2, Mercury, Automated Cold Vapor Technique. Issued 
1974. Table IB, Note 1.
    (H) Method 252.2, Osmium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (I) Method 253.2, Palladium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (J) Method 255.2, Platinum, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (K) Method 265.2, Rhodium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.

[[Page 54]]

    (L) Method 279.2, Thallium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (M) Method 283.2, Titanium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (N) Method 289.2, Zinc, Atomic Absorption, Furnace Technique. Issued 
1978. Table IB, Note 1.
    (O) Method 310.2, Alkalinity, Colorimetric, Automated, Methyl 
Orange. Revision 1974. Table IB, Note 1.
    (P) Method 351.1, Nitrogen, Kjeldahl, Total, Colorimetric, Automated 
Phenate. Revision 1978. Table IB, Note 1.
    (Q) Method 352.1, Nitrogen, Nitrate, Colorimetric, Brucine. Issued 
1971. Table IB, Note 1.
    (R) Method 365.3, Phosphorus, All Forms, Colorimetric, Ascorbic 
Acid, Two Reagent. Issued 1978. Table IB, Note 1.
    (S) Method 365.4, Phosphorus, Total, Colorimetric, Automated, Block 
Digestor AA II. Issued 1974. Table IB, Note 1.
    (T) Method 410.3, Chemical Oxygen Demand, Titrimetric, High Level 
for Saline Waters. Revision 1978. Table IB, Note 1.
    (U) Method 420.1, Phenolics, Total Recoverable, Spectrophotometric, 
Manual 4-AAP With Distillation. Revision 1978. Table IB, Note 1.
    (iv) Prescribed Procedures for Measurement of Radioactivity in 
Drinking Water. 1980. EPA-600/4-80-032. Table IE.
    (A) Method 900.0, Gross Alpha and Gross Beta Radioactivity. Table 
IE.
    (B) Method 903.0, Alpha-Emitting iRadio Isotopes. Table IE.
    (C) Method 903.1, Radium-226, Radon Emanation Technique. Table IE.
    (D) Appendix B, Error and Statistical Calculations. Table IE.
    (6) Office of Science and Technology, U.S. Environmental Protection 
Agency, Washington DC (US EPA). Available at http://water.epa.gov/
scitech/methods/cwa/index.cfm.
    (i) Method 1625C, Semivolatile Organic Compounds by Isotope Dilution 
GCMS. 1989. Table IF.
    (ii) [Reserved]
    (7) Office of Water, U.S. Environmental Protection Agency, 
Washington DC (US EPA). Available at http://water.epa.gov/scitech/
methods/cwa/index.cfm or from National Technical Information Service, 
5285 Port Royal Road, Springfield, Virginia 22161.
    (i) Method 1631, Mercury in Water by Oxidation, Purge and Trap, and 
Cold Vapor Atomic Fluorescence Spectrometry. Revision E, August 2002. 
EPA-821-R-02-019, Pub. No. PB2002-108220. Table IB, Note 43.
    (ii) Kelada-01, Kelada Automated Test Methods for Total Cyanide, 
Acid Dissociable Cyanide, and Thiocyanate. Revision 1.2, August 2001. 
EPA 821-B-01-009, Pub. No. PB 2001-108275. Table IB, Note 55.
    (iii) In the compendium Analytical Methods for the Determination of 
Pollutants in Pharmaceutical Manufacturing Industry Wastewaters. July 
1998. EPA 821-B-98-016, Pub. No. PB95201679. Table IF, Note 1.
    (A) EPA Method 1666, Volatile Organic Compounds Specific to the 
Pharmaceutical Industry by Isotope Dilution GC/MS. Table IF, Note 1.
    (B) EPA Method 1667, Formaldehyde, Isobutyraldehyde, and Furfural by 
Derivatization Followed by High Performance Liquid Chromatography. Table 
IF.
    (C) Method 1671, Volatile Organic Compounds Specific to the 
Pharmaceutical Manufacturing Industry by GC/FID. Table IF.
    (iv) Methods For The Determination of Nonconventional Pesticides In 
Municipal and Industrial Wastewater, Volume I. Revision I, August 1993. 
EPA 821-R-93-010A, Pub. No. PB 94121654. Tables ID, IG.
    (A) Method 608.1, Organochlorine Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (B) Method 608.2, Certain Organochlorine Pesticides. Table ID, Note 
10; Table IG, Note 3.
    (C) Method 614, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (D) Method 614.1, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (E) Method 615, Chlorinated Herbicides. Table ID, Note 10; Table IG, 
Note 3.
    (F) Method 617, Organohalide Pesticides and PCBs. Table ID, Note 10; 
Table IG, Note 3.

[[Page 55]]

    (G) Method 619, Triazine Pesticides. Table ID, Note 10; Table IG, 
Note 3.
    (H) Method 622, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (I) Method 622.1, Thiophosphate Pesticides. Table ID, Note 10; Table 
IG, Note 3.
    (J) Method 627, Dinitroaniline Pesticides. Table ID, Note 10; Table 
IG, Notes 1 and 3.
    (K) Method 629, Cyanazine. Table IG, Note 3.
    (L) Method 630, Dithiocarbamate Pesticides. Table IG, Note 3.
    (M) Method 630.1, Dithiocarbamate Pesticides. Table IG, Note 3.
    (N) Method 631, Benomyl and Carbendazim. Table IG, Note 3.
    (O) Method 632, Carbamate and Urea Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (P) Method 632.1, Carbamate and Amide Pesticides. Table IG, Note 3.
    (Q) Method 633, Organonitrogen Pesticides. Table IG, Note 3.
    (R) Method 633.1, Neutral Nitrogen-Containing Pesticides. Table IG, 
Note 3.
    (S) Method 637, MBTS and TCMTB. Table IG, Note 3.
    (T) Method 644, Picloram. Table IG, Note 3.
    (U) Method 645, Certain Amine Pesticides and Lethane. Table IG, Note 
3.
    (V) Method 1656, Organohalide Pesticides. Table ID, Note 10; Table 
IG, Notes 1 and 3.
    (W) Method 1657, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (X) Method 1658, Phenoxy-Acid Herbicides. Table IG, Note 3.
    (Y) Method 1659, Dazomet. Table IG, Note 3.
    (Z) Method 1660, Pyrethrins and Pyrethroids. Table IG, Note 3.
    (AA) Method 1661, Bromoxynil. Table IG, Note 3.
    (BB) Ind-01. Methods EV-024 and EV-025, Analytical Procedures for 
Determining Total Tin and Triorganotin in Wastewater. Table IG, Note 3.
    (v) Methods For The Determination of Nonconventional Pesticides In 
Municipal and Industrial Wastewater, Volume II. August 1993. EPA 821-R-
93-010B, Pub. No. PB 94166311. Table IG.
    (A) Method 200.9, Determination of Trace Elements by Stabilized 
Temperature Graphite Furnace Atomic Absorption Spectrometry. Table IG, 
Note 3.
    (B) Method 505, Analysis of Organohalide Pesticides and Commercial 
Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and 
Gas Chromatography. Table ID, Note 10; Table IG, Note 3.
    (C) Method 507, The Determination of Nitrogen- and Phosphorus-
Containing Pesticides in Water by Gas Chromatography with a Nitrogen-
Phosphorus Detector. Table ID, Note 10; Table IG, Note 3.
    (D) Method 508, Determination of Chlorinated Pesticides in Water by 
Gas Chromatography with an Electron Capture Detector. Table ID, Note 10; 
Table IG, Note 3.
    (E) Method 515.1, Determination of Chlorinated Acids in Water by Gas 
Chromatography with an Electron Capture Detector. Table IG, Notes 2 and 
3.
    (F) Method 515.2, Determination of Chlorinated Acids in Water Using 
Liquid-Solid Extraction and Gas Chromatography with an Electron Capture 
Detector. Table IG, Notes 2 and 3.
    (G) Method 525.1, Determination of Organic Compounds in Drinking 
Water by Liquids-Solid Extraction and Capillary Column Gas 
Chromatography/Mass Spectrometry. Table ID, Note 10; Table IG, Note 3.
    (H) Method 531.1, Measurement of N-Methylcarbamoyloximes and N-
Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-
Column Derivatization. Table ID, Note 10; Table IG, Note 3.
    (I) Method 547, Determination of Glyphosate in Drinking Water by 
Direct-Aqueous-Injection HPLC, Post-Column Derivatization, and 
Fluorescence Detection. Table IG, Note 3.
    (J) Method 548, Determination of Endothall in Drinking Water by 
Aqueous Derivatization, Liquid-Solid Extraction, and Gas Chromatography 
with Electron-Capture Detector. Table IG, Note 3.
    (K) Method 548.1, Determination of Endothall in Drinking Water by 
Ion-Exchange Extraction, Acidic Methanol Methylation and Gas 
Chromatography/Mass Spectrometry. Table IG, Note 3.

[[Page 56]]

    (L) Method 553, Determination of Benzidines and Nitrogen-Containing 
Pesticides in Water by Liquid-Liquid Extraction or Liquid-Solid 
Extraction and Reverse Phase High Performance Liquid Chromatography/
Particle Beam/Mass Spectrometry Table ID, Note 10; Table IG, Note 3.
    (M) Method 555, Determination of Chlorinated Acids in Water by High 
Performance Liquid Chromatography With a Photodiode Array Ultraviolet 
Detector. Table IG, Note 3.
    (vi) In the compendium Methods for the Determination of Organic 
Compounds in Drinking Water. Revised July 1991, December 1998. EPA-600/
4-88-039, Pub. No. PB92-207703. Table IF.
    (A) EPA Method 502.2, Volatile Organic Compounds in Water by Purge 
and Trap Capillary Column Gas Chromatography with Photoionization and 
Electrolytic Conductivity Detectors in Series. Table IF.
    (B) [Reserved]
    (vii) In the compendium Methods for the Determination of Organic 
Compounds in Drinking Water-Supplement II. August 1992. EPA-600/R-92-
129, Pub. No. PB92-207703. Table IF.
    (A) EPA Method 524.2, Measurement of Purgeable Organic Compounds in 
Water by Capillary Column Gas Chromatography/Mass Spectrometry. Table 
IF.
    (B) [Reserved]
    (viii) Methods for Measuring the Acute Toxicity of Effluents and 
Receiving Waters to Freshwater and Marine Organisms, Fifth Edition. 
October 2002. EPA 821-R-02-012, Pub. No. PB2002-108488. Table IA, Note 
26.
    (ix) Short-Term Methods for Measuring the Chronic Toxicity of 
Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition. 
October 2002. EPA 821-R-02-013, Pub. No. PB2002-108489. Table IA, Note 
27.
    (x) Short-Term Methods for Measuring the Chronic Toxicity of 
Effluents and Receiving Waters to Marine and Estuarine Organisms, Third 
Edition. October 2002. EPA 821-R-02-014, Pub. No. PB2002-108490. Table 
IA, Note 28.
    (8) Office of Water, U.S. Environmental Protection Agency, 
Washington DC (US EPA). Available at http://water.epa.gov/scitech/
methods/cwa/index.cfm.
    (i) Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence 
Spectrometry. Revision 2.0, February 2005. EPA-821-R-05-001. Table IB, 
Note 17.
    (ii) Method 1103.1: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). 
March 2010. EPA-621-R-10-002. Table IH, Note 19.
    (iii) Method 1106.1: Enterococci in Water by Membrane Filtration 
Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). December 2009. 
EPA-621-R-09-015. Table IH, Note 23.
    (iv) Method 1600: Enterococci in Water by Membrane Filtration Using 
membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). September 
2014. EPA-821-R-14-011. Table IA, Note 25; Table IH, Note 24.
    (v) Method 1603: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar 
(Modified mTEC). September 2014. EPA-821-R-14-010. Table IA, Note 22; 
Table IH, Note 20.
    (vi) Method 1604: Total Coliforms and Escherichia coli (E. coli) in 
Water by Membrane Filtration Using a Simultaneous Detection Technique 
(MI Medium). September 2002. EPA-821-R-02-024. Table IH, Note 21.
    (vii) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. 
December 2005. EPA-821-R-05-001. Table IH, Note 25.
    (viii) Method 1623: Cryptosporidium and Giardia in Water by 
Filtration/IMS/FA. December 2005. EPA-821-R-05-002. Table IH, Note 26.
    (ix) Method 1627, Kinetic Test Method for the Prediction of Mine 
Drainage Quality. December 2011. EPA-821-R-09-002. Table IB, Note 69.
    (x) Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) 
and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar 
Material) by Extraction and Gravimetry. Revision A, February 1999. EPA-
821-R-98-002. Table IB, Notes 38 and 42.
    (xi) Method 1664, n-Hexane Extractable Material (HEM; Oil and 
Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; 
Non-polar Material) by Extraction and Gravimetry. Revision B, February 
2010.

[[Page 57]]

EPA-821-R-10-001. Table IB, Notes 38 and 42.
    (xii) Method 1669, Sampling Ambient Water for Trace Metals at EPA 
Water Quality Criteria Levels. July 1996. Table IB, Note 43.
    (xiii) Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by 
Multiple-Tube Fermentation using Lauryl Tryptose Broth (LTB) and EC 
Medium. September 2014. EPA-821-R-14-009. Table IA, Note 15.
    (xiv) Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by 
Multiple-Tube Fermentation using A-1 Medium. July 2006. EPA 821-R-06-
013. Table IA, Note 20.
    (xv) Method 1682: Salmonella in Sewage Sludge (Biosolids) by 
Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. September 2014. 
EPA 821-R-14-012. Table IA, Note 23.
    (9) American National Standards Institute, 1430 Broadway, New York 
NY 10018.
    (i) ANSI. American National Standard on Photographic Processing 
Effluents. April 2, 1975. Table IB, Note 9.
    (ii) [Reserved]
    (10) American Public Health Association, 1015 15th Street NW., 
Washington, DC 20005. Standard Methods Online is available through the 
Standard Methods Web site (http://www.standardmethods.org).
    (i) Standard Methods for the Examination of Water and Wastewater. 
14th Edition, 1975. Table IB, Notes 17 and 27.
    (ii) Standard Methods for the Examination of Water and Wastewater. 
15th Edition, 1980, Table IB, Note 30; Table ID.
    (iii) Selected Analytical Methods Approved and Cited by the United 
States Environmental Protection Agency, Supplement to the 15th Edition 
of Standard Methods for the Examination of Water and Wastewater. 1981. 
Table IC, Note 6; Table ID, Note 6.
    (iv) Standard Methods for the Examination of Water and Wastewater. 
18th Edition, 1992. Tables IA, IB, IC, ID, IE, and IH.
    (v) Standard Methods for the Examination of Water and Wastewater. 
19th Edition, 1995. Tables IA, IB, IC, ID, IE, and IH.
    (vi) Standard Methods for the Examination of Water and Wastewater. 
20th Edition, 1998. Tables IA, IB, IC, ID, IE, and IH.
    (vii) Standard Methods for the Examination of Water and Wastewater. 
21st Edition, 2005. Table IB, Notes 17 and 27.
    (viii) 2120, Color. 2011. Table IB.
    (ix) 2130, Turbidity. 2011. Table IB.
    (x) 2310, Acidity. 2011. Table IB.
    (xi) 2320, Alkalinity. 2011. Table IB.
    (xii) 2340, Hardness. 2011. Table IB.
    (xiii) 2510, Conductivity. 2011. Table IB.
    (xiv) 2540, Solids. 2011. Table IB.
    (xv) 2550, Temperature. 2010. Table IB.
    (xvi) 3111, Metals by Flame Atomic Absorption Spectrometry. 2011. 
Table IB.
    (xvii) 3112, Metals by Cold-Vapor Atomic Absorption Spectrometry. 
2011. Table IB.
    (xviii) 3113, Metals by Electrothermal Atomic Absorption 
Spectrometry. 2010. Table IB.
    (xix) 3114, Arsenic and Selenium by Hydride Generation/Atomic 
Absorption Spectrometry. 2011. Table IB.
    (xx) 3120, Metals by Plasma Emission Spectroscopy. 2011. Table IB.
    (xxi) 3125, Metals by Inductively Coupled Plasma-Mass Spectrometry. 
2011. Table IB.
    (xxii) 3500-Al, Aluminum. 2011. Table IB.
    (xxiii) 3500-As, Arsenic. 2011. Table IB.
    (xxiv) 3500-Ca, Calcium. 2011. Table IB.
    (xxv) 3500-Cr, Chromium. 2011. Table IB.
    (xxvi) 3500-Cu, Copper. 2011. Table IB.
    (xxvii) 3500-Fe, Iron. 2011. Table IB.
    (xxviii) 3500-Pb, Lead. 2011. Table IB.
    (xxix) 3500-Mn, Manganese. 2011. Table IB.
    (xxx) 3500-K, Potassium. 2011. Table IB.
    (xxxi) 3500-Na, Sodium. 2011. Table IB.
    (xxxii) 3500-V, Vanadium. 2011. Table IB.
    (xxxiii) 3500-Zn, Zinc. 2011. Table IB.
    (xxxiv) 4110, Determination of Anions by Ion Chromatography. 2011. 
Table IB.
    (xxxv) 4140, Inorganic Anions by Capillary Ion Electrophoresis. 
2011. Table IB.

[[Page 58]]

    (xxxvi) 4500-B, Boron. 2011. Table IB.
    (xxxvii) 4500-Cl-, Chloride. 2011. Table IB.
    (xxxviii) 4500-Cl, Chlorine (Residual). 2011. Table IB.
    (xxxix) 4500-CN-, Cyanide. 2011. Table IB.
    (xl) 4500-F-, Fluoride. 2011. Table IB.
    (xli) 4500-H\+\, pH Value. 2011. Table IB.
    (xlii) 4500-NH3, Nitrogen (Ammonia). 2011. Table IB.
    (xliii) 4500-NO2-, Nitrogen (Nitrite). 2011. 
Table IB.
    (xliv) 4500-NO3-, Nitrogen (Nitrate). 2011. 
Table IB.
    (xlv) 4500-Norg, Nitrogen (Organic). 2011. Table IB.
    (xlvi) 4500-O, Oxygen (Dissolved). 2011. Table IB.
    (xlvii) 4500-P, Phosphorus. 2011. Table IB.
    (xlviii) 4500-SiO2, Silica. 2011. Table IB.
    (xlix) 4500-S2-, Sulfide. 2011. Table IB.
    (l) 4500-SO32-, Sulfite. 2011. Table IB.
    (li) 4500-SO42-, Sulfate. 2011. Table IB.
    (lii) 5210, Biochemical Oxygen Demand (BOD). 2011. Table IB.
    (liii) 5220, Chemical Oxygen Demand (COD). 2011. Table IB.
    (liv) 5310, Total Organic Carbon (TOC). 2011. Table IB.
    (lv) 5520, Oil and Grease. 2011. Table IB.
    (lvi) 5530, Phenols. 2010. Table IB.
    (lvii) 5540, Surfactants. 2011. Table IB.
    (lviii) 6200, Volatile Organic Compounds. 2011. Table IC.
    (lix) 6410, Extractable Base/Neutrals and Acids. 2000. Tables IC, 
ID.
    (lx) 6420, Phenols. 2000. Table IC.
    (lxi) 6440, Polynuclear Aromatic Hydrocarbons. 2005. Table IC.
    (lxii) 6630, Organochlorine Pesticides. 2007. Table ID.
    (lxiii) 6640, Acidic Herbicide Compounds. 2006. Table ID.
    (lxiv) 7110, Gross Alpha and Gross Beta Radioactivity (Total, 
Suspended, and Dissolved). 2000. Table IE.
    (lxv) 7500, Radium. 2001. Table IE.
    (lxvi) 9213, Recreational Waters. 2007. Table IH.
    (lxvii) 9221, Multiple-Tube Fermentation Technique for Members of 
the Coliform Group. 2006. Table IA, Notes 12 and 14; Table IH, Notes 11 
and 13.
    (lxviii) 9222, Membrane Filter Technique for Members of the Coliform 
Group. 2006. Table IA; Table IH, Note 18.
    (lxix) 9223, Enzyme Substrate Coliform Test. 2004. Table IA; Table 
IH.
    (lxx) 9230, Fecal Enterococcus/Streptococcus Groups. 2007. Table IA; 
Table IH.
    (11) The Analyst, The Royal Society of Chemistry, RSC Publishing, 
Royal Society of Chemistry, Thomas Graham House, Science Park, Milton 
Road, Cambridge CB4 0WF, United Kingdom. (Also available from most 
public libraries.)
    (i) Spectrophotometric Determination of Ammonia: A Study of a 
Modified Berthelot Reaction Using Salicylate and Dichloroisocyanurate. 
Krom, M.D. 105:305-316, April 1980. Table IB, Note 60.
    (ii) [Reserved]
    (12) Analytical Chemistry, ACS Publications, 1155 Sixteenth St. NW., 
Washington DC 20036. (Also available from most public libraries.)
    (i) Spectrophotometric and Kinetics Investigation of the Berthelot 
Reaction for the Determination of Ammonia. Patton, C.J. and S.R. Crouch. 
49(3):464-469, March 1977. Table IB, Note 60.
    (ii) [Reserved]
    (13) AOAC International, 481 North Frederick Avenue, Suite 500, 
Gaithersburg, MD 20877-2417.
    (i) Official Methods of Analysis of AOAC International. 16th 
Edition, 4th Revision, 1998.
    (A) 920.203, Manganese in Water, Persulfate Method. Table IB, Note 
3.
    (B) 925.54, Sulfate in Water, Gravimetric Method. Table IB, Note 3.
    (C) 973.40, Specific Conductance of Water. Table IB, Note 3.
    (D) 973.41, pH of Water. Table IB, Note 3.
    (E) 973.43, Alkalinity of Water, Titrimetric Method. Table IB, Note 
3.
    (F) 973.44, Biochemical Oxygen Demand (BOD) of Water, Incubation 
Method. Table IB, Note 3.
    (G) 973.45, Oxygen (Dissolved) in Water, Titrimetric Methods. Table 
IB, Note 3.
    (H) 973.46, Chemical Oxygen Demand (COD) of Water, Titrimetric 
Methods. Table IB, Note 3.

[[Page 59]]

    (I) 973.47, Organic Carbon in Water, Infrared Analyzer Method. Table 
IB, Note 3.
    (J) 973.48, Nitrogen (Total) in Water, Kjeldahl Method. Table IB, 
Note 3.
    (K) 973.49, Nitrogen (Ammonia) in Water, Colorimetric Method. Table 
IB, Note 3.
    (L) 973.50, Nitrogen (Nitrate) in Water, Brucine Colorimetric 
Method. Table IB, Note 3.
    (M) 973.51, Chloride in Water, Mercuric Nitrate Method. Table IB, 
Note 3.
    (N) 973.52, Hardness of Water. Table IB, Note 3.
    (O) 973.53, Potassium in Water, Atomic Absorption Spectrophotometric 
Method. Table IB, Note 3.
    (P) 973.54, Sodium in Water, Atomic Absorption Spectrophotometric 
Method. Table IB, Note 3.
    (Q) 973.55, Phosphorus in Water, Photometric Method. Table IB, Note 
3.
    (R) 973.56, Phosphorus in Water, Automated Method. Table IB, Note 3.
    (S) 974.27, Cadmium, Chromium, Copper, Iron, Lead, Magnesium, 
Manganese, Silver, Zinc in Water, Atomic Absorption Spectrophotometric 
Method. Table IB, Note 3.
    (T) 977.22, Mercury in Water, Flameless Atomic Absorption 
Spectrophotometric Method. Table IB, Note 3.
    (U) 991.15. Total Coliforms and Escherichia coli in Water Defined 
Substrate Technology (Colilert) Method. Table IA, Note 10; Table IH, 
Note 10.
    (V) 993.14, Trace Elements in Waters and Wastewaters, Inductively 
Coupled Plasma-Mass Spectrometric Method. Table IB, Note 3.
    (W) 993.23, Dissolved Hexavalent Chromium in Drinking Water, Ground 
Water, and Industrial Wastewater Effluents, Ion Chromatographic Method. 
Table IB, Note 3.
    (X) 993.30, Inorganic Anions in Water, Ion Chromatographic Method. 
Table IB, Note 3.
    (ii) [Reserved]
    (14) Applied and Environmental Microbiology, American Society for 
Microbiology, 1752 N Street NW., Washington DC 20036. (Also available 
from most public libraries.)
    (i) New Medium for the Simultaneous Detection of Total Coliforms and 
Escherichia coli in Water. Brenner, K.P., C.C. Rankin, Y.R. Roybal, G.N. 
Stelma, Jr., P.V. Scarpino, and A.P. Dufour. 59:3534-3544, November 
1993. Table IH, Note 21.
    (ii) [Reserved]
    (15) ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West 
Conshohocken, PA 19428-2959, or online at http://www.astm.org.
    (i) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1994. Tables IA, IB, 
IC, ID, IE, and IH.
    (ii) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1996. Tables IA, IB, 
IC, ID, IE, and IH.
    (iii) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1999. Tables IA, IB, 
IC, ID, IE, and IH.
    (iv) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 2000. Tables IA, IB, 
IC, ID, IE, and IH.
    (v) ASTM D511-09, Standard Test Methods for Calcium and Magnesium in 
Water. May 2009. Table IB.
    (vi) ASTM D512-04, Standard Test Methods for Chloride Ion in Water. 
July 2004. Table IB.
    (vii) ASTM D515-88, Test Methods for Phosphorus in Water, March 
1989. Table IB.
    (viii) ASTM D516-11, Standard Test Method for Sulfate Ion in Water, 
September 2011. Table IB.
    (ix) ASTM D858-12, Standard Test Methods for Manganese in Water. 
September 2012. Table IB.
    (x) ASTM D859-10, Standard Test Method for Silica in Water. July 
2010. Table IB.
    (xi) ASTM D888-09, Standard Test Methods for Dissolved Oxygen in 
Water. December 2009. Table IB.
    (xii) ASTM D1067-11, Standard Test Methods for Acidity or Alkalinity 
of Water. April 2011. Table IB.
    (xiii) ASTM D1068-10, Standard Test Methods for Iron in Water. 
October 2010. Table IB.
    (xiv) ASTM D1125-95 (Reapproved 1999), Standard Test Methods for 
Electrical Conductivity and Resistivity of Water. December 1995. Table 
IB.

[[Page 60]]

    (xv) ASTM D1126-12, Standard Test Method for Hardness in Water. 
March 2012. Table IB.
    (xvi) ASTM D1179-10, Standard Test Methods for Fluoride Ion in 
Water. July 2010. Table IB.
    (xvii) ASTM D1246-10, Standard Test Method for Bromide Ion in Water. 
July 2010. Table IB.
    (xviii) ASTM D1252-06, Standard Test Methods for Chemical Oxygen 
Demand (Dichromate Oxygen Demand) of Water. February 2006. Table IB.
    (xix) ASTM D1253-08, Standard Test Method for Residual Chlorine in 
Water. October 2008. Table IB.
    (xx) ASTM D1293-99, Standard Test Methods for pH of Water. March 
2000. Table IB.
    (xxi) ASTM D1426-08, Standard Test Methods for Ammonia Nitrogen in 
Water. September 2008. Table IB.
    (xxii) ASTM D1687-12 (Approved September 1, 2012), Standard Test 
Methods for Chromium in Water. August 2007. Table IB.
    (xxiii) ASTM D1688-12, Standard Test Methods for Copper in Water. 
September 2012. Table IB.
    (xxiv) ASTM D1691-12, Standard Test Methods for Zinc in Water. 
September 2012. Table IB.
    (xxv) ASTM D1783-01 (Reapproved 2007), Standard Test Methods for 
Phenolic Compounds in Water. January 2008). Table IB.
    (xxvi) ASTM D1886-08, Standard Test Methods for Nickel in Water. 
October 2008. Table IB.
    (xxvii) ASTM D1889-00, Standard Test Method for Turbidity of Water. 
October 2000. Table IB.
    (xxviii) ASTM D1890-96, Standard Test Method for Beta Particle 
Radioactivity of Water. April 1996. Table IE.
    (xxix) ASTM D1943-96, Standard Test Method for Alpha Particle 
Radioactivity of Water. April 1996. Table IE.
    (xxx) ASTM D1976-12, Standard Test Method for Elements in Water by 
Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy. March 
2012. Table IB.
    (xxxi) ASTM D2036-09, Standard Test Methods for Cyanides in Water. 
October 2009. Table IB.
    (xxxii) ASTM D2330-02, Standard Test Method for Methylene Blue 
Active Substances. August 2002. Table IB.
    (xxxiii) ASTM D2460-97, Standard Test Method for Alpha-Particle-
Emitting Isotopes of Radium in Water. October 1997. Table IE.
    (xxxiv) ASTM D2972-08, Standard Tests Method for Arsenic in Water. 
October 2008. Table IB.
    (xxxv) ASTM D3223-12, Standard Test Method for Total Mercury in 
Water. September 2012. Table IB.
    (xxxvi) ASTM D3371-95, Standard Test Method for Nitriles in Aqueous 
Solution by Gas-Liquid Chromatography, February 1996. Table IF.
    (xxxvii) ASTM D3373-12, Standard Test Method for Vanadium in Water. 
September 2012. Table IB.
    (xxxviii) ASTM D3454-97, Standard Test Method for Radium-226 in 
Water. February 1998. Table IE.
    (xxxix) ASTM D3557-12, Standard Test Method for Cadmium in Water. 
September 2012. Table IB.
    (xl) ASTM D3558-08, Standard Test Method for Cobalt in Water. 
November 2008. Table IB.
    (xli) ASTM D3559-08, Standard Test Methods for Lead in Water. 
October 2008. Table IB.
    (xlii) ASTM D3590-11, Standard Test Methods for Total Kjeldahl 
Nitrogen in Water. April 2011. Table IB.
    (xliii) ASTM D3645-08, Standard Test Methods for Beryllium in Water. 
October 2008. Table IB.
    (xliv) ASTM D3695-95, Standard Test Method for Volatile Alcohols in 
Water by Direct Aqueous-Injection Gas Chromatography. April 1995. Table 
IF.
    (xlv) ASTM D3859-08, Standard Test Methods for Selenium in Water. 
October 2008. Table IB.
    (xlvi) ASTM D3867-04, Standard Test Method for Nitrite-Nitrate in 
Water. July 2004. Table IB.
    (xlvii) ASTM D4190-08, Standard Test Method for Elements in Water by 
Direct-Current Plasma Atomic Emission Spectroscopy. October 2008. Table 
IB.
    (xlviii) ASTM D4282-02, Standard Test Method for Determination of 
Free Cyanide in Water and Wastewater by Microdiffusion. August 2002. 
Table IB.
    (xlix) ASTM D4327-03, Standard Test Method for Anions in Water by 
Chemically Suppressed Ion Chromatography. January 2003. Table IB.
    (l) ASTM D4382-12, Standard Test Method for Barium in Water, Atomic

[[Page 61]]

Absorption Spectrophotometry, Graphite Furnace. September 2012. Table 
IB.
    (li) ASTM D4657-92 (Reapproved 1998), Standard Test Method for 
Polynuclear Aromatic Hydrocarbons in Water. January 1993. Table IC.
    (lii) ASTM D4658-09, Standard Test Method for Sulfide Ion in Water. 
May 2009. Table IB.
    (liii) ASTM D4763-88 (Reapproved 2001), Standard Practice for 
Identification of Chemicals in Water by Fluorescence Spectroscopy. 
September 1988. Table IF.
    (liv) ASTM D4839-03, Standard Test Method for Total Carbon and 
Organic Carbon in Water by Ultraviolet, or Persulfate Oxidation, or 
Both, and Infrared Detection. January 2003. Table IB.
    (lv) ASTM D5257-11, Standard Test Method for Dissolved Hexavalent 
Chromium in Water by Ion Chromatography. April 2011. Table IB.
    (lvi) ASTM D5259-92, Standard Test Method for Isolation and 
Enumeration of Enterococci from Water by the Membrane Filter Procedure. 
October 1992. Table IH, Note 9.
    (lvii) ASTM D5392-93, Standard Test Method for Isolation and 
Enumeration of Escherichia coli in Water by the Two-Step Membrane Filter 
Procedure. September 1993. Table IH, Note 9.
    (lviii) ASTM D5673-10, Standard Test Method for Elements in Water by 
Inductively Coupled Plasma--Mass Spectrometry. September 2010. Table IB.
    (lix) ASTM D5(19)907-13, Standard Test Method for Filterable Matter 
(Total Dissolved Solids) and Nonfilterable Matter (Total Suspended 
Solids) in Water. July 2013. Table IB.
    (lx) ASTM D6503-99, Standard Test Method for Enterococci in Water 
Using Enterolert. April 2000. Table IA Note 9, Table IH, Note 9.
    (lxi) ASTM. D6508-10, Standard Test Method for Determination of 
Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion 
Electrophoresis and Chromate Electrolyte. October 2010. Table IB, Note 
54.
    (lxii) ASTM. D6888-09, Standard Test Method for Available Cyanide 
with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas 
Diffusion Separation and Amperometric Detection. October 2009. Table IB, 
Note 59.
    (lxiii) ASTM. D6919-09, Standard Test Method for Determination of 
Dissolved Alkali and Alkaline Earth Cations and Ammonium in Water and 
Wastewater by Ion Chromatography. May 2009. Table IB.
    (lxiv) ASTM. D7065-11, Standard Test Method for Determination of 
Nonylphenol, Bisphenol A, p-tert-Octylphenol, Nonylphenol Monoethoxylate 
and Nonylphenol Diethoxylate in Environmental Waters by Gas 
Chromatography Mass Spectrometry. July 2011. Table IB.
    (lxv) ASTM. D7237-10, Standard Test Method for Free Cyanide with 
Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and 
Amperometric Detection. June 2010. Table IB.
    (lxvi) ASTM. D7284-13, Standard Test Method for Total Cyanide in 
Water by Micro Distillation followed by Flow Injection Analysis with Gas 
Diffusion Separation and Amperometric Detection. July 2013. Table IB.
    (lxvii) ASTM. D7365-09a, Standard Practice for Sampling, 
Preservation, and Mitigating Interferences in Water Samples for Analysis 
of Cyanide. October 2009. Table II, Notes 5 and 6.
    (lxviii) ASTM. D7511-12, Standard Test Method for Total Cyanide by 
Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and 
Amperometric Detection. January 2012. Table IB.
    (lxix) ASTM. D7573-09, Standard Test Method for Total Carbon and 
Organic Carbon in Water by High Temperature Catalytic Combustion and 
Infrared Detection. November 2009. Table IB.
    (16) Bran & Luebbe Analyzing Technologies, Inc., Elmsford NY 10523.
    (i) Industrial Method Number 378-75WA, Hydrogen Ion (pH) Automated 
Electrode Method, Bran & Luebbe (Technicon) Auto Analyzer II. October 
1976. Table IB, Note 21.
    (ii) [Reserved]
    (17) CEM Corporation, P.O. Box 200, Matthews NC 28106-0200.
    (i) Closed Vessel Microwave Digestion of Wastewater Samples for 
Determination of Metals. April 16, 1992. Table IB, Note 36.
    (ii) [Reserved]
    (18) Craig R. Chinchilla, 900 Jorie Blvd., Suite 35, Oak Brook IL 
60523. Telephone: 630-645-0600.

[[Page 62]]

    (i) Nitrate by Discrete Analysis Easy (1-Reagent) Nitrate Method, 
(Colorimetric, Automated, 1 Reagent). Revision 1, November 12, 2011. 
Table IB, Note 62.
    (ii) [Reserved]
    (19) Hach Company, P.O. Box 389, Loveland CO 80537.
    (i) Method 8000, Chemical Oxygen Demand. Hach Handbook of Water 
Analysis. 1979. Table IB, Note 14.
    (ii) Method 8008, 1,10-Phenanthroline Method using FerroVer Iron 
Reagent for Water. 1980. Table IB, Note 22.
    (iii) Method 8009, Zincon Method for Zinc. Hach Handbook for Water 
Analysis. 1979. Table IB, Note 33.
    (iv) Method 8034, Periodate Oxidation Method for Manganese. Hach 
Handbook for Water Analysis. 1979. Table IB, Note 23.
    (v) Method 8506, Bicinchoninate Method for Copper. Hach Handbook of 
Water Analysis. 1979. Table IB, Note 19.
    (vi) Method 8507, Nitrogen, Nitrite--Low Range, Diazotization Method 
for Water and Wastewater. 1979. Table IB, Note 25.
    (vii) Method 10206, Hach Company TNTplus 835/836 Nitrate Method 
10206, Spectrophotometric Measurement of Nitrate in Water and 
Wastewater. Revision 2.1, January 10, 2013. Table IB, Note 75.
    (viii) Method 10242, Hach Company TNTplus 880 Total Kjeldahl 
Nitrogen Method 10242, Simplified Spectrophotometric Measurement of 
Total Kjeldahl Nitrogen in Water and Wastewater. Revision 1.1, January 
10, 2013. Table IB, Note 76.
    (ix) Hach Method 10360, Luminescence Measurement of Dissolved Oxygen 
in Water and Wastewater and for Use in the Determination of 
BOD5 and cBOD5. Revision 1.2, October 2011. Table 
IB, Note 63.
    (x) m-ColiBlue24[supreg] Method, for total Coliforms and E. coli. 
Revision 2, 1999. Table IA, Note 18; Table IH, Note 17.
    (20) IDEXX Laboratories Inc., One Idexx Drive, Westbrook ME 04092.
    (i) Colilert. 2013. Table IA, Notes 17 and 18; Table IH, Notes 14, 
15 and 16.
    (ii) Colilert-18. 2013. Table IA, Notes 17 and 18; Table IH, Notes 
14, 15 and 16.
    (iii) Enterolert. 2013. Table IA, Note 24; Table IH, Note 12.
    (iv) Quanti-Tray Insert and Most Probable Number (MPN) Table. 2013. 
Table IA, Note 18; Table IH, Notes 14 and 16.
    (21) In-Situ Incorporated, 221 E. Lincoln Ave., Ft. Collins CO 
80524. Telephone: 970-498-1500.
    (i) In-Situ Inc. Method 1002-8-2009, Dissolved Oxygen Measurement by 
Optical Probe. 2009. Table IB, Note 64.
    (ii) In-Situ Inc. Method 1003-8-2009, Biochemical Oxygen Demand 
(BOD) Measurement by Optical Probe. 2009. Table IB, Note 10.
    (iii) In-Situ Inc. Method 1004-8-2009, Carbonaceous Biochemical 
Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. Table IB, Note 
35.
    (22) Journal of Chromatography, Elsevier/North-Holland, Inc., 
Journal Information Centre, 52 Vanderbilt Avenue, New York NY 10164. 
(Also available from most public libraries.
    (i) Direct Determination of Elemental Phosphorus by Gas-Liquid 
Chromatography. Addison, R.F. and R.G. Ackman. 47(3): 421-426, 1970. 
Table IB, Note 28.
    (ii) [Reserved]
    (23) Lachat Instruments, 6645 W. Mill Road, Milwaukee WI 53218, 
Telephone: 414-358-4200.
    (i) QuikChem Method 10-204-00-1-X, Digestion and Distillation of 
Total Cyanide in Drinking and Wastewaters using MICRO DIST and 
Determination of Cyanide by Flow Injection Analysis. Revision 2.2, March 
2005. Table IB, Note 56.
    (ii) [Reserved]
    (24) Leck Mitchell, Ph.D., P.E., 656 Independence Valley Dr., Grand 
Junction CO 81507. Telephone: 970-244-8661.
    (i) Mitchell Method M5271, Determination of Turbidity by 
Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 66.
    (ii) Mitchell Method M5331, Determination of Turbidity by 
Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 65.
    (25) National Council of the Paper Industry for Air and Stream 
Improvements, Inc. (NCASI), 260 Madison Avenue, New York NY 10016.
    (i) NCASI Method TNTP-W10900, Total Nitrogen and Total Phophorus in 
Pulp and Paper Biologically Treated

[[Page 63]]

Effluent by Alkaline Persulfate Digestion. June 2011. Table IB, Note 77.
    (ii) NCASI Technical Bulletin No. 253, An Investigation of Improved 
Procedures for Measurement of Mill Effluent and Receiving Water Color. 
December 1971. Table IB, Note 18.
    (iii) NCASI Technical Bulletin No. 803, An Update of Procedures for 
the Measurement of Color in Pulp Mill Wastewaters. May 2000. Table IB, 
Note 18.
    (26) The Nitrate Elimination Co., Inc. (NECi), 334 Hecla St., Lake 
Linden NI 49945.
    (i) NECi Method N07-0003, Method for Nitrate Reductase Nitrate-
Nitrogen Analysis. Revision 9.0. March 2014. Table IB, Note 73.
    (ii) [Reserved]
    (27) Oceanography International Corporation, 512 West Loop, P.O. Box 
2980, College Station TX 77840.
    (i) OIC Chemical Oxygen Demand Method. 1978. Table IB, Note 13.
    (ii) [Reserved]
    (28) OI Analytical, Box 9010, College Station TX 77820-9010.
    (i) Method OIA-1677-09, Available Cyanide by Ligand Exchange and 
Flow Injection Analysis (FIA). Copyright 2010. Table IB, Note 59.
    (ii) Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, 
Steam Distillation, Titrimetric Detection. Revised December 22, 1994. 
Table IB, Note 39.
    (iii) Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, 
Steam Distillation, Colorimetric Detection. Revised December 22, 1994. 
Table IB, Note 40.
    (iv) Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, 
Automated FIA Gas Diffusion. Revised December 22, 1994. Table IB, Note 
41.
    (29) ORION Research Corporation, 840 Memorial Drive, Cambridge, 
Massachusetts 02138.
    (i) ORION Research Instruction Manual, Residual Chlorine Electrode 
Model 97-70. 1977. Table IB, Note 16.
    (ii) [Reserved]
    (30) Technicon Industrial Systems, Tarrytown NY 10591.
    (i) Industrial Method Number 379-75WE Ammonia, Automated Electrode 
Method, Technicon Auto Analyzer II. February 19, 1976. Table IB, Note 7.
    (ii) [Reserved]
    (31) Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin MA 
02038.
    (i) Method AES0029. Direct Current Plasma (DCP) Optical Emission 
Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 
1986, Revised 1991. Table IB, Note 34.
    (ii) [Reserved]
    (32) Thermo Scientific, 166 Cummings Center, Beverly MA 01915. 
Telephone: 1-800-225-1480. www.thermoscientific.com.
    (i) Thermo Scientific Orion Method AQ4500, Determination of 
Turbidity by Nephelometry. Revision 5, March 12, 2009. Table IB, Note 
67.
    (ii) [Reserved]
    (33) 3M Corporation, 3M Center Building 220-9E-10, St. Paul MN 
55144-1000.
    (i) Organochlorine Pesticides and PCBs in Wastewater Using Empore 
\TM\ Disk'' Test Method 3M 0222. Revised October 28, 1994. Table IC, 
Note 8; Table ID, Note 8.
    (ii) [Reserved]
    (34) Timberline Instruments, LLC, 1880 South Flatiron Ct., Unit I, 
Boulder CO 80301.
    (i) Timberline Amonia-001, Determination of Inorganic Ammonia by 
Continuous Flow Gas Diffusion and Conductivity Cell Analysis. June 24, 
2011. Table IB, Note 74.
    (ii) [Reserved]
    (35) U.S. Geological Survey (USGS), U.S. Department of the Interior, 
Reston, Virginia. Available from USGS Books and Open-File Reports (OFR) 
Section, Federal Center, Box 25425, Denver, CO 80225.
    (i) Colorimetric determination of nitrate plus nitrite in water by 
enzymatic reduction, automated discrete analyzer methods. U.S. 
Geological Survey Techniques and Methods, Book 5--Laboratory Analysis, 
Section B--Methods of the National Water Quality Laboratory, Chapter 8. 
2011. Table IB, Note 72.
    (ii) Methods for Determination of Inorganic Substances in Water and 
Fluvial Sediments, editors, Techniques of Water-Resources Investigations 
of the U.S. Geological Survey, Book 5, Chapter A1. 1979. Table IB, Note 
8.
    (iii) Methods for Determination of Inorganic Substances in Water and 
Fluvial Sediments, Techniques of Water-Resources Investigations of the 
U.S.

[[Page 64]]

Geological Survey, Book 5, Chapter A1. 1989. Table IB, Note 2.
    (iv) Methods for the Determination of Organic Substances in Water 
and Fluvial Sediments. Techniques of Water-Resources Investigations of 
the U.S. Geological Survey, Book 5, Chapter A3. 1987. Table IB, Note 24; 
Table ID, Note 4.
    (v) OFR 76-177, Selected Methods of the U.S. Geological Survey of 
Analysis of Wastewaters. 1976. Table IE, Note 2.
    (vi) OFR 91-519, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Organonitrogen 
Herbicides in Water by Solid-Phase Extraction and Capillary-Column Gas 
Chromatography/Mass Spectrometry With Selected-Ion Monitoring. 1992. 
Table ID, Note 14.
    (vii) OFR 92-146, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Total Phosphorus by 
a Kjeldahl Digestion Method and an Automated Colorimetric Finish That 
Includes Dialysis. 1992. Table IB, Note 48.
    (viii) OFR 93-125, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Inorganic and 
Organic Constituents in Water and Fluvial Sediments. 1993. Table IB, 
Note 51; Table IC, Note 9.
    (ix) OFR 93-449, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Chromium in Water by 
Graphite Furnace Atomic Absorption Spectrophotometry. 1993. Table IB, 
Note 46.
    (x) OFR 94-37, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Triazine and Other 
Nitrogen-containing Compounds by Gas Chromatography With Nitrogen 
Phosphorus Detectors. 1994. Table ID, Note 9.
    (xi) OFR 95-181, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Pesticides in Water 
by C-18 Solid-Phase Extraction and Capillary-Column Gas Chromatography/
Mass Spectrometry With Selected-Ion Monitoring. 1995. Table ID, Note 11.
    (xii) OFR 97-198, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Molybdenum in Water 
by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. Table IB, 
Note 47.
    (xiii) OFR 98-165, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Elements in Whole-
Water Digests Using Inductively Coupled Plasma-Optical Emission 
Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. 
Table IB, Note 50.
    (xiv) OFR 98-639, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Arsenic and Selenium 
in Water and Sediment by Graphite Furnace--Atomic Absorption 
Spectrometry. 1999. Table IB, Note 49.
    (xv) OFR 00-170, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Ammonium Plus 
Organic Nitrogen by a Kjeldahl Digestion Method and an Automated 
Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. 
Table IB, Note 45.
    (xvi) Techniques and Methods Book 5-B1, Determination of Elements in 
Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction 
Cell Inductively Coupled Plasma-Mass Spectrometry. Chapter 1, Section B, 
Methods of the National Water Quality Laboratory, Book 5, Laboratory 
Analysis. 2006. Table IB, Note 70.
    (xvii) U.S. Geological Survey Techniques of Water-Resources 
Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for 
Collection and Analysis of Aquatic Biological and Microbiological 
Samples. 1989. Table IA, Note 4; Table IH, Note 4.
    (xviii) Water-Resources Investigation Report 01-4098, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Moderate-Use Pesticides and Selected 
Degradates in Water by C-18 Solid-Phase Extraction and Gas 
Chromatography/Mass Spectrometry. 2001. Table ID, Note 13.
    (xix) Water-Resources Investigations Report 01-4132, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Organic Plus Inorganic Mercury

[[Page 65]]

in Filtered and Unfiltered Natural Water With Cold Vapor-Atomic 
Fluorescence Spectrometry. 2001. Table IB, Note 71.
    (xx) Water-Resources Investigation Report 01-4134, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Pesticides in Water by Graphitized Carbon-
Based Solid-Phase Extraction and High-Performance Liquid Chormatography/
Mass Spectrometry. 2001. Table ID, Note 12.
    (xxi) Water Temperature--Influential Factors, Field Measurement and 
Data Presentation, Techniques of Water-Resources Investigations of the 
U.S. Geological Survey, Book 1, Chapter D1. 1975. Table IB, Note 32.
    (36) Waters Corporation, 34 Maple Street, Milford MA 01757, 
Telephone: 508-482-2131, Fax: 508-482-3625.
    (i) Method D6508, Test Method for Determination of Dissolved 
Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis 
and Chromate Electrolyte. Revision 2, December 2000. Table IB, Note 54.
    (ii) [Reserved]
    (c) Under certain circumstances, the Director may establish 
limitations on the discharge of a parameter for which there is no test 
procedure in this part or in 40 CFR parts 405 through 499. In these 
instances the test procedure shall be specified by the Director.
    (d) Under certain circumstances, the Administrator may approve 
additional alternate test procedures for nationwide use, upon 
recommendation by the Alternate Test Procedure Program Coordinator, 
Washington, DC.
    (e) Sample preservation procedures, container materials, and maximum 
allowable holding times for parameters are cited in Tables IA, IB, IC, 
ID, IE, IF, IG, and IH are prescribed in Table II. Information in the 
table takes precedence over information in specific methods or 
elsewhere. Any person may apply for a change from the prescribed 
preservation techniques, container materials, and maximum holding times 
applicable to samples taken from a specific discharge. Applications for 
such limited use changes may be made by letters to the Regional 
Alternative Test Procedure (ATP) Program Coordinator or the permitting 
authority in the Region in which the discharge will occur. Sufficient 
data should be provided to assure such changes in sample preservation, 
containers or holding times do not adversely affect the integrity of the 
sample. The Regional ATP Coordinator or permitting authority will review 
the application and then notify the applicant and the appropriate State 
agency of approval or rejection of the use of the alternate test 
procedure. A decision to approve or deny any request on deviations from 
the prescribed Table II requirements will be made within 90 days of 
receipt of the application by the Regional Administrator. An analyst may 
not modify any sample preservation and/or holding time requirements of 
an approved method unless the requirements of this section are met.

                    Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
                                                                                           Maximum holding time
        Parameter number/name               Container \1\         Preservation \2\ \3\             \4\
----------------------------------------------------------------------------------------------------------------
                                            Table IA--Bacterial Tests
----------------------------------------------------------------------------------------------------------------
1-5. Coliform, total, fecal, and E.    PA, G..................  Cool, <10 [deg]C,        8 hours.\22\ \23\
 coli.                                                           0.008% Na2S2O3 \5\.
6. Fecal streptococci................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.008% Na2S2O3 \5\.
7. Enterococci.......................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.008% Na2S2O3 \5\.
8. Salmonella........................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.008% Na2S2O3 \5\.
----------------------------------------------------------------------------------------------------------------
                                        Table IA--Aquatic Toxicity Tests
----------------------------------------------------------------------------------------------------------------
9-12. Toxicity, acute and chronic....  P, FP, G...............  Cool, <=6 [deg]C \16\..  36 hours.
----------------------------------------------------------------------------------------------------------------
                                            Table IB--Inorganic Tests
----------------------------------------------------------------------------------------------------------------
1. Acidity...........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  14 days.
2. Alkalinity........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  14 days.

[[Page 66]]

 
4. Ammonia...........................  P, FP, G...............  Cool, <=6 [deg]C,\18\    28 days.
                                                                 H2SO4 to pH <2.
9. Biochemical oxygen demand.........  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
10. Boron............................  P, FP, or Quartz.......  HNO3 to pH <2..........  6 months.
11. Bromide..........................  P, FP, G...............  None required..........  28 days.
14. Biochemical oxygen demand,         P, FP G................  Cool, <=6 [deg]C \18\..  48 hours.
 carbonaceous.
15. Chemical oxygen demand...........  P, FP, G...............  Cool, <=6 [deg]C,\18\    28 days.
                                                                 H2SO4 to pH <2.
16. Chloride.........................  P, FP, G...............  None required..........  28 days.
17. Chlorine, total residual.........  P, G...................  None required..........  Analyze within 15
                                                                                          minutes.
21. Color............................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
23-24. Cyanide, total or available     P, FP, G...............  Cool, <=6 [deg]C,\18\    14 days.
 (or CATC) and free.                                             NaOH to pH 10,5 6 reducing
                                                                 agent if oxidizer
                                                                 present.
25. Fluoride.........................  P......................  None required..........  28 days.
27. Hardness.........................  P, FP, G...............  HNO3 or H2SO4 to pH <2.  6 months.
28. Hydrogen ion (pH)................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
31, 43. Kjeldahl and organic N.......  P, FP, G...............  Cool, <=6 [deg]C,\18\    28 days.
                                                                 H2SO4 to pH <2.
----------------------------------------------------------------------------------------------------------------
                                              Table IB--Metals \7\
----------------------------------------------------------------------------------------------------------------
18. Chromium VI......................  P, FP, G...............  Cool, <=6 [deg]C,\18\    28 days.
                                                                 pH = 9.3-9.7 \20\.
35. Mercury (CVAA)...................  P, FP, G...............  HNO3 to pH <2..........  28 days.
35. Mercury (CVAFS)..................  FP, G; and FP-lined cap  5 mL/L 12N HCl or 5 mL/  90 days.\17\
                                        \17\.                    L BrCl \17\.
3, 5-8, 12, 13, 19, 20, 22, 26, 29,    P, FP, G...............  HNO3 to pH <2, or at     6 months.
 30, 32-34, 36, 37, 45, 47, 51, 52,                              least 24 hours prior
 58-60, 62, 63, 70-72, 74, 75.                                   to analysis \19\.
 Metals, except boron, chromium VI,
 and mercury.
38. Nitrate..........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
39. Nitrate-nitrite..................  P, FP, G...............  Cool, <=6                28 days.
                                                                 [deg]C,\18\H2SO4 to pH
                                                                 <2.
40. Nitrite..........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
41. Oil and grease...................  G......................  Cool to <=6 [deg]C,\18\  28 days.
                                                                 HCl or H2SO4 to pH <2.
42. Organic Carbon...................  P, FP, G...............  Cool to <=6 [deg]C,\18\  28 days.
                                                                 HCl, H2SO4, or H3PO4
                                                                 to pH <2.
44. Orthophosphate...................  P, FP, G...............  Cool, to <=6 [deg]C 18   Filter within 15
                                                                 24.                      minutes; Analyze
                                                                                          within 48 hours.
46. Oxygen, Dissolved Probe..........  G, Bottle and top......  None required..........  Analyze within 15
                                                                                          minutes.
47. Winkler..........................  G, Bottle and top......  Fix on site and store    8 hours.
                                                                 in dark.
48. Phenols..........................  G......................  Cool, <=6 [deg]C,\18\    28 days.
                                                                 H2SO4 to pH <2.
49. Phosphorous (elemental)..........  G......................  Cool, <=6 [deg]C \18\..  48 hours.
50. Phosphorous, total...............  P, FP, G...............  Cool, <=6 [deg]C,\18\    28 days.
                                                                 H2SO4 to pH <2.
53. Residue, total...................  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
54. Residue, Filterable..............  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
55. Residue, Nonfilterable (TSS).....  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
56. Residue, Settleable..............  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
57. Residue, Volatile................  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
61. Silica...........................  P or Quartz............  Cool, <=6 [deg]C \18\..  28 days.
64. Specific conductance.............  P, FP, G...............  Cool, <=6 [deg]C \18\..  28 days.
65. Sulfate..........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  28 days.
66. Sulfide..........................  P, FP, G...............  Cool, <=6 [deg]C,\18\    7 days.
                                                                 add zinc acetate plus
                                                                 sodium hydroxide to pH
                                                                 9.
67. Sulfite..........................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
68. Surfactants......................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
69. Temperature......................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
73. Turbidity........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
----------------------------------------------------------------------------------------------------------------

[[Page 67]]

 
                                           Table IC--Organic Tests \8\
----------------------------------------------------------------------------------------------------------------
13, 18-20, 22, 24, 25, 27,28, 34-37,   G, FP-lined septum.....  Cool, <=6 [deg]C,\18\    14 days.
 39-43, 45-47, 56, 76, 104, 105, 108-                            0.008% Na2S2O3,\5\ HCl
 111, 113. Purgeable Halocarbons.                                to pH 2.
26. 2-Chloroethylvinyl ether.........  G, FP-lined septum.....  Cool, <=6 [deg]C,\18\    14 days.
                                                                 0.008% Na2S2O3\5\.
6, 57, 106. Purgeable aromatic         G, FP-lined septum.....  Cool, <=6 [deg]C,\18\    14 days.\9\
 hydrocarbons.                                                   0.008% Na2S2O3,\5\ HCl
                                                                 to pH 2 \9\.
3, 4. Acrolein and acrylonitrile.....  G, FP-lined septum.....  Cool, <=6 [deg]C,\18\    14 days.\10\
                                                                 0.008% Na2S2O3, pH to
                                                                 4-5 \10\.
23, 30, 44, 49, 53, 77, 80, 81, 98,    G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
 100, 112. Phenols \11\.                                         0.008% Na2S2O3.          extraction, 40 days
                                                                                          after extraction.
7, 38. Benzidines 11 12..............  G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
                                                                 0.008% Na2S2O3\5\.       extraction.\13\
14, 17, 48, 50-52. Phthalate esters    G, FP-lined cap........  Cool, <=6 [deg]C \18\..  7 days until
 \11\.                                                                                    extraction, 40 days
                                                                                          after extraction.
82-84. Nitrosamines 11 14............  G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
                                                                 store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3 \5\.             after extraction.
88-94. PCBs \11\.....................  G, FP-lined cap........  Cool, <=6 [deg]C \18\..  1 year until
                                                                                          extraction, 1 year
                                                                                          after extraction.
54, 55, 75, 79. Nitroaromatics and     G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
 isophorone \11\.                                                store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3 \5\.             after extraction.
1, 2, 5, 8-12, 32, 33, 58, 59, 74,     G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
 78, 99, 101. Polynuclear aromatic                               store in dark, 0.008%    extraction, 40 days
 hydrocarbons \11\.                                              Na2S2O3 \5\.             after extraction.
15, 16, 21, 31, 87. Haloethers \11\..  G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
                                                                 0.008% Na2S2O3 \5\.      extraction, 40 days
                                                                                          after extraction.
29, 35-37, 63-65, 107. Chlorinated     G, FP-lined cap........  Cool, <=6 [deg]C \18\..  7 days until
 hydrocarbons \11\.                                                                       extraction, 40 days
                                                                                          after extraction.
60-62, 66-72, 85, 86, 95-97, 102,      G......................  See footnote 11........  See footnote 11.
 103. CDDs/CDFs \11\.
    Aqueous Samples: Field and Lab     G......................  Cool, <=6 [deg]C,\18\    1 year.
     Preservation.                                               0.008% Na2S2O3,\5\ pH
                                                                 <9.
    Solids and Mixed-Phase Samples:    G......................  Cool, <=6 [deg]C \18\..  7 days.
     Field Preservation.
    Tissue Samples: Field              G......................  Cool, <=6 [deg]C \18\..  24 hours.
     Preservation.
    Solids, Mixed-Phase, and Tissue    G......................  Freeze, <=-10 [deg]C...  1 year.
     Samples: Lab Preservation.
114-118. Alkylated phenols...........  G......................  Cool, <6 [deg]C, H2SO4   28 days until
                                                                 to pH <2.                extraction, 40 days
                                                                                          after extraction.
119. Adsorbable Organic Halides (AOX)  G......................  Cool, <6 [deg]C, 0.008%  Hold at least 3 days,
                                                                 Na2S2O3, HNO3 to pH <2.  but not more than 6
                                                                                          months.
120. Chlorinated Phenolics...........  G, FP-lined cap........  Cool, <6 [deg]C, 0.008%  30 days until
                                                                 Na2S2O3, H2SO4 to pH     acetylation, 30 days
                                                                 <2.                      after acetylation.
----------------------------------------------------------------------------------------------------------------
                                           Table ID--Pesticides Tests
----------------------------------------------------------------------------------------------------------------
1-70. Pesticides \11\................  G, FP-lined cap........  Cool, <=6 [deg]C,\18\    7 days until
                                                                 pH 5-9 \15\.             extraction, 40 days
                                                                                          after extraction.
----------------------------------------------------------------------------------------------------------------
                                          Table IE--Radiological Tests
----------------------------------------------------------------------------------------------------------------
1-5. Alpha, beta, and radium.........  P, FP, G...............  HNO3 to pH <2..........  6 months.
----------------------------------------------------------------------------------------------------------------
                                            Table IH--Bacterial Tests
----------------------------------------------------------------------------------------------------------------
1-4. Coliform, total, fecal..........  PA, G..................  Cool, <10 [deg]C,        8 hours.22 23
                                                                 0.008% Na2S2O3\5\.
5. E. coli...........................  PA, G..................  Cool, <10 [deg]C, 0.     8 hours.\22\
                                                                 008% Na2S2O3 \5\.
6. Fecal streptococci................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.008% Na2S2O3 \5\.
7. Enterococci.......................  PA, G..................  Cool, <10 [deg]C, 0.     8 hours.\22\
                                                                 008% Na2S2O3 \5\.
----------------------------------------------------------------------------------------------------------------
                                            Table IH--Protozoan Tests
----------------------------------------------------------------------------------------------------------------
8. Cryptosporidium...................  LDPE; field filtration.  1-10 [deg]C............  96 hours.\21\

[[Page 68]]

 
9. Giardia...........................  LDPE; field filtration.  1-10 [deg]C............  96 hours.\21\
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is for polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE); Teflon[supreg]), or
  other fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is
  made of a sterilizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density
  polyethylene.
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
  minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour
  composite sample; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), refrigerate the sample at <=6
  [deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
  sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <=6 [deg]C,
  unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
  is completed. Add the preservative to the sample container prior to sample collection when the preservative
  will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite
  sample within 15 minutes of collection. If a composite measurement is required but a composite sample would
  compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4
  samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the
  concentrations averaged. Alternatively, grab samples may be collected in the field and composited in the
  laboratory if the compositing procedure produces results equivalent to results produced by arithmetic
  averaging of results of analysis of individual grab samples. For examples of laboratory compositing
  procedures, see EPA Method 1664 Rev. A (oil and grease) and the procedures at 40 CFR 141.24(f)(14)(iv) and (v)
  (volatile organics).
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
  the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering such
  material for transportation is responsible for ensuring such compliance. For the preservation requirement of
  Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
  determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
  (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater; Nitric acid
  (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
  acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
  Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
  less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
  samples may be held before the start of analysis and still be considered valid. Samples may be held for longer
  periods only if the permittee or monitoring laboratory have data on file to show that, for the specific types
  of samples under study, the analytes are stable for the longer time, and has received a variance from the
  Regional ATP Coordinator under Sec.   136.3(e). For a grab sample, the holding time begins at the time of
  collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
  sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), the holding time begins at the time of
  the end of collection of the composite sample. For a set of grab samples composited in the field or
  laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
  may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
  obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
  sample stability. See Sec.   136.3(e) for details. The date and time of collection of an individual grab
  sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and
  that are all collected on the same calendar date, the date of collection is the date on which the samples are
  collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
  date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
  automatically on a given date, the date of collection is the date on which the sample is collected. For a
  composite sample collected automatically, and that is collected across two calendar dates, the date of
  collection is the dates of the two days; e.g., November 14-15. For static-renewal toxicity tests, each grab or
  composite sample may also be used to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after first
  use, if stored at 0-6 [deg]C, with minimum head space.
\5\ ASTM D7365-09a specifies treatment options for samples containing oxidants (e.g., chlorine) for cyanide
  analyses. Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st
  editions) addresses dechlorination procedures for microbiological analyses.
\6\ Sampling, preservation and mitigating interferences in water samples for analysis of cyanide are described
  in ASTM D7365-09a. There may be interferences that are not mitigated by the analytical test methods or D7365-
  09a. Any technique for removal or suppression of interference may be employed, provided the laboratory
  demonstrates that it more accurately measures cyanide through quality control measures described in the
  analytical test method. Any removal or suppression technique not described in D7365-09a or the analytical test
  method must be documented along with supporting data.
\7\ For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives.
  For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40
  CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), filter the sample within 15 minutes after completion of
  collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will
  be compromised during collection of a composite sample collected automatically over time (e.g., by interchange
  of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote
  2) in place of a composite sample collected automatically.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
\10\ The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
  adjustment must be analyzed within 3 days of sampling.
\11\ When the extractable analytes of concern fall within a single chemical category, the specified preservative
  and maximum holding times should be observed for optimum safeguard of sample integrity (i.e., use all
  necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two
  or more chemical categories, the sample may be preserved by cooling to <=6 [deg]C, reducing residual chlorine
  with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this
  manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this
  optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
  thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
\12\ If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 
  0.2 to prevent rearrangement to benzidine.
\13\ Extracts may be stored up to 30 days at <0 [deg]C.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
  of sampling.
\15\ The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
  extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Place sufficient ice with the samples in the shipping container to ensure that ice is still present when
  the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately
  measure the temperature of the samples and confirm that the preservation temperature maximum has not been
  exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the
  permittee can be given the option of on-site testing or can request a variance. The request for a variance
  should include supportive data which show that the toxicity of the effluent samples is not reduced because of
  the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day
  of collection do not need to be cooled to 0 to 6 [deg]C prior to test initiation.

[[Page 69]]

 
\17\ Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be
  collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48
  hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
  sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory
  within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample
  should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669.
  If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be
  filtered in a designated clean area in the field within the time period necessary to maintain sample
  integrity. A sample that has been collected for determination of total or dissolved trace level mercury must
  be analyzed within 90 days of sample collection.
\18\ Aqueous samples must be preserved at <=6 [deg]C, and should not be frozen unless data demonstrating that
  sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
  regulatory authority. Also, for purposes of NPDES monitoring, the specification of ``<= [deg]C'' is used in
  place of the ``4 [deg]C'' and ``<4 [deg]C'' sample temperature requirements listed in some methods. It is not
  necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three
  significant figures are specified so that rounding down to 6 [deg]C may not be used to meet the <=6 [deg]C
  requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than
  15 minutes).
\19\ An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at
  least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must
  be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment
  samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and
  holding time requirements in the approved metals methods.
\20\ To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6.
  The allowance in this footnote supersedes preservation and holding time requirements in the approved
  hexavalent chromium methods, unless this supersession would compromise the measurement, in which case
  requirements in the method must be followed.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
  in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
\22\ Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later
  than 8 hours from time of collection.
\23\ For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for
  the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B
  aerobically digested, and Class B anaerobically digested.
\24\ The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-
  available form of orthophosphorus (i.e., that which passes through a 0.45-micron filter), hence the
  requirement to filter the sample immediately upon collection (i.e., within 15 minutes of collection).


[38 FR 28758, Oct. 16, 1973]

    Editorial Note: For Federal Register citations affecting Sec.  
136.3, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  136.4  Application for and approval of alternate test procedures 
for nationwide use.

    (a) A written application for review of an alternate test procedure 
(alternate method) for nationwide use may be made by letter via email or 
by hard copy in triplicate to the National Alternate Test Procedure 
(ATP) Program Coordinator (National Coordinator), Office of Science and 
Technology (4303T), Office of Water, U.S. Environmental Protection 
Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460. Any 
application for an ATP under this paragraph (a) shall:
    (1) Provide the name and address of the responsible person or firm 
making the application.
    (2) Identify the pollutant(s) or parameter(s) for which nationwide 
approval of an alternate test procedure is being requested.
    (3) Provide a detailed description of the proposed alternate test 
procedure, together with references to published or other studies 
confirming the general applicability of the alternate test procedure for 
the analysis of the pollutant(s) or parameter(s) in wastewater 
discharges from representative and specified industrial or other 
categories.
    (4) Provide comparability data for the performance of the proposed 
alternative test procedure compared to the performance of the reference 
method.
    (b) The National Coordinator may request additional information and 
analyses from the applicant in order to evaluate whether the alternate 
test procedure satisfies the applicable requirements of this part.
    (c) Approval for nationwide use. (1) After a review of the 
application and any additional analyses requested from the applicant, 
the National Coordinator will notify the applicant, in writing, of 
whether the National Coordinator will recommend approval or disapproval 
of the alternate test procedure for nationwide use in CWA programs. If 
the application is not recommended for approval, the National 
Coordinator may specify what additional information might lead to a 
reconsideration of the application and notify the Regional Alternate 
Test Procedure Coordinators of the disapproval recommendation. Based on 
the National Coordinator's recommended disapproval of a proposed

[[Page 70]]

alternate test procedure and an assessment of any current approvals for 
limited uses for the unapproved method, the Regional ATP Coordinator may 
decide to withdraw approval of the method for limited use in the Region.
    (2) Where the National Coordinator has recommended approval of an 
applicant's request for nationwide use of an alternate test procedure, 
the National Coordinator will notify the applicant. The National 
Coordinator will also notify the Regional ATP Coordinators that they may 
consider approval of this alternate test procedure for limited use in 
their Regions based on the information and data provided in the 
application until the alternate test procedure is approved by 
publication in a final rule in the Federal Register.
    (3) EPA will propose to amend this part to include the alternate 
test procedure in Sec.  136.3. EPA shall make available for review all 
the factual bases for its proposal, including the method, any 
performance data submitted by the applicant and any available EPA 
analysis of those data.
    (4) Following public comment, EPA shall publish in the Federal 
Register a final decision on whether to amend this part to include the 
alternate test procedure as an approved analytical method for nationwide 
use.
    (5) Whenever the National Coordinator has recommended approval of an 
applicant's ATP request for nationwide use, any person may request an 
approval of the method for limited use under Sec.  136.5 from the EPA 
Region.

[77 FR 29809, May 18, 2012, as amended at 82 FR 40874, Aug. 28, 2017]



Sec.  136.5  Approval of alternate test procedures for limited use.

    (a) Any person may request the Regional ATP Coordinator to approve 
the use of an alternate test procedure in the Region.
    (b) When the request for the use of an alternate test procedure 
concerns use in a State with an NPDES permit program approved pursuant 
to section 402 of the Act, the requestor shall first submit an 
application for limited use to the Director of the State agency having 
responsibility for issuance of NPDES permits within such State (i.e., 
permitting authority). The Director will forward the application to the 
Regional ATP Coordinator with a recommendation for or against approval.
    (c) Any application for approval of an alternate test procedure for 
limited use may be made by letter, email or by hard copy. The 
application shall include the following:
    (1) Provide the name and address of the applicant and the applicable 
ID number of the existing or pending permit(s) and issuing agency for 
which use of the alternate test procedure is requested, and the 
discharge serial number.
    (2) Identify the pollutant or parameter for which approval of an 
alternate test procedure is being requested.
    (3) Provide justification for using testing procedures other than 
those specified in Tables IA through IH of Sec.  136.3, or in the NPDES 
permit.
    (4) Provide a detailed description of the proposed alternate test 
procedure, together with references to published studies of the 
applicability of the alternate test procedure to the effluents in 
question.
    (5) Provide comparability data for the performance of the proposed 
alternate test procedure compared to the performance of the reference 
method.
    (d) Approval for limited use. (1) The Regional ATP Coordinator will 
review the application and notify the applicant and the appropriate 
State agency of approval or rejection of the use of the alternate test 
procedure. The approval may be restricted to use only with respect to a 
specific discharge or facility (and its laboratory) or, at the 
discretion of the Regional ATP Coordinator, to all dischargers or 
facilities (and their associated laboratories) specified in the approval 
for the Region. If the application is not approved, the Regional ATP 
Coordinator shall specify what additional information might lead to a 
reconsideration of the application.
    (2) The Regional ATP Coordinator will forward a copy of every 
approval and rejection notification to the National Alternate Test 
Procedure Coordinator.

[77 FR 29809, May 18, 2012, as amended at 82 FR 40875, Aug. 28, 2017]

[[Page 71]]



Sec.  136.6  Method modifications and analytical requirements.

    (a) Definitions of terms used in this section--(1) Analyst means the 
person or laboratory using a test procedure (analytical method) in this 
part.
    (2) Chemistry of the method means the reagents and reactions used in 
a test procedure that allow determination of the analyte(s) of interest 
in an environmental sample.
    (3) Determinative technique means the way in which an analyte is 
identified and quantified (e.g., colorimetry, mass spectrometry).
    (4) Equivalent performance means that the modified method produces 
results that meet or exceed the QC acceptance criteria of the approved 
method.
    (5) Method-defined analyte means an analyte defined solely by the 
method used to determine the analyte. Such an analyte may be a physical 
parameter, a parameter that is not a specific chemical, or a parameter 
that may be comprised of a number of substances. Examples of such 
analytes include temperature, oil and grease, total suspended solids, 
total phenolics, turbidity, chemical oxygen demand, and biochemical 
oxygen demand.
    (6) QC means ``quality control.''
    (b) Method modifications. (1) If the underlying chemistry and 
determinative technique in a modified method are essentially the same as 
an approved Part 136 method, then the modified method is an equivalent 
and acceptable alternative to the approved method provided the 
requirements of this section are met. However, those who develop or use 
a modification to an approved (Part 136) method must document that the 
performance of the modified method, in the matrix to which the modified 
method will be applied, is equivalent to the performance of the approved 
method. If such a demonstration cannot be made and documented, then the 
modified method is not an acceptable alternative to the approved method. 
Supporting documentation must, if applicable, include the routine 
initial demonstration of capability and ongoing QC including 
determination of precision and accuracy, detection limits, and matrix 
spike recoveries. Initial demonstration of capability typically includes 
analysis of four replicates of a mid-level standard and a method 
detection limit study. Ongoing quality control typically includes method 
blanks, mid-level laboratory control samples, and matrix spikes (QC is 
as specified in the method). The method is considered equivalent if the 
quality control requirements in the reference method are achieved. Where 
the laboratory is using a vendor-supplied method, it is the QC criteria 
in the reference method, not the vendor's method, that must be met to 
show equivalency. Where a sample preparation step is required (i.e., 
digestion, distillation), QC tests are to be run using standards treated 
in the same way as the samples. The method user's Standard Operating 
Procedure (SOP) must clearly document the modifications made to the 
reference method. Examples of allowed method modifications are listed in 
this section. If the method user is uncertain whether a method 
modification is allowed, the Regional ATP Coordinator or Director should 
be contacted for approval prior to implementing the modification. The 
method user should also complete necessary performance checks to verify 
that acceptable performance is achieved with the method modification 
prior to analyses of compliance samples.
    (2) Requirements. The modified method must meet or exceed 
performance of the approved method(s) for the analyte(s) of interest, as 
documented by meeting the initial and ongoing quality control 
requirements in the method.
    (i) Requirements for establishing equivalent performance. If the 
approved method contains QC tests and QC acceptance criteria, the 
modified method must use these QC tests and the modified method must 
meet the QC acceptance criteria with the following conditions:
    (A) The analyst may only rely on QC tests and QC acceptance criteria 
in a method if it includes wastewater matrix QC tests and QC acceptance 
criteria (e.g., matrix spikes) and both initial (start-up) and ongoing 
QC tests and QC acceptance criteria.
    (B) If the approved method does not contain QC tests and QC 
acceptance criteria or if the QC tests and QC acceptance criteria in the 
method do not

[[Page 72]]

meet the requirements of this section, then the analyst must employ QC 
tests published in the ``equivalent'' of a Part 136 method that has such 
QC, or the essential QC requirements specified at 136.7, as applicable. 
If the approved method is from a compendium or VCSB and the QA/QC 
requirements are published in other parts of that organization's 
compendium rather than within the Part 136 method then that part of the 
organization's compendium must be used for the QC tests.
    (C) In addition, the analyst must perform ongoing QC tests, 
including assessment of performance of the modified method on the sample 
matrix (e.g., analysis of a matrix spike/matrix spike duplicate pair for 
every twenty samples), and analysis of an ongoing precision and recovery 
sample (e.g., laboratory fortified blank or blank spike) and a blank 
with each batch of 20 or fewer samples.
    (D) If the performance of the modified method in the wastewater 
matrix or reagent water does not meet or exceed the QC acceptance 
criteria, the method modification may not be used.
    (ii) Requirements for documentation. The modified method must be 
documented in a method write-up or an addendum that describes the 
modification(s) to the approved method prior to the use of the method 
for compliance purposes. The write-up or addendum must include a 
reference number (e.g., method number), revision number, and revision 
date so that it may be referenced accurately. In addition, the 
organization that uses the modified method must document the results of 
QC tests and keep these records, along with a copy of the method write-
up or addendum, for review by an auditor.
    (3) Restrictions. An analyst may not modify an approved Clean Water 
Act analytical method for a method-defined analyte. In addition, an 
analyst may not modify an approved method if the modification would 
result in measurement of a different form or species of an analyte. 
Changes in method procedures are not allowed if such changes would alter 
the defined chemistry (i.e., method principle) of the unmodified method. 
For example, phenol method 420.1 or 420.4 defines phenolics as ferric 
iron oxidized compounds that react with 4-aminoantipyrine (4-AAP) at pH 
10 after being distilled from acid solution. Because total phenolics 
represents a group of compounds that all react at different efficiencies 
with 4-AAP, changing test conditions likely would change the behavior of 
these different phenolic compounds. An analyst may not modify any sample 
collection, preservation, or holding time requirements of an approved 
method. Such modifications to sample collection, preservation, and 
holding time requirements do not fall within the scope of the 
flexibility allowed at Sec.  136.6. Method flexibility refers to 
modifications of the analytical procedures used for identification and 
measurement of the analyte only and does not apply to sample collection, 
preservation, or holding time procedures, which may only be modified as 
specified in Sec.  136.3(e).
    (4) Allowable changes. Except as noted under paragraph (b)(3) of 
this section, an analyst may modify an approved test procedure 
(analytical method) provided that the underlying reactions and 
principles used in the approved method remain essentially the same, and 
provided that the requirements of this section are met. If equal or 
better performance can be obtained with an alternative reagent, then it 
is allowed. A laboratory wishing to use these modifications must 
demonstrate acceptable method performance by performing and documenting 
all applicable initial demonstration of capability and ongoing QC tests 
and meeting all applicable QC acceptance criteria as described in Sec.  
136.7. Some examples of the allowed types of changes, provided the 
requirements of this section are met include:
    (i) Changes between manual method, flow analyzer, and discrete 
instrumentation.
    (ii) Changes in chromatographic columns or temperature programs.
    (iii) Changes between automated and manual sample preparation, such 
as digestions, distillations, and extractions; in-line sample 
preparation is an acceptable form of automated sample preparation for 
CWA methods.
    (iv) In general, ICP-MS is a sensitive and selective detector for 
metal analysis; however isobaric interference can

[[Page 73]]

cause problems for quantitative determination, as well as identification 
based on the isotope pattern. Interference reduction technologies, such 
as collision cells or reaction cells, are designed to reduce the effect 
of spectroscopic interferences that may bias results for the element of 
interest. The use of interference reduction technologies is allowed, 
provided the method performance specifications relevant to ICP-MS 
measurements are met.
    (v) The use of EPA Method 200.2 or the sample preparation steps from 
EPA Method 1638, including the use of closed-vessel digestion, is 
allowed for EPA Method 200.8, provided the method performance 
specifications relevant to the ICP-MS are met.
    (vi) Changes in pH adjustment reagents. Changes in compounds used to 
adjust pH are acceptable as long as they do not produce interference. 
For example, using a different acid to adjust pH in colorimetric 
methods.
    (vii) Changes in buffer reagents are acceptable provided that the 
changes do not produce interferences.
    (viii) Changes in the order of reagent addition are acceptable 
provided that the change does not alter the chemistry and does not 
produce an interference. For example, using the same reagents, but 
adding them in different order, or preparing them in combined or 
separate solutions (so they can be added separately), is allowed, 
provided reagent stability or method performance is equivalent or 
improved.
    (ix) Changes in calibration range (provided that the modified range 
covers any relevant regulatory limit and the method performance 
specifications for calibration are met).
    (x) Changes in calibration model. (A) Linear calibration models do 
not adequately fit calibration data with one or two inflection points. 
For example, vendor-supplied data acquisition and processing software on 
some instruments may provide quadratic fitting functions to handle such 
situations. If the calibration data for a particular analytical method 
routinely display quadratic character, using quadratic fitting functions 
may be acceptable. In such cases, the minimum number of calibrators for 
second order fits should be six, and in no case should concentrations be 
extrapolated for instrument responses that exceed that of the most 
concentrated calibrator. Examples of methods with nonlinear calibration 
functions include chloride by SM4500-Cl-E-1997, hardness by EPA Method 
130.1, cyanide by ASTM D6888 or OIA1677, Kjeldahl nitrogen by PAI-DK03, 
and anions by EPA Method 300.0.
    (B) As an alternative to using the average response factor, the 
quality of the calibration may be evaluated using the Relative Standard 
Error (RSE). The acceptance criterion for the RSE is the same as the 
acceptance criterion for Relative Standard Deviation (RSD), in the 
method. RSE is calculated as:
[GRAPHIC] [TIFF OMITTED] TR18MY12.000

Where:

x[min]i = Calculated concentration at level i
xi = Actual concentration of the calibration level i
n = Number of calibration points
p = Number of terms in the fitting equation (average = 1, linear = 2, 
          quadratic = 3)

    (C) Using the RSE as a metric has the added advantage of allowing 
the same numerical standard to be applied to the calibration model, 
regardless of the form of the model. Thus, if a method states that the 
RSD should be <=20% for the traditional linear model

[[Page 74]]

through the origin, then the RSE acceptance limit can remain <=20% as 
well. Similarly, if a method provides an RSD acceptance limit of <=15%, 
then that same figure can be used as the acceptance limit for the RSE. 
The RSE may be used as an alternative to correlation coefficients and 
coefficients of determination for evaluating calibration curves for any 
of the methods at part 136. If the method includes a numerical criterion 
for the RSD, then the same numerical value is used for the RSE. Some 
older methods do not include any criterion for the calibration curve--
for these methods, if RSE is used the value should be <=20%. Note that 
the use of the RSE is included as an alternative to the use of the 
correlation coefficient as a measure of the suitability of a calibration 
curve. It is not necessary to evaluate both the RSE and the correlation 
coefficient.
    (xi) Changes in equipment such as equipment from a vendor different 
from the one specified in the method.
    (xii) The use of micro or midi distillation apparatus in place of 
macro distillation apparatus.
    (xiii) The use of prepackaged reagents.
    (xiv) The use of digital titrators and methods where the underlying 
chemistry used for the determination is similar to that used in the 
approved method.
    (xv) Use of selected ion monitoring (SIM) mode for analytes that 
cannot be effectively analyzed in full-scan mode and reach the required 
sensitivity. False positives are more of a concern when using SIM 
analysis, so at a minimum, one quantitation and two qualifying ions must 
be monitored for each analyte (unless fewer than three ions with 
intensity greater than 15% of the base peak are available). The ratio of 
each of the two qualifying ions to the quantitation ion must be 
evaluated and should agree with the ratio observed in an authentic 
standard within 20 percent. Analyst judgment must 
be applied to the evaluation of ion ratios because the ratios can be 
affected by co-eluting compounds present in the sample matrix. The 
signal-to-noise ratio of the least sensitive ion should be at least 3:1. 
Retention time in the sample should match within 0.05 minute of an 
authentic standard analyzed under identical conditions. Matrix 
interferences can cause minor shifts in retention time and may be 
evident as shifts in the retention times of the internal standards. The 
total scan time should be such that a minimum of eight scans are 
obtained per chromatographic peak.
    (xvi) Changes are allowed in purge-and-trap sample volumes or 
operating conditions. Some examples are:
    (A) Changes in purge time and purge-gas flow rate. A change in purge 
time and purge-gas flow rate is allowed provided that sufficient total 
purge volume is used to achieve the required minimum detectible 
concentration and calibration range for all compounds. In general, a 
purge rate in the range 20-200 mL/min and a total purge volume in the 
range 240-880 mL are recommended.
    (B) Use of nitrogen or helium as a purge gas, provided that the 
required sensitivities for all compounds are met.
    (C) Sample temperature during the purge state. Gentle heating of the 
sample during purging (e.g., 40 [deg]C) increases purging efficiency of 
hydrophilic compounds and may improve sample-to-sample repeatability 
because all samples are purged under precisely the same conditions.
    (D) Trap sorbent. Any trap design is acceptable, provided that the 
data acquired meet all QC criteria.
    (E) Changes to the desorb time. Shortening the desorb time (e.g., 
from4 minutes to 1 minute) may not affect compound recoveries, and can 
shorten overall cycle time and significantly reduce the amount of water 
introduced to the analytical system, thus improving the precision of 
analysis, especially for water-soluble analytes. A desorb time of four 
minutes is recommended, however a shorter desorb time may be used, 
provided that all QC specifications in the method are met.
    (F) Use of water management techniques is allowed. Water is always 
collected on the trap along with the analytes and is a significant 
interference for analytical systems (GC and GC/MS). Modern water 
management techniques (e.g., dry purge or condensation points) can 
remove moisture from

[[Page 75]]

the sample stream and improve analytical performance.
    (xvii) If the characteristics of a wastewater matrix prevent 
efficient recovery of organic pollutants and prevent the method from 
meeting QC requirements, the analyst may attempt to resolve the issue by 
adding salts to the sample, provided that such salts do not react with 
or introduce the target pollutant into the sample (as evidenced by the 
analysis of method blanks, laboratory control samples, and spiked 
samples that also contain such salts), and that all requirements of 
paragraph (b)(2) of this section are met. Samples having residual 
chlorine or other halogen must be dechlorinated prior to the addition of 
such salts.
    (xviii) If the characteristics of a wastewater matrix result in poor 
sample dispersion or reagent deposition on equipment and prevent the 
analyst from meeting QC requirements, the analyst may attempt to resolve 
the issue by adding a inert surfactant that does not affect the 
chemistry of the method, such as Brij-35 or sodium dodecyl sulfate 
(SDS), provided that such surfactant does not react with or introduce 
the target pollutant into the sample (as evidenced by the analysis of 
method blanks, laboratory control samples, and spiked samples that also 
contain such surfactant) and that all requirements of paragraph (b)(1) 
and (b)(2) of this section are met. Samples having residual chlorine or 
other halogen must be dechlorinated prior to the addition of such 
surfactant.
    (xix) The use of gas diffusion (using pH change to convert the 
analyte to gaseous form and/or heat to separate an analyte contained in 
steam from the sample matrix) across a hydrophobic semi-permeable 
membrane to separate the analyte of interest from the sample matrix may 
be used in place of manual or automated distillation in methods for 
analysis such as ammonia, total cyanide, total Kjeldahl nitrogen, and 
total phenols. These procedures do not replace the digestion procedures 
specified in the approved methods and must be used in conjunction with 
those procedures.
    (xx) Changes in equipment operating parameters such as the 
monitoring wavelength of a colorimeter or the reaction time and 
temperature as needed to achieve the chemical reactions defined in the 
unmodified CWA method. For example, molybdenum blue phosphate methods 
have two absorbance maxima, one at about 660 nm and another at about 880 
nm. The former is about 2.5 times less sensitive than the latter. 
Wavelength choice provides a cost-effective, dilution-free means to 
increase sensitivity of molybdenum blue phosphate methods.
    (xxi) Interchange of oxidants, such as the use of titanium oxide in 
UV-assisted automated digestion of TOC and total phosphorus, as long as 
complete oxidation can be demonstrated.
    (xxii) Use of an axially viewed torch with Method 200.7.
    (c) The permittee must notify their permitting authority of the 
intent to use a modified method. Such notification should be of the form 
``Method xxx has been modified within the flexibility allowed in 40 CFR 
136.6.'' The permittee may indicate the specific paragraph of Sec.  
136.6 allowing the method modification. Specific details of the 
modification need not be provided, but must be documented in the 
Standard Operating Procedure (SOP) and maintained by the analytical 
laboratory that performs the analysis.

[77 FR 29810, May 18, 2012, as amended at 82 FR 40875, Aug. 28, 2017]



Sec.  136.7  Quality assurance and quality control.

    The permittee/laboratory shall use suitable QA/QC procedures when 
conducting compliance analyses with any part 136 chemical method or an 
alternative method specified by the permitting authority. These QA/QC 
procedures are generally included in the analytical method or may be 
part of the methods compendium for approved Part 136 methods from a 
consensus organization. For example, Standard Methods contains QA/QC 
procedures in the Part 1000 section of the Standard Methods Compendium. 
The permittee/laboratory shall follow these QA/QC procedures, as 
described in the method or methods compendium. If the method lacks QA/QC 
procedures, the permittee/laboratory has the following options to comply 
with the QA/QC requirements:

[[Page 76]]

    (a) Refer to and follow the QA/QC published in the ``equivalent'' 
EPA method for that parameter that has such QA/QC procedures;
    (b) Refer to the appropriate QA/QC section(s) of an approved part 
136 method from a consensus organization compendium;
    (c)(1) Incorporate the following twelve quality control elements, 
where applicable, into the laboratory's documented standard operating 
procedure (SOP) for performing compliance analyses when using an 
approved part 136 method when the method lacks such QA/QC procedures. 
One or more of the twelve QC elements may not apply to a given method 
and may be omitted if a written rationale is provided indicating why the 
element(s) is/are inappropriate for a specific method.
    (i) Demonstration of Capability (DOC);
    (ii) Method Detection Limit (MDL);
    (iii) Laboratory reagent blank (LRB), also referred to as method 
blank (MB);
    (iv) Laboratory fortified blank (LFB), also referred to as a spiked 
blank, or laboratory control sample (LCS);
    (v) Matrix spike (MS) and matrix spike duplicate (MSD), or 
laboratory fortified matrix (LFM) and LFM duplicate, may be used for 
suspected matrix interference problems to assess precision;
    (vi) Internal standards (for GC/MS analyses), surrogate standards 
(for organic analysis) or tracers (for radiochemistry);
    (vii) Calibration (initial and continuing), also referred to as 
initial calibration verification (ICV) and continuing calibration 
verification (CCV);
    (viii) Control charts (or other trend analyses of quality control 
results);
    (ix) Corrective action (root cause analysis);
    (x) QC acceptance criteria;
    (xi) Definitions of preparation and analytical batches that may 
drive QC frequencies; and
    (xii) Minimum frequency for conducting all QC elements.
    (2) These twelve quality control elements must be clearly documented 
in the written standard operating procedure for each analytical method 
not containing QA/QC procedures, where applicable.

[77 FR 29813, May 18, 2012]



 Sec. Appendix A to Part 136--Methods for Organic Chemical Analysis of 
                   Municipal and Industrial Wastewater

                    Method 601--Purgeable Halocarbons

                        1. Scope and Application

    1.1 This method covers the determination of 29 purgeable 
halocarbons.
    The following parameters may be determined by this method:

------------------------------------------------------------------------
                                                  STORET
                   Parameter                       No.        CAS No.
------------------------------------------------------------------------
Bromodichloromethane...........................    32101         75-27-4
Bromoform......................................    32104         75-25-2
Bromomethane...................................    34413         74-83-9
Carbon tetrachloride...........................    32102         56-23-5
Chlorobenzene..................................    34301        108-90-7
Chloroethane...................................    34311         75-00-3
2-Chloroethylvinyl ether.......................    34576        100-75-8
Chloroform.....................................    32106         67-66-3
Chloromethane..................................    34418         74-87-3
Dibromochloromethane...........................    32105        124-48-1
1,2-Dichlorobenzene............................    34536         95-50-1
1,3-Dichlorobenzene............................    34566        541-73-1
1,4-Dichlorobenzene............................    34571        106-46-7
Dichlorodifluoromethane........................    34668         75-71-8
1,1-Dichloroethane.............................    34496         75-34-3
1,2-Dichloroethane.............................    34531        107-06-2
1,1-Dichloroethane.............................    34501         75-35-4
trans-1,2-Dichloroethene.......................    34546        156-60-5
1,2-Dichloropropane............................    34541         78-87-5
cis-1,3-Dichloropropene........................    34704      10061-01-5
trans-1,3-Dichloropropene......................    34699      10061-02-6
Methylene chloride.............................    34423         75-09-2
1,1,2,2-Tetrachloroethane......................    34516         79-34-5
Tetrachloroethene..............................    34475        127-18-4
1,1,1-Trichloroethane..........................    34506         71-55-6
1,1,2-Trichloroethane..........................    34511         79-00-5
Tetrachloroethene..............................    39180         79-01-6
Trichlorofluoromethane.........................    34488         75-69-4
Vinyl chloride.................................    39715         75-01-4
------------------------------------------------------------------------

    1.2 This is a purge and trap gas chromatographic (GC) method 
applicable to the determination of the compounds listed above in 
municipal and industrial discharges as provided under 40 CFR 136.1. When 
this method is used to analyze unfamiliar samples for any or all of the 
compounds above, compound identifications should be supported by at 
least one additional qualitative technique. This method describes 
analytical conditions for a second gas chromatographic column that can 
be used to confirm measurements made with the primary column. Method 624 
provides gas chromatograph/mass spectrometer (GC/MS) conditions 
appropriate for the qualitative and quantitative confirmation of results 
for most of the parameters listed above.
    1.3 The method detection limit (MDL, defined in Section 12.1) \1\ 
for each parameter is

[[Page 77]]

listed in Table 1. The MDL for a specific wastewater may differ from 
those listed, depending upon the nature of interferences in the sample 
matrix.
    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the operation of a purge and trap system and a 
gas chromatograph and in the interpretation of gas chromatograms. Each 
analyst must demonstrate the ability to generate acceptable results with 
this method using the procedure described in Section 8.2.

                          2. Summary of Method

    2.1 An inert gas is bubbled through a 5-mL water sample contained in 
a specially-designed purging chamber at ambient temperature. The 
halocarbons are efficiently transferred from the aqueous phase to the 
vapor phase. The vapor is swept through a sorbent trap where the 
halocarbons are trapped. After purging is completed, the trap is heated 
and backflushed with the inert gas to desorb the halocarbons onto a gas 
chromatographic column. The gas chromatograph is temperature programmed 
to separate the halocarbons which are then detected with a halide-
specific detector. \2 3\
    2.2 The method provides an optional gas chromatographic column that 
may be helpful in resolving the compounds of interest from interferences 
that may occur.

                            3. Interferences

    3.1 Impurities in the purge gas and organic compounds outgassing 
from the plumbing ahead of the trap account for the majority of 
contamination problems. The analytical system must be demonstrated to be 
free from contamination under the conditions of the analysis by running 
laboratory reagent blanks as described in Section 8.1.3. The use of non-
Teflon plastic tubing, non-Teflon thread sealants, or flow controllers 
with rubber components in the purge and trap system should be avoided.
    3.2 Samples can be contaminated by diffusion of volatile organics 
(particularly fluorocarbons and methylene chloride) through the septum 
seal ilto the sample during shipment and storage. A field reagent blank 
prepared from reagent water and carried through the sampling and 
handling protocol can serve as a check on such contamination.
    3.3 Contamination by carry-over can occur whenever high level and 
low level samples are sequentially analyzed. To reduce carry-over, the 
purging device and sample syringe must be rinsed with reagent water 
between sample analyses. Whenever an unusually concentrated sample is 
encountered, it should be followed by an analysis of reagent water to 
check for cross contamination. For samples containing large amounts of 
water-soluble materials, suspended solids, high boiling compounds or 
high organohalide levels, it may be necessary to wash out the purging 
device with a detergent solution, rinse it with distilled water, and 
then dry it in a 105 [deg]C oven between analyses. The trap and other 
parts of the system are also subject to contamination; therefore, 
frequent bakeout and purging of the entire system may be required.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \4 6\ for 
the information of the analyst.
    4.2 The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: carbon tetrachloride, chloroform, 1,4-dichlorobenzene, and 
vinyl chloride. Primary standards of these toxic compounds should be 
prepared in a hood. A NIOSH/MESA approved toxic gas respirator should be 
worn when the analyst handles high concentrations of these toxic 
compounds.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete sampling.
    5.1.1 Vial--25-mL capacity or larger, equipped with a screw cap with 
a hole in the center (Pierce 13075 or equivalent). Detergent wash, 
rinse with tap and distilled water, and dry at 105 [deg]C before use.
    5.1.2 Septum--Teflon-faced silicone (Pierce 12722 or equivalent). 
Detergent wash, rinse with tap and distilled water, and dry at 105 
[deg]C for 1 h before use.
    5.2 Purge and trap system--The purge and trap system consists of 
three separate pieces of equipment: a purging device, trap, and 
desorber. Several complete systems are now commercially available.
    5.2.1 The purging device must be designed to accept 5-mL samples 
with a water column at least 3 cm deep. The gaseous head space between 
the water column and the trap must have a total volume of less than 15 
mL. The

[[Page 78]]

purge gas must pass through the water column as finely divided bubbles 
with a diameter of less than 3 mm at the origin. The purge gas must be 
introduced no more than 5 mm from the base of the water column. The 
purging device illustrated in Figure 1 meets these design criteria.
    5.2.2 The trap must be at least 25 cm long and have an inside 
diameter of at least 0.105 in. The trap must be packed to contain the 
following minimum lengths of adsorbents: 1.0 cm of methyl silicone 
coated packing (Section 6.3.3), 7.7 cm of 2,6-diphenylene oxide polymer 
(Section 6.3.2), 7.7 cm of silica gel (Section 6.3.4), 7.7 cm of coconut 
charcoal (Section 6.3.1). If it is not necessary to analyze for 
dichlorodifluoromethane, the charcoal can be eliminated, and the polymer 
section lengthened to 15 cm. The minimum specifications for the trap are 
illustrated in Figure 2.
    5.2.3 The desorber must be capable of rapidly heating the trap to 
180 [deg]C. The polymer section of the trap should not be heated higher 
than 180 [deg]C and the remaining sections should not exceed 200 [deg]C. 
The desorber illustrated in Figure 2 meets these design criteria.
    5.2.4 The purge and trap system may be assembled as a separate unit 
or be coupled to a gas chromatograph as illustrated in Figures 3 and 4.
    5.3 Gas chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph suitable for on-column 
injection and all required accessories including syringes, analytical 
columns, gases, detector, and strip-chart recorder. A data system is 
recommended for measuring peak areas.
    5.3.1 Column 1--8 ft long x 0.1 in. ID stainless steel or glass, 
packed with 1% SP-1000 on Carbopack B (60/80 mesh) or equivalent. This 
column was used to develop the method performance statements in Section 
12. Guidelines for the use of alternate column packings are provided in 
Section 10.1.
    5.3.2 Column 2--6 ft long x 0.1 in. ID stainless steel or glass, 
packed with chemically bonded n-octane on Porasil-C (100/120 mesh) or 
equivalent.
    5.3.3 Detector--Electrolytic conductivity or microcoulometric 
detector. These types of detectors have proven effective in the analysis 
of wastewaters for the parameters listed in the scope (Section 1.1). The 
electrolytic conductivity detector was used to develop the method 
performance statements in Section 12. Guidelines for the use of 
alternate detectors are provided in Section 10.1.
    5.4 Syringes--5-mL glass hypodermic with Luerlok tip (two each), if 
applicable to the purging device.
    5.5 Micro syringes--25-[micro]L, 0.006 in. ID needle.
    5.6 Syringe valve--2-way, with Luer ends (three each).
    5.7 Syringe--5-mL, gas-tight with shut-off valve.
    5.8 Bottle--15-mL, screw-cap, with Teflon cap liner.
    5.9 Balance--Analytical, capable of accurately weighing 0.0001 g.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.1.1 Reagent water can be generated by passing tap water through a 
carbon filter bed containing about 1 lb of activated carbon (Filtrasorb-
300, Calgon Corp., or equivalent).
    6.1.2 A water purification system (Millipore Super-Q or equivalent) 
may be used to generate reagent water.
    6.1.3 Reagent water may also be prepared by boiling water for 15 
min. Subsequently, while maintaining the temperature at 90 [deg]C, 
bubble a contaminant-free inert gas through the water for 1 h. While 
still hot, transfer the water to a narrow mouth screw-cap bottle and 
seal with a Teflon-lined septum and cap.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Trap Materials:
    6.3.1 Coconut charcoal--6/10 mesh sieved to 26 mesh, Barnabey 
Cheney, CA-580-26 lot  M-2649 or equivalent.
    6.3.2 2,6-Diphenylene oxide polymer--Tenax, (60/80 mesh), 
chromatographic grade or equivalent.
    6.3.3 Methyl silicone packing--3% OV-1 on Chromosorb-W (60/80 mesh) 
or equivalent.
    6.3.4 Silica gel--35/60 mesh, Davison, grade-15 or equivalent.
    6.4 Methanol--Pesticide quality or equivalent.
    6.5 Stock standard solutions--Stock standard solutions may be 
prepared from pure standard materials or purchased as certified 
solutions. Prepare stock standard solutions in methanol using assayed 
liquids or gases as appropriate. Because of the toxicity of some of the 
organohalides, primary dilutions of these materials should be prepared 
in a hood. A NIOSH/MESA approved toxic gas respirator should be used 
when the analyst handles high concentrations of such materials.
    6.5.1 Place about 9.8 mL of methanol into a 10-mL ground glass 
stoppered volumetric flask. Allow the flask to stand, unstoppered, for 
about 10 min or until all alcohol wetted surfaces have dried. Weigh the 
flask to the learest 0.1 mg.
    6.5.2 Add the assayed reference material:
    6.5.2.1 Liquid--Using a 100 [micro]L syringe, immediately add two or 
more drops of assayed reference material to the flask, then reweigh. Be 
sure that the drops fall directly into the alcohol without contacting 
the neck of the flask.

[[Page 79]]

    6.5.2.2 Gases--To prepare standards for any of the six halocarbons 
that boil below 30 [deg]C (bromomethane, chloroethane, chloromethane, 
dichlorodifluoromethane, trichlorofluoromethane, vinyl chloride), fill a 
5-mL valved gas-tight syringe with the reference standard to the 5.0-mL 
mark. Lower the needle to 5 mm above the methanol meniscus. Slowly 
introduce the reference standard above the surface of the liquid (the 
heavy gas will rapidly dissolve into the methanol).
    6.5.3 Reweigh, dilute to volume, stopper, then mix by inverting the 
flask several times. Calculate the concentration in [micro]g/[micro]L 
from the net gain in weight. When compound purity is assayed to be 96% 
or greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
malufacturer or by an independent source.
    6.5.4 Transfer the stock standard solution into a Teflon-sealed 
screw-cap bottle. Store, with minimal headspace, at -10 to -20 [deg]C 
and protect from light.
    6.5.5 Prepare fresh standards weekly for the six gases and 2-
chloroethylvinyl ether. All other standards must be replaced after one 
month, or sooner if comparison with check standards indicates a problem.
    6.6 Secondary dilution standards--Using stock standard solutions, 
prepare secondary dilution standards in methanol that contain the 
compounds of interest, either singly or mixed together. The secondary 
dilution standards should be prepared at concentrations such that the 
aqueous calibration standards prepared in Section 7.3.1 or 7.4.1 will 
bracket the working range of the analytical system. Secondary dilution 
standards should be stored with minimal headspace and should be checked 
frequently for signs of degradation or evaporation, especially just 
prior to preparing calibration standards from them.
    6.7 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Assemble a purge and trap system that meets the specifications 
in Section 5.2. Condition the trap overnight at 180 [deg]C by 
backflushing with an inert gas flow of at least 20 mL/min. Condition the 
trap for 10 min once daily prior to use.
    7.2 Connect the purge and trap system to a gas chromatograph. The 
gas chromatograph must be operated using temperature and flow rate 
conditions equivalent to those given in Table 1. Calibrate the purge and 
trap-gas chromatographic system using either the external standard 
technique (Section 7.3) or the internal standard technique (Section 
7.4).
    7.3 External standard calibration procedure:
    7.3.1 Prepare calibration standards at a miminum of three 
concentration levels for each parameter by carefully adding 20.0 
[micro]L of one or more secondary dilution standards to 100, 500, or 
1000 [micro]L of reagent water. A 25-[micro]L syringe with a 0.006 in. 
ID needle should be used for this operation. One of the external 
standards should be at a concentration near, but above, the MDL (Table 
1) and the other concentrations should correspond to the expected range 
of concentrations found in real samples or should define the working 
range of the detector. These aqueous standards can be stored up to 24 h, 
if held in sealed vials with zero headspace as described in Section 9.2. 
If not so stored, they must be discarded after 1 h.
    7.3.2 Analyze each calibration standard according to Section 10, and 
tabulate peak height or area responses versus the concentration in the 
standard. The results can be used to prepare a calibration curve for 
each compound. Alternatively, if the ratio of response to concentration 
(calibration factor) is a constant over the working range (<10% relative 
standard deviation, RSD), linearity through the origin can be assumed 
and the average ratio or calibration factor can be used in place of a 
calibration curve.
    7.4 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples. The compounds recommended for use as surrogate spikes in 
Section 8.7 have been used successfully as internal standards, because 
of their generally unique retention times.
    7.4.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest as described in 
Section 7.3.1.
    7.4.2 Prepare a spiking solution containing each of the internal 
standards using the procedures described in Sections 6.5 and 6.6. It is 
recommended that the secondary dilution standard be prepared at a 
concentration of 15 [micro]g/mL of each internal standard compound. The 
addition of 10 [micro]L of this standard to 5.0 mL of sample or 
calibration standard would be equivalent to 30 [micro]g/L.
    7.4.3 Analyze each calibration standard according to Section 10, 
adding 10 [micro]L of internal standard spiking solution directly to the 
syringe (Section 10.4). Tabulate peak height or area responses against 
concentration for each compound and internal standard, and calculate 
response factors (RF) for each compound using Equation 1.

[[Page 80]]

[GRAPHIC] [TIFF OMITTED] TC15NO91.094

                                                              Equation 1
where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard.
Cs = Concentration of the parameter to be measured.

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.5 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of a QC check sample.
    7.5.1 Prepare the QC check sample as described in Section 8.2.2.
    7.5.2 Analyze the QC check sample according to Section 10.
    7.5.3 For each parameter, compare the response (Q) with the 
corresponding calibration acceptance criteria found in Table 2. If the 
responses for all parameters of interest fall within the designated 
ranges, analysis of actual samples can begin. If any individual Q falls 
outside the range, proceed according to Section 7.5.4.
    Note: The large number of parameters in Table 2 present a 
substantial probability that one or more will not meet the calibration 
acceptance criteria when all parameters are analyzed.
    7.5.4 Repeat the test only for those parameters that failed to meet 
the calibration acceptance criteria. If the response for a parameter 
does not fall within the range in this second test, a new calibration 
curve, calibration factor, or RF must be prepared for that parameter 
according to Section 7.3 or 7.4.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Section 10.1) to improve the separations or lower the cost of 
measurements. Each time such a modification is made to the method, the 
analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Each day, the analyst must analyze a reagent water blank to 
demonstrate that interferences from the analytical system are under 
control.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 10 [micro]g/
mL in methanol. The QC check sample concentrate must be obtained from 
the U.S. Environmental Protection Agency, Environmental Monitoring and 
Support Laboratory in Cincinnati, Ohio, if available. If not available 
from that source, the QC check sample concentrate must be obtained from 
another external source. If not available from either source above, the 
QC check sample concentrate must be prepared by the laboratory using 
stock standards prepared independently from those used for calibration.
    8.2.2 Prepare a QC check sample to contain 20 [micro]g/L of each 
parameter by adding 200 [micro]L of QC check sample concentrate to 100 
mL of reagent water.
    8.2.3 Analyze four 5-mL aliquots of the well-mixed QC check sample 
according to Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
of interest using the four results.

[[Page 81]]

    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, then the system 
performance is unacceptable for that parameter.
    Note: The large number of parameters in Table 2 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when all parameters are analyzed.
    8.2.6 When one or more of the parameters tested fail at least one of 
the acceptance criteria, the analyst must proceed according to Section 
8.2.6.1 or 8.2.6.2.
    8.2.6.1 Locate and correct the source of the problem and repeat the 
test for all parameters of interest beginning with Section 8.2.3.
    8.2.6.2 Beginning with Section 8.2.3, repeat the test only for those 
parameters that failed to meet criteria. Repeated failure, however, will 
confirm a general problem with the measurement system. If this occurs, 
locate and correct the source of the problem and repeat the test for all 
compounds of interest beginning with Section 8.2.3.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 20 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.2 Analyze one 5-mL sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second 5-mL sample aliquot with 10 
[micro]L of the QC check sample concentrate and analyze it to determine 
the concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than 20 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 2, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 3, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T)2.44(100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory. If the entire list of parameters in Table 2 must be measured 
in the sample in Section 8.3, the probability that the analysis of a QC 
check standard will be required is high. In this case the QC check 
standard should be routinely analyzed with the spiked sample.
    8.4.1 Prepare the QC check standard by adding 10 [micro]L of QC 
check sample concentrate (Section 8.2.1 or 8.3.2) to 5 mL of reagent 
water. The QC check standard needs only to contain the parameters that 
failed criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the

[[Page 82]]

unspiked sample is suspect and may not be reported for regulatory 
compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If p = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.
    8.7 The analyst should monitor both the performance of the 
analytical system and the effectiveness of the method in dealing with 
each sample matrix by spiking each sample, standard, and reagent water 
blank with surrogate halocarbons. A combination of bromochloromethane, 
2-bromo-1-chloropropane, and 1,4-dichlorobutane is recommended to 
encompass the range of the temperature program used in this method. From 
stock standard solutions prepared as in Section 6.5, add a volume to 
give 750 [micro]g of each surrogate to 45 mL of reagent water contained 
in a 50-mL volumetric flask, mix and dilute to volume for a 
concentration of 15 ng/[micro]L. Add 10 [micro]L of this surrogate 
spiking solution directly into the 5-mL syringe with every sample and 
reference standard analyzed. Prepare a fresh surrogate spiking solution 
on a weekly basis. If the internal standard calibration procedure is 
being used, the surrogate compounds may be added directly to the 
internal standard spiking solution (Section 7.4.2).

            9. Sample Collection, Preservation, and Handling

    9.1 All samples must be iced or refrigerated from the time of 
collection until analysis. If the sample contains free or combined 
chlorine, add sodium thiosulfate preservative (10 mg/40 mL is sufficient 
for up to 5 ppm Cl2) to the empty sample bottle just prior to 
shipping to the sampling site. EPA Methods 330.4 and 330.5 may be used 
for measurement of residual chlorine. \8\ Field test kits are available 
for this purpose.
    9.2 Grab samples must be collected in glass containers having a 
total volume of at least 25 mL. Fill the sample bottle just to 
overflowing in such a manner that no air bubbles pass through the sample 
as the bottle is being filled. Seal the bottle so that no air bubbles 
are entrapped in it. If preservative has been added, shake vigorously 
for 1 min. Maintain the hermetic seal on the sample bottle until time of 
analysis.
    9.3 All samples must be analyzed within 14 days of collection. \3\

                              10. Procedure

    10.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are estimated retention times 
and MDL that can be achieved under these conditions. An example of the 
separations achieved by Column 1 is shown in Figure 5. Other packed 
columns, chromatographic conditions, or detectors may be used if the 
requirements of Section 8.2 are met.
    10.2 Calibrate the system daily as described in Section 7.
    10.3 Adjust the purge gas (nitrogen or helium) flow rate to 40 mL/
min. Attach the trap inlet to the purging device, and set the purge and 
trap system to purge (Figure 3). Open the syringe valve located on the 
purging device sample introduction needle.
    10.4 Allow the sample to come to ambient temperature prior to 
introducing it to the syringe. Remove the plunger from a 5-mL syringe 
and attach a closed syringe valve. Open the sample bottle (or standard) 
and carefully pour the sample into the syringe barrel to just short of 
overflowing. Replace the syringe plunger and compress the sample. Open 
the syringe valve and vent any residual air while adjusting the sample 
volume to 5.0 mL. Since this process of taking an aliquot destroys the 
validity of the sample for future analysis, the analyst should fill a 
second syringe at this time to protect against possible loss of data. 
Add 10.0 [micro]L of the surrogate spiking solution (Section 8.7) and 
10.0 [micro]L of the internal standard spiking solution (Section 7.4.2), 
if applicable, through the valve bore, then close the valve.
    10.5 Attach the syringe-syringe valve assembly to the syringe valve 
on the purging device. Open the syringe valves and inject the sample 
into the purging chamber.
    10.6 Close both valves and purge the sample for 11.0 0.1 min at ambient temperature.
    10.7 After the 11-min purge time, attach the trap to the 
chromatograph, adjust the purge and trap system to the desorb mode 
(Figure 4), and begin to temperature program the gas chromatograph. 
Introduce the trapped materials to the GC column by rapidly heating the 
trap to 180 [deg]C while

[[Page 83]]

backflushing the trap with an inert gas between 20 and 60 mL/min for 4 
min. If rapid heating of the trap cannot be achieved, the GC column must 
be used as a secondary trap by cooling it to 30 [deg]C (subambient 
temperature, if poor peak geometry or random retention time problems 
persist) instead of the initial program temperature of 45 [deg]C
    10.8 While the trap is being desorbed into the gas chromatograph, 
empty the purging chamber using the sample introduction syringe. Wash 
the chamber with two 5-mL flushes of reagent water.
    10.9 After desorbing the sample for 4 min, recondition the trap by 
returning the purge and trap system to the purge mode. Wait 15 s then 
close the syringe valve on the purging device to begin gas flow through 
the trap. The trap temperature should be maintained at 180 [deg]C After 
approximately 7 min, turn off the trap heater and open the syringe valve 
to stop the gas flow through the trap. When the trap is cool, the next 
sample can be analyzed.
    10.10 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    10.11 If the response for a peak exceeds the working range of the 
system, prepare a dilution of the sample with reagent water from the 
aliquot in the second syringe and reanalyze.

                            11. Calculations

    11.1 Determine the concentration of individual compounds in the 
sample.
    11.1.1 If the external standard calibration procedure is used, 
calculate the concentration of the parameter being measured from the 
peak response using the calibration curve or calibration factor 
determined in Section 7.3.2.
    11.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.4.3 and Equation 2.
                                                              Equation 2
[GRAPHIC] [TIFF OMITTED] TC15NO91.095

where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard.

    11.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         12. Method Performance

    12.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentration 
listed in Table 1 were obtained using reagent water. \11\. Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.

    12.2 This method is recommended for use in the concentration range 
from the MDL to 1000 x MDL. Direct aqueous injection techniques should 
be used to measure concentration levels above 1000 x MDL.
    12.3 This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 8.0 to 500 [micro]g/L. \9\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. Bellar, T.A., and Lichtenberg, J.J. ``Determining Volatile 
Organics at Microgram-per-Litre-Levels by Gas Chromatography,'' Journal 
of the American Water Works Association, 66, 739 (1974).
    3. Bellar, T.A., and Lichtenberg, J.J. ``Semi-Automated Headspace 
Analysis of Drinking Waters and Industrial Waters for Purgeable Volatile 
Organic Compounds,'' Proceedings from Symposium on Measurement of 
Organic Pollutants in Water and Wastewater, American Society for Testing 
and Materials, STP 686, C.E. Van Hall, editor, 1978.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).

[[Page 84]]

    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    8. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA 600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    9. ``EPA Method Study 24, Method 601--Purgeable Halocarbons by the 
Purge and Trap Method,'' EPA 600/4-84-064, National Technical 
Information Service, PB84-212448, Springfield, Virginia 22161, July 
1984.
    10. ``Method Validation Data for EPA Method 601,'' Memorandum from 
B. Potter, U.S. Environmental Protection Agency, Environmental 
Monitoring and Support Laboratory, Cincinnati, Ohio 45268, November 10, 
1983.
    11. Bellar, T. A., Unpublished data, U.S. Environmental Protection 
Agency, Environmental Monitoring and Support Laboratory, Cincinnati, 
Ohio 45268, 1981.

                         Table 1--Chromatographic Conditions and Method Detection Limits
----------------------------------------------------------------------------------------------------------------
                                                                   Retention time (min)         Method detection
                         Parameter                         ------------------------------------ limit ([micro]g/
                                                                Column 1          Column 2             L)
----------------------------------------------------------------------------------------------------------------
Chloromethane.............................................         1.50              5.28              0.08
Bromomethane..............................................         2.17              7.05              1.18
Dichlorodifluoromethane...................................         2.62             nd                 1.81
Vinyl chloride............................................         2.67              5.28              0.18
Chloroethane..............................................         3.33              8.68              0.52
Methylene chloride........................................         5.25             10.1               0.25
Trichlorofluoromethane....................................         7.18             nd                nd
1,1-Dichloroethene........................................         7.93              7.72              0.13
1,1-Dichloroethane........................................         9.30             12.6               0.07
trans-1,2-Dichloroethene..................................        10.1               9.38              0.10
Chloroform................................................        10.7              12.1               0.05
1,2-Dichloroethane........................................        11.4              15.4               0.03
1,1,1-Trichloroethane.....................................        12.6              13.1               0.03
Carbon tetrachloride......................................        13.0              14.4               0.12
Bromodichloromethane......................................        13.7              14.6               0.10
1,2-Dichloropropane.......................................        14.9              16.6               0.04
cis-1,3-Dichloropropene...................................        15.2              16.6               0.34
Trichloroethene...........................................        15.8              13.1               0.12
Dibromochloromethane......................................        16.5              16.6               0.09
1,1,2-Trichloroethane.....................................        16.5              18.1               0.02
trans-1,3-Dichloropropene.................................        16.5              18.0               0.20
2-Chloroethylvinyl ether..................................        18.0              nd                 0.13
Bromoform.................................................        19.2              19.2               0.20
1,1,2,2-Tetrachloroethane.................................        21.6              nd                 0.03
Tetrachloroethene.........................................        21.7              15.0               0.03
Chlorobenzene.............................................        24.2              18.8               0.25
1,3-Dichlorobenzene.......................................        34.0              22.4               0.32
1,2-Dichlorobenzene.......................................        34.9              23.5               0.15
1,4-Dichlorobenzene.......................................        35.4              22.3               0.24
----------------------------------------------------------------------------------------------------------------
Column 1 conditions: Carbopack B (60/80 mesh) coated with 1% SP-1000 packed in an 8 ft x 0.1 in. ID stainless
  steel or glass column with helium carrier gas at 40 mL/min flow rate. Column temperature held at 45 [deg]C for
  3 min then programmed at 8 [deg]C/min to 220 [deg]C and held for 15 min.
Column 2 conditions: Porisil-C (100/120 mesh) coated with n-octane packed in a 6 ft x 0.1 in. ID stainless steel
  or glass column with helium carrier gas at 40 mL/min flow rate. Column temperature held at 50 [deg]C for 3 min
  then programmed at 6 [deg]C/min to 170 [deg]C and held for 4 min.
nd = not determined.


                         Table 2--Calibration and QC Acceptance Criteria--Method 601 \a\
----------------------------------------------------------------------------------------------------------------
                                                                           Limit for
                                                            Range for Q        s        Range for X    Range P,
                        Parameter                          ([micro]g/L)   ([micro]g/   ([micro]g/L)     Ps (%)
                                                                              L)
----------------------------------------------------------------------------------------------------------------
Bromodichloromethane....................................       15.2-24.8         4.3       10.7-32.0      42-172
Bromoform...............................................       14.7-25.3         4.7        5.0-29.3      13-159
Bromomethane............................................       11.7-28.3         7.6        3.4-24.5       D-144
Carbon tetrachloride....................................       13.7-26.3         5.6       11.8-25.3      43-143
Chlorobenzene...........................................       14.4-25.6         5.0       10.2-27.4      38-150
Chloroethane............................................       15.4-24.6         4.4       11.3-25.2      46-137
2-Chloroethylvinyl ether................................       12.0-28.0         8.3        4.5-35.5      14-186
Chloroform..............................................       15.0-25.0         4.5       12.4-24.0      49-133
Chloromethane...........................................       11.9-28.1         7.4          D-34.9       D-193

[[Page 85]]

 
Dibromochloromethane....................................       13.1-26.9         6.3        7.9-35.1      24-191
1,2-Dichlorobenzene.....................................       14.0-26.0         5.5        1.7-38.9       D-208
1,3-Dichlorobenzene.....................................        9.9-30.1         9.1        6.2-32.6       7-187
1,4-Dichlorobenzene.....................................       13.9-26.1         5.5       11.5-25.5      42-143
1,1-Dichloroethane......................................       16.8-23.2         3.2       11.2-24.6      47-132
1,2-Dichloroethane......................................       14.3-25.7         5.2       13.0-26.5      51-147
1,1-Dichloroethene......................................       12.6-27.4         6.6       10.2-27.3      28-167
trans-1,2-Dichloroethene................................       12.8-27.2         6.4       11.4-27.1      38-155
1,2-Dichloropropane.....................................       14.8-25.2         5.2       10.1-29.9      44-156
cis-1,3-Dichloropropene.................................       12.8-27.2         7.3        6.2-33.8      22-178
trans-1,3-Dichloropropene...............................       12.8-27.2         7.3        6.2-33.8      22-178
Methylene chloride......................................       15.5-24.5         4.0        7.0-27.6      25-162
1,1,2,2-Tetrachloroethane...............................        9.8-30.2         9.2        6.6-31.8       8-184
Tetrachloroethene.......................................       14.0-26.0         5.4        8.1-29.6      26-162
1,1,1-Trichloroethane...................................       14.2-25.8         4.9       10.8-24.8      41-138
1,1,2-Trichloroethane...................................       15.7-24.3         3.9        9.6-25.4      39-136
Trichloroethene.........................................       15.4-24.6         4.2        9.2-26.6      35-146
Trichlorofluoromethane..................................       13.3-26.7         6.0        7.4-28.1      21-156
Vinyl chloride..........................................       13.7-26.3         5.7        8.2-29.9      28-163
----------------------------------------------------------------------------------------------------------------
\a\ Criteria were calculated assuming a QC check sample concentration of 20 [micro]g/L.
Q = Concentration measured in QC check sample, in [micro]g/L (Section 7.5.3).
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 601
----------------------------------------------------------------------------------------------------------------
                                                                     Single analyst
              Parameter                Accuracy, as recovery,        precision, sr'       Overall precision, S'
                                           X' ([micro]g/L)            ([micro]g/L)             ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Bromodichloromethane................  1.12C-1.02                0.11X + 0.04             0.20X + 1.00
Bromoform...........................  0.96C-2.05                0.12X + 0.58             0.21X + 2.41
Bromomethane........................  0.76C-1.27                0.28X + 0.27             0.36X + 0.94
Carbon tetrachloride................  0.98C-1.04                0.15X + 0.38             0.20X + 0.39
Chlorobenzene.......................  1.00C-1.23                0.15X-0.02               0.18X + 1.21
Choroethane.........................  0.99C-1.53                0.14X-0.13               0.17X + 0.63
2-Chloroethylvinyl ether \a\........  1.00C                     0.20X                    0.35X
Chloroform..........................  0.93C-0.39                0.13X + 0.15             0.19X-0.02
Chloromethane.......................  0.77C + 0.18              0.28X-0.31               0.52X + 1.31
Dibromochloromethane................  0.94C + 2.72              0.11X + 1.10             0.24X + 1.68
1,2-Dichlorobenzene.................  0.93C + 1.70              0.20X + 0.97             0.13X + 6.13
1,3-Dichlorobenzene.................  0.95C + 0.43              0.14X + 2.33             0.26X + 2.34
1,4-Dichlorobenzene.................  0.93C-0.09                0.15X + 0.29             0.20X + 0.41
1,1-Dichloroethane..................  0.95C-1.08                0.09X + 0.17             0.14X + 0.94
1,2-Dichloroethane..................  1.04C-1.06                0.11X + 0.70             0.15X + 0.94
1,1-Dichloroethene..................  0.98C-0.87                0.21X-0.23               0.29X-0.40
trans-1,2-Dichloroethene............  0.97C-0.16                0.11X + 1.46             0.17X + 1.46
1,2-Dichloropropane \a\.............  1.00C                     0.13X                    0.23X
cis-1,3-Dichloropropene \a\.........  1.00C                     0.18X                    0.32X
trans-1,3-Dichloropropene \a\.......  1.00C                     0.18X                    0.32X
Methylene chloride..................  0.91C-0.93                0.11X + 0.33             0.21X + 1.43
1,1,2,2-Tetrachloroethene...........  0.95C + 0.19              0.14X + 2.41             0.23X + 2.79
Tetrachloroethene...................  0.94C + 0.06              0.14X + 0.38             0.18X + 2.21
1,1,1-Trichloroethane...............  0.90C-0.16                0.15X + 0.04             0.20X + 0.37
1,1,2-Trichloroethane...............  0.86C + 0.30              0.13X-0.14               0.19X + 0.67
Trichloroethene.....................  0.87C + 0.48              0.13X-0.03               0.23X + 0.30
Trichlorofluoromethane..............  0.89C-0.07                0.15X + 0.67             0.26X + 0.91
Vinyl chloride......................  0.97C-0.36                0.13X + 0.65             0.27X + 0.40
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sn' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S\1\ = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.
\a\ Estimates based upon the performance in a single laboratory. \10\


[[Page 86]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.000


[[Page 87]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.001


[[Page 88]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.002


[[Page 89]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.003


[[Page 90]]

                     Method 602--Purgeable Aromatics

                        1. Scope and Application

    1.1 This method covers the determination of various purgeable 
aromatics. The following parameters may be determined by this method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
Benzene..........................................     34030      71-43-2
Chlorobenzene....................................     34301     108-90-7
1,2-Dichlorobenzene..............................     34536      95-50-1
1,3-Dichlorobenzene..............................     34566     541-73-1
1,4-Dichlorobenzene..............................     34571     106-46-7
Ethylbenzene.....................................     34371     100-41-4
Toluene..........................................     34010     108-88-3
------------------------------------------------------------------------

    1.2 This is a purge and trap gas chromatographic (GC) method 
applicable to the determination of the compounds listed above in 
municipal and industrial discharges as provided under 40 CFR 136.1. When 
this method is used to analyze unfamiliar samples for any or all of the 
compounds above, compound identifications should be supported by at 
least one additional qualitative technique. This method describes 
analytical conditions for a second gas chromatographic column that can 
be used to confirm measurements made with the primary column. Method 624 
provides gas chromatograph/mass spectrometer (GC/MS) conditions 
appropriate for the qualitative and quantitative confirmation of results 
for all of the parameters listed above.
    1.3 The method detection limit (MDL, defined in Section 12.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the operation of a purge and trap system and a 
gas chromatograph and in the interpretation of gas chromatograms. Each 
analyst must demonstrate the ability to generate acceptable results with 
this method using the procedure described in Section 8.2.

                          2. Summary of Method

    2.1 An inert gas is bubbled through a 5-mL water sample contained in 
a specially-designed purging chamber at ambient temperature. The 
aromatics are efficiently transferred from the aqueous phase to the 
vapor phase. The vapor is swept through a sorbent trap where the 
aromatics are trapped. After purging is completed, the trap is heated 
and backflushed with the inert gas to desorb the aromatics onto a gas 
chromatographic column. The gas chromatograph is temperature programmed 
to separate the aromatics which are then detected with a photoionization 
detector. \2 3\
    2.2 The method provides an optional gas chromatographic column that 
may be helpful in resolving the compounds of interest from interferences 
that may occur.

                            3. Interferences

    3.1 Impurities in the purge gas and organic compounds outgassing 
from the plumbing ahead of the trap account for the majority of 
contamination problems. The analytical system must be demonstrated to be 
free from contamination under the conditions of the analysis by running 
laboratory reagent blanks as described in Section 8.1.3. The use of non-
Teflon plastic tubing, non-Teflon thread sealants, or flow controllers 
with rubber components in the purge and trap system should be avoided.
    3.2 Samples can be contaminated by diffusion of volatile organics 
through the septum seal into the sample during shipment and storage. A 
field reagent blank prepared from reagent water and carried through the 
sampling and handling protocol can serve as a check on such 
contamination.
    3.3 Contamination by carry-over can occur whenever high level and 
low level samples are sequentially analyzed. To reduce carry-over, the 
purging device and sample syringe must be rinsed with reagent water 
between sample analyses. Whenever an unusually concentrated sample is 
encountered, it should be followed by an analysis of reagent water to 
check for cross contamination. For samples containing large amounts of 
water-soluble materials, suspended solids, high boiling compounds or 
high aromatic levels, it may be necessary to wash the purging device 
with a detergent solution, rinse it with distilled water, and then dry 
it in an oven at 105 [deg]C between analyses. The trap and other parts 
of the system are also subject to contamination; therefore, frequent 
bakeout and purging of the entire system may be required.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety

[[Page 91]]

are available and have been identified 4 6 for the 
information of the analyst.
    4.2 The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: benzene and 1,4-dichlorobenzene. Primary standards of these 
toxic compounds should be prepared in a hood. A NIOSH/MESA approved 
toxic gas respirator should be worn when the analyst handles high 
concentrations of these toxic compounds.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete sampling.
    5.1.1 Vial]25-mL capacity or larger, equipped with a screw cap with 
a hole in the center (Pierce 13075 or equivalent). Detergent wash, 
rinse with tap and distilled water, and dry at 105 [deg]C before use.
    5.1.2 Septum--Teflon-faced silicone (Pierce 12722 or equivalent). 
Detergent wash, rinse with tap and distilled water, and dry at 105 
[deg]C for 1 h before use.
    5.2 Purge and trap system--The purge and trap system consists of 
three separate pieces of equipment: A purging device, trap, and 
desorber. Several complete systems are now commercially available.
    5.2.1 The purging device must be designed to accept 5-mL samples 
with a water column at least 3 cm deep. The gaseous head space between 
the water column and the trap must have a total volume of less than 15 
mL. The purge gas must pass through the water column as finely divided 
bubbles with a diameter of less than 3 mm at the origin. The purge gas 
must be introduced no more than 5 mm from the base of the water column. 
The purging device illustrated in Figure 1 meets these design criteria.
    5.2.2 The trap must be at least 25 cm long and have an inside 
diameter of at least 0.105 in.
    5.2.2.1 The trap is packed with 1 cm of methyl silicone coated 
packing (Section 6.4.2) and 23 cm of 2,6-diphenylene oxide polymer 
(Section 6.4.1) as shown in Figure 2. This trap was used to develop the 
method performance statements in Section 12.
    5.2.2.2 Alternatively, either of the two traps described in Method 
601 may be used, although water vapor will preclude the measurement of 
low concentrations of benzene.
    5.2.3 The desorber must be capable of rapidly heating the trap to 
180 [deg]C. The polymer section of the trap should not be heated higher 
than 180 [deg]C and the remaining sections should not exceed 200 [deg]C. 
The desorber illustrated in Figure 2 meets these design criteria.
    5.2.4 The purge and trap system may be assembled as a separate unit 
or be coupled to a gas chromatograph as illustrated in Figures 3, 4, and 
5.
    5.3 Gas chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph suitable for on-column 
injection and all required accessories including syringes, analytical 
columns, gases, detector, and strip-chart recorder. A data system is 
recommended for measuring peak areas.
    5.3.1 Column 1--6 ft long x 0.082 in. ID stainless steel or glass, 
packed with 5% SP-1200 and 1.75% Bentone-34 on Supelcoport (100/120 
mesh) or equivalent. This column was used to develop the method 
performance statements in Section 12. Guidelines for the use of 
alternate column packings are provided in Section 10.1.
    5.3.2 Column 2--8 ft long x 0.1 in ID stainless steel or glass, 
packed with 5% 1,2,3-Tris(2-cyanoethoxy)propane on Chromosorb W-AW (60/
80 mesh) or equivalent.
    5.3.3 Detector--Photoionization detector (h-Nu Systems, Inc. Model 
PI-51-02 or equivalent). This type of detector has been proven effective 
in the analysis of wastewaters for the parameters listed in the scope 
(Section 1.1), and was used to develop the method performance statements 
in Section 12. Guidelines for the use of alternate detectors are 
provided in Section 10.1.
    5.4 Syringes--5-mL glass hypodermic with Luerlok tip (two each), if 
applicable to the purging device.
    5.5 Micro syringes--25-[micro]L, 0.006 in. ID needle.
    5.6 Syringe valve--2-way, with Luer ends (three each).
    5.7 Bottle--15-mL, screw-cap, with Teflon cap liner.
    5.8 Balance--Analytical, capable of accurately weighing 0.0001 g.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.1.1 Reagent water can be generated by passing tap water through a 
carbon filter bed containing about 1 lb of activated carbon (Filtrasorb-
300, Calgon Corp., or equivalent).
    6.1.2 A water purification system (Millipore Super-Q or equivalent) 
may be used to generate reagent water.
    6.1.3 Reagent water may also be prepared by boiling water for 15 
min. Subsequently, while maintaining the temperature at 90 [deg]C, 
bubble a contaminant-free inert gas through the water for 1 h. While 
still hot, transfer the water to a narrow mouth screw-cap bottle and 
seal with a Teflon-lined septum and cap.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Hydrochloric acid (1 + 1)--Add 50 mL of concentrated HCl (ACS) 
to 50 mL of reagent water.
    6.4 Trap Materials:

[[Page 92]]

    6.4.1 2,6-Diphenylene oxide polymer--Tenax, (60/80 mesh), 
chromatographic grade or equivalent.
    6.4.2 Methyl silicone packing--3% OV-1 on Chromosorb-W (60/80 mesh) 
or equivalent.
    6.5 Methanol--Pesticide quality or equivalent.
    6.6 Stock standard solutions--Stock standard solutions may be 
prepared from pure standard materials or purchased as certified 
solutions. Prepare stock standard solutions in methanol using assayed 
liquids. Because of the toxicity of benzene and 1,4-dichlorobenzene, 
primary dilutions of these materials should be prepared in a hood. A 
NIOSH/MESA approved toxic gas respirator should be used when the analyst 
handles high concentrations of such materials.
    6.6.1 Place about 9.8 mL of methanol into a 10-mL ground glass 
stoppered volumetric flask. Allow the flask to stand, unstoppered, for 
about 10 min or until all alcohol wetted surfaces have dried. Weigh the 
flask to the nearest 0.1 mg.
    6.6.2 Using a 100-[micro]L syringe, immediately add two or more 
drops of assayed reference material to the flask, then reweigh. Be sure 
that the drops fall directly into the alcohol without contacting the 
neck of the flask.
    6.6.3 Reweigh, dilute to volume, stopper, then mix by inverting the 
flask several times. Calculate the concentration in [micro]g/[micro]L 
from the net gain in weight. When compound purity is assayed to be 96% 
or greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.6.4 Transfer the stock standard solution into a Teflon-sealed 
screw-cap bottle. Store at 4 [deg]C and protect from light.
    6.6.5 All standards must be replaced after one month, or sooner if 
comparison with check standards indicates a problem.
    6.7 Secondary dilution standards--Using stock standard solutions, 
prepare secondary dilution standards in methanol that contain the 
compounds of interest, either singly or mixed together. The secondary 
dilution standards should be prepared at concentrations such that the 
aqueous calibration standards prepared in Section 7.3.1 or 7.4.1 will 
bracket the working range of the analytical system. Secondary solution 
standards must be stored with zero headspace and should be checked 
frequently for signs of degradation or evaporation, especially just 
prior to preparing calibration standards from them.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Assemble a purge and trap system that meets the specifications 
in Section 5.2. Condition the trap overnight at 180 [deg]C by 
backflushing with an inert gas flow of at least 20 mL/min. Condition the 
trap for 10 min once daily prior to use.
    7.2 Connect the purge and trap system to a gas chromatograph. The 
gas chromatograph must be operated using temperature and flow rate 
conditions equivalent to those given in Table 1. Calibrate the purge and 
trap-gas chromatographic system using either the external standard 
technique (Section 7.3) or the internal standard technique (Section 
7.4).
    7.3 External standard calibration procedure:
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter by carefully adding 20.0 
[micro]L of one or more secondary dilution standards to 100, 500, or 
1000 mL of reagent water. A 25-[micro]L syringe with a 0.006 in. ID 
needle should be used for this operation. One of the external standards 
should be at a concentration near, but above, the MDL (Table 1) and the 
other concentrations should correspond to the expected range of 
concentrations found in real samples or should define the working range 
of the detector. These aqueous standards must be prepared fresh daily.
    7.3.2 Analyze each calibration standard according to Section 10, and 
tabulate peak height or area responses versus the concentration in the 
standard. The results can be used to prepare a calibration curve for 
each compound. Alternatively, if the ratio of response to concentration 
(calibration factor) is a constant over the working range (<10% relative 
standard deviation, RSD), linearity through the origin can be assumed 
and the average ratio or calibration factor can be used in place of a 
calibration curve.
    7.4 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples. The compound, [alpha],[alpha],[alpha],-trifluorotoluene, 
recommended as a surrogate spiking compound in Section 8.7 has been used 
successfully as an internal standard.
    7.4.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest as described in 
Section 7.3.1.
    7.4.2 Prepare a spiking solution containing each of the internal 
standards using the procedures described in Sections 6.6 and 6.7. It is 
recommended that the secondary dilution standard be prepared at a 
concentration of 15 [micro]g/mL of each internal standard compound. The 
addition of 10 [micro]l of this

[[Page 93]]

standard to 5.0 mL of sample or calibration standard would be equivalent 
to 30 [micro]g/L.
    7.4.3 Analyze each calibration standard according to Section 10, 
adding 10 [micro]L of internal standard spiking solution directly to the 
syringe (Section 10.4). Tabulate peak height or area responses against 
concentration for each compound and internal standard, and calculate 
response factors (RF) for each compound using Equation 1.

RF = (As)(Cis (Ais)(Cs)

Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard
Cs = Concentration of the parameter to be measured.

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.5 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of a QC check sample.
    7.5.1 Prepare the QC check sample as described in Section 8.2.2.
    7.5.2 Analyze the QC check sample according to Section 10.
    7.5.3 For each parameter, compare the response (Q) with the 
corresponding calibration acceptance criteria found in Table 2. If the 
responses for all parameters of interest fall within the designated 
ranges, analysis of actual samples can begin. If any individual Q falls 
outside the range, a new calibration curve, calibration factor, or RF 
must be prepared for that parameter according to Section 7.3 or 7.4.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Section 10.1) to improve the separations or lower the cost of 
measurements. Each time such a modification is made to the method, the 
analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Each day, the analyst must analyze a reagent water blank to 
demonstrate that interferences from the analytical system are under 
control.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 10 [micro]g/
mL in methanol. The QC check sample concentrate must be obtained from 
the U.S. Environmental Protection Agency, Environmental Monitoring and 
Support Laboratory in Cincinnati, Ohio, if available. If not available 
from that source, the QC check sample concentrate must be obtained from 
another external source. If not available from either source above, the 
QC check sample concentrate must be prepared by the laboratory using 
stock standards prepared independently from those used for calibration.
    8.2.2 Prepare a QC check sample to contain 20 [micro]g/L of each 
parameter by adding 200 [micro]L of QC check sample concentrate to 100 
mL of reagant water.
    8.2.3 Analyze four 5-mL aliquots of the well-mixed QC check sample 
according to Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
of interest using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively,

[[Page 94]]

found in Table 2. If s and X for all parameters of interest meet the 
acceptance criteria, the system performance is acceptable and analysis 
of actual samples can begin. If any individual s exceeds the precision 
limit or any individual X falls outside the range for accuracy, the 
system performance is unacceptable for that parameter.
    Note: The large number of parameters in Table 2 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when all parameters are analyzed.
    8.2.6 When one or more of the parameters tested fail at least one of 
the acceptance criteria, the analyst must proceed according to Section 
8.2.6.1 or 8.2.6.2.
    8.2.6.1 Locate and correct the source of the problem and repeat the 
test for all parameters of interest beginning with Section 8.2.3.
    8.2.6.2 Beginning with Section 8.2.3, repeat the test only for those 
parameters that failed to meet criteria. Repeated failure, however, will 
confirm a general problem with the measurement system. If this occurs, 
locate and correct the source of the problem and repeat the test for all 
compounds of interest beginning with Section 8.2.3.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 20 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.2 Analyze one 5-mL sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second 5-mL sample aliquot with 10 
[micro]L of the QC check sample concentrate and analyze it to determine 
the concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than 20 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 2, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 3, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T) 2.44(100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 10 [micro]L of QC 
check sample concentrate (Section 8.2.1 or 8.3.2) to 5 mL of reagent 
water. The QC check standard needs only to contain the parameters that 
failed criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P)

[[Page 95]]

and the standard deviation of the percent recovery (sp). 
Express the accuracy assessment as a percent recovery interval from P-
2sp to P + 2sp. If P = 90% and sp = 
10%, for example, the accuracy interval is expressed as 70-110%. Update 
the accuracy assessment for each parameter on a regular basis (e.g. 
after each five to ten new accuracy measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.
    8.7 The analyst should monitor both the performance of the 
analytical system and the effectiveness of the method in dealing with 
each sample matrix by spiking each sample, standard, and reagent water 
blank with surrogate compounds (e.g. [alpha], [alpha], [alpha],-
trifluorotoluene) that encompass the range of the temperature program 
used in this method. From stock standard solutions prepared as in 
Section 6.6, add a volume to give 750 [micro]g of each surrogate to 45 
mL of reagent water contained in a 50-mL volumetric flask, mix and 
dilute to volume for a concentration of 15 mg/[micro]L. Add 10 [micro]L 
of this surrogate spiking solution directly into the 5-mL syringe with 
every sample and reference standard analyzed. Prepare a fresh surrogate 
spiking solution on a weekly basis. If the internal standard calibration 
procedure is being used, the surrogate compounds may be added directly 
to the internal standard spiking solution (Section 7.4.2).

            9. Sample Collection, Preservation, and Handling

    9.1 The samples must be iced or refrigerated from the time of 
collection until analysis. If the sample contains free or combined 
chlorine, add sodium thiosulfate preservative (10 mg/40 mL is sufficient 
for up to 5 ppm Cl2) to the empty sample bottle just prior to 
shipping to the sampling site. EPA Method 330.4 or 330.5 may be used for 
measurement of residual chlorine. \8\ Field test kits are available for 
this purpose.
    9.2 Collect about 500 mL of sample in a clean container. Adjust the 
pH of the sample to about 2 by adding 1 + 1 HCl while stirring. Fill the 
sample bottle in such a manner that no air bubbles pass through the 
sample as the bottle is being filled. Seal the bottle so that no air 
bubbles are entrapped in it. Maintain the hermetic seal on the sample 
bottle until time of analysis.
    9.3 All samples must be analyzed within 14 days of collection. \3\

                              10. Procedure

    10.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are estimated retention times 
and MDL that can be achieved under these conditions. An example of the 
separations achieved by Column 1 is shown in Figure 6. Other packed 
columns, chromatographic conditions, or detectors may be used if the 
requirements of Section 8.2 are met.
    10.2 Calibrate the system daily as described in Section 7.
    10.3 Adjust the purge gas (nitrogen or helium) flow rate to 40 mL/
min. Attach the trap inlet to the purging device, and set the purge and 
trap system to purge (Figure 3). Open the syringe valve located on the 
purging device sample introduction needle.
    10.4 Allow the sample to come to ambient temperature prior to 
introducing it to the syringe. Remove the plunger from a 5-mL syringe 
and attach a closed syringe valve. Open the sample bottle (or standard) 
and carefully pour the sample into the syringe barrel to just short of 
overflowing. Replace the syringe plunger and compress the sample. Open 
the syringe valve and vent any residual air while adjusting the sample 
volume to 5.0 mL. Since this process of taking an aliquot destroys the 
validity of the sample for future analysis, the analyst should fill a 
second syringe at this time to protect against possible loss of data. 
Add 10.0 [micro]L of the surrogate spiking solution (Section 8.7) and 
10.0 [micro]L of the internal standard spiking solution (Section 7.4.2), 
if applicable, through the valve bore, then close the valve.
    10.5 Attach the syringe-syringe valve assembly to the syringe valve 
on the purging device. Open the syringe valves and inject the sample 
into the purging chamber.
    10.6 Close both valves and purge the sample for 12.0 0.1 min at ambient temperature.
    10.7 After the 12-min purge time, disconnect the purging device from 
the trap. Dry the trap by maintaining a flow of 40 mL/min of dry purge 
gas through it for 6 min (Figure 4). If the purging device has no 
provision for bypassing the purger for this step, a dry purger should be 
inserted into the device to minimize moisture in the gas. Attach the 
trap to the chromatograph, adjust the purge and trap system to the 
desorb mode (Figure 5), and begin to temperature program the gas 
chromatograph. Introduce the trapped materials to the GC column by 
rapidly heating the trap to 180 [deg]C while backflushing the trap with 
an inert gas between 20 and 60 mL/min for 4 min. If rapid heating of the 
trap cannot be achieved, the GC column must be used as

[[Page 96]]

a secondary trap by cooling it to 30 [deg]C (subambient temperature, if 
poor peak geometry and random retention time problems persist) instead 
of the initial program temperature of 50 [deg]C.
    10.8 While the trap is being desorbed into the gas chromatograph 
column, empty the purging chamber using the sample introduction syringe. 
Wash the chamber with two 5-mL flushes of reagent water.
    10.9 After desorbing the sample for 4 min, recondition the trap by 
returning the purge and trap system to the purge mode. Wait 15 s, then 
close the syringe valve on the purging device to begin gas flow through 
the trap. The trap temperature should be maintained at 180 [deg]C. After 
approximately 7 min, turn off the trap heater and open the syringe valve 
to stop the gas flow through the trap. When the trap is cool, the next 
sample can be analyzed.
    10.10 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    10.11 If the response for a peak exceeds the working range of the 
system, prepare a dilution of the sample with reagent water from the 
aliquot in the second syringe and reanalyze.

                            11. Calculations

    11.1 Determine the concentration of individual compounds in the 
sample.
    11.1.1 If the external standard calibration procedure is used, 
calculate the concentration of the parameter being measured from the 
peak response using the calibration curve or calibration factor 
determined in Section 7.3.2.
    11.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.4.3 and Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.096

    Equation 2
where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard.

    11.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         12. Method Performance

    12.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \9\ Similar results 
were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    12.2 This method has been demonstrated to be applicable for the 
concentration range from the MDL to 100 x MDL. \9\ Direct aqueous 
injection techniques should be used to measure concentration levels 
above 1000 x MDL.
    12.3 This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 2.1 to 550 [micro]g/L. \9\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. Lichtenberg, J.J. ``Determining Volatile Organics at Microgram-
per-Litre-Levels by Gas Chromatography,'' Journal American Water Works 
Association, 66, 739 (1974).
    3. Bellar, T.A., and Lichtenberg, J.J. ``Semi-Automated Headspace 
Analysis of Drinking Waters and Industrial Waters for Purgeable Volatile 
Organic Compounds,'' Proceedings of Symposium on Measurement of Organic 
Pollutants in Water and Wastewater. American Society for Testing and 
Materials, STP 686, C.E. Van Hall, editor, 1978.
    4. ``Carcinogens--Working with Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health. 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3. is two times the value 1.22 
derived in this report.)

[[Page 97]]

    8.``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Office of Research and Development, 
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio 45268. 
March 1979.
    9. ``EPA Method Study 25, Method 602, Purgeable Aromatics,'' EPA 
600/4-84-042, National Technical Information Service, PB84-196682, 
Springfield, Virginia 22161, May 1984.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                        Retention time (min)    Method
                                       ----------------------  detection
               Parameter                                         limit
                                         Column 1   Column 2  ([micro]g/
                                                                  L)
------------------------------------------------------------------------
Benzene...............................       3.33       2.75        0.2
Toluene...............................       5.75       4.25        0.2
Ethylbenzene..........................       8.25       6.25        0.2
Chlorobenzene.........................       9.17       8.02        0.2
1,4-Dichlorobenzene...................      16.8       16.2         0.3
1,3-Dichlorobenzene...................      18.2       15.0         0.4
1,2-Dichlorobenzene...................      25.9       19.4         0.4
------------------------------------------------------------------------
Column 1 conditions: Supelcoport (100/120 mesh) coated with 5% SP-1200/
  1.75% Bentone-34 packed in a 6 ft x 0.085 in. ID stainless steel
  column with helium carrier gas at 36 mL/min flow rate. Column
  temperature held at 50 [deg]C for 2 min then programmed at 6 [deg]C/
  min to 90 [deg]C for a final hold.
Column 2 conditions: Chromosorb W-AW (60/80 mesh) coated with 5% 1,2,3-
  Tris(2-cyanoethyoxy)propane packed in a 6 ft x 0.085 in. ID stainless
  steel column with helium carrier gas at 30 mL/min flow rate. Column
  temperature held at 40 [deg]C for 2 min then programmed at 2 [deg]C/
  min to 100 [deg]C for a final hold.


                         Table 2--Calibration and QC Acceptance Criteria--Method 602 \a\
----------------------------------------------------------------------------------------------------------------
                                                                               Limit for
                                                                 Range for Q       s      Range for X  Range for
                           Parameter                              ([micro]g/  ([micro]g/   ([micro]g/   P, Ps(%)
                                                                      L)          L)           L)
----------------------------------------------------------------------------------------------------------------
Benzene........................................................    15.4-24.6        4.1     10.0-27.9     39-150
Chlorobenzene..................................................    16.1-23.9        3.5     12.7-25.4     55-135
1,2-Dichlorobenzene............................................    13.6-26.4        5.8     10.6-27.6     37-154
1,3-Dichlorobenzene............................................    14.5-25.5        5.0     12.8-25.5     50-141
1,4-Dichlorobenzene............................................    13.9-26.1        5.5     11.6-25.5     42-143
Ethylbenzene...................................................    12.6-27.4        6.7     10.0-28.2     32-160
Toluene........................................................    15.5-24.5        4.0     11.2-27.7     46-148
----------------------------------------------------------------------------------------------------------------
Q = Concentration measured in QC check sample, in [micro]g/L (Section 7.5.3).
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
Ps, P = Percent recovery measured (Section 8.3.2, Section 8.4.2).
\a\ Criteria were calculated assuming a QC check sample concentration of 20 [micro]g/L.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 602
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                              recovery, X'    precision, s'   precision, S'
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Benzene.........................................................    0.92C + 0.57    0.09X + 0.59    0.21X + 0.56
Chlorobenzene...................................................    0.95C + 0.02    0.09X + 0.23    0.17X + 0.10
1,2-Dichlorobenzene.............................................    0.93C + 0.52      0.17X-0.04    0.22X + 0.53
1,3-Dichlorobenzene.............................................      0.96C-0.05      0.15X-0.10    0.19X + 0.09
1,4-Dichlorobenzene.............................................      0.93C-0.09    0.15X + 0.28    0.20X + 0.41
Ethylbenzene....................................................    0.94C + 0.31    0.17X + 0.46    0.26X + 0.23
Toluene.........................................................    0.94C + 0.65    0.09X + 0.48    0.18X + 0.71
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
S' = Expected single analyst standard deviation of measurements at an average concentration found of X, in X
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the Concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


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                 Method 603--Acrolein and Acrylonitrile

                        1. Scope and Application

    1.1 This method covers the determination of acrolein and 
acrylonitrile. The following parameters may be determined by this 
method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
Acrolein.........................................     34210     107-02-8
Acrylonitrile....................................     34215     107-13-1
------------------------------------------------------------------------
 

    1.2 This is a purge and trap gas chromatographic (GC) method 
applicable to the determination of the compounds listed above in 
municipal and industrial discharges as provided under 40 CFR 136.1. When 
this method is used to analyze unfamiliar samples for either or both of 
the compounds above, compound identifications should be supported by at 
least one additional qualitative technique. This method describes 
analytical conditions for a second gas chromatographic column that can 
be used to confirm measurements made with the primary column. Method 624 
provides gas chromatograph/mass spectrometer (GC/MS) conditions 
appropriate for the qualitative and quantitative confirmation of results 
for the parameters listed above, if used with the purge and trap 
conditions described in this method.
    1.3 The method detection limit (MDL, defined in Section 12.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the operation of a purge and trap system and a 
gas chromatograph and in the interpretation of gas chromatograms. Each 
analyst must demonstrate the ability to generate acceptable results with 
this method using the procedure described in Section 8.2.

                          2. Summary of Method

    2.1 An inert gas is bubbled through a 5-mL water sample contained in 
a heated purging chamber. Acrolein and acrylonitrile are transferred 
from the aqueous phase to the vapor phase. The vapor is swept through a 
sorbent trap where the analytes are trapped. After the purge is 
completed, the trap is heated and backflushed with the inert gas to 
desorb the compound onto a gas chromatographic column. The gas 
chromatograph is temperature programmed to separate the analytes which 
are then detected with a flame ionization detector. \2 3\
    2.2 The method provides an optional gas chromatographic column that 
may be helpful in resolving the compounds of interest from the 
interferences that may occur.

                            3. Interferences

    3.1 Impurities in the purge gas and organic compound outgassing from 
the plumbing of the trap account for the majority of contamination 
problems. The analytical system must be demonstrated to be free from 
contamination under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3. The use of non-Teflon 
plastic tubing, non-Teflon thread sealants, or flow controllers with 
rubber components in the purge and trap system should be avoided.
    3.2 Samples can be contaminated by diffusion of volatile organics 
through the septum seal into the sample during shipment and storage. A 
field reagent blank prepared from reagent water and carried through the 
sampling and handling protocol can serve as a check on such 
contamination.
    3.3 Contamination by carry-over can occur whenever high level and 
low level samples are sequentially analyzed. To reduce carry-over, the 
purging device and sample syringe must be rinsed between samples with 
reagent water. Whenever an unusually concentrated sample is encountered, 
it should be followed by an analysis of reagent water to check for cross 
contamination. For samples containing large amounts of water-soluble 
materials, suspended solids, high boiling compounds or high analyte 
levels, it may be necessary to wash the purging device with a detergent 
solution, rinse it with distilled water, and then dry it in an oven at 
105 [deg]C between analyses. The trap and other parts of the system are 
also subject to contamination, therefore, frequent bakeout and purging 
of the entire system may be required.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this view point, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified 
4 6 for the information of the analyst.

[[Page 103]]

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete sampling.
    5.1.1 Vial--25-mL capacity or larger, equipped with a screw cap with 
a hole in the center (Pierce 13075 or equivalent). Detergent wash, 
rinse with tap and distilled water, and dry at 105 [deg]C before use.
    5.1.2 Septum--Teflon-faced silicone (Pierce 12722 or equivalent). 
Detergent wash, rinse with tap and distilled water and dry at 105 [deg]C 
for 1 h before use.
    5.2 Purge and trap system--The purge and trap system consists of 
three separate pieces of equipment: a purging device, trap, and 
desorber. Several complete systems are now commercially available.
    5.2.1 The purging device must be designed to accept 5-mL, samples 
with a water column at least 3 cm deep. The gaseous head space between 
the water column and the trap must have a total volume of less than 15 
mL. The purge gas must pass through the water column as finely divided 
bubbles with a diameter of less than 3 mm at the origin. The purge gas 
must be introduced no more than 5 mm from the base of the water column. 
The purging device must be capable of being heated to 85 [deg]C within 
3.0 min after transfer of the sample to the purging device and being 
held at 85 2 [deg]C during the purge cycle. The 
entire water column in the purging device must be heated. Design of this 
modification to the standard purging device is optional, however, use of 
a water bath is suggested.
    5.2.1.1 Heating mantle--To be used to heat water bath.
    5.2.1.2 Temperature controller--Equipped with thermocouple/sensor to 
accurately control water bath temperature to 2 
[deg]C. The purging device illustrated in Figure 1 meets these design 
criteria.
    5.2.2 The trap must be at least 25 cm long and have an inside 
diameter of at least 0.105 in. The trap must be packed to contain 1.0 cm 
of methyl silicone coated packing (Section 6.5.2) and 23 cm of 2,6-
diphenylene oxide polymer (Section 6.5.1). The minimum specifications 
for the trap are illustrated in Figure 2.
    5.2.3 The desorber must be capable of rapidly heating the trap to 
180 [deg]C, The desorber illustrated in Figure 2 meets these design 
criteria.
    5.2.4 The purge and trap system may be assembled as a separate unit 
as illustrated in Figure 3 or be coupled to a gas chromatograph.
    5.3 pH paper--Narrow pH range, about 3.5 to 5.5 (Fisher Scientific 
Short Range Alkacid No. 2, 14-837-2 or equivalent).
    5.4 Gas chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph suitable for on-column 
injection and all required accessories including syringes, analytical 
columns, gases, detector, and strip-chart recorder. A data system is 
recommended for measuring peak areas.
    5.4.1 Column 1--10 ft long x 2 mm ID glass or stainless steel, 
packed with Porapak-QS (80/100 mesh) or equivalent. This column was used 
to develop the method performance statements in Section 12. Guidelines 
for the use of alternate column packings are provided in Section 10.1.
    5.4.2 Column 2--6 ft long x 0.1 in. ID glass or stainless steel, 
packed with Chromosorb 101 (60/80 mesh) or equivalent.
    5.4.3 Detector--Flame ionization detector. This type of detector has 
proven effective in the analysis of wastewaters for the parameters 
listed in the scope (Section 1.1), and was used to develop the method 
performance statements in Section 12. Guidelines for the use of 
alternate detectors are provided in Section 10.1.
    5.5 Syringes--5-mL, glass hypodermic with Luerlok tip (two each).
    5.6 Micro syringes--25-[micro]L, 0.006 in. ID needle.
    5.7 Syringe valve--2-way, with Luer ends (three each).
    5.8 Bottle--15-mL, screw-cap, with Teflon cap liner.
    5.9 Balance--Analytical, capable of accurately weighing 0.0001 g.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.1.1 Reagent water can be generated by passing tap water through a 
carbon filter bed containing about 1 lb of activated carbon (Filtrasorb-
300, Calgon Corp., or equivalent).
    6.1.2 A water purification system (Millipore Super-Q or equivalent) 
may be used to generate reagent water.
    6.1.3 Regent water may also be prepared by boiling water for 15 min. 
Subsequently, while maintaining the temperature at 90 [deg]C, bubble a 
contaminant-free inert gas through the water for 1 h. While still hot, 
transfer the water to a narrow mouth screw-cap bottle and seal with a 
Teflon-lined septum and cap.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.4 Hydrochloric acid (1 + 1)--Slowly, add 50 mL of concentrated HCl 
(ACS) to 50 mL of reagent water.
    6.5 Trap Materials:
    6.5.1 2,6-Diphenylene oxide polymer--Tenax (60/80 mesh), 
chromatographic grade or equivalent.
    6.5.2 Methyl silicone packing--3% OV-1 on Chromosorb-W (60/80 mesh) 
or equivalent.

[[Page 104]]

    6.6 Stock standard solutions--Stock standard solutions may be 
prepared from pure standard materials or purchased as certified 
solutions. Prepare stock standard solutions in reagent water using 
assayed liquids. Since acrolein and acrylonitrile are lachrymators, 
primary dilutions of these compounds should be prepared in a hood. A 
NIOSH/MESA approved toxic gas respirator should be used when the analyst 
handles high concentrations of such materials.
    6.6.1 Place about 9.8 mL of reagent water into a 10-mL ground glass 
stoppered volumetric flask. For acrolein standards the reagent water 
must be adjusted to pH 4 to 5. Weight the flask to the nearest 0.1 mg.
    6.6.2 Using a 100-[micro]L syringe, immediately add two or more 
drops of assayed reference material to the flask, then reweigh. Be sure 
that the drops fall directly into the water without contacting the neck 
of the flask.
    6.6.3 Reweigh, dilute to volume, stopper, then mix by inverting the 
flask several times. Calculate the concentration in [micro]g/[micro]L 
from the net gain in weight. When compound purity is assayed to be 96% 
or greater, the weight can be used without correction to calculate the 
concentration of the stock staldard. Optionally, stock standard 
solutions may be prepared using the pure standard material by 
volumetrically measuring the appropriate amounts and determining the 
weight of the material using the density of the material. Commercially 
prepared stock standards may be used at any concentration if they are 
certified by the manufactaurer or by an independent source.
    6.6.4 Transfer the stock standard solution into a Teflon-sealed 
screw-cap bottle. Store at 4 [deg]C and protect from light.
    6.6.5 Prepare fresh standards daily.
    6.7 Secondary dilution standards--Using stock standard solutions, 
prepare secondary dilution standards in reagent water that contain the 
compounds of interest, either singly or mixed together. The secondary 
dilution standards should be prepared at concentrations such that the 
aqueous calibration standards prepared in Section 7.3.1 or 7.4.1 will 
bracket the working range of the analytical system. Secondary dilution 
standards should be prepared daily and stored at 4 [deg]C.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Assemble a purge and trap system that meets the specifications 
in Section 5.2. Condition the trap overnight at 180 [deg]C by 
backflushing with an inert gas flow of at least 20 mL/min. Condition the 
trap for 10 min once daily prior to use.
    7.2 Connect the purge and trap system to a gas chromatograph. The 
gas chromatograph must be operated using temperature and flow rate 
conditions equivalent to those given in Table 1. Calibrate the purge and 
trap-gas chromatographic system using either the external standard 
technique (Section 7.3) or the internal standard technique (Section 
7.4).
    7.3 External standard calibration procedure:
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter by carefully adding 20.0 
[micro]L of one or more secondary dilution standards to 100, 500, or 
1000 mL of reagent water. A 25-[micro]L syringe with a 0.006 in. ID 
needle should be used for this operation. One of the external standards 
should be at a concentration near, but above, the MDL and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector. These standards must be prepared fresh daily.
    7.3.2 Analyze each calibration standard according to Section 10, and 
tabulate peak height or area responses versus the concentration of the 
standard. The results can be used to prepare a calibration curve for 
each compound. Alternatively, if the ratio of response to concentration 
(calibration factor) is a constant over the working range (<10% relative 
standard deviation, RSD), linearity through the origin can be assumed 
and the average ratio or calibration factor can be used in place of a 
calibration curve.
    7.4 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.4.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest as described in 
Section 7.3.1.
    7.4.2 Prepare a spiking solution containing each of the internal 
standards using the procedures described in Sections 6.6 and 6.7. It is 
recommended that the secondary dilution standard be prepared at a 
concentration of 15 [micro]g/mL of each internal standard compound. The 
addition of 10 [micro]L of this standard to 5.0 mL of sample or 
calibration standard would be equivalent to 30 [micro]g/L.
    7.4.3 Analyze each calibration standard according to Section 10, 
adding 10 [micro]L of internal standard spiking solution directly to the 
syringe (Section 10.4). Tabulate peak height or area responses against 
concentration for each compound and internal standard, and calculate 
response factors (RF) for each compound using Equation 1.

   RF = (As)(Cis (Ais)(Cs)

                                                              Equation 1


[[Page 105]]


where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard.
Cs = Concentration of the parameter to be measured.

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.5 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of a QC check sample.
    7.5.1 Prepare the QC check sample as described in Section 8.2.2.
    7.5.2 Analyze the QC check sample according to Section 10.
    7.5.3 For each parameter, compare the response (Q) with the 
corresponding calibration acceptance criteria found in Table 2. If the 
responses for all parameters of interest fall within the designated 
ranges, analysis of actual samples can begin. If any individual Q falls 
outside the range, a new calibration curve, calibration factor, or RF 
must be prepared for that parameter according to Section 7.3 or 7.4.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Section 10.1) to improve the separations or lower the cost of 
measurements. Each time such a modification is made to the method, the 
analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Each day, the analyst must analyze a reagent water blank to 
demonstrate that interferences from the analytical system are under 
control.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 25 [micro]g/
mL in reagent water. The QC check sample concentrate must be obtained 
from the U.S. Environmental Protection Agency, Environmental Monitoring 
and Support Laboratory in Cincinnati, Ohio, if available. If not 
available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Prepare a QC check sample to contain 50 [micro]g/L of each 
parameter by adding 200 [micro]L of QC check sample concentrate to 100 
mL of reagent water.
    8.2.3 Analyze four 5-mL aliquots of the well-mixed QC check sample 
according to Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 3. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If either s exceeds the precision limit or X falls 
outside the range for accuracy, the system performance is unacceptable 
for that parameter. Locate and correct the source of the problem and 
repeat the test for each compound of interest.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to

[[Page 106]]

ten samples per month, at least one spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 50 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.2 Analyze one 5-mL sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second 5-mL sample aliquot with 10 
[micro]L of the QC check sample concentrate and analyze it to determine 
the concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 3. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 10 [micro]L of QC 
check sample concentrate (Section 8.2.1 or 8.3.2) to 5 mL of reagent 
water. The QC check standard needs only to contain the parameters that 
failed criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
3. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column or mass spectrometer 
must be used. Whenever possible, the laboratory should analyze standard 
reference materials and participate in relevant performance evaluation 
studies.

            9. Sample Collection, Preservation, and Handling

    9.1 All samples must be iced or refrigerated from the time of 
collection until analysis. If the sample contains free or combined 
chlorine, add sodium thiosulfate preservative (10 mg/40 mL is sufficient 
for up to 5 ppm Cl2) to the empty sample bottle just prior to 
shipping to the sampling site. EPA Methods 330.4 and 330.5 may be used 
for measurement of residual chlorine. \8\ Field test kits are available 
for this purpose.
    9.2 If acrolein is to be analyzed, collect about 500 mL of sample in 
a clean glass container. Adjust the pH of the sample to 4 to 5 using 
acid or base, measuring with narrow range pH paper. Samples for acrolein 
analysis receiving no pH adjustment must be analyzed within 3 days of 
sampling.

[[Page 107]]

    9.3 Grab samples must be collected in glass containers having a 
total volume of at least 25 mL. Fill the sample bottle just to 
overflowing in such a manner that no air bubbles pass through the sample 
as the bottle is being filled. Seal the bottle so that no air bubbles 
are entrapped in it. If preservative has been added, shake vigorously 
for 1 min. Maintain the hermetic seal on the sample bottle until time of 
analysis.
    9.4 All samples must be analyzed within 14 days of collection. \3\

                              10. Procedure

    10.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are estimated retention times 
and MDL that can be achieved under these conditions. An example of the 
separations achieved by Column 1 is shown in Figure 5. Other packed 
columns, chromatographic conditions, or detectors may be used if the 
requirements of Section 8.2 are met.
    10.2 Calibrate the system daily as described in Section 7.
    10.3 Adjust the purge gas (nitrogen or helium) flow rate to 20 mL-
min. Attach the trap inlet to the purging device, and set the purge and 
trap system to purge (Figure 3). Open the syringe valve located on the 
purging device sample introduction needle.
    10.4 Remove the plunger from a 5-mL syringe and attach a closed 
syringe valve. Open the sample bottle (or standard) and carefully pour 
the sample into the syringe barrel to just short of overflowing. Replace 
the syringe plunger and compress the sample. Open the syringe valve and 
vent any residual air while adjusting the sample volume to 5.0 mL. Since 
this process of taking an aliquot destroys the validity of the sample 
for future analysis, the analyst should fill a second syringe at this 
time to protect against possible loss of data. Add 10.0 [micro]L of the 
internal standard spiking solution (Section 7.4.2), if applicable, 
through the valve bore then close the valve.
    10.5 Attach the syringe-syringe valve assembly to the syringe valve 
on the purging device. Open the syringe valves and inject the sample 
into the purging chamber.
    10.6 Close both valves and purge the sample for 15.0 0.1 min while heating at 85 2 
[deg]C.
    10.7 After the 15-min purge time, attach the trap to the 
chromatograph, adjust the purge and trap system to the desorb mode 
(Figure 4), and begin to temperature program the gas chromatograph. 
Introduce the trapped materials to the GC column by rapidly heating the 
trap to 180 [deg]C while backflushing the trap with an inert gas between 
20 and 60 mL/min for 1.5 min.
    10.8 While the trap is being desorbed into the gas chromatograph, 
empty the purging chamber using the sample introduction syringe. Wash 
the chamber with two 5-mL flushes of reagent water.
    10.9 After desorbing the sample for 1.5 min, recondition the trap by 
returning the purge and trap system to the purge mode. Wait 15 s then 
close the syringe valve on the purging device to begin gas flow through 
the trap. The trap temperature should be maintained at 210 [deg]C. After 
approximately 7 min, turn off the trap heater and open the syringe valve 
to stop the gas flow through the trap. When the trap is cool, the next 
sample can be analyzed.
    10.10 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.

                            11. Calculations

    11.1 Determine the concentration of individual compounds in the 
sample.
    11.1.1 If the external standard calibration procedure is used, 
calculate the concentration of the parameter being measured from the 
peak response using the calibration curve or calibration factor 
determined in Section 7.3.2.
    11.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.4.3 and Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.097

                                                              Equation 2

where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard.

    11.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         12. Method Performance

    12.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \9\

[[Page 108]]

The MDL actually achieved in a given analysis will vary depending on 
instrument sensitivity and matrix effects.
    12.2 This method is recommended for the concentration range from the 
MDL to 1,000 x MDL. Direct aqueous injection techniques should be used 
to measure concentration levels above 1,000 x MDL.
    12.3 In a single laboratory (Battelle-Columbus), the average 
recoveries and standard deviations presented in Table 2 were obtained. 
\9\ Seven replicate samples were analyzed at each spike level.

                               References

    1. 40 CFR part 136, appendix B.
    2. Bellar, T.A., and Lichtenberg, J.J. ``Determining Volatile 
Organics at Microgram-per-Litre-Levels by Gas Chromatography,'' Journal 
American Water Works Association, 66, 739 (1974).
    3. ``Evaluate Test Procedures for Acrolein and Acrylonitrile,'' 
Special letter report for EPA Project 4719-A, U.S. Environmental 
Protection Agency, Environmental Monitoring and Support Laboratory, 
Cincinnati, Ohio 45268, 27 June 1979.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983).
    8. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    9. ``Evaluation of Method 603 (Modified),'' EPA-600/4-84-ABC, 
National Technical Information Service, PB84-, Springfield, Virginia 
22161, Nov. 1984.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                       Retention time (min)     Method
                                     ------------------------  detection
              Parameter                                          limit
                                       Column 1    Column 2   ([micro]g/
                                                                  L)
------------------------------------------------------------------------
Acrolein............................     10.6         8.2         0.7
Acrylonitrile.......................     12.7         9.8         0.5
------------------------------------------------------------------------
Column 1 conditions: Porapak-QS (80/100 mesh) packed in a 10 ft x 2 mm
  ID glass or stainless steel column with helium carrier gas at 30 mL/
  min flow rate. Column temperature held isothermal at 110 [deg]C for
  1.5 min (during desorption), then heated as rapidly as possible to 150
  [deg]C and held for 20 min; column bakeout at 190 [deg]C for 10 min.
  \9\
Column 2 conditions: Chromosorb 101 (60/80 mesh) packed in a 6 ft. x 0.1
  in. ID glass or stainless steel column with helium carrier gas at 40
  mL/min flow rate. Column temperature held isothermal at 80 [deg]C for
  4 min, then programmed at 50 [deg]C/min to 120 [deg]C and held for 12
  min.


                          Table 2--Single Laboratory Accuracy and Precision--Method 603
----------------------------------------------------------------------------------------------------------------
                                                                      Spike      Average    Standard
                                                          Sample      conc.     recovery    deviation   Average
                       Parameter                          matrix   ([micro]g/  ([micro]g/  ([micro]g/   percent
                                                                       L)          L)          L)       recovery
----------------------------------------------------------------------------------------------------------------
Acrolein...............................................        RW        5.0          5.2         0.2        104
                                                               RW       50.0         51.4         0.7        103
                                                             POTW        5.0          4.0         0.2         80
                                                             POTW       50.0         44.4         0.8         89
                                                               IW        5.0          0.1         0.1          2
                                                               IW      100.0          9.3         1.1          9
Acrylonitrile..........................................        RW        5.0          4.2         0.2         84
                                                               RW       50.0         51.4         1.5        103
                                                             POTW       20.0         20.1         0.8        100
                                                             POTW      100.0        101.3         1.5        101
                                                               IW       10.0          9.1         0.8         91
                                                               IW      100.0        104.0         3.2        104
----------------------------------------------------------------------------------------------------------------
RW = Reagent water.
POTW = Prechlorination secondary effluent from a municipal sewage treatment plant.
IW = Industrial wastewater containing an unidentified acrolein reactant.


                         Table 3--Calibration and QC Acceptance Criteria--Method 603 \a\
----------------------------------------------------------------------------------------------------------------
                                                                             Limit for
                                                               Range for Q       S      Range for X   Range for
                          Parameter                             ([micro]g/  ([micro]g/   ([micro]g/   P, Ps (%)
                                                                    L)          L)           L)
----------------------------------------------------------------------------------------------------------------
Acrolein.....................................................    45.9-54.1         4.6    42.9-60.1       88-118

[[Page 109]]

 
Acrylonitrile................................................    41.2-58.8         9.9    33.1-69.9       71-135
----------------------------------------------------------------------------------------------------------------
\a\ = Criteria were calculated assuming a QC check sample concentration of 50 [micro]g/L. \9\
Q = Concentration measured in QC check sample, in [micro]g/L (Section 7.5.3).
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).

[GRAPHIC] [TIFF OMITTED] TC02JY92.008


[[Page 110]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.009


[[Page 111]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.010


[[Page 112]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.011

                           Method 604--Phenols

                        1. Scope and Application

    1.1 This method covers the determination of phenol and certain 
substituted phenols. The following parameters may be determined by this 
method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
4-Chloro-3-methylphenol..........................     34452      59-50-7
2--Chlorophenol..................................     34586      95-57-8
2,4-Dichlorophenol...............................     34601     120-83-2
2,4-Dimethylphenol...............................     34606     105-67-9
2,4-Dinitrophenol................................     34616      51-28-5
2-Methyl-4,6-dinitrophenol.......................     34657     534-52-1
2-Nitrophenol....................................     34591      88-75-5
4-Nitrophenol....................................     34646     100-02-7
Pentachlorophenol................................     39032      87-86-5
Phenol...........................................     34694     108-95-2
2,4,6-Trichlorophenol............................     34621      88-06-2
------------------------------------------------------------------------

    1.2 This is a flame ionization detector gas chromatographic (FIDGC) 
method applicable to the determination of the compounds listed above in 
municipal and industrial discharges as provided under 40 CFR 136.1. When 
this method is used to analyze unfamiliar samples for any or all of the 
compounds above, compound identifications should be supported by at 
least one additional qualitative technique. This method describes 
analytical conditions for derivatization, cleanup, and electron capture 
detector gas chromatography (ECDGC) that can be used to confirm 
measurements made by FIDGC. Method 625 provides gas chromatograph/mass 
spectrometer (GC/MS) conditions appropriate for the qualitative and 
quantitative confirmation of results for all of the parameters listed 
above, using the extract produced by this method.
    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix. The MDL listed in Table 1 for each 
parameter was achieved with a flame ionization detector (FID). The MDLs 
that were achieved when the derivatization cleanup and electron capture 
detector (ECD) were employed are presented in Table 2.

[[Page 113]]

    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is acidified and 
extracted with methylene chloride using a separatory funnel. The 
methylene chloride extract is dried and exchanged to 2-propanol during 
concentration to a volume of 10 mL or less. The extract is separated by 
gas chromatography and the phenols are then measured with an FID. \2\
    2.2 A preliminary sample wash under basic conditions can be employed 
for samples having high general organic and organic base interferences.
    2.3 The method also provides for a derivatization and column 
chromatography cleanup procedure to aid in the elimination of 
interferences. 2 3 The derivatives are analyzed by ECDGC.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \4\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are 
coextracted from the sample. The extent of matrix interferences will 
vary considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
derivatization cleanup procedure in Section 12 can be used to overcome 
many of these interferences, but unique samples may require additional 
cleanup approaches to achieve the MDL listed in Tables 1 and 2.
    3.3 The basic sample wash (Section 10.2) may cause significantly 
reduced recovery of phenol and 2,4-dimethylphenol. The analyst must 
recognize that results obtained under these conditions are minimum 
concentrations.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
mothod has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified 
5 7 for the information of analyst.
    4.2 Special care should be taken in handling pentafluorobenzyl 
bromide, which is a lachrymator, and 18-crown-6-ether, which is highly 
toxic.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be

[[Page 114]]

used. Before use, however, the compressible tubing should be thoroughly 
rinsed with methanol, followed by repeated rinsings with distilled water 
to minimize the potential for contamination of the sample. An 
integrating flow meter is required to collect flow proportional 
composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, 400 mm long x 19 mm ID, 
with coarse frit filter disc.
    5.2.3 Chromatographic column--100 mm long x 10 mm ID, with Teflon 
stopcock.
    5.2.4 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.5 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.6 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.7 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.8 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.9 Reaction flask--15 to 25-mL round bottom flask, with standard 
tapered joint, fitted with a water-cooled condenser and U-shaped drying 
tube containing granular calcium chloride.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighting 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph suitable for on-column 
injection and all required accessories including syringes, analytical 
columns, gases, detector, and strip-chart recorder. A data system is 
recommended for measuring peak areas.
    5.6.1 Column for underivatized phenols--1.8 m long x 2 mm ID glass, 
packed with 1% SP-1240DA on Supelcoport (80/100 mesh) or equivalent. 
This column was used to develop the method performance statements in 
Section 14. Guidelines for the use of alternate column packings are 
provided in Section 11.1.
    5.6.2 Column for derivatized phenols--1.8 m long x 2 mm ID glass, 
packed with 5% OV-17 on Chromosorb W-AW-DMCS (80/100 mesh) or 
equivalent. This column has proven effective in the analysis of 
wastewaters for derivatization products of the parameters listed in the 
scope (Section 1.1), and was used to develop the method performance 
statements in Section 14. Guidelines for the use of alternate column 
packings are provided in Section 11.1.
    5.6.3 Detectors--Flame ionization and electron capture detectors. 
The FID is used when determining the parent phenols. The ECD is used 
when determining the derivatized phenols. Guidelines for the use of 
alternatve detectors are provided in Section 11.1.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.3 Sodium hydroxide solution (1 N)--Dissolve 4 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.4 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.5 Sodium thiosulfate--(ACS) Granular.
    6.6 Sulfuric acid (1 + 1)--Slowly, add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.7 Sulfuric acid (1 N)--Slowly, add 58 mL of 
H2SO4 (ACS, sp. gr. 1.84) to reagent water and 
dilute to 1 L.
    6.8 Potassium carbonate--(ACS) Powdered.
    6.9 Pentafluorobenzyl bromide ([alpha]-Bromopentafluorotoluene)--97% 
minimum purity.
    Note: This chemical is a lachrymator. (See Section 4.2.)
    6.10 18-crown-6-ether (1,4,7,10,13,16-Hexaoxacyclooctadecane)--98% 
minimum purity.
    Note: This chemical is highly toxic.
    6.11 Derivatization reagent--Add 1 mL of pentafluorobenzyl bromide 
and 1 g of 18-crown-6-ether to a 50-mL volumetric flask and dilute to 
volume with 2-propanol. Prepare fresh weekly. This operation should be 
carried out in a hood. Store at 4 [deg]C and protect from light.
    6.12 Acetone, hexane, methanol, methylene chloride, 2-propanol, 
toluene--Pesticide quality or equivalent.
    6.13 Silica gel--100/200 mesh, Davison, grade-923 or equivalent. 
Activate at 130 [deg]C overnight and store in a desiccator.
    6.14 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions may be prepared from pure standard materials or 
purchased as certified solutions.
    6.14.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in 2-propanol

[[Page 115]]

and dilute to volume in a 10-mL volumetric flask. Larger volumes can be 
used at the convenience of the analyst. When compound purity is assayed 
to be 96% or greater, the weight can be used without correction to 
calculate the concentration of the stock standard. Commercially prepared 
stock standards can be used at any concentration if they are certified 
by the manufacturer or by an independent source.
    6.14.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.14.3 Stock standard solutions must be replaced after six months, 
or sooner if comparison with check standards indicates a problem.
    6.15 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 To calibrate the FIDGC for the anaylsis of underivatized 
phenols, establish gas chromatographic operating conditions equivalent 
to those given in Table 1. The gas chromatographic system can be 
calibrated using the external standard technique (Section 7.2) or the 
internal standard technique (Section 7.3).
    7.2 External standard calibration procedure for FIDGC:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with 2-propanol. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using injections of 2 to 5 [micro]l, analyze each calibration 
standard according to Section 11 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD), linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure for FIDGC--To use this 
approach, the analyst must select one or more internal standards that 
are similar in analytical behavior to the compounds of interest. The 
analyst must further demonstrate that the measurement of the internal 
standard is not affected by method or matrix interferences. Because of 
these limitations, no internal standard can be suggested that is 
applicable to all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with 2-propanol. One of the standards should be at 
a concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 11 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.

   RF = (As)(Cis (Ais)(Cs)

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).

Cs = Concentration of the parameter to be measured ([micro]g/
          L).

    If the RF value over the working range is a constant (<10% RSD), the 
RF can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 To calibrate the ECDGC for the analysis of phenol derivatives, 
establish gas chromatographic operating conditions equivalent to those 
given in Table 2.
    7.5.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with 2-propanol. One of the external standards should be at a 
concentration near, but above, the MDL (Table 2) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.

[[Page 116]]

    7.5.2 Each time samples are to be derivatized, simultaneously treat 
a 1-mL aliquot of each calibration standard as described in Section 12.
    7.5.3 After derivatization, analyze 2 to 5 [micro]L of each column 
eluate collected according to the method beginning in Section 12.8 and 
tabulate peak height or area responses against the calculated equivalent 
mass of underivatized phenol injected. The results can be used to 
prepare a calibration curve for each compound.
    7.6 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.6 and 11.1) to improve the separations or lower the cost of 
measurements. Each time such a modification is made to the method, the 
analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 100 
[micro]g/mL in 2-propanol. The QC check sample concentrate must be 
obtained from the U.S. Environmental Protection Agency, Environmental 
Monitoring and Support Laboratory in Cincinnati, Ohio, if available. If 
not available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Using a pipet, prepare QC check samples at a concentration of 
100 [micro]g/L by adding 1.00 mL of QC check sample concentrate to each 
of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 3. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter.
    Note: The large number of parameters in Talbe 3 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when all parameters are analyzed.
    8.2.6 When one or more of the parameters tested fail at least one of 
the acceptance criteria, the analyst must proceed according to Section 
8.2.6.1 or 8.2.6.2.
    8.2.6.1 Locate and correct the source of the problem and repeat the 
test for all parameters of interest beginning with Section 8.2.2.
    8.2.6.2 Beginning with Section 8.2.2, repeat the test only for those 
parameters that failed to meet criteria. Repeated failure, however, will 
confirm a general problem

[[Page 117]]

with the measurement system. If this occurs, locate and correct the 
source of the problem and repeat the test for all compounds of interest 
beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 100 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any, 
or, if none, (2) the larger of either 5 times higher than the expected 
background concentration or 100 [micro]g/L.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 3. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\8\ If spiking was performed at a concentration lower than 100 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 3, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 4, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 4, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T)2.44(100 S'/T)%. \8\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.

    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.

    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
3. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6. It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When

[[Page 118]]

doubt exists over the identification of a peak on the chromatogram, 
confirmatory techniques such as gas chromatography with a dissimilar 
column, specific element detector, or mass spectrometer must be used. 
Whenever possible, the laboratory should analyze standard reference 
materials and participate in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \9\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction. Fill the sample bottles and, if 
residual chlorine is present, add 80 mg of sodium thiosulfate per liter 
of sample and mix well. EPA Methods 330.4 and 330.5 may be used for 
measurement of residual chlorine. \10\ Field test kits are available for 
this purpose.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of sample bottle for later 
determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.
    10.2 For samples high in organic content, the analyst may solvent 
wash the sample at basic pH as prescribed in Sections 10.2.1 and 10.2.2 
to remove potential method interferences. Prolonged or exhaustive 
contact with solvent during the wash may result in low recovery of some 
of the phenols, notably phenol and 2,4-dimethylphenol. For relatively 
clean samples, the wash should be omitted and the extraction, beginning 
with Section 10.3, should be followed.
    10.2.1 Adjust the pH of the sample to 12.0 or greater with sodium 
hydroxide solution.
    10.2.2 Add 60 mL of methylene chloride to the sample by shaking the 
funnel for 1 min with periodic venting to release excess pressure. 
Discard the solvent layer. The wash can be repeated up to two additional 
times if significant color is being removed.
    10.3 Adjust the sample to a pH of 1 to 2 with sulfuric acid.
    10.4 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 
min. with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.5 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.6 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.7 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.8 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.9 Increase the temperature of the hot water bath to 95 to 100 
[deg]C. Remove the Synder column and rinse the flask and its lower joint 
into the concentrator tube with 1 to 2 mL of 2-propanol. A 5-mL syringe 
is recommended for this operation. Attach a two-ball micro-Snyder column 
to the concentrator tube and prewet the column by adding about 0.5 mL of 
2-propanol to the top. Place the micro-K-D apparatus on the water bath 
so that the concentrator tube is partially immersed in the hot water. 
Adjust the vertical position of the apparatus and the water temperature 
as required to complete concentration in 5 to 10 min. At the proper rate 
of distillation the balls of the column will actively chatter but the 
chambers will

[[Page 119]]

not flood. When the apparent volume of liquid reaches 2.5 mL, remove the 
K-D apparatus and allow it to drain and cool for at least 10 min. Add an 
additional 2 mL of 2-propanol through the top of the micro-Snyder column 
and resume concentrating as before. When the apparent volume of liquid 
reaches 0.5 mL, remove the K-D apparatus and allow it to drain and cool 
for at least 10 min.
    10.10 Remove the micro-Snyder column and rinse its lower joint into 
the concentrator tube with a minimum amount of 2-propanol. Adjust the 
extract volume to 1.0 mL. Stopper the concentrator tube and store 
refrigerated at 4 [deg]C if further processing will not be performed 
immediately. If the extract will be stored longer than two days, it 
should be transferred to a Teflon-sealed screw-cap vial. If the sample 
extract requires no further cleanup, proceed with FIDGC analysis 
(Section 11). If the sample requires further cleanup, proceed to Section 
12.
    10.11 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

            11. Flame Ionization Detector Gas Chromatography

    11.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. An example of the 
separations achieved by this column is shown in Figure 1. Other packed 
or capillary (open-tubular) columns, chromatographic conditions, or 
detectors may be used if the requirements of Section 8.2 are met.
    11.2 Calibrate the system daily as described in Section 7.
    11.3 If the internal standard calibration procedure is used, the 
internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    11.4 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush technique. \11\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, and 
the resulting peak size in area or peak height units.
    11.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
may be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    11.6 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    11.7 If the measurement of the peak response is prevented by the 
presence of interferences, an alternative gas chromatographic procedure 
is required. Section 12 describes a derivatization and column 
chromatographic procedure which has been tested and found to be a 
practical means of analyzing phenols in complex extracts.

   12. Derivatization and Electron Capture Detector Gas Chromatography

    12.1 Pipet a 1.0-mL aliquot of the 2-propanol solution of standard 
or sample extract into a glass reaction vial. Add 1.0 mL of derivatizing 
reagent (Section 6.11). This amount of reagent is sufficient to 
derivatize a solution whose total phenolic content does not exceed 0.3 
mg/mL.
    12.2 Add about 3 mg of potassium carbonate to the solution and shake 
gently.
    12.3 Cap the mixture and heat it for 4 h at 80 [deg]C in a hot water 
bath.
    12.4 Remove the solution from the hot water bath and allow it to 
cool.
    12.5 Add 10 mL of hexane to the reaction flask and shake vigorously 
for 1 min. Add 3.0 mL of distilled, deionized water to the reaction 
flask and shake for 2 min. Decant a portion of the organic layer into a 
concentrator tube and cap with a glass stopper.
    12.6 Place 4.0 g of silica gel into a chromatographic column. Tap 
the column to settle the silica gel and add about 2 g of anhydrous 
sodium sulfate to the top.
    12.7 Preelute the column with 6 mL of hexane. Discard the eluate and 
just prior to exposure of the sodium sulfate layer to the air, pipet 
onto the column 2.0 mL of the hexane solution (Section 12.5) that 
contains the derivatized sample or standard. Elute the column with 10.0 
mL of hexane and discard the eluate. Elute the column, in order, with: 
10.0 mL of 15% toluene in hexane (Fraction 1); 10.0 mL of 40% toluene in 
hexane (Fraction 2); 10.0 mL of 75% toluene in hexane (Fraction 3); and 
10.0 mL of 15% 2-propanol in toluene (Fraction 4). All elution mixtures 
are prepared on a volume: volume basis. Elution patterns for the 
phenolic derivatives are shown in Table 2. Fractions may be combined as 
desired, depending upon the specific phenols of interest or level of 
interferences.
    12.8 Analyze the fractions by ECDGC. Table 2 summarizes the 
recommended operating conditions for the gas chromatograph. Included in 
this table are retention times and MDL that can be achieved under these 
conditions. An example of the separations achieved by this column is 
shown in Figure 2.

[[Page 120]]

    12.9 Calibrate the system daily with a minimum of three aliquots of 
calibration standards, containing each of the phenols of interest that 
are derivatized according to Section 7.5.
    12.10 Inject 2 to 5 [micro]L of the column fractions into the gas 
chromatograph using the solvent-flush technique. Smaller (1.0 [micro]L) 
volumes can be injected if automatic devices are employed. Record the 
volume injected to the nearest 0.05 [micro]L, and the resulting peak 
size in area or peak height units. If the peak response exceeds the 
linear range of the system, dilute the extract and reanalyze.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample analyzed by FIDGC (without derivatization) as indicated below.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.098

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.099

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Determine the concentration of individual compounds in the 
sample analyzed by derivatization and ECDGC according to Equation 4.
[GRAPHIC] [TIFF OMITTED] TC15NO91.100

                                                              Equation 4

where:
A = Mass of underivatized phenol represented by area of peak in sample 
          chromatogram, determined from calibration curve in Section 
          7.5.3 (ng).
Vi = Volume of eluate injected ([micro]L).
Vt = Total volume of column eluate or combined fractions from 
          which Vi was taken ([micro]L).
Vs = Volume of water extracted in Section 10.10 (mL).
B = Total volume of hexane added in Section 12.5 (mL).
C = Volume of hexane sample solution added to cleanup column in Section 
          12.7 (mL).
D = Total volume of 2-propanol extract prior to derivatization (mL).
E = Volume of 2-propanol extract carried through derivatization in 
          Section 12.1 (mL).

    13.3 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Tables 1 and 2 were obtained using reagent water. \12\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
as six concentrations over the range 12 to 450 [micro]g/L. \13\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships for a flame ionization detector are 
presented in Table 4.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Phenols in Industrial and Municipal 
Wastewaters,'' EPA 600/4-84-ABC, National Technical Information Service, 
PBXYZ, Springfield, Virginia 22161, November 1984.
    3. Kawahara, F. K. ``Microdetermination of Derivatives of Phenols 
and Mercaptans by Means of Electron Capture Gas Chromatography,'' 
Analytical Chemistry, 40, 1009 (1968).
    4. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American

[[Page 121]]

Society for Testing and Materials, Philadelphia.
    5. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    6. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    7. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    8. Provost, L. P., and Elder, R. S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    9. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    10. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methmds for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    11. Burke, J. A. ``Gas Chromatography for Pesticide Residue 
Analysis; Some Practical Aspects,'' Journal of the Association of 
Official Analytical Chemists, 48, 1037 (1965).
    12. ``Development of Detection Limits, EPA Method 604, Phenols,'' 
Special letter report for EPA Contract 68-03-2625, U.S. Environmental 
Protection Agency, Environmental Monitoring and Support Laboratory, 
Cincinnati, Ohio 45268.
    13. ``EPA Method Study 14 Method 604-Phenols,'' EPA 600/4-84-044, 
National Technical Information Service, PB84-196211, Springfield, 
Virginia 22161, May 1984.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                                               Method
                                                 Retention    detection
                   Parameter                    time (min)      limit
                                                            ([micro]g/L)
------------------------------------------------------------------------
2-Chlorophenol................................        1.70          0.31
2-Nitrophenol.................................        2.00          0.45
Phenol........................................        3.01          0.14
2,4-Dimethylphenol............................        4.03          0.32
2,4-Dichlorophenol............................        4.30          0.39
2,4,6-Trichlorophenol.........................        6.05          0.64
4-Chloro-3-methylphenol.......................        7.50          0.36
2,4-Dinitrophenol.............................       10.00         13.0
2-Methyl-4,6-dinitrophenol....................       10.24         16.0
Pentachlorophenol.............................       12.42          7.4
4-Nitrophenol.................................       24.25          2.8
------------------------------------------------------------------------
Column conditions: Supelcoport (80/100 mesh) coated with 1% SP-1240DA
  packed in a 1.8 m long x 2 mm ID glass column with nitrogen carrier
  gas at 30 mL/min flow rate. Column temperature was 80 [deg]C at
  injection, programmed immediately at 8 [deg]C/min to 150 [deg]C final
  temperature. MDL were determined with an FID.


          Table 2--Silica Gel Fractionation and Electron Capture Gas Chromatography of PFBB Derivatives
----------------------------------------------------------------------------------------------------------------
                                                                   Percent recovery by                  Method
                                                                      fraction \a\         Retention   detection
                       Parent compound                        ----------------------------    time       limit
                                                                                             (min)    ([micro]g/
                                                                 1      2      3      4                   L)
----------------------------------------------------------------------------------------------------------------
2-Chlorophenol...............................................  .....     90      1  .....        3.3        0.58
2-Nitrophenol................................................  .....  .....      9     90        9.1        0.77
Phenol.......................................................  .....     90     10  .....        1.8        2.2
2,4-Dimethylphenol...........................................  .....     95      7  .....        2.9        0.63
2,4-Dichlorophenol...........................................  .....     95      1  .....        5.8        0.68
2,4,6-Trichlorophenol........................................     50     50  .....  .....        7.0        0.58
4-Chloro-3-methylphenol......................................  .....     84     14  .....        4.8        1.8
Pentachlorophenol............................................     75     20  .....  .....       28.8        0.59
4-Nitrophenol................................................  .....  .....      1     90       14.0        0.70
----------------------------------------------------------------------------------------------------------------
Column conditions: Chromosorb W-AW-DMCS (80/100 mesh) coated with 5% OV-17 packed in a 1.8 m long x 2.0 mm ID
  glass column with 5% methane/95% argon carrier gas at 30 mL/min flow rate. Column temperature held isothermal
  at 200 [deg]C. MDL were determined with an ECD.
 
\a\ Eluant composition:
 Fraction 1--15% toluene in hexane.
 Fraction 2--40% toluene in hexane.
 Fraction 3--75% toluene in hexane.
 Fraction 4--15% 2-propanol in toluene.


[[Page 122]]


                                   Table 3--QC Acceptance Criteria--Method 604
----------------------------------------------------------------------------------------------------------------
                                                                             Limit for
                                                                Test conc.       s      Range for X   Range for
                           Parameter                            ([micro]g/  ([micro]g/   ([micro]g/     P, Ps
                                                                    L)          L)           L)       (percent)
----------------------------------------------------------------------------------------------------------------
4-Chloro-3-methylphenol.......................................       100          16.6   56.7-113.4       49-122
2-Chlorophenol................................................       100          27.0   54.1-110.2       38-126
2,4-Dichlorophenol............................................       100          25.1   59.7-103.3       44-119
2,4-Dimethylphenol............................................       100          33.3   50.4-100.0       24-118
4,6-Dinitro-2-methylphenol....................................       100          25.0   42.4-123.6       30-136
2,4-Dinitrophenol.............................................       100          36.0   31.7-125.1       12-145
2-Nitrophenol.................................................       100          22.5   56.6-103.8       43-117
4-Nitrophenol.................................................       100          19.0   22.7-100.0       13-110
Pentachlorophenol.............................................       100          32.4   56.7-113.5       36-134
Phenol........................................................       100          14.1   32.4-100.0       23-108
2,4,6-Trichlorophenol.........................................       100          16.6   60.8-110.4       53-119
----------------------------------------------------------------------------------------------------------------
s--Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X--Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps--Percent recovery measured (Section 8.3.2, Section 8.4.2).
 
Note: These criteria are based directly upon the method performance data in Table 4. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 4.


                Table 4--Method Accuracy and Precision as Functions of Concentration--Method 604
----------------------------------------------------------------------------------------------------------------
                                                            Accuracy, as      Single Analyst        Overall
                       Parameter                            recovery, X'      precision, sr'     precision, S'
                                                            ([micro]g/L)       ([micro]g/L)       ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
4-Chloro-3-methylphenol................................         0.87C-1.97        0.11X090.21       0.16X + 1.41
2-Chlorophenol.........................................         0.83C-0.84       0.18X + 0.20       0.21X + 0.75
2,4-Dichlorophenol.....................................       0.81C + 0.48        0.17X090.02       0.18X + 0.62
2,4-Dimethylphenol.....................................         0.62C-1.64        0.30X090.89       0.25X + 0.48
4,6-Dinitro-2-methylphenol.............................         0.84C-1.01       0.15X + 1.25       0.19X + 5.85
2,4-Dinitrophenol......................................         0.80C-1.58        0.27X091.15       0.29X + 4.51
2-Nitrophenol..........................................         0.81C-0.76       0.15X + 0.44       0.14X + 3.84
4-Nitrophenol..........................................       0.46C + 0.18       0.17X + 2.43       0.19X + 4.79
Pentachlorophenol......................................       0.83C + 2.07        0.22X090.58       0.23X + 0.57
Phenol.................................................       0.43C + 0.11        0.20X090.88       0.17X + 0.77
2,4,6-Trichlorophenol..................................         0.86C-0.40       0.10X + 0.53       0.13X + 2.40
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


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[GRAPHIC] [TIFF OMITTED] TC02JY92.012


[[Page 124]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.013

                         Method 605--Benzidines

                        1. Scope and Application

    1.1 This method covers the determination of certain benzidines. The 
following parameters can be determined by this method:

------------------------------------------------------------------------
                   Parameter                     Storet No     CAS No.
------------------------------------------------------------------------
Benzidine.....................................        39120      92-87-5
3,3'-Dichlorobenzidine........................        34631      91-94-1
------------------------------------------------------------------------

    1.2 This is a high performance liquid chromatography (HPLC) method 
applicable to the determination of the compounds listed above in 
municipal and industrial discharges as provided under 40 CFR 136.1. When 
this method is used to analyze unfamiliar samples for the compounds 
above, identifications should be supported by at least one additional 
qualitative technique. This method describes electrochemical conditions 
at a second potential which can be used to confirm measurements made 
with this method. Method 625 provides gas chromatograph/mass 
spectrometer (GC/MS) conditions appropriate for the qualitative and 
quantitative confirmation of results for the parameters listed above, 
using the extract produced by this method.
    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is

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listed in Table 1. The MDL for a specific wastewater may differ from 
those listed, depending upon the nature of the interferences in the 
sample matrix.
    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the use of HPLC instrumentation and in the 
interpretation of liquid chromatograms. Each analyst must demonstrate 
the ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with chloroform using liquid-liquid extractions in a separatory funnel. 
The chloroform extract is extracted with acid. The acid extract is then 
neutralized and extracted with chloroform. The final chloroform extract 
is exchanged to methanol while being concentrated using a rotary 
evaporator. The extract is mixed with buffer and separated by HPLC. The 
benzidine compounds are measured with an electrochemical detector. \2\
    2.2 The acid back-extraction acts as a general purpose cleanup to 
aid in the elimination of interferences.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in chromatograms. All of 
these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials may not be eliminated 
by this treatment. Solvent rinses with acetone and pesticide quality 
hexane may be substituted for the muffle furnace heating. Volumetric 
ware should not be heated in a muffle furnace. After drying and cooling, 
glassware should be sealed and stored in a clean environment to prevent 
any accumulation of dust or other contaminants. Store inverted or capped 
with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedures that are inherent in the extraction step are used to 
overcome many of these interferences, but unique samples may require 
additional cleanup approaches to achieve the MDL listed in Table 1.
    3.3 Some dye plant effluents contain large amounts of components 
with retention times closed to benzidine. In these cases, it has been 
found useful to reduce the electrode potential in order to eliminate 
interferences and still detect benzidine. (See Section 12.7.)

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health harzard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \4 6\ for 
the information of the analyst.
    4.2 The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: benzidine and 3,3'-dichlorobenzidine. Primary standards of 
these toxic compounds should be prepared in a hood. A NIOSH/MESA 
approved toxic gas respirator should be worn when the analyst handles 
high concentrations of these toxic compounds.
    4.3 Exposure to chloroform should be minimized by performing all 
extractions and extract concentrations in a hood or other well-
ventiliated area.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene

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chloride, and dried before use to minimize contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested):
    5.2.1 Separatory funnels--2000, 1000, and 250-mL, with Teflon 
stopcock.
    5.2.2 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.3 Rotary evaporator.
    5.2.4 Flasks--Round bottom, 100-mL, with 24/40 joints.
    5.2.5 Centrifuge tubes--Conical, graduated, with Teflon-lined screw 
caps.
    5.2.6 Pipettes--Pasteur, with bulbs.
    5.3 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.4 High performance liquid chromatograph (HPLC)--An analytical 
system complete with column supplies, high pressure syringes, detector, 
and compatible recorder. A data system is recommended for measuring peak 
areas and retention times.
    5.4.1 Solvent delivery system--With pulse damper, Altex 110A or 
equivalent.
    5.4.2 Injection valve (optional)--Waters U6K or equivalent.
    5.4.3 Electrochemical detector--Bioanalytical Systems LC-2A with 
glassy carbon electrode, or equivalent. This detector has proven 
effective in the analysis of wastewaters for the parameters listed in 
the scope (Section 1.1), and was used to develop the method performance 
statements in Section 14. Guidelines for the use of alternate detectors 
are provided in Section 12.1.
    5.4.4 Electrode polishing kit--Princeton Applied Research Model 9320 
or equivalent.
    5.4.5 Column--Lichrosorb RP-2, 5 micron particle diameter, in a 25 
cm x 4.6 mm ID stainless steel column. This column was used to develop 
the method performance statements in Section 14. Guidelines for the use 
of alternate column packings are provided in Section 12.1.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium hydroxide solution (5 N)--Dissolve 20 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.3 Sodium hydroxide solution (1 M)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 1 L.
    6.4 Sodium thiosulfate--(ACS) Granular.
    6.5 Sodium tribasic phosphate (0.4 M)--Dissolve 160 g of trisodium 
phosphate decahydrate (ACS) in reagent water and dilute to 1 L.
    6.6 Sulfuric acid (1 + 1)--Slowly, add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.7 Sulfuric acid (1 M)--Slowly, add 58 mL of 
H2SO4 (ACS, sp. gr. 1.84) to reagent water and 
dilute to 1 L.
    6.8 Acetate buffer (0.1 M, pH 4.7)--Dissolve 5.8 mL of glacial 
acetic acid (ACS) and 13.6 g of sodium acetate trihydrate (ACS) in 
reagent water which has been purified by filtration through a RO-4 
Millipore System or equivalent and dilute to 1 L.
    6.9 Acetonitrile, chloroform (preserved with 1% ethanol), methanol--
Pesticide quality or equivalent.
    6.10 Mobile phase--Place equal volumes of filtered acetonitrile 
(Millipore type FH filter or equivalent) and filtered acetate buffer 
(Millipore type GS filter or equivalent) in a narrow-mouth, glass 
container and mix thoroughly. Prepare fresh weekly. Degas daily by 
sonicating under vacuum, by heating and stirring, or by purging with 
helium.
    6.11 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions may be prepared from pure standard materials or 
purchased as certified solutions.
    6.11.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in methanol and dilute 
to volume in a 10-mL volumetric flask. Larger volumes can be used at the 
convenience of the analyst. When compound purity is assayed to be 96% or 
greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.11.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.11.3 Stock standard solutions must be replaced after six months, 
or sooner if comparison with check standards indicates a problem.
    6.12 Quality control check sample concentrate--See Section 8.2.1.

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                             7. Calibration

    7.1 Establish chromatographic operating conditions equivalent to 
those given in Table 1. The HPLC system can be calibrated using the 
external standard technique (Section 7.2) or the internal standard 
technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with mobile phase. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using syringe injections of 5 to 25 [micro]L or a constant 
volume injection loop, analyze each calibration standard according to 
Section 12 and tabulate peak height or area responses against the mass 
injected. The results can be used to prepare a calibration curve for 
each compound. Alternatively, if the ratio of response to amount 
injected (calibration factor) is a constant over the working range (<10% 
relative standard deviation, RSD), linearity through the origin can be 
assumed and the average ratio or calibration factor can be used in place 
of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with mobile phase. One of the standards should be 
at a concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using syringe injections of 5 to 25 [micro]L or a constant 
volume injection loop, analyze each calibration standard according to 
Section 12 and tabulate peak height or area responses against 
concentration for each compound and internal standard. Calculate 
response factors (RF) for each compound using Equation 1.

   RF = (As)(Cis (Ais)(Cs)

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

    If the RF value over the working range is a constant (<10% RSD), the 
RF can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound. If serious loss of 
response occurs, polish the electrode and recalibrate.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.9, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.

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    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing benzidine and/or 3,3'-dichlorobenzidine at a concentration of 
50 [micro]g/mL each in methanol. The QC check sample concentrate must be 
obtained from the U.S. Environmental Protection Agency, Environmental 
Monitoring and Support Laboratory in Cincinnati, Ohio, if available. If 
not available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Using a pipet, prepare QC check samples at a concentration of 
50 [micro]g/L by adding 1.00 mL of QC check sample concentrate to each 
of four 1-L-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter. Locate and correct the 
source of the problem and repeat the test for all parameters of interest 
beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 50 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none (2) the larger of either 5 times higher than the expected 
background concentration or 50 [micro]g/L.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than 50 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 2, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting

[[Page 129]]

the spike concentration (T) for C; (2) calculate overall precision (S') 
using the equation in Table 3, substituting X' for X; (3) calculate the 
range for recovery at the spike concentration as (100 X'/T)2.44(100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.

    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.

    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Sections 8.2.1 or 8.3.2) to 1 L of reagent water. 
The QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as HPLC with a dissimilar column, gas chromatography, or mass 
spectrometer must be used. Whenever possible, the laboratory should 
analyze standard reference materials and participate in relevant 
performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \8\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C and stored 
in the dark from the time of collection until extraction. Both benzidine 
and 3,3'-dichlorobenzidine are easily oxidized. Fill the sample bottles 
and, if residual chlorine is present, add 80 mg of sodium thiosulfate 
per liter of sample and mix well. EPA Methods 330.4 and 330.5 may be 
used for measurement of residual chlorine. \9\ Field test kits are 
available for this purpose. After mixing, adjust the pH of the sample to 
a range of 2 to 7 with sulfuric acid.
    9.3 If 1,2-diphenylhydrazine is likely to be present, adjust the pH 
of the sample to 4.0 0.2 to prevent rearrangement 
to benzidine.
    9.4 All samples must be extracted within 7 days of collection. 
Extracts may be held up to 7 days before analysis, if stored under an 
inert (oxidant free) atmosphere. \2\ The extract should be protected 
from light.

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel. Check the pH of the sample with wide-range pH paper 
and adjust to within the range of 6.5 to 7.5 with sodium hydroxide 
solution or sulfuric acid.
    10.2 Add 100 mL of chloroform to the sample bottle, seal, and shake 
30 s to rinse the inner surface. (Caution: Handle chloroform in a well 
ventilated area.) Transfer the solvent to the separatory funnel and 
extract the sample by shaking the funnel for 2 min with periodic venting 
to release excess pressure. Allow the organic layer to separate from the 
water phase for a minimum of 10 min. If the emulsion interface between 
layers is more than one-third the volume of the solvent layer, the 
analyst must employ mechanical techniques to complete the phase

[[Page 130]]

separation. The optimum technique depends upon the sample, but may 
include stirring, filtration of the emulsion through glass wool, 
centrifugation, or other physical methods. Collect the chloroform 
extract in a 250-mL separatory funnel.
    10.3 Add a 50-mL volume of chloroform to the sample bottle and 
repeat the extraction procedure a second time, combining the extracts in 
the separatory funnel. Perform a third extraction in the same manner.
    10.4 Separate and discard any aqueous layer remaining in the 250-mL 
separatory funnel after combining the organic extracts. Add 25 mL of 1 M 
sulfuric acid and extract the sample by shaking the funnel for 2 min. 
Transfer the aqueous layer to a 250-mL beaker. Extract with two 
additional 25-mL portions of 1 M sulfuric acid and combine the acid 
extracts in the beaker.
    10.5 Place a stirbar in the 250-mL beaker and stir the acid extract 
while carefully adding 5 mL of 0.4 M sodium tribasic phosphate. While 
monitoring with a pH meter, neutralize the extract to a pH between 6 and 
7 by dropwise addition of 5 N sodium hydroxide solution while stirring 
the solution vigorously. Approximately 25 to 30 mL of 5 N sodium 
hydroxide solution will be required and it should be added over at least 
a 2-min period. Do not allow the sample pH to exceed 8.
    10.6 Transfer the neutralized extract into a 250-mL separatory 
funnel. Add 30 mL of chloroform and shake the funnel for 2 min. Allow 
the phases to separate, and transfer the organic layer to a second 250-
mL separatory funnel.
    10.7 Extract the aqueous layer with two additional 20-mL aliquots of 
chloroform as before. Combine the extracts in the 250-mL separatory 
funnel.
    10.8 Add 20 mL of reagent water to the combined organic layers and 
shake for 30 s.
    10.9 Transfer the organic extract into a 100-mL round bottom flask. 
Add 20 mL of methanol and concentrate to 5 mL with a rotary evaporator 
at reduced pressure and 35 [deg]C. An aspirator is recommended for use 
as the source of vacuum. Chill the receiver with ice. This operation 
requires approximately 10 min. Other concentration techniques may be 
used if the requirements of Section 8.2 are met.
    10.10 Using a 9-in. Pasteur pipette, transfer the extract to a 15-
mL, conical, screw-cap centrifuge tube. Rinse the flask, including the 
entire side wall, with 2-mL portions of methanol and combine with the 
original extract.
    10.11 Carefully concentrate the extract to 0.5 mL using a gentle 
stream of nitrogen while heating in a 30 [deg]C water bath. Dilute to 2 
mL with methanol, reconcentrate to 1 mL, and dilute to 5 mL with acetate 
buffer. Mix the extract thoroughly. Cap the centrifuge tube and store 
refrigerated and protected from light if further processing will not be 
performed immediately. If the extract will be stored longer than two 
days, it should be transferred to a Teflon-sealed screw-cap vial. If the 
sample extract requires no further cleanup, proceed with HPLC analysis 
(Section 12). If the sample requires further cleanup, proceed to Section 
11.
    10.12 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1,000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst first must demonstrate that the requirements of 
Section 8.2 can be met using the method as revised to incorporate the 
cleanup procedure.

               12. High Performance Liquid Chromatography

    12.1 Table 1 summarizes the recommended operating conditions for the 
HPLC. Included in this table are retention times, capacity factors, and 
MDL that can be achieved under these conditions. An example of the 
separations achieved by this HPLC column is shown in Figure 1. Other 
HPLC columns, chromatographic conditions, or detectors may be used if 
the requirements of Section 8.2 are met. When the HPLC is idle, it is 
advisable to maintain a 0.1 mL/min flow through the column to prolong 
column life.
    12.2 Calibrate the system daily as described in Section 7.
    12.3 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the instrument.
    12.4 Inject 5 to 25 [micro]L of the sample extract or standard into 
the HPLC. If constant volume injection loops are not used, record the 
volume injected to the nearest 0.05 [micro]L, and the resulting peak 
size in area or peak height units.
    12.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    12.6 If the response for a peak exceeds the working range of the 
system, dilute the extract with mobile phase and reanalyze.

[[Page 131]]

    12.7 If the measurement of the peak response for benzidine is 
prevented by the presence of interferences, reduce the electrode 
potential to + 0.6 V and reanalyze. If the benzidine peak is still 
obscured by interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.101

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.102

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \10\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 7 x MDL to 3000 x MDL. \10\
    14.3 This method was tested by 17 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 1.0 to 70 [micro]g/L. \11\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Benzidines in Industrial and Muncipal 
Wastewaters,'' EPA 600/4-82-022, National Technical Information Service, 
PB82-196320, Springfield, Virginia 22161, April 1982.
    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    8. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    9. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    10. ``EPA Method Study 15, Method 605 (Benzidines),'' EPA 600/4-84-
062, National Technical Information Service, PB84-211176, Springfield, 
Virginia 22161, June 1984.
    11. ``EPA Method Validation Study 15, Method 605 (Benzidines),'' 
Report for EPA Contract 68-03-2624 (In preparation).

[[Page 132]]



     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                                                Method
                                                   Column     detection
            Parameter               Retention     capacity      limit
                                    time (min)  factor (k')   ([micro]g/
                                                                  L)
------------------------------------------------------------------------
Benzidine........................          6.1         1.44         0.08
3,3'-Dichlorobenzidine...........         12.1         3.84         0.13
------------------------------------------------------------------------
HPLC Column conditions: Lichrosorb RP-2, 5 micron particle size, in a 25
  cm x 4.6 mm ID stainless steel column. Mobile Phase: 0.8 mL/min of 50%
  acetonitrile/50% 0.1M pH 4.7 acetate buffer. The MDL were determined
  using an electrochemical detector operated at + 0.8 V.


                                   Table 2--QC Acceptance Criteria--Method 605
----------------------------------------------------------------------------------------------------------------
                                                                                Limit for   Range for
                                                                   Test conc.       s           X      Range for
                            Parameter                              ([micro]g/  ([micro]g/  ([micro]g/    P, Ps
                                                                       L)          L)          L)      (percent)
----------------------------------------------------------------------------------------------------------------
Benzidine........................................................          50        18.7    9.1-61.0      D-140
3.3'-Dichlorobenzidine...........................................          50        23.6   18.7-50.0      5-128
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 605
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                                recovery,    precision, sr'   precision, S'
                                                                  X'([micro]g/L)   ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Benzidine.......................................................    0.70C + 0.06    0.28X + 0.19    0.40X + 0.18
3,3'-Dichlorobenzidine..........................................    0.66C + 0.23      0.39X-0.05    0.38X + 0.02
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


[[Page 133]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.014


[[Page 134]]

                       Method 606--Phthalate Ester

                        1. Scope and Application

    1.1 This method covers the determination of certain phthalate 
esters. The following parameters can be determined by this method:

------------------------------------------------------------------------
                                                      STORET
                     Parameter                         No.      CAS No.
------------------------------------------------------------------------
Bis(2-ethylhexyl) phthalate........................    39100    117-81-7
Butyl benzyl phthalate.............................    34292     85-68-7
Di-n-butyl phthalate...............................    39110     84-74-2
Diethyl phthalate..................................    34336     84-66-2
Dimethyl phthalate.................................    34341    131-11-3
Di-n-octyl phthalate...............................    34596    117-84-0
------------------------------------------------------------------------

    1.2 This is a gas chromatographic (GC) method applicable to the 
determination of the compounds listed above in municipal and industrial 
discharges as provided under 40 CFR 136.1. When this method is used to 
analyze unfamiliar samples for any or all of the compounds above, 
compound identifications should be supported by at least one additional 
qualitative technique. This method describes analytical conditions for a 
second gas chromatographic column that can be used to confirm 
measurements made with the primary column. Method 625 provides gas 
chromatograph/mass spectrometer (GC/MS) conditions appropriate for the 
qualitative and quantitative confirmation of results for all of the 
parameters listed above, using the extract produced by this method.
    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 The sample extraction and concentration steps in this method are 
essentially the same as in Methods 608, 609, 611, and 612. Thus, a 
single sample may be extracted to measure the parameters included in the 
scope of each of these methods. When cleanup is required, the 
concentration levels must be high enough to permit selecting aliquots, 
as necessary, to apply appropriate cleanup procedures. The analyst is 
allowed the latitude, under Section 12, to select chromatographic 
conditions appropriate for the simultaneous measurement of combinations 
of these parameters.
    1.5 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is dried and exchanged to hexane during concentration 
to a volume of 10 mL or less. The extract is separated by gas 
chromatography and the phthalate esters are then measured with an 
electron capture detector. \2\
    2.2 Analysis for phthalates is especially complicated by their 
ubiquitous occurrence in the environment. The method provides Florisil 
and alumina column cleanup procedures to aid in the elimination of 
interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Phthalate esters are contaminants in many products commonly 
found in the laboratory. It is particularly important to avoid the use 
of plastics because phthalates are commonly used as plasticizers and are 
easily extracted from plastic materials. Serious phthalate contamination 
can result at any time, if consistent quality control is not practiced. 
Great care must be experienced to prevent such contamination. Exhaustive 
cleanup of reagents and glassware may be required to eliminate 
background phthalate contamination. \4 5\

[[Page 135]]

    3.3 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedures in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \6 8\ for 
the information of the analyst.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only).
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Chromatographic column--300 mm long x 10 mm ID, with Teflon 
stopcock and coarse frit filter disc at bottom (Kontes K-420540-0213 or 
equivalent).
    5.2.4 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.5 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.6 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.7 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.8 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with gas 
chromatograph suitable for on-column injection and all required 
accessories including syringes, analytical columns, gases, detector, and 
strip-chart recorder. A data system is recommended for measuring peak 
areas.
    5.6.1 Column 1--1.8 m long x 4 mm ID glass, packed with 1.5% SP-
2250/1.95% SP-2401 Supelcoport (100/120 mesh) or equivalent. This column 
was used to develop the method performance statemelts in Section 14. 
Guidelines for the use of alternate column packings are provided in 
Section 12.1.
    5.6.2 Column 2--1.8 m long x 4 mm ID glass, packed with 3% OV-1 on 
Supelcoport (100/120 mesh) or equivalent.
    5.6.3 Detector--Electron capture detector. This detector has proven 
effective in the analysis of wastewaters for the parameters listed in 
the scope (Section 1.1), and was used to develop the method performance 
statements in Section 14. Guidelines for the use of alternate detectors 
are provided in Section 12.1.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Acetone, hexane, isooctane, methylene chloride, methanol--
Pesticide quality or equivalent.
    6.3 Ethyl ether--nanograde, redistilled in glass if necessary.
    6.3.1 Ethyl ether must be shown to be free of peroxides before it is 
used as indicated by

[[Page 136]]

EM Laboratories Quant test strips. (Available from Scientific Products 
Co., Cat. No. P1126-8, and other suppliers.)
    6.3.2 Procedures recommended for removal of peroxides are provided 
with the test strips. After cleanup, 20 mL of ethyl alcohol preservative 
must be added to each liter of ether.
    6.4 Sodium sulfate--(ACS) Granular, anhydrous. Several levels of 
purification may be required in order to reduce background phthalate 
levels to an acceptable level: 1) Heat 4 h at 400 [deg]C in a shallow 
tray, 2) Heat 16 h at 450 to 500 [deg]C in a shallow tray, 3) Soxhlet 
extract with methylene chloride for 48 h.
    6.5 Florisil--PR grade (60/100 mesh). Purchase activated at 1250 
[deg]F and store in the dark in glass containers with ground glass 
stoppers or foil-lined screw caps. To prepare for use, place 100 g of 
Florisil into a 500-mL beaker and heat for approximately 16 h at 40 
[deg]C. After heating transfer to a 500-mL reagent bottle. Tightly seal 
and cool to room temperature. When cool add 3 mL of reagent water. Mix 
thoroughly by shaking or rolling for 10 min and let it stand for at 
least 2 h. Keep the bottle sealed tightly.
    6.6 Alumina--Neutral activity Super I, W200 series (ICN Life 
Sciences Group, No. 404583). To prepare for use, place 100 g of alumina 
into a 500-mL beaker and heat for approximately 16 h at 400 [deg]C. 
After heating transfer to a 500-mL reagent bottle. Tightly seal and cool 
to room temperature. When cool add 3 mL of reagent water. Mix thoroughly 
by shaking or rolling for 10 min and let it stand for at least 2 h. Keep 
the bottle sealed tightly.
    6.7 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions can be prepared from pure standard materials or 
purchased as certified solutions.
    6.7.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in isooctane and dilute 
to volume in a 10-mL volumetric flask. Larger volumes can be used at the 
convenience of the analyst. When compound purity is assayed to be 96% or 
greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.7.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.7.3 Stock standard solutions must be replaced after six months, or 
sooner if comparison with check standards indicates a problem.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatograph operating conditions equivalent to 
those given in Table 1. The gas chromatographic system can be calibrated 
using the external standard technique (Section 7.2) or the internal 
standard technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepared calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with isooctane. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD), linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flash. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with isooctane. One of the standards should be at a 
concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.

[[Page 137]]

    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.

   RF = (As)(Cis (Ais)(Cs)

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

    If the RF value over the working range is a constant (<10% RSD), the 
RF can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality contrml (QC) check sample concentrate is required 
containing each parameter of interest at the following concentrations in 
acetone: butyl benzyl phthalate, 10 [micro]g/mL; bis(2-ethylhexyl) 
phthalate, 50 [micro]g/mL; di-n-octyl phthalate, 50 [micro]g/mL; any 
other phthlate, 25 [micro]g/mL. The QC check sample concentrate must be 
obtained from the U.S. Environmental Protection Agancy, Environmental 
Monitoring and Support Laboratory in Cincinnati, Ohio, if available. If 
not available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Using a pipet, prepare QC check samples at the test 
concentrations shown in Table 2 by adding 1.00 mL of QC check sample 
concentrate to each of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively,

[[Page 138]]

found in Table 2. If s and X for all parameters of interest meet the 
acceptance criteria, the system performance is acceptable and analysis 
of actual samples can begin. If any individual s exceeds the precision 
limit or any individual X falls outside the range for accuracy, the 
system performance is unacceptable for that parameter. Locate and 
correct the source of the problem and repeat the test for all parameters 
of interest beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at the test concentration in Section 8.2.2 or 1 to 5 
times higher than the background concentration determined in Section 
8.3.2, whichever concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none (2) the larger of either 5 times higher than the expected 
background concentration or the test concentration in Section 8.2.2.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\9\ If spiking was performed at a concentration lower than the test 
concentration in Section 8.2.2, the analyst must use either the QC 
acceptance criteria in Table 2, or optional QC acceptance criteria 
calculated for the specific spike concentration. To calculate optional 
acceptance criteria for the recovery of a parameter: (1) Calculate 
accuracy (X') using the equation in Table 3, substituting the spike 
concentration (T) for C; (2) calculate overall precision (S') using the 
equation in Table 3, substituting X' for X; (3) calculate the range for 
recovery at the spike concentration as (100 X'/T)2.44(100 S'/T)%. \9\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).

[[Page 139]]

    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \10\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.
    10.2 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 
min. with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phrase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentrator 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.6 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.7 Increase the temperature of the hot water bath to about 80 
[deg]C. Momentarily remove the Snyder column, add 50 mL of hexane and a 
new boiling chip, and reattach the Snyder column. Concentrate the 
extract as in Section 10.6, except use hexane to prewet the column. The 
elapsed time of concentration should be 5 to 10 min.
    10.8 Remove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of hexane. A 5-mL 
syringe is recommended for this operation. Adjust the extract volume to 
10 mL. Stopper the concentrator tube and store refrigerated if further 
processing will not be performed immediately. If the extract will be 
stored longer than two days, it should be transferred to a Teflon-sealed 
screw-cap vial. If the sample extract requires no further cleanup, 
proceed with gas chromatographic analysis (Section 12). If the sample 
requires further cleanup, proceed to Section 11.
    10.9 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11. Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use either procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of

[[Page 140]]

Section 8.2 can be met using the method as revised to incorporate the 
cleanup procedure.
    11.2 If the entire extract is to be cleaned up by one of the 
following procedures, it must be concentrated to 2.0 mL. To the 
concentrator tube in Section 10.8, add a clean boiling chip and attach a 
two-ball micro-Snyder column. Prewet the column by adding about 0.5 mL 
of hexane to the top. Place the micro-K-D apparatus on a hot water bath 
(80 [deg]C) so that the concentrator tube is partially immersed in the 
hot water. Adjust the vertical position of the apparatus and the water 
temperature as required to complete the concentration in 5 to 10 min. At 
the proper rate of distillation the balls of the column will actively 
chatter but the chambers will not flood. When the apparent volume of 
liquid reaches about 0.5 mL, remove the K-D apparatus and allow it to 
drain and cool for at least 10 min. Remove the micro-Snyder column and 
rinse its lower joint into the concentrator tube with 0.2 mL of hexane. 
Adjust the final volume to 2.0 mL and proceed with one of the following 
cleanup procedures.
    11.3 Florisil column cleanup for phthalate esters:
    11.3.1 Place 10 g of Florisil into a chromatographic column. Tap the 
column to settle the Florisil and add 1 cm of anhydrous sodium sulfate 
to the top.
    11.3.2 Preelute the column with 40 mL of hexane. The rate for all 
elutions should be about 2 mL/min. Discard the eluate and just prior to 
exposure of the sodium sulfate layer to the air, quantitatively transfer 
the 2-mL sample extract onto the column using an additional 2 mL of 
hexane to complete the transfer. Just prior to exposure of the sodium 
sulfate layer to the air, add 40 mL of hexane and continue the elution 
of the column. Discard this hexane eluate.
    11.3.3 Next, elute the column with 100 mL of 20% ethyl ether in 
hexane (V/V) into a 500-mL K-D flask equipped with a 10-mL concentrator 
tube. Concentrate the collected fraction as in Section 10.6. No solvent 
exchange is necessary. Adjust the volume of the cleaned up extract to 10 
mL in the concentrator tube and analyze by gas chromatography (Section 
12).
    11.4 Alumina column cleanup for phthalate esters:
    11.4.1 Place 10 g of alumina into a chromatographic column. Tap the 
column to settle the alumina and add 1 cm of anhydrous sodium sulfate to 
the top.
    11.4.2 Preelute the column with 40 mL of hexane. The rate for all 
elutions should be about 2 mL/min. Discard the eluate and just prior to 
exposure of the sodium sulfate layer to the air, quantitatively transfer 
the 2-mL sample extract onto the column using an additional 2 mL of 
hexane to complete the transfer. Just prior to exposure of the sodium 
sulfate layer to the air, add 35 mL of hexane and continue the elution 
of the column. Discard this hexane eluate.
    11.4.3 Next, elute the column with 140 mL of 20% ethyl ether in 
hexane (V/V) into a 500-mL K-D flask equipped with a 10-mL concentrator 
type. Concentrate the collected fraction as in Section 10.6. No solvent 
exchange is necessary. Adjust the volume of the cleaned up extract to 10 
mL in the concentrator tube and analyze by gas chromatography (Section 
12).

                         12. Gas Chromatography

    12.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. Examples of the separations 
achieved by Column 1 are shown in Figures 1 and 2. Other packed or 
capillary (open-tubular) columns, chromatographic conditions, or 
detectors may be used if the requirements of Section 8.2 are met.
    12.2 Calibrate the system daily as described in Section 7.
    12.3 If the internal standard calibration procedure is being used, 
the internal staldard must be added to the sample extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    12.4 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas-chromatograph using the solvent-flush technique. \11\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, and 
the resulting peak size in area or peak height units.
    12.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    12.6 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    12.7 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration

[[Page 141]]

factor determined in Section 7.2.2. The concentration in the sample can 
be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.103

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.104

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \12\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 5 x MDL to 1000 x MDL with the following 
exceptions: dimethyl and diethyl phthalate recoveries at 1000 x MDL were 
low (70%); bis-2-ethylhexyl and di-n-octyl phthalate recoveries at 5 x 
MDL were low (60%). \12\
    14.3 This method was tested by 16 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 0.7 to 106 [micro]g/L. \13\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Phthalates in Industrial and Muncipal 
Wastewaters,'' EPA 600/4-81-063, National Technical Information Service, 
PB81-232167, Springfield, Virginia 22161, July 1981.
    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    4. Giam, C.S., Chan, H.S., and Nef, G.S. ``Sensitive Method for 
Determination of Phthalate Ester Plasticizers in Open-Ocean Biota 
Samples,'' Analytical Chemistry, 47, 2225 (1975).
    5. Giam, C.S., and Chan, H.S. ``Control of Blanks in the Analysis of 
Phthalates in Air and Ocean Biota Samples,'' U.S. National Bureau of 
Standards, Special Publication 442, pp. 701-708, 1976.
    6. ``Carcinogens--Working with Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    7. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    8. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    9. Provost L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    10. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    11. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    12. ``Method Detection Limit and Analytical Curve Studies, EPA 
Methods 606, 607, and 608,'' Special letter report for EPA Contract 68-
03-2606, U.S. Environmental Protection Agency, Environmental Monitoring 
and Support Laboratory, Cincinnati, Ohio 45268, June 1980.
    13. ``EPA Method Study 16 Method 606 (Phthalate Esters),'' EPA 600/
4-84-056, National Technical Information Service, PB84-211275, 
Springfield, Virginia 22161, June 1984.

[[Page 142]]



     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                   Retention time (min)        Method
                               ----------------------------   detection
           Parameter                                            limit
                                  Column 1      Column 2    ([micro]g/L)
------------------------------------------------------------------------
Dimethyl phthalate............          2.03          0.95          0.29
Diethyl phthalate.............          2.82          1.27          0.49
Di-n-butyl phthalate..........          8.65          3.50          0.36
Butyl benzyl phthalate........      \a\ 6.94      \a\ 5.11          0.34
Bis(2-ethylhexyl) phthalate...      \a\ 8.92     \a\ 10.5           2.0
Di-n-octyl phthalate..........     \a\ 16.2      \a\ 18.0           3.0
------------------------------------------------------------------------
Column 1 conditions: Supelcoport (100/120 mesh) coated with 1.5% SP-2250/
  1.95% SP-2401 packed in a 1.8 m long x 4 mm ID glass column with 5%
  methane/95% argon carrier gas at 60 mL/min flow rate. Column
  temperature held isothermal at 180 [deg]C, except where otherwise
  indicated.
Column 2 conditions: Supelcoport (100/120 mesh) coated with 3% OV-1
  packed in a 1.8 m long x 4 mm ID glass column with 5% methane/95%
  argon carrier gas at 60 mL/min flow rate. Column temperature held
  isothermal at 200 [deg]C, except where otherwise indicated.
\a\ 220 [deg]C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 606
----------------------------------------------------------------------------------------------------------------
                                                                                Limit for   Range for
                                                                   Test conc.       s           X      Range for
                            Parameter                              ([micro]g/  ([micro]g/  ([micro]g/    P, Ps
                                                                       L)          L)          L)      (percent)
----------------------------------------------------------------------------------------------------------------
Bis(2-ethylhexyl) phthalate......................................          50        38.4    1.2-55.9      D-158
Butyl benzyl phthalate...........................................          10         4.2    5.7-11.0     30-136
Di-n-butyl phthalate.............................................          25         8.9   10.3-29.6     23-136
Diethyl phthalate................................................          25         9.0    1.9-33.4      D-149
Dimethyl phathalate..............................................          25         9.5    1.3-35.5      D-156
Di-n-octyl phthalate.............................................          50        13.4      D-50.0      D-114
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 606
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                              recovery, X'   precision, sr'   precision, S'
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Bis(2-ethylhexyl) phthalate.....................................    0.53C + 2.02      0.80X-2.54      0.73X-0.17
Butyl benzyl phthalate..........................................    0.82C + 0.13    0.26X + 0.04    0.25X + 0.07
Di-n-butyl phthalate............................................    0.79C + 0.17    0.23X + 0.20    0.29X + 0.06
Diethyl phthalate...............................................    0.70C + 0.13    0.27X + 0.05    0.45X + 0.11
Dimethyl phthalate..............................................    0.73C + 0.17    0.26X + 0.14    0.44X + 0.31
Di-n-octyl phthalate............................................      0.35C-0.71    0.38X + 0.71    0.62X + 0.34
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


[[Page 143]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.015


[[Page 144]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.016


[[Page 145]]

                        Method 607--Nitrosamines

                        1. Scope and Application

    1.1 This method covers the determination of certain nitrosamines. 
The following parameters can be determined by this method:

------------------------------------------------------------------------
                   Parameter                     Storet No.    CAS No.
------------------------------------------------------------------------
N-Nitrosodimethylamine........................        34438      62-75-9
N-Nitrosodiphenylamine........................        34433      86-30-6
N-Nitrosodi-n-propylamine.....................        34428     621-64-7
------------------------------------------------------------------------

    1.2 This is a gas chromatographic (GC) method applicable to the 
determination of the parameters listed above in municipal and industrial 
discharges as provided under 40 CFR 136.1. When this method is used to 
analyze unfamiliar samples for any or all of the compmunds above, 
compound identifications should be supported by at least one additional 
qualitative technique. This method describes analytical conditimns for a 
second gas chromatographic column that can be used to confirm 
measurements made with the primary column. Method 625 provides gas 
chromatograph/mass spectrometer (GC/MS) conditions appropriate for the 
qualitative and quantitative confirmation of results for N-nitrosodi-n-
propylamine. In order to confirm the presence of N-nitrosodiphenylamine, 
the cleanup procedure specified in Section 11.3 or 11.4 must be used. In 
order to confirm the presence of N-nitrosodimethylamine by GC/MS, Column 
1 of this method must be substituted for the column recommended in 
Method 625. Confirmation of these parameters using GC-high resolution 
mass spectrometry or a Thermal Energy Analyzer is also recommended. \1 
2\
    1.3 The method detection limit (MDL, defined in Section 14.1) \3\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.5 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is washed with dilute hydrochloric acid to remove free 
amines, dried, and concentrated to a volume of 10 mL or less. After the 
extract has been exchanged to methanol, it is separated by gas 
chromatography and the parameters are then measured with a nitrogen-
phosphorus detector. \4\
    2.2 The method provides Florisil and alumina column cleanup 
procedures to separate diphenylamine from the nitrosamines and to aid in 
the elimination of interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \5\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Solvent rinses with acetone and pesticide quality 
hexane may be substituted for the muffle furnace heating. Volumetric 
ware should not be heated in a muffle furnace. After drying and cooling, 
glassware should be sealed and stored in a clean environment to prevent 
any accumulation of dust or other contaminants. Store inverted or capped 
with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedures in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.
    3.3 N-Nitrosodiphenylamine is reported \6-9\ to undergo 
transnitrosation reactions. Care must be exercised in the heating or 
concentrating of solutions containing this compound in the presence of 
reactive amines.
    3.4 The sensitive and selective Thermal Energy Analyzer and the 
reductive Hall detector may be used in place of the nitrogen-phosphorus 
detector when interferences are encountered. The Thermal Energy Analyzer 
offers the highest selectivity of the non-MS detectors.

[[Page 146]]

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \10-12\ for 
the information of the analyst.
    4.2 These nitrosamines are known carcinogens, \13-17\ therefore, 
utmost care must be exercised in the handling of these materials. 
Nitrosamine reference standards and standard solutions should be handled 
and prepared in a ventilated glove box within a properly ventilated 
room.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flowmeter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnels--2-L and 250-mL, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.4 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.5 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.6 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.7 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.8 Chromatographic column--Approximately 400 mm long x 22 mm ID, 
with Teflon stopcock and coarse frit filter disc at bottom (Kontes K-
420540-0234 or equivalent), for use in Florisil column cleanup 
procedure.
    5.2.9 Chromatographic column--Approximately 300 mm long x 10 mm ID, 
with Teflon stopcock and coarse frit filter disc at bottom (Kontes K-
420540-0213 or equivalent), for use in alumina column cleanup procedure.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with gas 
chromatograph suitable for on-column injection and all required 
accessories including syringes, analytical columns, gases, detector, and 
strip-chart recorder. A data system is recommended for measuring peak 
areas.
    5.6.1 Column 1--1.8 m long x 4 mm ID glass, packed with 10% Carbowax 
20 M/2% KOH on Chromosorb W-AW (80/100 mesh) or equivalent. This column 
was used to develop the method performance statements in Section 14. 
Guidelines for the use of alternate column packings are provided in 
Section 12.2.
    5.6.2 Column 2--1.8 m long x 4 mm ID glass, packed with 10% SP-2250 
on Supel-coport (100/120 mesh) or equivalent.
    5.6.3 Detector--Nitrogen-phosphorus, reductive Hall, or Thermal 
Energy Analyzer detector. \1 2\ These detectors have proven effective in 
the analysis of wastewaters for the parameters listed in the scope 
(Section 1.1). A nitrogen-phosphorus detector was used to develop the 
method performance statements in Section 14. Guidelines for the use of 
alternate detectors are provided in Section 12.2.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 ml.

[[Page 147]]

    6.3 Sodium thiosulfate--(ACS) Granular.
    6.4 Sulfuric acid (1 + 1)--Slowly, add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.5 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.6 Hydrochloric acid (1 + 9)--Add one volume of concentrated HCl 
(ACS) to nine volumes of reagent water.
    6.7 Acetone, methanol, methylene chloride, pentane--Pesticide 
quality or equivalent.
    6.8 Ethyl ether--Nanograde, redistilled in glass if necessary.
    6.8.1 Ethyl ether must be shown to be free of peroxides before it is 
used as indicated by EM Laboratories Quant test strips. (Available from 
Scientific Products Co., Cat No. P1126-8, and other suppliers.)
    6.8.2 Procedures recommended for removal of peroxides are provided 
with the test strips. After cleanup, 20 mL of ethyl alcohol preservative 
must be added to each liter of ether.
    6.9 Florisil--PR grade (60/100 mesh). Purchase activated at 1250 
[deg]F and store in the dark in glass containers with ground glass 
stoppers or foil-lined screw caps. Before use, activate each batch at 
least 16 h at 130 [deg]C in a foil-covered glass container and allow to 
cool.
    6.10 Alumina--Basic activity Super I, W200 series (ICN Life Sciences 
Group, No. 404571, or equivalent). To prepare for use, place 100 g of 
alumina into a 500-mL reagent bottle and add 2 mL of reagent water. Mix 
the alumina preparation thoroughly by shaking or rolling for 10 min and 
let it stand for at least 2 h. The preparation should be homogeneous 
before use. Keep the bottle sealed tightly to ensure proper activity.
    6.11 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions can be prepared from pure standard materials or 
purchased as certified solutions.
    6.11.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in methanol and dilute 
to volume in a 10-mL volumetric flask. Larger volumes can be used at the 
convenience of the analyst. When compound purity is assayed to be 96% or 
greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.11.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.11.3 Stock standard solutions must be replaced after six months, 
or sooner if comparison with check standards indicates a problem.
    6.12 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatographic operating conditions equivalent to 
those given in Table 1. The gas chromatographic system can be calibrated 
using the external standard technique (Section 7.2) or the internal 
standard technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with methanol. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD), linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with methanol. One of the standards should be at a 
concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.

[[Page 148]]

    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.

   RF = (As)(Cis (Ais)(Cs)

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

    If the RF value over the working range is a constant (<10% RSD), the 
RF can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, and 12.2) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 20 [micro]g/
mL in methanol. The QC check sample concentrate must be obtained from 
the U.S. Environmental Protection Agency, Environmental Monitoring and 
Support Laboratory in Cincinnati, Ohio, if available. If not available 
from that source, the QC check sample concentrate must be obtained from 
another external source. If not available from either source above, the 
QC check sample concentrate must be prepared by the laboratory using 
stock standards prepared independently from those used for calibration.
    8.2.2 Using a pipet, prepare QC check samples at a concentration of 
20 [micro]g/L by adding 1.00 mL of QC check sample concentrate to each 
of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If

[[Page 149]]

any individual s exceeds the precision limit or any individual X falls 
outside the range for accuracy, the system performance is unacceptable 
for that parameter. Locate and correct the source of the problem and 
repeat the test for all parameters of interest beginning with Section 
8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 20 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none (2) the larger of either 5 times higher than the expected 
background concentration or 20 [micro]g/L.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100(A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were caluclated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\18\ If spiking was performed at a concentration lower than 20 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 2, or 
optional QC acceptance criteria caluclated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 3, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T) 2.44(100 S'/T)%. \18\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of

[[Page 150]]

the samples. Field duplicates may be analyzed to assess the precision of 
the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \19\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction. Fill the sample bottles and, if 
residual chlorine is present, add 80 mg of sodium thiosulfate per liter 
of sample and mix well. EPA Methods 330.4 and 330.5 may be used for 
measurement of residual chlorine. \20\ Field test kits are available for 
this purpose. If N-nitrosodiphenylamine is to be determined, adjust the 
sample pH to 7 to 10 with sodium hydroxide solution or sulfuric acid.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \4\
    9.4 Nitrosamines are known to be light sensitive. \7\ Samples should 
be stored in amber or foil-wrapped bottles in order to minimize 
photolytic decomposition.

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel. Check the pH of the sample with wide-range pH paper 
and adjust to within the range of 5 to 9 with sodium hydroxide solution 
or sulfuric acid.
    10.2 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 min 
with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Add 10 mL of hydrochloric acid to the combined extracts and 
shake for 2 min. Allow the layers to separate. Pour the combined extract 
through a solvent-rinsed drying column containing about 10 cm of 
anhydrous sodium sulfate, and collect the extract in the K-D 
concentrator. Rinse the Erlenmeyer flask and column with 20 to 30 mL of 
methylene chloride to complete the quantitative transfer.
    10.6 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.7 Remove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of methylene chloride. A 
5-mL syringe is recommended for this operation. Stopper the concentrator 
tube and store refrigerated if further processing will not be performed 
immediately. If the extract will be stored longer than two days, it 
should be transferred to a Teflon-sealed screw-cap vial. If N-
nitrosodiphenylamine is to be measured by gas chromatography, the 
analyst must first use a cleanup column to eliminate diphenylamine 
interference (Section 11). If N-nitrosodiphenylamine is of no interest, 
the analyst may proceed directly with gas chromatographic analysis 
(Section 12).
    10.8 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-
mL graduated cylinder. Record the sample volume to the nearest 5 mL.

[[Page 151]]

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use either procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of Section 8.2 can be met using the method as revised 
to incorporate the cleanup procedure. Diphenylamine, if present in the 
original sample extract, must be separated from the nitrosamines if N-
nitrosodiphenylamine is to be determined by this method.
    11.2 If the entire extract is to be cleaned up by one of the 
following procedures, it must be concentrated to 2.0 mL. To the 
concentrator tube in Section 10.7, add a clean boiling chip and attach a 
two-ball micro-Snyder column. Prewet the column by adding about 0.5 mL 
of methylene chloride to the top. Place the micr-K-D apparatus on a hot 
water bath (60 to 65 [deg]C) so that the concentrator tube is partially 
immersed in the hot water. Adjust the vertical position of the apparatus 
and the water temperature as required to complete the concentration in 5 
to 10 min. At the proper rate of distillation the balls of the column 
will actively chatter but the chambers will not flood. When the apparent 
volume of liquid reaches about 0.5 mL, remove the K-D apparatus and 
allow it to drain and cool for at least 10 min. Remove the micro-Snyder 
column and rinse its lower joint into the concentrator tube with 0.2 mL 
of methylene chloride. Adjust the final volume to 2.0 mL and proceed 
with one of the following cleanup procedures.
    11.3 Florisil column cleanup for nitrosamines:
    11.3.1 Place 22 g of activated Florisil into a 22-mm ID 
chromatographic column. Tap the column to settle the Florisil and add 
about 5 mm of anhydrous sodium sulfate to the top.
    11.3.2 Preelute the column with 40 mL of ethyl ether/pentane (15 + 
85)(V/V). Discard the eluate and just prior to exposure of the sodium 
sulfate layer to the air, quantitatively transfer the 2-mL sample 
extract onto the column using an additional 2 mL of pentane to complete 
the transfer.
    11.3.3 Elute the column with 90 mL of ethyl ether/pentane (15 + 
85)(V/V) and discard the eluate. This fraction will contain the 
diphenylamine, if it is present in the extract.
    11.3.4 Next, elute the column with 100 mL of acetone/ethyl ether (5 
+ 95)(V/V) into a 500-mL K-D flask equipped with a 10-mL concentrator 
tube. This fraction will contain all of the nitrosamines listed in the 
scope of the method.
    11.3.5 Add 15 mL of methanol to the collected fraction and 
concentrate as in Section 10.6, except use pentane to prewet the column 
and set the water bath at 70 to 75 [deg]C. When the apparatus is cool, 
remove the Snyder column and rinse the flask and its lower joint into 
the concentrator tube with 1 to 2 mL of pentane. Analyze by gas 
chromatography (Section 12).
    11.4 Alumina column cleanup for nitrosamines:
    11.4.1 Place 12 g of the alumina preparation (Section 6.10) into a 
10-mm ID chromatographic column. Tap the column to settle the alumina 
and add 1 to 2 cm of anhydrous sodium sulfate to the top.
    11.4.2 Preelute the column with 10 mL of ethyl ether/pentane (3 + 
7)(V/V). Discard the eluate (about 2 mL) and just prior to exposure of 
the sodium sulfate layer to the air, quantitatively transfer the 2 mL 
sample extract onto the column using an additional 2 mL of pentane to 
complete the transfer.
    11.4.3 Just prior to exposure of the sodium sulfate layer to the 
air, add 70 mL of ethyl ether/pentane (3 + 7)(V/V). Discard the first 10 
mL of eluate. Collect the remainder of the eluate in a 500-mL K-D flask 
equipped with a 10 mL concentrator tube. This fraction contains N-
nitrosodiphenylamine and probably a small amount of N-nitrosodi-n-
propylamine.
    11.4.4 Next, elute the column with 60 mL of ethyl ether/pentane (1 + 
1)(V/V), collecting the eluate in a second K-D flask equipped with a 10-
mL concentrator tube. Add 15 mL of methanol to the K-D flask. This 
fraction will contain N-nitrosodimethylamine, most of the N-nitrosodi-n-
propylamine and any diphenylamine that is present.
    11.4.5 Concentrate both fractions as in Section 10.6, except use 
pentane to prewet the column. When the apparatus is cool, remove the 
Snyder column and rinse the flask and its lower joint into the 
concentrator tube with 1 to 2 mL of pentane. Analyze the fractions by 
gas chromatography (Section 12).

                         12. Gas Chromatography

    12.1 N-nitrosodiphenylamine completely reacts to form diphenylamine 
at the normal operating temperatures of a GC injection port (200 to 250 
[deg]C). Thus, N-nitrosodiphenylamine is chromatographed and detected as 
diphenylamine. Accurate determination depends on removal of 
diphenylamine that may be present in the original extract prior to GC 
analysis (See Section 11).
    12.2 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. Examples of the separations 
achieved by Column 1 are shown in Figures 1 and 2. Other packed or 
capillary (open-tubular) columns, chromatographic conditions, or 
detectors may be used if the requirements of Section 8.2 are met.
    12.3 Calibrate the system daily as described in Section 7.

[[Page 152]]

    12.4 If the extract has not been subjected to one of the cleanup 
procedures in Section 11, it is necessary to exchange the solvent from 
methylene chloride to methanol before the thermionic detector can be 
used. To a 1 to 10-mL volume of methylene chloride extract in a 
concentrator tube, add 2 mL of methanol and a clean boiling chip. Attach 
a two-ball micro-Snyder column to the concentrator tube. Prewet the 
column by adding about 0.5 mL of methylene chloride to the top. Place 
the micro-K-D apparatus on a boiling (100 [deg]C) water bath so that the 
concentrator tube is partially immersed in the hot water. Adjust the 
vertical position of the apparatus and the water temperature as required 
to complete the concentration in 5 to 10 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood. When the apparent volume of liquid reaches 
about 0.5 mL, remove the K-D apparatus and allow it to drain and cool 
for at least 10 min. Remove the micro-Snyder column and rinse its lower 
joint into the concentrator tube with 0.2 mL of methanol. Adjust the 
final volume to 2.0 mL.
    12.5 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    12.6 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush technique. \21\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, and 
the resulting peak size in area or peak height units.
    12.7 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    12.8 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    12.9 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.105

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.106

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \3\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \22\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 4 x MDL to 1000 x MDL. \22\
    14.3 This method was tested by 17 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 0.8 to 55 [micro]g/L. \23\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

[[Page 153]]

                               References

    1. Fine, D.H., Lieb, D., and Rufeh, R. ``Principle of Operation of 
the Thermal Energy Analyzer for the Trace Analysis of Volatile and Non-
volatile N-nitroso Compounds,'' Journal of Chromatography, 107, 351 
(1975).
    2. Fine, D.H., Hoffman, F., Rounbehler, D.P., and Belcher, N.M. 
``Analysis of N-nitroso Compounds by Combined High Performance Liquid 
Chromatography and Thermal Energy Analysis,'' Walker, E.A., Bogovski, P. 
and Griciute, L., Editors, N-nitroso Compounds--Analysis and Formation, 
Lyon, International Agency for Research on Cancer (IARC Scientific 
Publications No. 14), pp. 43-50 (1976).
    3. 40 CFR part 136, appendix B.
    4. ``Determination of Nitrosamines in Industrial and Municipal 
Wastewaters,'' EPA 600/4-82-016, National Technical Information Service, 
PB82-199621, Springfield, Virginia 22161, April 1982.
    5. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    6. Buglass, A.J., Challis, B.C., and Osborn, M.R. ``Transnitrosation 
and Decomposition of Nitrosamines,'' Bogovski, P. and Walker, E.A., 
Editors, N-nitroso Compounds in the Environment, Lyon, International 
Agency for Research on Cancer (IARC Scientific Publication No. 9), pp. 
94-100 (1974).
    7. Burgess, E.M., and Lavanish, J.M. ``Photochemical Decomposition 
of N-nitrosamines,'' Tetrahedon Letters, 1221 (1964)
    8. Druckrey, H., Preussmann, R., Ivankovic, S., and Schmahl, D. 
``Organotrope Carcinogene Wirkungen bei 65 Verschiedenen N-
NitrosoVerbindungen an BD-Ratten,'' Z. Krebsforsch., 69, 103 (1967).
    9. Fiddler, W. ``The Occurrence and Determination of N-nitroso 
Compounds,'' Toxicol. Appl. Pharmacol., 31, 352 (1975).
    10. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    11. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
Part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    12. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    13. Lijinsky, W. ``How Nitrosamines Cause Cancer,'' New Scientist, 
73, 216 (1977).
    14. Mirvish, S.S. ``N-Nitroso compounds: Their Chemical and in vivo 
Formation and Possible Importance as Environmental Carcinogens,'' J. 
Toxicol. Environ. Health, 3, 1267 (1977).
    15. ``Reconnaissance of Environmental Levels of Nitrosamines in the 
Central United States,'' EPA-330/1-77-001, National Enforcement 
Investigations Center, U.S. Environmental Protection Agency (1977).
    16. ``Atmospheric Nitrosamine Assessment Report,'' Office of Air 
Quality Planning and Standards, U.S. Environmental Protection Agency, 
Research Triangle Park, North Carolina (1976).
    17. ``Scientific and Technical Assessment Report on Nitrosamines,'' 
EPA-660/6-7-001, Office of Research and Development, U.S. Environmental 
Protection Agency (1976).
    18. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value of 1.22 
derived in this report.)
    19. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    20. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    21. Burke, J. A. ``Gas Chromatography for Pesticide Residue 
Analysis; Some Practical Aspects,'' Journal of the Association of 
Official Analytical Chemists, 48, 1037 (1965).
    22. ``Method Detection Limit and Analytical Curve Studies EPA 
Methods 606, 607, and 608,'' Special letter report for EPA Contract 68-
03-2606, U.S. Environmental Protection Agency, Environmental Monitoring 
and Support Laboratory, Cincinnati, Ohio 45268, June 1980.
    23. ``EPA Method Study 17 Method 607--Nitrosamines,'' EPA 600/4-84-
051, National Technical Information Service, PB84-207646, Springfield, 
Virginia 22161, June 1984.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                     Retention time (min)       Method
                                  --------------------------  detection
            Parameter                                           limit
                                     Column 1     Column 2    ([micro]g/
                                                                  L)
------------------------------------------------------------------------
N-Nitrosodimethylamine...........          4.1         0.88         0.15
N-Nitrosodi-n-propylamine........         12.1          4.2          .46

[[Page 154]]

 
N-Nitrosodiphenylamine \a\.......     \b\ 12.8      \c\ 6.4          .81
------------------------------------------------------------------------
Column 1 conditions: Chromosorb W-AW (80/100 mesh) coated with 10%
  Carbowax 20 M/2% KOH packed in a 1.8 m long x 4mm ID glass column with
  helium carrier gas at 40 mL/min flow rate. Column temperature held
  isothermal at 110 [deg]C, except where otherwise indicated.
Column 2 conditions: Supelcoport (100/120 mesh) coated with 10% SP-2250
  packed in a 1.8 m long x 4 mm ID glass column with helium carrier gas
  at 40 mL/min flow rate. Column temperature held isothermal at 120
  [deg]C, except where otherwise indicated.
\a\ Measured as diphenylamine.
\b\ 220 [deg]C column temperature.
\c\ 210 [deg]C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 607
----------------------------------------------------------------------------------------------------------------
                                                               Test conc.  Limit for s  Range for X   Range for
                          Parameter                            ([micro]g/   ([micro]g/   ([micro]g/     P, Ps
                                                                   L)           L)           L)       (percent)
----------------------------------------------------------------------------------------------------------------
N-Nitrosodimethylamine......................................           20          3.4     4.6-20.0       13-109
N-Nitrosodiphenyl...........................................           20          6.1     2.1-24.5        D-139
N-Nitrosodi-n-propylamine...................................           20          5.7    11.5-26.8      45-146
----------------------------------------------------------------------------------------------------------------
s = Standard deviation for four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 607
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                              recovery, X'   precision, sr'   precision, S'
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
N-Nitrosodimethylamine..........................................    0.37C + 0.06      0.25X-0.04    0.25X + 0.11
N-Nitrosodiphenylamine..........................................    0.64C + 0.52      0.36X-1.53      0.46X-0.47
N-Nitrosodi-n-propylamine.......................................      0.96C-0.07    0.15X + 0.13    0.21X + 0.15
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


[[Page 155]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.017


[[Page 156]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.018


[[Page 157]]

       Method 608.3--Organochlorine Pesticides And PCBs By GC/HSD

                        1. Scope and Application

    1.1 This method is for determination of organochlorine pesticides 
and polychlorinated biphenyls (PCBs) in industrial discharges and other 
environmental samples by gas chromatography (GC) combined with a 
halogen-specific detector (HSD; e.g., electron capture, electrolytic 
conductivity), as provided under 40 CFR 136.1. This revision is based on 
a previous protocol (Reference 1), on the revision promulgated October 
26, 1984, on an inter-laboratory method validation study (Reference 2), 
and on EPA Method 1656 (Reference 16). The analytes that may be 
qualitatively and quantitatively determined using this method and their 
CAS Registry numbers are listed in Table 1.
    1.2 This method may be extended to determine the analytes listed in 
Table 2. However, extraction or gas chromatography challenges for some 
of these analytes may make quantitative determination difficult.
    1.3 When this method is used to analyze unfamiliar samples for an 
analyte listed in Table 1 or Table 2, analyte identification must be 
supported by at least one additional qualitative technique. This method 
gives analytical conditions for a second GC column that can be used to 
confirm and quantify measurements. Additionally, Method 625.1 provides 
gas chromatograph/mass spectrometer (GC/MS) conditions appropriate for 
the qualitative confirmation of results for the analytes listed in 
Tables 1 and 2 using the extract produced by this method, and Method 
1699 (Reference 18) provides high resolution GC/MS conditions for 
qualitative confirmation of results using the original sample. When such 
methods are used to confirm the identifications of the target analytes, 
the quantitative results should be derived from the procedure with the 
calibration range and sensitivity that are most appropriate for the 
intended application.
    1.4 The large number of analytes in Tables 1 and 2 makes testing 
difficult if all analytes are determined simultaneously. Therefore, it 
is necessary to determine and perform quality control (QC) tests for the 
``analytes of interest'' only. The analytes of interest are those 
required to be determined by a regulatory/control authority or in a 
permit, or by a client. If a list of analytes is not specified, the 
analytes in Table 1 must be determined, at a minimum, and QC testing 
must be performed for these analytes. The analytes in Table 1 and some 
of the analytes in Table 2 have been identified as Toxic Pollutants (40 
CFR 401.15), expanded to a list of Priority Pollutants (40 CFR part 423, 
appendix A).
    1.5 In this revision to Method 608, Chlordane has been listed as the 
alpha- and gamma- isomers in Table 1. Reporting may be by the individual 
isomers, or as the sum of the concentrations of these isomers, as 
requested or required by a regulatory/control authority or in a permit. 
Technical Chlordane is listed in Table 2 and may be used in cases where 
historical reporting has only been the Technical Chlordane. Toxaphene 
and the PCBs have been moved from Table 1 to Table 2 (Additional 
Analytes) to distinguish these analytes from the analytes required in 
quality control tests (Table 1). QC acceptance criteria for Toxaphene 
and the PCBs have been retained in Table 4 and may continue to be 
applied if desired, or if these analytes are requested or required by a 
regulatory/control authority or in a permit. Method 1668C (Reference 17) 
may be useful for determination of PCBs as individual chlorinated 
biphenyl congeners, and Method 1699 (Reference 18) may be useful for 
determination of the pesticides listed in this method. However, at the 
time of writing of this revision, Methods 1668C and 1699 had not been 
approved for use at 40 CFR part 136.
    1.6 Method detection limits (MDLs; Reference 3) for the analytes in 
Tables 1 and some of the analytes in Table 2 are listed in those tables. 
These MDLs were determined in reagent water (Reference 3). Advances in 
analytical technology, particularly the use of capillary (open-tubular) 
columns, allowed laboratories to routinely achieve MDLs for the analytes 
in this method that are 2-10 times lower than those in the version 
promulgated in 1984. The MDL for an analyte in a specific wastewater may 
differ from those listed, depending upon the nature of interferences in 
the sample matrix.
    1.6.1 EPA has promulgated this method at 40 CFR part 136 for use in 
wastewater compliance monitoring under the National Pollutant Discharge 
Elimination System (NPDES). The data reporting practices described in 
section 15.6 are focused on such monitoring needs and may not be 
relevant to other uses of the method.
    1.6.2 This method includes ``reporting limits'' based on EPA's 
``minimum level'' (ML) concept (see the glossary in section 23). Tables 
1 and 2 contain MDL values and ML values for many of the analytes.
    1.7 The separatory funnel and continuous liquid-liquid sample 
extraction and concentration steps in this method are essentially the 
same as those steps in Methods 606, 609, 611, and 612. Thus, a single 
sample may be extracted to measure the analytes included in the scope of 
each of these methods. Samples may also be extracted using a disk-based 
solid-phase extraction (SPE) procedure developed by the 3M Corporation 
and approved by EPA as an Alternate Test Procedure (ATP) for wastewater 
analyses in 1995 (Reference 20).
    1.8 This method is performance-based. It may be modified to improve 
performance (e.g., to overcome interferences or improve

[[Page 158]]

the accuracy of results) provided all performance requirements are met.
    1.8.1 Examples of allowed method modifications are described at 40 
CFR 136.6. Other examples of allowed modifications specific to this 
method are described in section 8.1.2.
    1.8.2 Any modification beyond those expressly permitted at 40 CFR 
136.6 or in section 8.1.2 of this method shall be considered a major 
modification subject to application and approval of an alternate test 
procedure under 40 CFR 136.4 and 136.5.
    1.8.3 For regulatory compliance, any modification must be 
demonstrated to produce results equivalent or superior to results 
produced by this method when applied to relevant wastewaters (section 
8.1.2).
    1.9 This method is restricted to use by or under the supervision of 
analysts experienced in the use of GC/HSD. The laboratory must 
demonstrate the ability to generate acceptable results with this method 
using the procedure in section 8.2.
    1.10 Terms and units of measure used in this method are given in the 
glossary at the end of the method.

                          2. Summary of Method

    2.1 A measured volume of sample, the amount required to meet an MDL 
or reporting limit (nominally 1-L), is extracted with methylene chloride 
using a separatory funnel, a continuous liquid/liquid extractor, or 
disk-based solid-phase extraction equipment. The extract is dried and 
concentrated for cleanup, if required. After cleanup, or if cleanup is 
not required, the extract is exchanged into an appropriate solvent and 
concentrated to the volume necessary to meet the required compliance or 
detection limit, and analyzed by GC/HSD.
    2.2 Qualitative identification of an analyte in the extract is 
performed using the retention times on dissimilar GC columns. 
Quantitative analysis is performed using the peak areas or peak heights 
for the analyte on the dissimilar columns with either the external or 
internal standard technique.
    2.3 Florisil[supreg], alumina, a C18 solid-phase cleanup, and an 
elemental sulfur cleanup procedure are provided to aid in elimination of 
interferences that may be encountered. Other cleanup procedures may be 
used if demonstrated to be effective for the analytes in a wastewater 
matrix.

                   3. Contamination and Interferences

    3.1 Solvents, reagents, glassware, and other sample processing lab 
ware may yield artifacts, elevated baselines, or matrix interferences 
causing misinterpretation of chromatograms. All materials used in the 
analysis must be demonstrated free from contamination and interferences 
by running blanks initially and with each extraction batch (samples 
started through the extraction process in a given 24-hour period, to a 
maximum of 20 samples--see Glossary for detailed definition), as 
described in section 8.5. Specific selection of reagents and 
purification of solvents by distillation in all-glass systems may be 
required. Where possible, labware is cleaned by extraction or solvent 
rinse, or baking in a kiln or oven.
    3.2 Glassware must be scrupulously cleaned (Reference 4). Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and reagent water. The glassware 
should then be drained dry, and heated at 400 [deg]C for 15-30 minutes. 
Some thermally stable materials, such as PCBs, may require higher 
temperatures and longer baking times for removal. Solvent rinses with 
pesticide quality acetone, hexane, or other solvents may be substituted 
for heating. Do not heat volumetric labware above 90 [deg]C. After 
drying and cooling, store inverted or capped with solvent-rinsed or 
baked aluminum foil in a clean environment to prevent accumulation of 
dust or other contaminants.
    3.3 Interferences by phthalate esters can pose a major problem in 
pesticide analysis when using the electron capture detector. The 
phthalate esters generally appear in the chromatogram as large late 
eluting peaks, especially in the 15 and 50% fractions from 
Florisil[supreg]. Common flexible plastics contain varying amounts of 
phthalates that may be extracted or leached from such materials during 
laboratory operations. Cross contamination of clean glassware routinely 
occurs when plastics are handled during extraction steps, especially 
when solvent-wetted surfaces are handled. Interferences from phthalates 
can best be minimized by avoiding use of non-fluoropolymer plastics in 
the laboratory. Exhaustive cleanup of reagents and glassware may be 
required to eliminate background phthalate contamination (References 5 
and 6). Interferences from phthalate esters can be avoided by using a 
microcoulometric or electrolytic conductivity detector.
    3.4 Matrix interferences may be caused by contaminants co-extracted 
from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. 
Interferences extracted from samples high in total organic carbon (TOC) 
may result in elevated baselines, or by enhancing or suppressing a 
signal at or near the retention time of an analyte of interest. Analyses 
of the matrix spike and matrix spike duplicate (Section 8.3) may be 
useful in identifying matrix interferences, and the cleanup procedures 
in Section 11 may aid in eliminating these interferences. EPA has 
provided guidance that may aid in overcoming matrix

[[Page 159]]

interferences (Reference 7); however, unique samples may require 
additional cleanup approaches to achieve the MDLs listed in Tables 1 and 
2.

                                4. Safety

    4.1 Hazards associated with each reagent used in this method have 
not been precisely defined; however, each chemical compound should be 
treated as a potential health hazard. From this viewpoint, exposure to 
these chemicals must be reduced to the lowest possible level by whatever 
means available. The laboratory is responsible for maintaining a current 
awareness file of OSHA regulations regarding the safe handling of the 
chemicals specified in this method. A reference file of safety data 
sheets (SDSs, OSHA, 29 CFR 1910.12009(g)) should also be made available 
to all personnel involved in sample handling and chemical analysis. 
Additional references to laboratory safety are available and have been 
identified (References 8 and 9) for the information of the analyst.
    4.2 The following analytes covered by this method have been 
tentatively classified as known or suspected human or mammalian 
carcinogens: 4,4[min]-DDT, 4,4[min]-DDD, the BHCs, and the PCBs. Primary 
standards of these toxic analytes should be prepared in a chemical fume 
hood, and a NIOSH/MESA approved toxic gas respirator should be worn when 
high concentrations are handled.
    4.3 This method allows the use of hydrogen as a carrier gas in place 
of helium (section 5.8.2). The laboratory should take the necessary 
precautions in dealing with hydrogen, and should limit hydrogen flow at 
the source to prevent buildup of an explosive mixture of hydrogen in 
air.

                       5. Apparatus and Materials

    Note: Brand names and suppliers are for illustration purposes only. 
No endorsement is implied. Equivalent performance may be achieved using 
equipment and materials other than those specified here. Demonstrating 
that the equipment and supplies used in the laboratory achieve the 
required performance is the responsibility of the laboratory. Suppliers 
for equipment and materials in this method may be found through an on-
line search. Please do not contact EPA for supplier information.

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--Amber glass bottle large enough to contain 
the necessary sample volume (nominally 1 L), fitted with a 
fluoropolymer-lined screw cap. Foil may be substituted for fluoropolymer 
if the sample is not corrosive. If amber bottles are not available, 
protect samples from light. Unless pre-cleaned, the bottle and cap liner 
must be washed, rinsed with acetone or methylene chloride, and dried 
before use to minimize contamination.
    5.1.2 Automatic sampler (optional)--The sampler must use a glass or 
fluoropolymer container and tubing for sample collection. If the sampler 
uses a peristaltic pump, a minimum length of compressible silicone 
rubber tubing may be used. Before use, rinse the compressible tubing 
thoroughly with methanol, followed by repeated rinsing with reagent 
water to minimize the potential for sample contamination. An integrating 
flow meter is required to collect flow proportional composites. The 
sample container must be kept refrigerated at <=6 [deg]C and protected 
from light during compositing.
    5.2. Lab ware.
    5.2.1 Extraction.
    5.2.1.1 pH measurement.
    5.2.1.1.1 pH meter, with combination glass electrode.
    5.2.1.1.2 pH paper, wide range (Hydrion Papers, or equivalent).
    5.2.1.2 Separatory funnel--Size appropriate to hold the sample and 
extraction solvent volumes, equipped with fluoropolymer stopcock.
    5.2.1.3 Continuous liquid-liquid extractor--Equipped with 
fluoropolymer or glass connecting joints and stopcocks requiring no 
lubrication. (Hershberg-Wolf Extractor, Ace Glass Company, Vineland, NJ, 
or equivalent.)
    5.2.1.3.1 Round-bottom flask, 500-mL, with heating mantle.
    5.2.1.3.2 Condenser, Graham, to fit extractor.
    5.2.1.4 Solid-phase extractor--90-mm filter apparatus (Figure 2) or 
multi-position manifold.

    Note: The approved ATP for solid-phase extraction is limited to 
disk-based extraction media and associated peripheral equipment.

    5.2.1.4.1 Vacuum system--Capable of achieving 0.1 bar (25 inch) Hg 
(house vacuum, vacuum pump, or water aspirator), equipped with shutoff 
valve and vacuum gauge.
    5.2.1.4.2 Vacuum trap--Made from 500-mL sidearm flask fitted with 
single-hole rubber stopper and glass tubing.
    5.2.2 Filtration.
    5.2.2.1 Glass powder funnel, 125- to 250-mL.
    5.2.2.2 Filter paper for above, Whatman 41, or equivalent.
    5.2.2.3 Prefiltering aids--90-mm 1-[micro]m glass fiber filter or 
Empore[supreg] Filter Aid 400.
    5.2.3 Drying column.
    5.2.3.1 Chromatographic column--Approximately 400 mm long x 15 mm 
ID, with fluoropolymer stopcock and coarse frit filter disc (Kontes or 
equivalent).
    5.2.3.2 Glass wool--Pyrex, extracted with methylene chloride or 
baked at 450 [deg]C for 1 hour minimum.

[[Page 160]]

    5.2.4 Column for Florisil[supreg] or alumina cleanup--Approximately 
300 mm long x 10 mm ID, with fluoropolymer stopcock. (This column is not 
required if cartridges containing Florisil[supreg] are used.)
    5.2.5 Concentration/evaporation.

    Note: Use of a solvent recovery system with the K-D or other solvent 
evaporation apparatus is strongly recommended.

    5.2.5.1 Kuderna-Danish concentrator.
    5.2.5.1.1 Concentrator tube, Kuderna-Danish--10-mL, graduated 
(Kontes or equivalent). Calibration must be checked at the volumes 
employed for extract volume measurement. A ground-glass stopper is used 
to prevent evaporation of extracts.
    5.2.5.1.2 Evaporative flask, Kuderna-Danish--500-mL (Kontes or 
equivalent). Attach to concentrator tube with connectors.
    5.2.5.1.3 Snyder column, Kuderna/Danish--Three-ball macro (Kontes or 
equivalent).
    5.2.5.1.4 Snyder column--Two-ball micro (Kontes or equivalent).
    5.2.5.1.5 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C), installed in a 
hood using appropriate engineering controls to limit exposure to solvent 
vapors.
    5.2.5.2 Nitrogen evaporation device--Equipped with heated bath that 
can be maintained at an appropriate temperature for the solvent and 
analytes. (N-Evap, Organomation Associates, Inc., or equivalent).
    5.2.5.3 Rotary evaporator--Buchi/Brinkman-American Scientific or 
equivalent, equipped with a variable temperature water bath, vacuum 
source with shutoff valve at the evaporator, and vacuum gauge.
    5.2.5.3.1 A recirculating water pump and chiller are recommended, as 
use of tap water for cooling the evaporator wastes large volumes of 
water and can lead to inconsistent performance as water temperatures and 
pressures vary.
    5.2.5.3.2 Round-bottom flask--100-mL and 500-mL or larger, with 
ground-glass fitting compatible with the rotary evaporator

    Note: This equipment is used to prepare copper foil or copper powder 
for removing sulfur from sample extracts (see Section 6.7.4).

    5.2.5.4 Automated concentrator--Equipped with glassware sufficient 
to concentrate 3-400 mL extract to a final volume of 1-10 mL under 
controlled conditions of temperature and nitrogen flow (Turbovap, or 
equivalent). Follow manufacturer's directions and requirements.
    5.2.5.5 Boiling chips--Glass, silicon carbide, or equivalent, 
approximately 10/40 mesh. Heat at 400 [deg]C for 30 minutes, or solvent 
rinse or Soxhlet extract with methylene chloride.
    5.2.6 Solid-phase extraction disks--90-mm extraction disks 
containing 2 g of 8-[micro]m octadecyl (C18) bonded silica uniformly 
enmeshed in a matrix of inert PTFE fibrils (3M Empore[supreg] or 
equivalent). The disks should not contain any organic compounds, either 
from the PTFE or the bonded silica, which will leach into the methylene 
chloride eluant. One liter of reagent water should pass through the 
disks in 2-5 minutes, using a vacuum of at least 25 inches of mercury.

    Note: Extraction disks from other manufacturers may be used in this 
procedure, provided that they use the same solid-phase materials (i.e., 
octadecyl bonded silica). Disks of other diameters also may be used, but 
may adversely affect the flow rate of the sample through the disk.

    5.3 Vials.
    5.3.1 Extract storage--10- to 15-mL, amber glass, with 
fluoropolymer-lined screw cap.
    5.3.2 GC autosampler--1- to 5-mL, amber glass, with fluoropolymer-
lined screw- or crimp-cap, to fit GC autosampler.
    5.4 Balances.
    5.4.1 Analytical--Capable of accurately weighing 0.1 mg.
    5.4.2 Top loading--Capable of weighing 10 mg.
    5.5 Sample cleanup.
    5.5.1 Oven--For baking and storage of adsorbents, capable of 
maintaining a constant temperature (5 [deg]C) in 
the range of 105-250 [deg]C.
    5.5.2 Muffle furnace--Capable of cleaning glassware or baking sodium 
sulfate in the range of 400-450 [deg]C.
    5.5.3 Vacuum system and cartridges for solid-phase cleanup (see 
Section 11.2).
    5.5.3.1 Vacuum system--Capable of achieving 0.1 bar (25 in.) Hg 
(house vacuum, vacuum pump, or water aspirator), equipped with shutoff 
valve and vacuum gauge.
    5.5.3.2 VacElute Manifold (Analytichem International, or 
equivalent).
    5.5.3.3 Vacuum trap--Made from 500-mL sidearm flask fitted with 
single-hole rubber stopper and glass tubing.
    5.5.3.4 Rack for holding 50-mL volumetric flasks in the manifold.
    5.5.3.5 Cartridge--Mega Bond Elute, Non-polar, C18 Octadecyl, 10 g/
60 mL (Analytichem International or equivalent), used for solid-phase 
cleanup of sample extracts (see Section 11.2).
    5.5.4 Sulfur removal tube--40- to 50-mL bottle, test tube, or 
Erlenmeyer flask with fluoropolymer-lined screw cap.
    5.6 Centrifuge apparatus.
    5.6.1 Centrifuge--Capable of rotating 500-mL centrifuge bottles or 
15-mL centrifuge tubes at 5,000 rpm minimum.
    5.6.2 Centrifuge bottle--500-mL, with screw cap, to fit centrifuge.
    5.6.3 Centrifuge tube--15-mL, with screw cap, to fit centrifuge.
    5.7 Miscellaneous lab ware--Graduated cylinders, pipettes, beakers, 
volumetric flasks, vials, syringes, and other lab ware

[[Page 161]]

necessary to support the operations in this method.
    5.8 Gas chromatograph--Dual-column with simultaneous split/
splitless, temperature programmable split/splitless (PTV), or on-column 
injection; temperature program with isothermal holds, and all required 
accessories including syringes, analytical columns, gases, and 
detectors. An autosampler is highly recommended because it injects 
volumes more reproducibly than manual injection techniques. 
Alternatively, two separate single-column gas chromatographic systems 
may be employed.
    5.8.1 Example columns and operating conditions.
    5.8.1.1 DB-608 (or equivalent), 30-m long x 0.53-mm ID fused-silica 
capillary, 0.83-[micro]m film thickness.
    5.8.1.2 DB-1701 (or equivalent), 30-m long x 0.53-mm ID fused-silica 
capillary, 1.0-[micro]m film thickness.
    5.8.1.3 Suggested operating conditions used to meet the retention 
times shown in Table 3 are:
    (a) Carrier gas flow rate: Approximately 7 mL/min,
    (b) Initial temperature: 150 [deg]C for 0.5 minute,
    (c) Temperature program: 150-270 [deg]C at 5 [deg]C/min, and
    (d) Final temperature: 270 [deg]C, until trans-Permethrin elutes.

    Note: Other columns, internal diameters, film thicknesses, and 
operating conditions may be used, provided that the performance 
requirements in this method are met. However, the column pair chosen 
must have dissimilar phases/chemical properties in order to separate the 
compounds of interest in different retention time order. Columns that 
only differ in the length, ID, or film thickness, but use the same 
stationary phase do not qualify as ``dissimilar.''

    5.8.2 Carrier gas--Helium or hydrogen. Data in the tables in this 
method were obtained using helium carrier gas. If hydrogen is used, 
analytical conditions may need to be adjusted for optimum performance, 
and calibration and all QC tests must be performed with hydrogen carrier 
gas. See Section 4.3 for precautions regarding the use of hydrogen as a 
carrier gas.
    5.8.3 Detector--Halogen-specific detector (electron capture detector 
[ECD], electrolytic conductivity detector [ELCD], or equivalent). The 
ECD has proven effective in the analysis of wastewaters for the analytes 
listed in Tables 1 and 2, and was used to develop the method performance 
data in Section 17 and Tables 4 and 5.
    5.8.4 Data system--A computer system must be interfaced to the GC 
that allows continuous acquisition and storage of data from the 
detectors throughout the chromatographic program. The computer must have 
software that allows searching GC data for specific analytes, and for 
plotting responses versus time. Software must also be available that 
allows integrating peak areas or peak heights in selected retention time 
windows and calculating concentrations of the analytes.

                        6. Reagents and Standards

    6.1 pH adjustment.
    6.1.1 Sodium hydroxide solutions.
    6.1.1.1 Concentrated (10 M)--Dissolve 40 g of NaOH (ACS) in reagent 
water and dilute to 100 mL.
    6.1.1.2 Dilute (1 M)--Dissolve 40 g NaOH in 1 L of reagent water.
    6.1.2 Sulfuric acid (1+1)--Slowly add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.1.3 Hydrochloric acid--Reagent grade, 6 N.
    6.2 Sodium thiosulfate--(ACS) granular.
    6.3 Sodium sulfate--Sodium sulfate, reagent grade, granular 
anhydrous (Baker or equivalent), rinsed with methylene chloride, baked 
in a shallow tray at 450 [deg]C for 1 hour minimum, cooled in a 
desiccator, and stored in a pre-cleaned glass bottle with screw cap 
which prevents moisture from entering. If, after heating, the sodium 
sulfate develops a noticeable grayish cast (due to the presence of 
carbon in the crystal matrix), that batch of reagent is not suitable for 
use and should be discarded. Extraction with methylene chloride (as 
opposed to simple rinsing) and baking at a lower temperature may produce 
sodium sulfate suitable for use.
    6.4 Reagent water--Reagent water is defined as water in which the 
analytes of interest and interfering compounds are not observed at the 
MDLs of the analytes in this method.
    6.5 Solvents--Methylene chloride, acetone, methanol, hexane, 
acetonitrile, and isooctane, high purity pesticide quality, or 
equivalent, demonstrated to be free of the analytes and interferences 
(section 3). Purification of solvents by distillation in all-glass 
systems may be required.

    Note: The standards and final sample extracts must be prepared in 
the same final solvent.

    6.6 Ethyl ether--Nanograde, redistilled in glass if necessary. Ethyl 
ether must be shown to be free of peroxides before use, as indicated by 
EM Laboratories Quant test strips (available from Scientific Products 
Co. and other suppliers). Procedures recommended for removal of 
peroxides are provided with the test strips. After removal of peroxides, 
add 20 mL of ethyl alcohol preservative to each liter of ether.
    6.7 Materials for sample cleanup.
    6.7.1 Florisil[supreg]--PR grade (60/100 mesh), activated at 650-700 
[deg]C, stored in the dark in a glass container with fluoropolymer-lined

[[Page 162]]

screw cap. Activate each batch immediately prior to use for 16 hours 
minimum at 130 [deg]C in a foil-covered glass container and allow to 
cool. Alternatively, 500 mg cartridges (J.T. Baker, or equivalent) may 
be used.
    6.7.1.1 Cartridge certification--Each cartridge lot must be 
certified to ensure recovery of the analytes of interest and removal of 
2,4,6-trichlorophenol. To make the test mixture, add the trichlorophenol 
solution (section 6.7.1.3) to the same standard used to prepare the 
Quality Control Check Sample (section 6.8.3). Transfer the mixture to 
the column and dry the column. Pre-elute with three 10-mL portions of 
elution solvent, drying the column between elutions. Elute the cartridge 
with 10 mL each of methanol and water, as in section 11.2.3.3.
    6.7.1.2 Concentrate the eluant to per section 10.3.3, exchange to 
isooctane or hexane per section 10.3.3, and inject 1.0 [micro]L of the 
concentrated eluant into the GC using the procedure in section 12. The 
recovery of all analytes (including the unresolved GC peaks) shall be 
within the ranges for calibration verification (section 13.6 and Table 
4), the recovery of trichlorophenol shall be less than 5%, and no peaks 
interfering with the target analytes shall be detected. Otherwise the 
Florisil cartridge is not performing properly and the cartridge lot 
shall be rejected.
    6.7.1.3 Florisil cartridge calibration solution--2,4,6-
Trichlorophenol, 0.1 [micro]g/mL in acetone.
    6.7.2 SPE elution solvent--Methylene chloride:acetonitrile:hexane 
(50:3:47).
    6.7.3 Alumina, neutral, Brockman Activity I, 80-200 mesh (Fisher 
Scientific certified, or equivalent). Heat in a glass bottle for 16 
hours at 400 to 450 [deg]C. Seal and cool to room temperature. Add 7% 
(w/w) reagent water and mix for 10 to 12 hours. Keep bottle tightly 
sealed.
    6.7.4 Sulfur removal.
    6.7.4.1 Copper foil or powder--Fisher, Alfa Aesar, or equivalent. 
Cut copper foil into approximately 1-cm squares. Copper must be 
activated before it may be used, as described below.
    6.7.4.1.1 Place the quantity of copper needed for sulfur removal 
(section 11.5.1.3) in a ground-glass-stoppered Erlenmeyer flask or 
bottle. Cover the foil or powder with methanol.
    6.7.4.1.2 Add HCl dropwise (0.5-1.0 mL) while swirling, until the 
copper brightens.
    6.7.4.1.3 Pour off the methanol/HCl and rinse 3 times with reagent 
water to remove all traces of acid, then 3 times with acetone, then 3 
times with hexane.
    6.7.4.1.4 For copper foil, cover with hexane after the final rinse. 
Store in a stoppered flask under nitrogen until used. For the powder, 
dry on a rotary evaporator. Store in a stoppered flask under nitrogen 
until used. Inspect the copper foil or powder before each use. It must 
have a bright, non-oxidized appearance to be effective. Copper foil or 
powder that has oxidized may be reactivated using the procedure 
described above.
    6.7.4.2 Tetrabutylammonium sulfite (TBA sulfite)--Prepare as 
described below.
    6.7.4.2.1 Tetrabutylammonium hydrogen sulfate, 
[CH3(CH2)3]4NHSO4.

    6.7.4.2.2 Sodium sulfite, Na2SO3.
    6.7.4.2.3 Dissolve approximately 3 g tetrabutylammonium hydrogen 
sulfate in 100 mL of reagent water in an amber bottle with 
fluoropolymer-lined screw cap. Extract with three 20-mL portions of 
hexane and discard the hexane extracts.
    6.7.4.2.4 Add 25 g sodium sulfite to produce a saturated solution. 
Store at room temperature. Replace after 1 month.
    6.7.5 Sodium chloride--Reagent grade, prepare at 5% (w/v) solution 
in reagent water.
    6.8 Stock standard solutions--Stock standard solutions may be 
prepared from pure materials, or purchased as certified solutions. 
Traceability must be to the National Institute of Standards and 
Technology (NIST) or other national or international standard, when 
available. Stock solution concentrations alternative to those below may 
be used. Because of the toxicity of some of the compounds, primary 
dilutions should be prepared in a hood, and a NIOSH/MESA approved toxic 
gas respirator should be worn when high concentrations of neat materials 
are handled. The following procedure may be used to prepare standards 
from neat materials.
    6.8.1 Accurately weigh about 0.0100 g of pure material in a 10-mL 
volumetric flask. Dilute to volume in pesticide quality hexane, 
isooctane, or other suitable solvent. Larger volumes may be used at the 
convenience of the laboratory. When compound purity is assayed to be 96% 
or greater, the weight may be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards may be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.8.1.1 Unless stated otherwise in this method, store non-aqueous 
standards in fluoropolymer-lined screw-cap, or heat-sealed, glass 
containers, in the dark at -20 to -10 [deg]C. Store aqueous standards; 
e.g., the aqueous LCS (section 8.4), in the dark at <=6 [deg]C, but do 
not freeze.
    6.8.1.2 Standards prepared by the laboratory may be stored for up to 
one year, except when comparison with QC check standards indicates that 
a standard has degraded or become more concentrated due to evaporation, 
or unless the laboratory has data on file to prove stability for a 
longer period. Commercially prepared standards may be stored until the 
expiration date provided by the vendor, except when comparison with QC 
check standards indicates that a standard

[[Page 163]]

has degraded or become more concentrated due to evaporation, or unless 
the laboratory has data from the vendor on file to prove stability for a 
longer period.
    6.8.2 Calibration solutions--It is necessary to prepare calibration 
solutions for the analytes of interest (section 1.4) only using an 
appropriate solvent (isooctane or hexane may be used). Whatever solvent 
is used, both the calibration standards and the final sample extracts 
must use the same solvent. Other analytes may be included as desired.
    6.8.2.1 Prepare calibration standards for the single-component 
analytes of interest and surrogates at a minimum of three concentration 
levels (five are suggested) by adding appropriate volumes of one or more 
stock standards to volumetric flasks. One of the calibration standards 
should be at a concentration at or below the ML specified in Table 1, or 
2, or as specified by a regulatory/control authority or in a permit. The 
ML value may be rounded to a whole number that is more convenient for 
preparing the standard, but must not exceed the ML value listed in 
Tables 1 or 2 for those analytes which list ML values. Alternatively, 
the laboratory may establish an ML for each analyte based on the 
concentration of the lowest calibration standard in a series of 
standards produced by the laboratory or obtained from a commercial 
vendor, again, provided that the ML does not exceed the ML in Table 1 
and 2, and provided that the resulting calibration meets the acceptance 
criteria in section 7.5.2 based on the RSD, RSE, or R\2\.
    (a) The other concentrations should correspond to the expected range 
of concentrations found in real samples or should define the working 
range of the GC system. A minimum of six concentration levels is 
required for a second order, non-linear (e.g., quadratic; ax\2\ + bx + c 
= 0) calibration (section 7.5.2 or 7.6.2). Calibrations higher than 
second order are not allowed. A separate standard near the MDL may be 
analyzed as a check on sensitivity, but should not be included in the 
linearity assessment. The solvent for the standards must match the final 
solvent for the sample extracts (e.g., isooctane or hexane).

    Note: The option for non-linear calibration may be necessary to 
address specific instrumental techniques. However, it is not EPA's 
intent to allow non-linear calibration to be used to compensate for 
detector saturation or to avoid proper instrument maintenance.

    (b) Given the number of analytes included in this method, it is 
highly likely that some will coelute on one or both of the GC columns 
used for the analysis. Divide the analytes into two or more groups and 
prepare separate calibration standards for each group, at multiple 
concentrations (e.g., a five-point calibration will require ten 
solutions to cover two groups of analytes). Table 7 provides information 
on dividing the target analytes into separate calibration mixtures that 
should minimize or eliminate co-elutions. This table is provided solely 
as guidance, based on the GC columns suggested in this method. If an 
analyte listed in Table 7 is not an analyte of interest in a given 
laboratory setting, then it need not be included in a calibration 
mixture.

    Note: Many commercially available standards are divided into 
separate mixtures to address this issue.

    (c) If co-elutions occur in analysis of a sample, a co-elution on 
one column is acceptable so long as effective separation of the co-
eluting compounds can be achieved on the second column.
    6.8.2.2 Multi-component analytes (e.g., PCBs as Aroclors, and 
Toxaphene).
    6.8.2.2.1 A standard containing a mixture of Aroclor 1016 and 
Aroclor 1260 will include many of the peaks represented in the other 
Aroclor mixtures. As a result, a multi-point initial calibration 
employing a mixture of Aroclors 1016 and 1260 at three to five 
concentrations should be sufficient to demonstrate the linearity of the 
detector response without the necessity of performing multi-point 
initial calibrations for each of the seven Aroclors. In addition, such a 
mixture can be used as a standard to demonstrate that a sample does not 
contain peaks that represent any one of the Aroclors. This standard can 
also be used to determine the concentrations of either Aroclor 1016 or 
Aroclor 1260, should they be present in a sample. Therefore, prepare a 
minimum of three calibration standards containing equal concentrations 
of both Aroclor 1016 and Aroclor 1260 by dilution of the stock standard 
with isooctane or hexane. The concentrations should correspond to the 
expected range of concentrations found in real samples and should 
bracket the linear range of the detector.
    6.8.2.2.2 Single standards of each of the other five Aroclors are 
required to aid the analyst in pattern recognition. Assuming that the 
Aroclor 1016/1260 standards described in Section 6.8.2.2.1 have been 
used to demonstrate the linearity of the detector, these single 
standards of the remaining five Aroclors also may be used to determine 
the calibration factor for each Aroclor. Prepare a standard for each of 
the other Aroclors. The concentrations should generally correspond to 
the mid-point of the linear range of the detector, but lower 
concentrations may be employed at the discretion of the analyst based on 
project requirements.
    6.8.2.2.3 For Toxaphene, prepare a minimum of three calibration 
standards containing Toxaphene by dilution of the stock

[[Page 164]]

standard with isooctane or hexane. The concentrations should correspond 
to the expected range of concentrations found in real samples and should 
bracket the linear range of the detector.
    6.8.3 Quality Control (QC) Check Sample Concentrate--Prepare one or 
more mid-level standard mixtures (concentrates) in acetone (or other 
water miscible solvent). The concentrate is used as the spiking solution 
with which to prepare the Demonstration of Capabilities (DOC) samples, 
the Laboratory Control Sample (LCS), and Matrix Spike (MS) and Matrix 
Spike Duplicate (MSD) samples described in section 8. If prepared by the 
laboratory (as opposed the purchasing it from a commercial supplier), 
the concentrate must be prepared independently from the standards used 
for calibration, but may be prepared from the same source as the second-
source standard used for calibration verification (section 7.7). 
Regardless of the source, the concentrate must be in a water-miscible 
solvent, as noted above. The concentrate is used to prepare the DOC and 
LCS (sections 8.2.1 and 8.4) and MS/MSD samples (section 8.3). Depending 
on the analytes of interest for a given sample (see Section 1.4), 
multiple solutions and multiple LCS or MS/MSD samples may be required to 
account for co-eluting analytes. However, a co-elution on one column is 
acceptable so long as effective separation of the co-eluting compounds 
can be achieved on the second column. In addition, the concentrations of 
the MS/MSD samples should reflect any relevant compliance limits for the 
analytes of interest, as described in section 8.3.1. If a custom spiking 
solution is required for a specific discharge (section 8.3.1), prepare 
it separately from the DOC and LCS solution.

    Note: Some commercially available standards are divided into 
separate mixtures to address the co-elution issue.

    6.8.4 Calibration Verification Standards--In order to verify the 
results of the initial calibration standards, prepare one or more mid-
level standard mixtures in isooctane or hexane, using standards obtained 
from a second source (different manufacturer or different certified lot 
from the calibration standards). These standards will be analyzed to 
verify the accuracy of the calibration (sections 7.7 and 13.6.2). As 
with the QC sample concentrate in section 6.8.3, multiple solutions may 
be required to address co-elutions among all of the analytes.
    6.8.5 Internal standard solution--If the internal standard 
calibration technique is to be used, prepare pentachloronitrobenzene 
(PCNB) at a concentration of 10 [micro]g/mL in ethyl acetate. 
Alternative and multiple internal standards; e.g., tetrachloro-m-xylene, 
4,4[min]-dibromobiphenyl, and/or decachlorobiphenyl may be used provided 
that the laboratory performs all QC tests and meets all QC acceptance 
criteria with the alternative or additional internal standard(s) as an 
integral part of this method.
    6.8.6 Surrogate solution--Prepare a solution containing one or more 
surrogates at a concentration of 2 [micro]g/mL in acetone. Potential 
surrogates include: dibutyl chlorendate (DBC), tetrachloro-m-xylene 
(TCMX), 4,4[min]-dibromobiphenyl, or decachlorobiphenyl. Alternative 
surrogates and concentrations may be used, provided the laboratory 
performs all QC tests and meets all QC acceptance criteria with the 
alternative surrogate(s) as an integral part of this method. If the 
internal standard calibration technique is used, do not use the internal 
standard as a surrogate.
    6.8.7 DDT and endrin decomposition (breakdown) solution--Prepare a 
solution containing endrin at a concentration of 50 ng/mL and 4,4'-DDT 
at a concentration of 100 ng/mL, in isooctane or hexane. A 1-[micro]L 
injection of this standard will contain 50 picograms (pg) of endrin and 
100 pg of DDT. The concentration of the solution may be adjusted by the 
laboratory to accommodate other injection volumes such that the same 
masses of the two analytes are introduced into the instrument.

                             7. Calibration

    7.1 Establish gas chromatographic operating conditions equivalent to 
those in Section 5.8.1 and Footnote 2 to Table 3. Alternative 
temperature program and flow rate conditions may be used. The system may 
be calibrated using the external standard technique (section 7.5) or the 
internal standard technique (section 7.6). It is necessary to calibrate 
the system for the analytes of interest (section 1.4) only.
    7.2 Separately inject the mid-level calibration standard for each 
calibration mixture. Store the retention time on each GC column.
    7.3 Injection of calibration solutions--Inject a constant volume in 
the range of 0.5 to 2.0 [micro]L of each calibration solution into the 
GC column/detector pairs. An alternative volume (see Section 12.3) may 
be used provided all requirements in this method are met. Beginning with 
the lowest level mixture and proceeding to the highest level mixture may 
limit the risk of carryover from one standard to the next, but other 
sequences may be used. An instrument blank should be analyzed after the 
highest standard to demonstrate that there is no carry-over within the 
system for this calibration range.
    7.4 For each analyte, compute, record, and store, as a function of 
the concentration injected, the retention time and peak area on each 
column/detector system. If multi-component analytes are to be analyzed, 
store the retention time and peak area for the three to five exclusive 
(unique large) peaks

[[Page 165]]

for each PCB or technical chlordane. Use four to six peaks for 
toxaphene.
    7.5 External standard calibration.
    7.5.1 From the calibration data (Section 7.4), calculate the 
calibration factor (CF) for each analyte at each concentration according 
to the following equation:
[GRAPHIC] [TIFF OMITTED] TR28AU17.000

Where:

Cs = Concentration of the analyte in the standard (ng/mL)
As = Peak height or area

    For multi-component analytes, choose a series of characteristic 
peaks for each analyte (3 to 5 for each Aroclor, 4 to 6 for toxaphene) 
and calculate individual calibration factors for each peak. 
Alternatively, for toxaphene, sum the areas of all of the peaks in the 
standard chromatogram and use the summed area to determine the 
calibration factor. (If this alternative is used, the same approach must 
be used to quantitate the analyte in the samples.)
    7.5.2 Calculate the mean (average) and relative standard deviation 
(RSD) of the calibration factors. If the RSD is less than 20%, linearity 
through the origin can be assumed and the average CF can be used for 
calculations. Alternatively, the results can be used to fit a linear or 
quadratic regression of response, As, vs. concentration 
Cs. If used, the regression must be weighted inversely 
proportional to concentration. The coefficient of determination (R\2\) 
of the weighted regression must be greater than 0.920. Alternatively, 
the relative standard error (Reference 10) may be used as an acceptance 
criterion. As with the RSD, the RSE must be less than 20%. If an RSE 
less than 20% cannot be achieved for a quadratic regression, system 
performance is unacceptable and the system must be adjusted and re-
calibrated.

    Note: Regression calculations are not included in this method 
because the calculations are cumbersome and because many GC/ECD data 
systems allow selection of weighted regression for calibration and 
calculation of analyte concentrations.

    7.6 Internal standard calibration.
    7.6.1 From the calibration data (Section 7.4), calculate the 
response factor (RF) for each analyte at each concentration according to 
the following equation:
[GRAPHIC] [TIFF OMITTED] TR28AU17.001

Where:

As = Response for the analyte to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard (ng/mL)
Cs = Concentration of the analyte to be measured (ng/mL).

    7.6.2 Calculate the mean (average) and relative standard deviation 
(RSD) of the response factors. If the RSD is less than 15%, linearity 
through the origin can be assumed and the average RF can be used for 
calculations. Alternatively, the results can be used to prepare a 
calibration curve of response ratios, As/Ais, vs. 
concentration ratios, Cs/Cis, for the analyte. A 
minimum of six concentration levels is required for a non-linear (e.g., 
quadratic) regression. If used, the regression must be weighted 
inversely proportional to concentration, and the coefficient of 
determination of the weighted regression must be greater than 0.920. 
Alternatively, the relative standard error (Reference 10) may be used as 
an acceptance criterion. As with the RSD, the RSE must be less than 15%. 
If an RSE less than 15% cannot be achieved for a quadratic regression, 
system performance is unacceptable and the system must be adjusted and 
re-calibrated.
    7.7 The working calibration curve, CF, or RF must be verified 
immediately after calibration and at the beginning and end of each 24-
hour shift by the analysis of a mid-level calibration standard. The 
calibration verification standard(s) must be obtained from a second 
manufacturer or a manufacturer's batch prepared independently from the 
batch used for calibration (Section 6.8.4). Requirements for calibration 
verification are given in Section 13.6 and Table 4. Alternatively, 
calibration verification may be performed after a set number of 
injections

[[Page 166]]

(e.g., every 20 injections), to include injection of extracts of field 
samples, QC samples, instrument blanks, etc. (i.e., it is based on the 
number of injections performed, not sample extracts). The time for the 
injections may not exceed 24 hours.

    Note: The 24-hour shift begins after analysis of the combined QC 
standard (calibration verification) and ends 24 hours later. The ending 
calibration verification standard is run immediately after the last 
sample run during the 24-hour shift, so the beginning and ending 
calibration verifications are outside of the 24-hour shift. If 
calibration verification is based on the number of injections instead of 
time, then the ending verification standard for one group of injections 
may be used as the beginning verification for the next group of 
injections.

    7.8 Florisil[supreg] calibration--The column cleanup procedure in 
Section 11.3 utilizes Florisil column chromatography. Florisil[supreg] 
from different batches or sources may vary in adsorptive capacity. To 
standardize the amount of Florisil[supreg] which is used, use of the 
lauric acid value (Reference 11) is suggested. The referenced procedure 
determines the adsorption from a hexane solution of lauric acid (mg) per 
g of Florisil[supreg]. The amount of Florisil[supreg] to be used for 
each column is calculated by dividing 110 by this ratio and multiplying 
by 20 g. If cartridges containing Florisil[supreg] are used, then this 
step is not necessary.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability and 
ongoing analysis of spiked samples and blanks to evaluate and document 
data quality. The laboratory must maintain records to document the 
quality of data generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet performance requirements of this method. A quality control check 
standard (LCS, section 8.4) must be prepared and analyzed with each 
batch of samples to confirm that the measurements were performed in an 
in-control mode of operation. A laboratory may develop its own 
performance criteria (as QC acceptance criteria), provided such criteria 
are as or more restrictive than the criteria in this method.
    8.1.1 The laboratory must make an initial demonstration of the 
capability (IDC) to generate acceptable precision and recovery with this 
method. This demonstration is detailed in Section 8.2. On a continuing 
basis, the laboratory must repeat demonstration of capability (DOC) at 
least annually.
    8.1.2 In recognition of advances that are occurring in analytical 
technology, and to overcome matrix interferences, the laboratory is 
permitted certain options (section 1.8 and 40 CFR 136.6(b) [Reference 
12]) to improve separations or lower the costs of measurements. These 
options may include alternative extraction (e.g., other solid-phase 
extraction materials and formats), concentration, and cleanup 
procedures, and changes in GC columns (Reference 12). Alternative 
determinative techniques, such as the substitution of spectroscopic or 
immunoassay techniques, and changes that degrade method performance, are 
not allowed. If an analytical technique other than the techniques 
specified in this method is used, that technique must have a specificity 
equal to or greater than the specificity of the techniques in this 
method for the analytes of interest. The laboratory is also encouraged 
to participate in performance evaluation studies (see section 8.8).
    8.1.2.1 Each time a modification listed above is made to this 
method, the laboratory is required to repeat the procedure in section 
8.2. If the detection limit of the method will be affected by the 
change, the laboratory is required to demonstrate that the MDLs (40 CFR 
part 136, appendix B) are lower than one-third the regulatory compliance 
limit or as low as the MDLs in this method, whichever are greater. If 
calibration will be affected by the change, the instrument must be 
recalibrated per section 7. Once the modification is demonstrated to 
produce results equivalent or superior to results produced by this 
method as written, that modification may be used routinely thereafter, 
so long as the other requirements in this method are met (e.g., matrix 
spike/matrix spike duplicate recovery and relative percent difference).
    8.1.2.1.1 If an allowed method modification, is to be applied to a 
specific discharge, the laboratory must prepare and analyze matrix 
spike/matrix spike duplicate (MS/MSD) samples (section 8.3) and LCS 
samples (section 8.4). The laboratory must include surrogates (Section 
8.7) in each of the samples. The MS/MSD and LCS samples must be 
fortified with the analytes of interest (section 1.4). If the 
modification is for nationwide use, MS/MSD samples must be prepared from 
a minimum of nine different discharges (See section 8.1.2.1.2), and all 
QC acceptance criteria in this method must be met. This evaluation only 
needs to be performed once other than for the routine QC required by 
this method (for example it could be performed by the vendor of an 
alternative material) but any laboratory using that specific material 
must have the results of the study available. This includes a full data 
package with the raw data that will allow an independent reviewer to 
verify each determination and calculation performed by the laboratory 
(see section 8.1.2.2.5, items (a)-(q)).

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    8.1.2.1.2 Sample matrices on which MS/MSD tests must be performed 
for nationwide use of an allowed modification:
    (a) Effluent from a publicly owned treatment works (POTW).
    (b) ASTM D5905 Standard Specification for Substitute Wastewater.
    (c) Sewage sludge, if sewage sludge will be in the permit.
    (d) ASTM D1141 Standard Specification for Substitute Ocean Water, if 
ocean water will be in the permit.
    (e) Untreated and treated wastewaters up to a total of nine matrix 
types (see https://www.epa.gov/eg/industrial-effluent-guidelines for a 
list of industrial categories with existing effluent guidelines).
    (i) At least one of the above wastewater matrix types must have at 
least one of the following characteristics:
    (A) Total suspended solids greater than 40 mg/L.
    (B) Total dissolved solids greater than 100 mg/L.
    (C) Oil and grease greater than 20 mg/L.
    (D) NaCl greater than 120 mg/L.
    (E) CaCO3 greater than 140 mg/L.
    (ii) The interim acceptance criteria for MS, MSD recoveries that do 
not have recovery limits in Table 4 or developed in section 8.3.3, and 
for surrogates that do not have recovery limits developed in section 
8.6, must be no wider than 60-140%, and the relative percent difference 
(RPD) of the concentrations in the MS and MSD that do not have RPD 
limits in Table 4 or developed in section 8.3.3, must be less than 30%. 
Alternatively, the laboratory may use the laboratory's in-house limits 
if they are tighter.
    (f) A proficiency testing (PT) sample from a recognized provider, in 
addition to tests of the nine matrices (section 8.1.2.1.1).
    8.1.2.2 The laboratory must maintain records of modifications made 
to this method. These records include the following, at a minimum:
    8.1.2.2.1 The names, titles, and business street addresses, 
telephone numbers, and email addresses, of the analyst(s) that performed 
the analyses and modification, and of the quality control officer that 
witnessed and will verify the analyses and modifications.
    8.1.2.2.2 A list of analytes, by name and CAS Registry number.
    8.1.2.2.3 A narrative stating reason(s) for the modifications.
    8.1.2.2.4 Results from all quality control (QC) tests comparing the 
modified method to this method, including:
    (a) Calibration (section 7).
    (b) Calibration verification (section 13.6).
    (c) Initial demonstration of capability (section 8.2).
    (d) Analysis of blanks (section 8.5).
    (e) Matrix spike/matrix spike duplicate analysis (section 8.3).
    (f) Laboratory control sample analysis (section 8.4).
    8.1.2.2.5 Data that will allow an independent reviewer to validate 
each determination by tracing the instrument output (peak height, area, 
or other signal) to the final result. These data are to include:
    (a) Sample numbers and other identifiers.
    (b) Extraction dates.
    (c) Analysis dates and times.
    (d) Analysis sequence/run chronology.
    (e) Sample weight or volume (section 10).
    (f) Extract volume prior to each cleanup step (sections 10 and 11).
    (g) Extract volume after each cleanup step (section 11).
    (h) Final extract volume prior to injection (sections 10 and 12).
    (i) Injection volume (sections 12.3 and 13.2).
    (j) Sample or extract dilution (section 15.4).
    (k) Instrument and operating conditions.
    (l) Column (dimensions, material, etc.).
    (m) Operating conditions (temperatures, flow rates, etc.).
    (n) Detector (type, operating conditions, etc.).
    (o) Chromatograms and other recordings of raw data.
    (p) Quantitation reports, data system outputs, and other data to 
link the raw data to the results reported.
    (q) A written Standard Operating Procedure (SOP).
    8.1.2.2.6 Each individual laboratory wishing to use a given 
modification must perform the start-up tests in section 8.1.2 (e.g., 
DOC, MDL), with the modification as an integral part of this method 
prior to applying the modification to specific discharges. Results of 
the DOC must meet the QC acceptance criteria in Table 5 for the analytes 
of interest (section 1.4), and the MDLs must be equal to or lower than 
the MDLs in Tables 1 and 2 for the analytes of interest.
    8.1.3 Before analyzing samples, the laboratory must analyze a blank 
to demonstrate that interferences from the analytical system, lab ware, 
and reagents, are under control. Each time a batch of samples is 
extracted or reagents are changed, a blank must be extracted and 
analyzed as a safeguard against laboratory contamination. Requirements 
for the blank are given in section 8.5.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze 
samples to monitor and evaluate method and laboratory performance on the 
sample matrix. The procedure for spiking and analysis is given in 
section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
analysis of a quality control check sample (laboratory control sample, 
LCS; on-going precision and

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recovery sample, OPR) that the measurement system is in control. This 
procedure is described in Section 8.4.
    8.1.6 The laboratory should maintain performance records to document 
the quality of data that is generated. This procedure is given in 
section 8.7.
    8.1.7 The large number of analytes tested in performance tests in 
this method present a substantial probability that one or more will fail 
acceptance criteria when all analytes are tested simultaneously, and a 
re-test (reanalysis) is allowed if this situation should occur. If, 
however, continued re-testing results in further repeated failures, the 
laboratory should document the failures and either avoid reporting 
results for the analytes that failed or report the problem and failures 
with the data. A QC failure does not relieve a discharger or permittee 
of reporting timely results.
    8.2 Demonstration of capability (DOC)--To establish the ability to 
generate acceptable recovery and precision, the laboratory must perform 
the DOC in sections 8.2.1 through 8.2.6 for the analytes of interest 
initially and in an on-going manner at least annually. The laboratory 
must also establish MDLs for the analytes of interest using the MDL 
procedure at 40 CFR part 136, appendix B. The laboratory's MDLs must be 
equal to or lower than those listed in Tables 1 or 2, or lower than one-
third the regulatory compliance limit, whichever is greater. For MDLs 
not listed in Tables 1 or 2, the laboratory must determine the MDLs 
using the MDL procedure at 40 CFR part 136, appendix B under the same 
conditions used to determine the MDLs for the analytes listed in Tables 
1 and 2. When analyzing the PCBs as Aroclors, it is only necessary to 
establish an MDL for one of the multi-component analytes (e.g., PCB 
1254), or the mixture of Aroclors 1016 and 1260 may be used to establish 
MDLs for all of the Aroclors. Similarly, MDLs for other multi-component 
analytes (e.g., Chlordanes) may be determined using only one of the 
major components. All procedures used in the analysis, including cleanup 
procedures, must be included in the DOC.
    8.2.1 For the DOC, a QC check sample concentrate containing each 
analyte of interest (section 1.4) is prepared in a water-miscible 
solvent using the solution in section 6.8.3.

    Note: QC check sample concentrates are no longer available from EPA.
    8.2.2 Using a pipet or syringe, prepare four QC check samples by 
adding an appropriate volume of the concentrate and of the surrogate(s) 
to each of four 1-L aliquots of reagent water. Swirl or stir to mix.
    8.2.3 Extract and analyze the well-mixed QC check samples according 
to the method beginning in section 10.
    8.2.4 Calculate the average percent recovery (X) and the standard 
deviation (s) of the percent recovery for each analyte using the four 
results.
    8.2.5 For each analyte, compare s and X with the corresponding 
acceptance criteria for precision and recovery in Table 4. For analytes 
in Table 2 that are not listed in Table 4, QC acceptance criteria must 
be developed by the laboratory. EPA has provided guidance for 
development of QC acceptance criteria (References 12 and 13). If s and X 
for all analytes of interest meet the acceptance criteria, system 
performance is acceptable and analysis of blanks and samples can begin. 
If any individual s exceeds the precision limit or any individual X 
falls outside the range for recovery, system performance is unacceptable 
for that analyte.

    Note: The large number of analytes in Tables 1 and 2 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when many or all analytes are determined 
simultaneously.
    8.2.6 When one or more of the analytes tested fail at least one of 
the acceptance criteria, repeat the test for only the analytes that 
failed. If results for these analytes pass, system performance is 
acceptable and analysis of samples and blanks may proceed. If one or 
more of the analytes again fail, system performance is unacceptable for 
the analytes that failed the acceptance criteria. Correct the problem 
and repeat the test (section 8.2). See section 8.1.7 for disposition of 
repeated failures.

    Note: To maintain the validity of the test and re-test, system 
maintenance and/or adjustment is not permitted between this pair of 
tests.
    8.3 Matrix spike and matrix spike duplicate (MS/MSD)--The purpose of 
the MS/MSD requirement is to provide data that demonstrate the 
effectiveness of the method as applied to the samples in question by a 
given laboratory, and both the data user (discharger, permittee, 
regulated entity, regulatory/control authority, customer, other) and the 
laboratory share responsibility for provision of such data. The data 
user should identify the sample and the analytes of interest (section 
1.4) to be spiked and provide sufficient sample volume to perform MS/MSD 
analyses. The laboratory must, on an ongoing basis, spike at least 5% of 
the samples in duplicate from each discharge being monitored to assess 
accuracy (recovery and precision). If direction cannot be obtained from 
the data user, the laboratory must spike at least one sample in 
duplicate per extraction batch of up to 20 samples with the analytes in 
Table 1. Spiked sample results should be reported only to the data user 
whose sample was spiked, or as requested or required by a regulatory/
control authority, or in a permit.
    8.3.1. If, as in compliance monitoring, the concentration of a 
specific analyte will be

[[Page 169]]

checked against a regulatory concentration limit, the concentration of 
the spike should be at that limit; otherwise, the concentration of the 
spike should be one to five times higher than the background 
concentration determined in section 8.3.2, at or near the midpoint of 
the calibration range, or at the concentration in the LCS (section 8.4) 
whichever concentration would be larger. When no information is 
available, the mid-point of the calibration may be used.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of the each analyte of interest. If necessary to meet 
the requirement in section 8.3.1, prepare a new check sample concentrate 
(section 8.2.1) appropriate for the background concentration. Spike and 
analyze two additional sample aliquots of the same volume as the 
original sample, and determine the concentrations after spiking 
(A1 and A2) of each analyte. Calculate the percent 
recoveries (P1 and P2) as:
[GRAPHIC] [TIFF OMITTED] TR28AU17.002

where T is the known true value of the spike.

    Also calculate the relative percent difference (RPD) between the 
concentrations (A1 and A2):
[GRAPHIC] [TIFF OMITTED] TR28AU17.003

    8.3.3 Compare the percent recoveries (P1 and 
P2) and the RPD for each analyte in the MS/MSD aliquots with 
the corresponding QC acceptance criteria for recovery (P) and RPD in 
Table 4.
    (a) If any individual P falls outside the designated range for 
recovery in either aliquot, or the RPD limit is exceeded, the result for 
the analyte in the unspiked sample is suspect and may not be reported or 
used for permitting or regulatory compliance. See section 8.1.7 for 
disposition of failures.
    (b) For analytes in Table 2 not listed in Table 4, QC acceptance 
criteria must be developed by the laboratory. EPA has provided guidance 
for development of QC acceptance criteria (References 12 and 13).
    8.3.4 After analysis of a minimum of 20 MS/MSD samples for each 
target analyte and surrogate, and if the laboratory chooses to develop 
and apply optional in-house QC limits, the laboratory should calculate 
and apply the optional in-house QC limits for recovery and RPD of future 
MS/MSD samples (Section 8.3). The optional in-house QC limits for 
recovery are calculated as the mean observed recovery 3 standard deviations, and the upper QC limit for RPD is 
calculated as the mean RPD plus 3 standard deviations of the RPDs. The 
in-house QC limits must be updated at least every two years and re-
established after any major change in the analytical instrumentation or 
process. At least 80% of the analytes tested in the MS/MSD must have in-
house QC acceptance criteria that are tighter than those in Table 4 and 
the remaining analytes (those not included in the 80%) must meet the 
acceptance criteria in Table 4. If an in-house QC limit for the RPD is 
greater than the limit in Table 4, then the limit in Table 4 must be 
used. Similarly, if an in-house lower limit for recovery is below the 
lower limit in Table 4, then the lower limit in Table 4 must be used, 
and if an in-house upper limit for recovery is above the upper limit in 
Table 4, then the upper limit in Table 4 must be used. The laboratory 
must evaluate surrogate recovery data in each sample against its in-
house surrogate recovery limits. The laboratory may use 60 -140% as 
interim acceptance criteria for surrogate recoveries until in-house 
limits are developed. Alternatively, surrogate recovery limits may be 
developed from laboratory control charts. In-house QC acceptance 
criteria must be updated at least every two years.
    8.4 Laboratory control sample (LCS)--A QC check sample (laboratory 
control sample, LCS; on-going precision and recovery sample, OPR) 
containing each single-component analyte of interest (section 1.4) must 
be extracted, concentrated, and analyzed with each extraction batch of 
up to 20 samples (section 3.1) to demonstrate acceptable recovery of the 
analytes of interest from a

[[Page 170]]

clean sample matrix. If multi-peak analytes are required, extract and 
prepare at least one as an LCS for each batch. Alternatively, the 
laboratory may set up a program where multi-peak LCS is rotated with a 
single-peak LCS.
    8.4.1 Prepare the LCS by adding QC check sample concentrate 
(sections 6.8.3 and 8.2.1) to reagent water. Include all analytes of 
interest (section 1.4) in the LCS. The volume of reagent water must be 
the same as the nominal volume used for the sample, the DOC (Section 
8.2), the blank (section 8.5), and the MS/MSD (section 8.3). Also add a 
volume of the surrogate solution (section 6.8.6).
    8.4.2 Analyze the LCS prior to analysis of samples in the extraction 
batch (Section 3.1). Determine the concentration (A) of each analyte. 
Calculate the percent recovery as:
[GRAPHIC] [TIFF OMITTED] TR28AU17.004

where T is the true value of the concentration in the LCS.

    8.4.3 For each analyte, compare the percent recovery (P) with its 
corresponding QC acceptance criterion in Table 4. For analytes of 
interest in Table 2 not listed in Table 4, use the QC acceptance 
criteria developed for the MS/MSD (section 8.3.3.2), or limits based on 
laboratory control charts. If the recoveries for all analytes of 
interest fall within the designated ranges, analysis of blanks and field 
samples may proceed. If any individual recovery falls outside the range, 
proceed according to section 8.4.4.
    Note: The large number of analytes in Tables 1 and 2 present a 
substantial probability that one or more will fail the acceptance 
criteria when all analytes are tested simultaneously. Because a re-test 
is allowed in event of failure (sections 8.1.7 and 8.4.4), it may be 
prudent to extract and analyze two LCSs together and evaluate results of 
the second analysis against the QC acceptance criteria only if an 
analyte fails the first test.
    8.4.4 Repeat the test only for those analytes that failed to meet 
the acceptance criteria (P). If these analytes now pass, system 
performance is acceptable and analysis of blanks and samples may 
proceed. Repeated failure, however, will confirm a general problem with 
the measurement system. If this occurs, repeat the test using a fresh 
LCS (section 8.2.1) or an LCS prepared with a fresh QC check sample 
concentrate (section 8.2.1), or perform and document system repair. 
Subsequent to analysis of the LCS prepared with a fresh sample 
concentrate, or to system repair, repeat the LCS test (Section 8.4). If 
failure of the LCS indicates a systemic problem with samples in the 
batch, re-extract and re-analyze the samples in the batch. See Section 
8.1.7 for disposition of repeated failures.
    8.4.5 After analysis of 20 LCS samples, and if the laboratory 
chooses to develop and apply optional in-house QC limits, the laboratory 
should calculate and apply the optional in-house QC limits for recovery 
of future LCS samples (section 8.4). Limits for recovery in the LCS 
should be calculated as the mean recovery 3 
standard deviations. A minimum of 80% of the analytes tested for in the 
LCS must have QC acceptance criteria tighter than those in Table 4, and 
the remaining analytes (those not included in the 80%) must meet the 
acceptance criteria in Table 4. If an in-house lower limit for recovery 
is lower than the lower limit in Table 4, the lower limit in Table 4 
must be used, and if an in-house upper limit for recovery is higher than 
the upper limit in Table 4, the upper limit in Table 4 must be used. 
Many of the analytes and surrogates do not contain acceptance criteria. 
The laboratory should use 60-140% as interim acceptance criteria for 
recoveries of spiked analytes and surrogates that do not have recovery 
limits specified in Table 4, and at least 80% of the surrogates must 
meet the 60-140% interim criteria until in-house LCS and surrogate 
limits are developed. Alternatively, acceptance criteria for analytes 
that do not have recovery limits in Table 4 may be based on laboratory 
control charts. In-house QC acceptance criteria must be updated at least 
every two years.
    8.5 Blank--Extract and analyze a blank with each extraction batch 
(section 3.1) to demonstrate that the reagents and equipment used for 
preparation and analysis are free from contamination.
    8.5.1 Prepare the blank from reagent water and spike it with the 
surrogates. The volume of reagent water must be the same as the volume 
used for samples, the DOC (section 8.2), the LCS (section 8.4), and the 
MS/MSD (section 8.3). Extract, concentrate, and analyze the blank using 
the same procedures and reagents used for the samples, LCS, and MS/MSD 
in the batch. Analyze the blank immediately after analysis of the LCS 
(section 8.4) and prior to analysis of the MS/MSD and samples to 
demonstrate freedom from contamination.
    8.5.2 If any analyte of interest is found in the blank at a 
concentration greater than the MDL for the analyte, at a concentration

[[Page 171]]

greater than one-third the regulatory compliance limit, or at a 
concentration greater than one-tenth the concentration in a sample in 
the batch (section 3.1), whichever is greatest, analysis of samples must 
be halted and samples in the batch must be re-extracted and the extracts 
reanalyzed. Samples in a batch must be associated with an uncontaminated 
blank before the results for those samples may be reported or used for 
permitting or regulatory compliance purposes. If re-testing of blanks 
results in repeated failures, the laboratory should document the 
failures and report the problem and failures with the data.
    8.6 Surrogate recovery--The laboratory must spike all samples with 
the surrogate standard spiking solution (section 6.8.6) per section 
10.2.2 or 10.4.2, analyze the samples, and calculate the percent 
recovery of each surrogate. QC acceptance criteria for surrogates must 
be developed by the laboratory (section 8.4). If any recovery fails its 
criterion, attempt to find and correct the cause of the failure, and if 
sufficient volume is available, re-extract another aliquot of the 
affected sample; otherwise, see section 8.1.7 for disposition of 
repeated failures.
    8.7 As part of the QC program for the laboratory, it is suggested 
but not required that method accuracy for wastewater samples be assessed 
and records maintained. After analysis of five or more spiked wastewater 
samples as in Section 8.3, calculate the average percent recovery (X) 
and the standard deviation of the percent recovery (sp). Express the 
accuracy assessment as a percent interval from X-2sp to X+2sp. For 
example, if X = 90% and sp = 10%, the accuracy interval is expressed as 
70-110%. Update the accuracy assessment for each analyte on a regular 
basis to ensure process control (e.g., after each 5-10 new accuracy 
measurements). If desired, statements of accuracy for laboratory 
performance, independent of performance on samples, may be developed 
using LCSs.
    8.8 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with another dissimilar column, specific 
element detector, or mass spectrometer must be used. Whenever possible, 
the laboratory should analyze standard reference materials and 
participate in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Collect samples as grab samples in glass bottles, or in 
refrigerated bottles using automatic sampling equipment. Collect 1-L of 
ambient waters, effluents, and other aqueous samples. If high 
concentrations of the analytes of interest are expected (e.g., for 
untreated effluents or in-process waters), collect a smaller volume 
(e.g., 250 mL), but not less than 100 mL, in addition to the 1-L sample. 
Follow conventional sampling practices, except do not pre-rinse the 
bottle with sample before collection. Automatic sampling equipment must 
be as free as possible of polyvinyl chloride or other tubing or other 
potential sources of contamination. If needed, collect additional 
sample(s) for the MS/MSD (section 8.3).
    9.2 Ice or refrigerate the sample at <=6 [deg]C from the time of 
collection until extraction, but do not freeze. If aldrin is to be 
determined and residual chlorine is present, add 80 mg/L of sodium 
thiosulfate but do not add excess. Any method suitable for field use may 
be employed to test for residual chlorine (Reference 14). If sodium 
thiosulfate interferes in the determination of the analytes, an 
alternative preservative (e.g., ascorbic acid or sodium sulfite) may be 
used.
    9.3 Extract all samples within seven days of collection and 
completely analyze within 40 days of extraction (Reference 1). If the 
sample will not be extracted within 72 hours of collection, adjust the 
sample pH to a range of 5.0-9.0 with sodium hydroxide solution or 
sulfuric acid. Record the volume of acid or base used.

                          10. Sample Extraction

    10.1 This section contains procedures for separatory funnel liquid-
liquid extraction (SFLLE, section 10.2), continuous liquid-liquid 
extraction (CLLE, section 10.4), and disk-based solid-phase extraction 
(SPE, section 10.5). SFLLE is faster, but may not be as effective as 
CLLE for extracting polar analytes. SFLLE is labor intensive and may 
result in formation of emulsions that are difficult to break. CLLE is 
less labor intensive, avoids emulsion formation, but requires more time 
(18-24 hours), more hood space, and may require more solvent. SPE can be 
faster, unless the particulate load in an aqueous sample is so high that 
it slows the filtration process. If an alternative extraction scheme to 
those detailed in this method is used, all QC tests must be performed 
and all QC acceptance criteria must be met with that extraction scheme 
as an integral part of this method.
    10.2 Separatory funnel liquid-liquid extraction (SFLLE).
    10.2.1 The SFLLE procedure below assumes a sample volume of 1 L. 
When a different sample volume is extracted, adjust the volume of 
methylene chloride accordingly.

[[Page 172]]

    10.2.2 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into the 
separatory funnel. Pipet the surrogate standard spiking solution 
(section 6.8.6) into the separatory funnel. If the sample will be used 
for the LCS or MS or MSD, pipet the appropriate QC check sample 
concentrate (section 8.3 or 8.4) into the separatory funnel. Mix well. 
If the sample arrives in a larger sample bottle, 1 L may be measured in 
a graduated cylinder, then added to the separatory funnel.
    Note: Instances in which the sample is collected in an oversized 
bottle should be reported by the laboratory to the data user. Of 
particular concern is that fact that this practice precludes rinsing the 
empty bottle with solvent as described below, which could leave 
hydrophobic pesticides on the wall of the bottle, and underestimate the 
actual sample concentrations.
    10.2.3 Add 60 mL of methylene chloride to the sample bottle, seal, 
and shake for 30 seconds to rinse the inner surface. Transfer the 
solvent to the separatory funnel and extract the sample by shaking the 
funnel for two minutes with periodic venting to release excess pressure. 
Allow the organic layer to separate from the water phase for a minimum 
of 10 minutes. If an emulsion forms and the emulsion interface between 
the layers is more than one-third the volume of the solvent layer, 
employ mechanical techniques to complete the phase separation. The 
optimum technique depends upon the sample, but may include stirring, 
filtration of the emulsion through glass wool, use of phase-separation 
paper, centrifugation, salting, freezing, or other physical methods. 
Collect the methylene chloride extract in a flask. If the emulsion 
cannot be broken (recovery of less than 80% of the methylene chloride, 
corrected for the water solubility of methylene chloride), transfer the 
sample, solvent, and emulsion into the extraction chamber of a 
continuous extractor and proceed as described in section 10.4.
    10.2.4 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the flask. Perform a third extraction in the same manner. 
Proceed to macro-concentration (section 10.3.1).
    10.2.5 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to an appropriately sized 
graduated cylinder. Record the sample volume to the nearest 5 mL. Sample 
volumes may also be determined by weighing the container before and 
after extraction or filling to the mark with water.
    10.3 Concentration.
    10.3.1 Macro concentration.
    10.3.1.1 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 
10-mL concentrator tube to a 500-mL evaporative flask. Other 
concentration devices or techniques may be used in place of the K-D 
concentrator so long as the requirements of section 8.2 are met.
    10.3.1.2 Pour the extract through a solvent-rinsed drying column 
containing about 10 cm of anhydrous sodium sulfate, and collect the 
extract in the K-D concentrator. Rinse the flask and column with 20-30 
mL of methylene chloride to complete the quantitative transfer.
    10.3.1.3 If no cleanup is to be performed on the sample, add 500 
[micro]L (0.5 mL) of isooctane to the extract to act as a keeper during 
concentration.
    10.3.1.4 Add one or two clean boiling chips and attach a three-ball 
Snyder column to the K-D evaporative flask. Pre-wet the Snyder column by 
adding about 1 mL of methylene chloride to the top. Place the K-D 
apparatus on a hot water bath (60-65 [deg]C) so that the concentrator 
tube is partially immersed in the hot water, and the entire lower 
rounded surface of the flask is bathed with hot vapor. Adjust the 
vertical position of the apparatus and the water temperature as required 
to complete the concentration in 15-20 minutes. At the proper rate of 
evaporation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL or other determined amount, remove the K-D 
apparatus from the water bath and allow it to drain and cool for at 
least 10 minutes.
    10.3.1.5 If the extract is to be cleaned up by sulfur removal or 
acid back extraction, remove the Snyder column and rinse the flask and 
its lower joint into the concentrator tube with 1 to 2 mL of methylene 
chloride. A 5-mL syringe is recommended for this operation. Adjust the 
final volume to 10 mL in methylene chloride and proceed to sulfur 
removal (section 11.5) or acid back extraction (section 11.6). If the 
extract is to cleaned up using one of the other cleanup procedures or is 
to be injected into the GC, proceed to Kuderna-Danish micro-
concentration (section 10.3.2) or nitrogen evaporation and solvent 
exchange (section 10.3.3).
    10.3.2 Kuderna-Danish micro concentration--Add another one or two 
clean boiling chips to the concentrator tube and attach a two-ball 
micro-Snyder column. Pre-wet the Snyder column by adding about 0.5 mL of 
methylene chloride to the top. Place the K-D apparatus on a hot water 
bath (60-65 [deg]C) so that the concentrator tube is partially immersed 
in hot water. Adjust the vertical position of the apparatus and the 
water temperature as required to complete the concentration in 5-10 
minutes. At the proper rate of distillation the balls of the column will 
actively chatter but the chambers will not flood with condensed solvent. 
When the

[[Page 173]]

apparent volume of liquid reaches approximately 1 mL or other required 
amount, remove the K-D apparatus from the water bath and allow it to 
drain and cool for at least 10 minutes. Remove the Snyder column and 
rinse the flask and its lower joint into the concentrator tube with 
approximately 0.2 mL of methylene chloride, and proceed to section 
10.3.3 for nitrogen evaporation and solvent exchange.
    10.3.3 Nitrogen evaporation and solvent exchange--Extracts to be 
subjected to solid-phase cleanup (SPE) are exchanged into 1.0 mL of the 
SPE elution solvent (section 6.7.2.2). Extracts to be subjected to 
Florisil[supreg] or alumina cleanups are exchanged into hexane. Extracts 
that have been cleaned up and are ready for analysis are exchanged into 
isooctane or hexane, to match the solvent used for the calibration 
standards.
    10.3.3.1 Transfer the vial containing the sample extract to the 
nitrogen evaporation (blowdown) device (section 5.2.5.2). Lower the vial 
into a 50-55 [deg]C water bath and begin concentrating. During the 
solvent evaporation process, do not allow the extract to become dry. 
Adjust the flow of nitrogen so that the surface of the solvent is just 
visibly disturbed. A large vortex in the solvent may cause analyte loss.
    10.3.3.2 Solvent exchange.
    10.3.3.2.1 When the volume of the liquid is approximately 500 
[micro]L, add 2 to 3 mL of the desired solvent (SPE elution solvent for 
SPE cleanup, hexane for Florisil or alumina, or isooctane for final 
injection into the GC) and continue concentrating to approximately 500 
[micro]L. Repeat the addition of solvent and concentrate once more.
    10.3.3.3.2 Adjust the volume of an extract to be cleaned up by SPE, 
Florisil[supreg], or alumina to 1.0 mL. Proceed to extract cleanup 
(section 11).
    10.3.3.3 Extracts that have been cleaned up and are ready for 
analysis--Adjust the final extract volume to be consistent with the 
volume extracted and the sensitivity desired. The goal is for a full-
volume sample (e.g., 1-L) to have a final extract volume of 10 mL, but 
other volumes may be used.
    10.3.4 Transfer the concentrated extract to a vial with 
fluoropolymer-lined cap. Seal the vial and label with the sample number. 
Store in the dark at room temperature until ready for GC analysis. If GC 
analysis will not be performed on the same day, store the vial in the 
dark at <=6 [deg]C. Analyze the extract by GC per the procedure in 
section 12.
    10.4 Continuous liquid/liquid extraction (CLLE).
    10.4.1 Use CLLE when experience with a sample from a given source 
indicates an emulsion problem, or when an emulsion is encountered using 
SFLLE. CLLE may be used for all samples, if desired.
    10.4.2 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Transfer the sample to the 
continuous extractor and, using a pipet, add surrogate standard spiking 
solution. If the sample will be used for the LCS, MS, or MSD, pipet the 
appropriate check sample concentrate (section 8.2.1 or 8.3.2) into the 
separatory funnel. Mix well. Add 60 mL of methylene chloride to the 
sample bottle, seal, and shake for 30 seconds to rinse the inner 
surface. Transfer the solvent to the extractor.
    10.4.3 Repeat the sample bottle rinse with two additional 50-100 mL 
portions of methylene chloride and add the rinses to the extractor.
    10.4.4 Add a suitable volume of methylene chloride to the distilling 
flask (generally 200-500 mL) and sufficient reagent water to ensure 
proper operation of the extractor, and extract the sample for 18-24 
hours. A shorter or longer extraction time may be used if all QC 
acceptance criteria are met. Test and, if necessary, adjust the pH of 
the water to a range of 5.0-9.0 during the second or third hour of the 
extraction. After extraction, allow the apparatus to cool, then detach 
the distilling flask. Dry, concentrate, solvent exchange, and transfer 
the extract to a vial with fluoropolymer-lined cap, per Section 10.3.
    10.4.5 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to an appropriately sized 
graduated cylinder. Record the sample volume to the nearest 5 mL. Sample 
volumes may also be determined by weighing the container before and 
after extraction or filling to the mark with water.
    10.5 Solid-phase extraction of aqueous samples. The steps in this 
section address the extraction of aqueous field samples using disk-based 
solid-phase extraction (SPE) media, based on an ATP approved by EPA in 
1995 (Reference 20). This application of SPE is distinct from that used 
in this method for the cleanup of sample extracts in section 11.2. 
Analysts must be careful not to confuse the equipment, supplies, or the 
procedural steps from these two different uses of SPE.
    Note: Changes to the extraction conditions described below may be 
made by the laboratory under the allowance for method flexibility 
described in section 8.1, provided that the performance requirements in 
section 8.2 are met. However, changes in SPE materials, formats, and 
solvents must meet the requirements in section 8.1.2 and its 
subsections.
    10.5.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. If the sample contains 
particulates, let stand to settle out the particulates before 
extraction.
    10.5.2 Extract the sample as follows:
    10.5.2.1 Place a 90-mm standard filter apparatus on a vacuum 
filtration flask or manifold and attach to a vacuum source. The vacuum 
gauge must read at least 25 in. of

[[Page 174]]

mercury when all valves are closed. Position a 90-mm C18 extraction disk 
onto the filter screen. Wet the entire disk with methanol. To aid in 
filtering samples with particulates, a 1-[micro]m glass fiber filter or 
Empore[supreg] Filter Aid 400 can be placed on the top of the disk and 
wetted with methanol. Install the reservoir and clamp. Resume vacuum to 
dry the disk. Interrupt the vacuum. Wash the disk and reservoir with 20 
mL of methylene chloride. Resume the vacuum briefly to pull methylene 
chloride through the disk. Interrupt the vacuum and allow the disk to 
soak for about a minute. Resume vacuum and completely dry the disk.
    10.5.2.2 Condition the disk with 20 mL of methanol. Apply vacuum 
until nearly all the solvent has passed through the disk, interrupting 
it while solvent remains on the disk. Allow the disk to soak for about a 
minute. Resume vacuum to pull most of the methanol through, but 
interrupting it to leave a layer of methanol on the surface of the disk. 
Do not allow disk to dry. For uniform flow and good recovery, it is 
critical the disk not be allowed to dry from now until the end of the 
extraction. Discard waste solvent. Rinse the disk with 20 mL of 
deionized water. Resume vacuum to pull most of the water through, but 
interrupt it to leave a layer of water on the surface of the disk. Do 
not allow the disk to dry. If disk does dry, recondition with methanol 
as above.
    10.5.2.3 Add the water sample to the reservoir and immediately apply 
the vacuum. If particulates have settled in the sample, gently decant 
the clear layer into the apparatus until most of the sample has been 
processed. Then pour the remainder including the particulates into the 
reservoir. Empty the sample bottle completely. When the filtration is 
complete, dry the disk for three minutes. Turn off the vacuum.
    10.5.3 Discard sample filtrate. Insert tube to collect the eluant. 
The tube should fit around the drip tip of the base. Reassemble the 
apparatus. Add 5.0 mL of acetone to the center of the disk, allowing it 
to spread evenly over the disk. Turn the vacuum on and quickly off when 
the filter surface nears dryness but still remains wet. Allow to soak 
for 15 seconds. Add 20 mL of methylene chloride to the sample bottle, 
seal and shake to rinse the inside of the bottle. Transfer the methylene 
chloride from the bottle to the filter. Resume the vacuum slowly so as 
to avoid splashing.
    Interrupt the vacuum when the filter surface nears dryness but still 
remains wet. Allow disk to soak in solvent for 20 seconds. Rinse the 
reservoir glass and disk with 10 mL of methylene chloride. Resume vacuum 
slowly. Interrupt vacuum when disk is covered with solvent. Allow to 
soak for 20 seconds. Resume vacuum to dry the disk. Remove the sample 
tube.
    10.5.4 Dry, concentrate, solvent exchange, and transfer the extract 
to a vial with fluoropolymer-lined cap, per section 10.3.
    10.5.5 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to an appropriately sized 
graduated cylinder. Record the sample volume to the nearest 5 mL. Sample 
volumes may also be determined by weighing the container before and 
after extraction or filling to the mark with water.

                           11. Extract Cleanup

    11.1 Cleanup may not be necessary for relatively clean samples 
(e.g., treated effluents, groundwater, drinking water). If particular 
circumstances require the use of a cleanup procedure, the laboratory may 
use any or all of the procedures below or any other appropriate 
procedure (e.g., gel permeation chromatography). However, the laboratory 
must first repeat the tests in sections 8.2, 8.3, and 8.4 to demonstrate 
that the requirements of those sections can be met using the cleanup 
procedure(s) as an integral part of this method. This is particularly 
important when the target analytes for the analysis include any of the 
single component pesticides in Table 2, because some cleanups have not 
been optimized for all of those analytes.
    11.1.1 The solid-phase cartridge (section 11.2) removes polar 
organic compounds such as phenols.
    11.1.2 The Florisil[supreg] column (section 11.3) allows for 
selected fractionation of the organochlorine analytes and will also 
eliminate polar interferences.
    11.1.3 Alumina column cleanup (section 11.4) also removes polar 
materials.
    11.1.4 Elemental sulfur, which interferes with the electron capture 
gas chromatography of some of the pesticides, may be removed using 
activated copper, or TBA sulfite. Sulfur removal (section 11.5) is 
required when sulfur is known or suspected to be present. Some 
chlorinated pesticides which also contain sulfur may be removed by this 
cleanup.
    11.1.5 Acid back extraction (section 11.6) may be useful for cleanup 
of PCBs and other compounds not adversely affected by sulfuric acid.
    11.2 Solid-phase extraction (SPE) as a cleanup. In order to use the 
C18 SPE cartridge in section 5.5.3.5 as a cleanup procedure, the sample 
extract must be exchanged from methylene chloride to methylene 
chloride:acetonitrile:hexane (50:3:47). Follow the solvent exchange 
steps in section 10.3.3.2 prior to attempting solid-phase cleanup.

    Note: This application of SPE is distinct from that used in this 
method for the extraction of aqueous samples in section 10.5. Analysts 
must be careful not to confuse the equipment, supplies, or procedural 
steps from these two different uses of SPE.


[[Page 175]]


    11.2.1 Setup.
    11.2.1.1 Attach the VacElute Manifold (section 5.5.3.2) to a water 
aspirator or vacuum pump with the trap and gauge installed between the 
manifold and vacuum source.
    11.2.1.2 Place the SPE cartridges in the manifold, turn on the 
vacuum source, and adjust the vacuum to 5 to 10 psi.
    11.2.2 Cartridge washing--Pre-elute each cartridge prior to use 
sequentially with 10-mL portions each of hexane, methanol, and water 
using vacuum for 30 seconds after each eluting solvent. Follow this pre-
elution with 1 mL methylene chloride and three 10-mL portions of the 
elution solvent (section 6.7.2.2) using vacuum for 5 minutes after each 
eluting solvent. Tap the cartridge lightly while under vacuum to dry 
between solvent rinses. The three portions of elution solvent may be 
collected and used as a cartridge blank, if desired. Finally, elute the 
cartridge with 10 mL each of methanol and water, using the vacuum for 30 
seconds after each eluant.
    11.2.3 Extract cleanup.
    11.2.3.1 After cartridge washing (section 11.2.2), release the 
vacuum and place the rack containing the 50-mL volumetric flasks 
(section 5.5.3.4) in the vacuum manifold. Re-establish the vacuum at 5 
to 10 psi.
    11.2.3.2 Using a pipette or a 1-mL syringe, transfer 1.0 mL of 
extract to the SPE cartridge. Apply vacuum for five minutes to dry the 
cartridge. Tap gently to aid in drying.
    11.2.3.3 Elute each cartridge into its volumetric flask sequentially 
with three 10-mL portions of the methylene chloride:acetonitrile:hexane 
(50:3:47) elution solvent (section 6.7.2.2), using vacuum for five 
minutes after each portion. Collect the eluants in the 50-mL volumetric 
flasks.
    11.2.3.4 Release the vacuum and remove the 50-mL volumetric flasks.
    11.2.3.5 Concentrate the eluted extracts per Section 10.3.
    11.3 Florisil[supreg]. In order to use Florisil cleanup, the sample 
extract must be exchanged from methylene chloride to hexane. Follow the 
solvent exchange steps in section 10.3.3.2 prior to attempting 
Florisil[supreg] cleanup.

    Note: Alternative formats for this cleanup may be used by the 
laboratory, including cartridges containing Florisil[supreg]. If an 
alternative format is used, consult the manufacturer's instructions and 
develop a formal documented procedure to replace the steps in section 
11.3 of this method and demonstrate that the alternative meets the 
relevant quality control requirements of this method.

    11.3.1 If the chromatographic column does not contain a frit at the 
bottom, place a small plug of pre-cleaned glass wool in the column 
(section 5.2.4) to retain the Florisil[supreg]. Place the mass of 
Florisil[supreg] (nominally 20 g) predetermined by calibration (section 
7.8 and Table 6) in a chromatographic column. Tap the column to settle 
the Florisil[supreg] and add 1 to 2 cm of granular anhydrous sodium 
sulfate to the top.
    11.3.2 Add 60 mL of hexane to wet and rinse the sodium sulfate and 
Florisil[supreg]. Just prior to exposure of the sodium sulfate layer to 
the air, stop the elution of the hexane by closing the stopcock on the 
chromatographic column. Discard the eluant.
    11.3.3 Transfer the concentrated extract (section 10.3.3) onto the 
column. Complete the transfer with two 1-mL hexane rinses, drawing the 
extract and rinses down to the level of the sodium sulfate.
    11.3.4 Place a clean 500-mL K-D flask and concentrator tube under 
the column. Elute Fraction 1 with 200 mL of 6% (v/v) ethyl ether in 
hexane at a rate of approximately 5 mL/min. Remove the K-D flask and set 
it aside for later concentration. Elute Fraction 2 with 200 mL of 15% 
(v/v) ethyl ether in hexane into a second K-D flask. Elute Fraction 3 
with 200 mL of 50% (v/v) ethyl ether in hexane into a third K-D flask. 
The elution patterns for the pesticides and PCBs are shown in Table 6.
    11.3.5 Concentrate the fractions as in Section 10.3, except use 
hexane to prewet the column and set the water bath at about 85 [deg]C. 
When the apparatus is cool, remove the Snyder column and rinse the flask 
and its lower joint into the concentrator tube with hexane. Adjust the 
volume of Fraction 1 to approximately 10 mL for sulfur removal (Section 
11.5), if required; otherwise, adjust the volume of the fractions to 10 
mL, 1.0 mL, or other volume needed for the sensitivity desired. Analyze 
the concentrated extract by gas chromatography (Section 12).
    11.4 Alumina. The sample extract must be exchanged from methylene 
chloride to hexane. Follow the solvent exchange steps in section 
10.3.3.2 prior to attempting alumina cleanup.
    11.4.1 If the chromatographic column does not contain a frit at the 
bottom, place a small plug of pre-cleaned glass wool in the 
chromatographic column (section 5.2.4) to retain the alumina. Add 10 g 
of alumina (section 6.7.3) on top of the plug. Tap the column to settle 
the alumina. Place 1-2 g of anhydrous sodium sulfate on top of the 
alumina.
    11.4.2 Close the stopcock and fill the column to just above the 
sodium sulfate with hexane. Add 25 mL of hexane. Open the stopcock and 
adjust the flow rate of hexane to approximately 2 mL/min. Do not allow 
the column to go dry throughout the elutions.
    11.4.3 When the level of the hexane is at the top of the column, 
quantitatively transfer the extract to the column. When the level of the 
extract is at the top of the column, slowly add 25 mL of hexane and 
elute the column to the level of the sodium sulfate. Discard the hexane.
    11.4.4 Place a K-D flask (section 5.2.5.1.2) under the column and 
elute the pesticides

[[Page 176]]

with approximately 150 mL of hexane:ethyl ether (80:20 v/v). It may be 
necessary to adjust the volume of elution solvent for slightly different 
alumina activities.
    11.4.5 Concentrate the extract per section 10.3.
    11.5 Sulfur removal--Elemental sulfur will usually elute in Fraction 
1 of the Florisil[supreg] column cleanup. If Florisil[supreg] cleanup is 
not used, or to remove sulfur from any of the Florisil[supreg] 
fractions, use one of the sulfur removal procedures below. These 
procedures may be applied to extracts in hexane, ethyl ether, or 
methylene chloride.

    Note: Separate procedures using copper or TBA sulfite are provided 
in this section for sulfur removal. They may be used separately or in 
combination, if desired.

    11.5.1 Removal with copper (Reference 15).

    Note: Some of the analytes in Table 2 are not amenable to sulfur 
removal with copper (e.g., atrazine and diazinon). Therefore, before 
using copper to remove sulfur from an extract that will be analyzed for 
any of the non-PCB analytes in Table 2, the laboratory must demonstrate 
that the analytes can be extracted from an aqueous sample matrix that 
contains sulfur and recovered from an extract treated with copper. 
Acceptable performance can be demonstrated through the preparation and 
analysis of a matrix spike sample that meets the QC requirements for 
recovery.

    11.5.1.1 Quantitatively transfer the extract to a 40- to 50-mL flask 
or bottle. If there is evidence of water in the K-D or round-bottom 
flask after the transfer, rinse the flask with small portions of 
hexane:acetone (40:60) and add to the flask or bottle. Mark and set 
aside the concentration flask for future use.
    11.5.1.2 Add 10-20 g of granular anhydrous sodium sulfate to the 
flask. Swirl to dry the extract.
    11.5.1.3 Add activated copper (section 6.7.4.1.4) and allow to stand 
for 30-60 minutes, swirling occasionally. If the copper does not remain 
bright, add more and swirl occasionally for another 30-60 minutes.
    11.5.1.4 After drying and sulfur removal, quantitatively transfer 
the extract to a nitrogen-evaporation vial or tube and proceed to 
section 10.3.3 for nitrogen evaporation and solvent exchange, taking 
care to leave the sodium sulfate and copper foil in the flask.
    11.5.2 Removal with TBA sulfite.
    11.5.2.1 Using small volumes of hexane, quantitatively transfer the 
extract to a 40- to 50-mL centrifuge tube with fluoropolymer-lined screw 
cap.
    11.5.2.2 Add 1-2 mL of TBA sulfite reagent (section 6.7.4.2.4), 2-3 
mL of 2-propanol, and approximately 0.7 g of sodium sulfite (section 
6.7.4.2.2) crystals to the tube. Cap and shake for 1-2 minutes. If the 
sample is colorless or if the initial color is unchanged, and if clear 
crystals (precipitated sodium sulfite) are observed, sufficient sodium 
sulfite is present. If the precipitated sodium sulfite disappears, add 
more crystalline sodium sulfite in approximately 0.5-g portions until a 
solid residue remains after repeated shaking.
    11.5.2.3 Add 5-10 mL of reagent water and shake for 1-2 minutes. 
Centrifuge to settle the solids.
    11.5.2.4 Quantitatively transfer the hexane (top) layer through a 
small funnel containing a few grams of granular anhydrous sodium sulfate 
to a nitrogen-evaporation vial or tube and proceed to section 10.3.3 for 
micro-concentration and solvent exchange.
    11.6 Acid back extraction (section 6.1.2).
    11.6.1 Quantitatively transfer the extract (section 10.3.1.5) to a 
250-mL separatory funnel.
    11.6.2 Partition the extract against 50 mL of sulfuric acid solution 
(section 6.1.2). Discard the aqueous layer. Repeat the acid washing 
until no color is visible in the aqueous layer, to a maximum of four 
washings.
    11.6.3 Partition the extract against 50 mL of sodium chloride 
solution (section 6.7.5). Discard the aqueous layer.
    11.6.4 Proceed to section 10.3.3 for micro-concentration and solvent 
exchange.

                         12. Gas Chromatography

    12.1 Establish the same operating conditions used in section 7.1 for 
instrument calibration.
    12.2 If the internal standard calibration procedure is used, add the 
internal standard solution (section 6.9.3) to the extract as close as 
possible to the time of injection to minimize the possibility of loss by 
evaporation, adsorption, or reaction. For example, add 1 [micro]L of 10 
[micro]g/mL internal standard solution into the extract, assuming no 
dilutions. Mix thoroughly.
    12.3 Simultaneously inject an appropriate volume of the sample 
extract or standard solution onto both columns, using split, splitless, 
solvent purge, large-volume, or on-column injection. Alternatively, if 
using a single-column GC configuration, inject an appropriate volume of 
the sample extract or standard solution onto each GC column 
independently. If the sample is injected manually, the solvent-flush 
technique should be used. The injection volume depends upon the 
technique used and the sensitivity needed to meet MDLs or reporting 
limits for regulatory compliance. Injection volumes must be the same for 
all extracts. Record the volume injected to the nearest 0.05 [micro]L.
    12.4 Set the data system or GC control to start the temperature 
program upon sample injection, and begin data collection after the 
solvent peak elutes. Set the data system to stop data collection after 
the last analyte is expected to elute and to return the column to the 
initial temperature.

[[Page 177]]

    12.5 Perform all qualitative and quantitative measurements as 
described in Sections 14 and 15. When standards and extracts are not 
being used for analyses, store them refrigerated at <6 [deg]C, protected 
from light, in screw-cap vials equipped with un-pierced fluoropolymer-
lined septa.

                  13. System and Laboratory Performance

    13.1 At the beginning of each shift during which standards or 
extracts are analyzed, GC system performance and calibration must be 
verified for all analytes and surrogates on both column/detector 
systems. Adjustment and/or recalibration (per section 7) are performed 
until all performance criteria are met. Only after all performance 
criteria are met may samples, blanks and other QC samples, and standards 
be analyzed.
    13.2 Inject an aliquot of the calibration verification standard 
(section 6.8.4) on both columns. Inject an aliquot of each of the multi-
component standards.
    13.3 Retention times--The absolute retention times of the peak 
maxima shall be within 2 seconds of the retention 
times in the calibration verification (section 7.8).
    13.4 GC resolution--Resolution is acceptable if the valley height 
between two peaks (as measured from the baseline) is less than 40% of 
the shorter of the two peaks.
    13.4.1 DB-608 column--DDT and endrin aldehyde
    13.4.2 DB-1701 column--alpha and gamma chlordane

    Note: If using other GC columns or stationary phases, these 
resolution criteria apply to these four target analytes and any other 
closely eluting analytes on those other GC columns.

    13.5 Decomposition of DDT and endrin--If DDT, endrin, or their 
breakdown products are to be determined, this test must be performed 
prior to calibration verification (section 13.6). DDT decomposes to DDE 
and DDD. Endrin decomposes to endrin aldehyde and endrin ketone.
    13.5.1 Inject 1 [micro]L of the DDT and endrin decomposition 
solution (section 6.8.7). As noted in section 6.8.7, other injection 
volumes may be used as long as the concentrations of DDT and endrin in 
the solution are adjusted to introduce the masses of the two analytes 
into the instrument that are listed in section 6.8.7.
    13.5.2 Measure the areas of the peaks for DDT, DDE, DDD, endrin, 
endrin aldehyde, and endrin ketone in the chromatogram and calculate the 
percent breakdown as shown in the equations below:
[GRAPHIC] [TIFF OMITTED] TR28AU17.005

    13.5.3 Both the % breakdown of DDT and of endrin must be less than 
20%, otherwise the system is not performing acceptably for DDT and 
endrin. In this case, repair the GC column system that failed and repeat 
the performance tests (sections 13.2 to 13.6) until the specification is 
met.

    Note: DDT and endrin decomposition are usually caused by 
accumulations of particulates in the injector and in the front end of 
the column. Cleaning and silanizing the injection port liner, and 
breaking off a short section of the front end of the column will usually 
eliminate the decomposition problem. Either of these corrective actions 
may affect retention times, GC resolution, and calibration linearity.

    13.6 Calibration verification.
    13.6.1 Compute the percent recovery of each analyte and of the 
coeluting analytes, based on the initial calibration data (section 7.5 
or 7.6).
    13.6.2 For each analyte or for coeluting analytes, compare the 
concentration with the limits for calibration verification in Table 4. 
For coeluting analytes, use the coeluting analyte with the least 
restrictive specification (the widest range). For analytes in Table 2 
not listed in Table 4, QC acceptance criteria must be developed by the 
laboratory. EPA has provided guidance for development of QC acceptance 
criteria (References 13 and 14). If the recoveries for all analytes meet 
the acceptance criteria, system performance is acceptable and analysis 
of blanks and samples may continue. If, however, any recovery falls 
outside the calibration verification range, system performance is 
unacceptable for that analyte. If this occurs, repair the system and 
repeat the test (section 13.6), or prepare a fresh calibration

[[Page 178]]

standard and repeat the test, or recalibrate (section 7). See Section 
8.1.7 for information on repeated test failures.
    13.7 Laboratory control sample.
    13.7.1 Analyze the extract of the LCS (section 6.8.3) extracted with 
each sample batch (Section 8.4). See Section 8.4 for criteria acceptance 
of the LCS.
    13.7.2 It is suggested, but not required, that the laboratory update 
statements of data quality. Add results that pass the specifications in 
section 13.7.3 to initial (section 8.7) and previous ongoing data. 
Update QC charts to form a graphic representation of continued 
laboratory performance. Develop a statement of laboratory data quality 
for each analyte by calculating the average percent recovery (R) and the 
standard deviation of percent recovery, sr. Express the accuracy as a 
recovery interval from R - 2sr to R + 2sr. For example, if R = 95% and 
sr = 5%, the accuracy is 85 to 105%.
    13.8 Internal standard response--If internal standard calibration is 
used, verify that detector sensitivity has not changed by comparing the 
response (area or height) of each internal standard in the sample, 
blank, LCS, MS, and MSD to the response in calibration verification 
(section 6.8.3). The peak area or height of the internal standard should 
be within 50% to 200% (\1/2\ to 2x) of its respective peak area or 
height in the verification standard. If the area or height is not within 
this range, compute the concentration of the analytes using the external 
standard method (section 7.5). If the analytes are affected, re-prepare 
and reanalyze the sample, blank, LCS, MS, or MSD, and repeat the 
pertinent test.

                     14. Qualitative Identification

    14.1 Identification is accomplished by comparison of data from 
analysis of a sample, blank, or other QC sample with data from 
calibration verification (section 7.7.1 or 13.5), and with data stored 
in the retention-time and calibration libraries (section 7.7). The 
retention time window is determined as described in section 14.2. 
Identification is confirmed when retention time agrees on both GC 
columns, as described below. Alternatively, GC/MS identification may be 
used to provide another means of identification.
    14.2 Establishing retention time windows.
    14.2.1 Using the data from the multi-point initial calibration 
(section 7.4), determine the retention time in decimal minutes (not 
minutes:seconds) of each peak representing a single-component target 
analyte on each column/detector system. For the multi-component 
analytes, use the retention times of the five largest peaks in the 
chromatograms on each column/detector system.
    14.2.2 Calculate the standard deviation of the retention times for 
each single-component analyte on each column/detector system and for the 
three to five exclusive (unique large) peaks for each multi-component 
analyte.
    14.2.3 Define the width of the retention time window as three times 
that standard deviation. Establish the center of the retention time 
window for each analyte by using the absolute retention time for each 
analyte from the calibration verification standard at the beginning of 
the analytical shift. For samples run during the same shift as an 
initial calibration, use the retention time of the mid-point standard of 
the initial calibration. If the calculated RT window is less than 0.02 
minutes, then use 0.02 minutes as the window.

    Note: Procedures for establishing retention time windows from other 
sources may be employed provided that they are clearly documented and 
provide acceptable performance. Such performance may be evaluated using 
the results for the spiked QC samples described in this method, such as 
laboratory control samples and matrix spike samples.

    14.2.4 The retention time windows must be recentered when a new GC 
column is installed or if a GC column has been shortened during 
maintenance to a degree that the retention times of analytes in the 
calibration verification standard have shifted close to the lower limits 
of the established retention time windows.
    14.2.5 RT windows should be checked periodically by examining the 
peaks in spiked samples such as the LCS or MS/MSD to confirm that peaks 
for known analytes are properly identified.
    14.2.6 If the retention time of an analyte in the calibration 
(Section 7.4) varies by more than 5 seconds across the calibration range 
as a function of the concentration of the standard, using the standard 
deviation of the retention times (section 14.2.3) to set the width of 
the retention time window may not adequately serve to identify the 
analyte in question under routine conditions. In such cases, data from 
additional analyses of standards may be required to adequately model the 
chromatographic behavior of the analyte.
    14.3 Identifying the analyte in a sample.
    14.3.1 In order to identify a single-component analyte from analysis 
of a sample, blank, or other QC sample, the peak representing the 
analyte must fall within its respective retention time windows on both 
column/detector systems (as defined in section 14.2). That 
identification is further supported by the comparison of the numerical 
results on both columns, as described in section 15.7.
    14.3.2 In order to identify a multi-component analyte, pattern 
matching (fingerprinting) may be used, or the three to five exclusive 
(unique and largest) peaks for that analyte must fall within their 
respective retention time windows on both column/detector systems (as 
defined in section 14.2).

[[Page 179]]

That identification is further supported by the comparison of the 
numerical results on both columns, as described in section 15.7. 
Alternatively, GC/MS identification may be used. Differentiation among 
some of the Aroclors may require evaluation of more than five peaks to 
ensure correct identification.
    14.4 GC/MS confirmation. When the concentration of an analyte is 
sufficient and the presence or identity is suspect, its presence should 
be confirmed by GC/MS. In order to match the sensitivity of the GC/ECD, 
confirmation would need to be by GC/MS-SIM, or the estimated 
concentration would need to be 100 times higher than the GC/ECD 
calibration range. The extract may be concentrated by an additional 
amount to allow a further attempt at GC/MS confirmation.
    14.5 Additional information that may aid the laboratory in the 
identification of an analyte. The occurrence of peaks eluting near the 
retention time of an analyte of interest increases the probability of a 
false positive for the analyte. If the concentration is insufficient for 
confirmation by GC/MS, the laboratory may use the cleanup procedures in 
this method (section 11) on a new sample aliquot to attempt to remove 
the interferent. After attempts at cleanup are exhausted, the following 
steps may be helpful to assure that the substance that appears in the RT 
windows on both columns is the analyte of interest.
    14.5.1 Determine the consistency of the RT data for the analyte on 
each column. For example, if the RT is very stable (i.e., varies by no 
more than a few seconds) for the calibration, calibration verification, 
blank, LCS, and MS/MSD, the RT for the analyte of interest in the sample 
should be within this variation regardless of the window established in 
Section 14.2. If the analyte is not within this variation on both 
columns, it is likely not present.
    14.5.2 The possibility exists that the RT for the analyte in a 
sample could shift if extraneous materials are present. This possibility 
may be able to be confirmed or refuted by the behavior of the surrogates 
in the sample. If multiple surrogates are used that span the length of 
the chromatographic run, the RTs for the surrogates on both columns are 
consistent with their RTs in calibration, calibration verification, 
blank, LCS, and MS/MSD, it is unlikely that the RT for the analyte of 
interest has shifted.
    14.5.3 If the RT for the analyte is shifted slightly later on one 
column and earlier on the other, and the surrogates have not shifted, it 
is highly unlikely that the analyte is present, because shifts nearly 
always occur in the same direction on both columns.

                     15. Quantitative Determination

    15.1 External standard quantitation--Calculate the concentration of 
the analyte in the extract using the calibration curve or average 
calibration factor determined in calibration (section 7.5.2) and the 
following equation:
[GRAPHIC] [TIFF OMITTED] TR28AU17.006

where:

Cex = Concentration of the analyte in the extract (ng/mL)
As = Peak height or area for the analyte in the standard or 
          sample
CF = Calibration factor, as defined in Section 7.5.1

    15.2 Internal standard quantitation--Calculate the concentration of 
the analyte in the extract using the calibration curve or average 
response factor determined in calibration (section 7.6.2) and the 
following equation:
[GRAPHIC] [TIFF OMITTED] TR28AU17.007

where:

Cex = Concentration of the analyte in the extract (ng/mL)
As = Peak height or area for the analyte in the standard or 
          sample
Cis = Concentration of the internal standard (ng/mL)
Ais = Area of the internal standard
RF = Response factor, as defined in section 7.6.1


[[Page 180]]


    15.3 Calculate the concentration of the analyte in the sample using 
the concentration in the extract, the extract volume, the sample volume, 
and the dilution factor, per the following equation:
[GRAPHIC] [TIFF OMITTED] TR28AU17.008

where:

Cs = Concentration of the analyte in the sample ([micro]g/L)
Vex = Final extract volume (mL)
Cex = Concentration in the extract (ng/mL)
Vs = Volume of sample (L)
DF = Dilution factor

and the factor of 1,000 in the denominator converts the final units from 
ng/L to [micro]g/L
    15.4 If the concentration of any target analyte exceeds the 
calibration range, either extract and analyze a smaller sample volume, 
or dilute and analyze the diluted extract.
    15.5 Quantitation of multi-component analytes.
    15.5.1 PCBs as Aroclors. Quantify an Aroclor by comparing the sample 
chromatogram to that of the most similar Aroclor standard as indicated 
in section 14.3.2. Compare the responses of 3 to 5 major peaks in the 
calibration standard for that Aroclor with the peaks observed in the 
sample extract. The amount of Aroclor is calculated using the individual 
calibration factor for each of the 3 to 5 characteristic peaks chosen in 
section 7.5.1. Determine the concentration of each of the characteristic 
peaks, using the average calibration factor calculated for that peak in 
section 7.5.2, and then those 3 to 5 concentrations are averaged to 
determine the concentration of that Aroclor.
    15.5.2 Other multi-component analytes. Quantify any other multi-
component analytes (technical chlordane or toxaphene) using the same 
peaks used to develop the average calibration factors in section 7.5.2. 
Determine the concentration of each of the characteristic peaks, and 
then the concentrations represented by those characteristic peaks are 
averaged to determine the concentration of the analyte. Alternatively, 
for toxaphene, the analyst may determine the calibration factor in 
section 7.5.2 by summing the areas of all of the peaks for the analyte 
and using the summed of the peak areas in the sample chromatogram to 
determine the concentration. However, the approach used for toxaphene 
must be the same for the calibration and the sample analyses.
    15.6 Reporting of results. As noted in section 1.6.1, EPA has 
promulgated this method at 40 CFR part 136 for use in wastewater 
compliance monitoring under the National Pollutant Discharge Elimination 
System (NPDES). The data reporting practices described here are focused 
on such monitoring needs and may not be relevant to other uses of the 
method.
    15.6.1 Report results for wastewater samples in [micro]g/L without 
correction for recovery. (Other units may be used if required by in a 
permit.) Report all QC data with the sample results.
    15.6.2 Reporting level. Unless specified otherwise by a regulatory 
authority or in a discharge permit, results for analytes that meet the 
identification criteria are reported down to the concentration of the ML 
established by the laboratory through calibration of the instrument (see 
section 7.5 or 7.6 and the glossary for the derivation of the ML). EPA 
considers the terms ``reporting limit,'' ``quantitation limit,'' and 
``minimum level'' to be synonymous.
    15.6.2.1 Report the lower result from the two columns (see section 
15.7 below) for each analyte in each sample or QC standard at or above 
the ML to 3 significant figures. Report a result for each analyte in 
each sample or QC standard below the ML as ``12, are hazardous and must 
be handled and disposed of as hazardous waste, or neutralized and 
disposed of in accordance with all federal, state, and local 
regulations. It is the laboratory's responsibility to comply with all 
federal, state, and local regulations governing waste management, 
particularly the hazardous waste identification rules and land disposal 
restrictions. The laboratory using this method has the responsibility to 
protect the air, water, and land by minimizing and controlling all 
releases from fume hoods and bench operations. Compliance is also 
required with any sewage discharge permits and regulations. For further 
information on waste management, see ``The Waste Management Manual for 
Laboratory Personnel,'' also available from the American Chemical 
Society at the address in section 18.3.
    19.3 Many analytes in this method decompose above 500 [deg]C. Low-
level waste such as absorbent paper, tissues, animal remains, and 
plastic gloves may be burned in an appropriate incinerator. Gross 
quantities of neat or highly concentrated solutions of toxic or 
hazardous chemicals should be packaged securely and disposed of through 
commercial or governmental channels that are capable of handling toxic 
wastes.
    19.4 For further information on waste management, consult The Waste 
Management Manual for Laboratory Personnel and

[[Page 183]]

Less is Better-Laboratory Chemical Management for Waste Reduction, 
available from the American Chemical Society's Department of Government 
Relations and Science Policy, 1155 16th Street NW., Washington, DC 
20036, 202-872-4477.

                             20. References

1. ``Determination of Pesticides and PCBs in Industrial and Municipal 
          Wastewaters,'' EPA 600/4-82-023, National Technical 
          Information Service, PB82-214222, Springfield, Virginia 22161, 
          April 1982.
2. ``EPA Method Study 18 Method 608-Organochlorine Pesticides and 
          PCBs,'' EPA 600/4-84-061, National Technical Information 
          Service, PB84-211358, Springfield, Virginia 22161, June 1984.
3. ``Method Detection Limit and Analytical Curve Studies, EPA Methods 
          606, 607, and 608,'' Special letter report for EPA Contract 
          68-03-2606, U.S. Environmental Protection Agency, 
          Environmental Monitoring and Support Laboratory, Cincinnati, 
          Ohio 45268, June 1980.
4. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard Practice 
          for Preparation of Sample Containers and for Preservation of 
          Organic Constituents,'' American Society for Testing and 
          Materials, Philadelphia.
5. Giam, C.S., Chan, H.S., and Nef, G.S. ``Sensitive Method for 
          Determination of Phthalate Ester Plasticizers in Open-Ocean 
          Biota Samples,'' Analytical Chemistry, 47:2225 (1975).
6. Giam, C.S. and Chan, H.S. ``Control of Blanks in the Analysis of 
          Phthalates in Air and Ocean Biota Samples,'' U.S. National 
          Bureau of Standards, Special Publication 442, pp. 701-708, 
          1976.
7. Solutions to Analytical Chemistry Problems with Clean Water Act 
          Methods, EPA 821-R-07-002, March 2007.
8. ``Carcinogens-Working With Carcinogens,'' Department of Health, 
          Education, and Welfare, Public Health Service, Center for 
          Disease Control, National Institute for Occupational Safety 
          and Health, Publication No. 77-206, August 1977.
9. ``Occupational Exposure to Hazardous Chemicals in Laboratories,'' (29 
          CFR 1910.1450), Occupational Safety and Health Administration, 
          OSHA.
10. 40 CFR 136.6(b)(4)(j).
11. Mills, P.A. ``Variation of Florisil Activity: Simple Method for 
          Measuring Absorbent Capacity and Its Use in Standardizing 
          Florisil Columns,'' Journal of the Association of Official 
          Analytical Chemists, 51:29, (1968).
12. 40 CFR 136.6(b)(2)(i).
13. Protocol for EPA Approval of New Methods for Organic and Inorganic 
          Analytes in Wastewater and Drinking Water (EPA-821-B-98-003) 
          March 1999.
14. Methods 4500 Cl F and 4500 Cl G, Standard Methods for the 
          Examination of Water and Wastewater, published jointly by the 
          American Public Health Association, American Water Works 
          Association, and Water Environment Federation, 1015 Fifteenth 
          St., Washington, DC 20005, 20th Edition, 2000.
15. ``Manual of Analytical Methods for the Analysis of Pesticides in 
          Human and Environmental Samples,'' EPA-600/8-80-038, U.S. 
          Environmental Protection Agency, Health Effects Research 
          Laboratory, Research Triangle Park, North Carolina.
16. USEPA, 2000, Method 1656 Organo-Halide Pesticides In Wastewater, 
          Soil, Sludge, Sediment, and Tissue by GC/HSD, EPA-821-R-00-
          017, September 2000.
17. USEPA, 2010, Method 1668C Chlorinated Biphenyl Congeners in Water, 
          Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS, EPA-820-R-
          10-005, April 2010.
18. USEPA, 2007, Method 1699: Pesticides in Water, Soil, Sediment, 
          Biosolids, and Tissue by HRGC/HRMS, EPA-821-R-08-001, December 
          2007.
19. ``Less is Better,'' American Chemical Society on-line publication, 
          http://www.acs.org/content/dam/acsorg/about/governance/
          committees/chemicalsafety/publications/less-is-better.pdf.
20. EPA Method 608 ATP 3M0222, An alternative test procedure for the 
          measurement of organochlorine pesticides and polychlorinated 
          biphenyls in waste water. Federal Register, Vol. 60, No. 148 
          August 2, 1995.

                               21. Tables

                                             Table 1--Pesticides \1\
----------------------------------------------------------------------------------------------------------------
                             Analyte                                  CAS No.     MDL \2\ (ng/L)   ML \3\ (ng/L)
----------------------------------------------------------------------------------------------------------------
Aldrin..........................................................        309-00-2               4              12
alpha-BHC.......................................................        319-84-6               3               9
beta-BHC........................................................        319-85-7               6              18
delta-BHC.......................................................        319-86-8               9              27
gamma-BHC (Lindane).............................................         58-89-9               4              12
alpha-Chlordane \ 4\............................................       5103-71-9              14              42
gamma-Chlordane \ 4\............................................       5103-74-2              14              42
4,4[min]-DDD....................................................         72-54-8              11              33
4,4[min]-DDE....................................................         72-55-9               4              12
4,4[min]-DDT....................................................         50-29-3              12              36

[[Page 184]]

 
Dieldrin........................................................         60-57-1               2               6
Endosulfan I....................................................        959-98-8              14              42
Endosulfan II...................................................      33213-65-9               4              12
Endosulfan sulfate..............................................       1031-07-8              66             198
Endrin..........................................................         72-20-8               6              18
Endrin aldehyde.................................................       7421-93-4              23              70
Heptachlor......................................................         76-44-8               3               9
Heptachlor epoxide..............................................       1024-57-3              83             249
----------------------------------------------------------------------------------------------------------------
\1\ All analytes in this table are Priority Pollutants (40 CFR part 423, appendix A).
\2\ 40 CFR part 136, appendix B, June 30, 1986.
\3\ ML = Minimum Level--see Glossary for definition and derivation, calculated as 3 times the MDL.
\4\ MDL based on the MDL for Chlordane.


                                          Table 2--Additional Analytes
----------------------------------------------------------------------------------------------------------------
                             Analyte                                  CAS No.     MDL \3\ (ng/L)   ML \4\ (ng/L)
----------------------------------------------------------------------------------------------------------------
Acephate........................................................      30560-19-1
Alachlor........................................................      15972-60-8
Atrazine........................................................       1912-24-9
Benfluralin (Benefin)...........................................       1861-40-1
Bromacil........................................................        314-40-9
Bromoxynil octanoate............................................       1689-99-2
Butachlor.......................................................      23184-66-9
Captafol........................................................       2425-06-1
Captan..........................................................        133-06-2
Carbophenothion (Trithion)......................................        786-19-6
Chlorobenzilate.................................................        510-15-6
Chloroneb (Terraneb)............................................       2675-77-6
Chloropropylate (Acaralate).....................................       5836-10-2
Chlorothalonil..................................................       1897-45-6
Cyanazine.......................................................      21725-46-2
DCPA (Dacthal)..................................................       1861-32-1
2,4[min]-DDD....................................................         53-19-0
2,4[min]-DDE....................................................       3424-82-6
2,4[min]-DDT....................................................        789-02-6
Diallate (Avadex)...............................................       2303-16-4
1,2-Dibromo-3-chloropropane (DBCP)..............................         96-12-8
Dichlone........................................................        117-80-6
Dichloran.......................................................         99-30-9
Dicofol.........................................................        115-32-2
Endrin ketone...................................................      53494-70-5
Ethalfluralin (Sonalan).........................................      55283-68-6
Etridiazole.....................................................       2593-15-9
Fenarimol (Rubigan).............................................      60168-88-9
Hexachlorobenzene \1\...........................................        118-74-1
Hexachlorocyclopentadiene \1\...................................         77-47-4
Isodrin.........................................................        465-73-6
Isopropalin (Paarlan)...........................................      33820-53-0
Kepone..........................................................        143-50-0
Methoxychlor....................................................         72-43-5
Metolachlor.....................................................      51218-45-2
Metribuzin......................................................      21087-64-9
Mirex...........................................................       2385-85-5
Nitrofen (TOK)..................................................       1836-75-5
cis-Nonachlor...................................................       5103-73-1
trans-Nonachlor.................................................      39765-80-5
Norfluorazon....................................................      27314-13-2
Octachlorostyrene...............................................      29082-74-4
Oxychlordane....................................................      27304-13-8
PCNB (Pentachloronitrobenzene)..................................         82-68-8
Pendamethalin (Prowl)...........................................      40487-42-1
cis-Permethrin..................................................      61949-76-6
trans-Permethrin................................................      61949-77-7
Perthane (Ethylan)..............................................         72-56-0
Propachlor......................................................       1918-16-7
Propanil........................................................        709-98-8
Propazine.......................................................        139-40-2
Quintozene......................................................         82-68-8
Simazine........................................................        122-34-9

[[Page 185]]

 
Strobane........................................................       8001-50-1
Technazene......................................................        117-18-0
Technical Chlordane \2\.........................................  ..............
Terbacil........................................................       5902-51-2
Terbuthylazine..................................................       5915-41-3
Toxaphene \1\...................................................       8001-35-2             240             720
Trifluralin.....................................................       1582-09-8
PCB-1016 \1\....................................................      12674-11-2
PCB-1221 \1\....................................................      11104-28-2
PCB-1232 \1\....................................................      11141-16-5
PCB-1242 \1\....................................................      53469-21-9              65              95
PCB-1248 \1\....................................................      12672-29-6
PCB-1254 \1\....................................................      11097-69-1
PCB-1260 \1\....................................................      11096-82-5
PCB-1268........................................................      11100-14-4  ..............
----------------------------------------------------------------------------------------------------------------
\1\ Priority Pollutants (40 CFR part 423, appendix A).
\2\ Technical Chlordane may be used in cases where historical reporting has only been for this form of
  Chlordane.
\3\ 40 CFR part 136, appendix B, June 30, 1986.
\4\ ML = Minimum Level--see Glossary for definition and derivation, calculated as 3 times the MDL.


                  Table 3--Example Retention Times \1\
------------------------------------------------------------------------
                                             Retention time (min) \2\
                 Analyte                 -------------------------------
                                              DB-608          DB-1701
------------------------------------------------------------------------
Acephate................................            5.03           (\3\)
Trifluralin.............................            5.16            6.79
Ethalfluralin...........................            5.28            6.49
Benfluralin.............................            5.53            6.87
Diallate-A..............................            7.15            6.23
Diallate-B..............................            7.42            6.77
alpha-BHC...............................            8.14            7.44
PCNB....................................            9.03            7.58
Simazine................................            9.06            9.29
Atrazine................................            9.12            9.12
Terbuthylazine..........................            9.17            9.46
gamma-BHC (Lindane).....................            9.52            9.91
beta-BHC................................            9.86           11.90
Heptachlor..............................           10.66           10.55
Chlorothalonil..........................           10.66           10.96
Dichlone................................           10.80           (\4\)
Terbacil................................           11.11           12.63
delta-BHC...............................           11.20           12.98
Alachlor................................           11.57           11.06
Propanil................................           11.60           14.10
Aldrin..................................           11.84           11.46
DCPA....................................           12.18           12.09
Metribuzin..............................           12.80           11.68
Triadimefon.............................           12.99           13.57
Isopropalin.............................           13.06           13.37
Isodrin.................................           13.47           11.12
Heptachlor epoxide......................           13.97           12.56
Pendamethalin...........................           14.21           13.46
Bromacil................................           14.39           (\3\)
alpha-Chlordane.........................           14.63           14.20
Butachlor...............................           15.03           15.69
gamma-Chlordane.........................           15.24           14.36
Endosulfan I............................           15.25           13.87
4,4[min]-DDE............................           16.34           14.84
Dieldrin................................           16.41           15.25
Captan..................................           16.83           15.43
Chlorobenzilate.........................           17.58           17.28
Endrin..................................           17.80           15.86
Nitrofen (TOK)..........................           17.86           17.47
Kepone..................................           17.92           (3 5)
4,4[min]-DDD............................           18.43           17.77
Endosulfan II...........................           18.45           18.57
Bromoxynil octanoate....................           18.85           18.57
4,4[min]-DDT............................           19.48           18.32

[[Page 186]]

 
Carbophenothion.........................           19.65           18.21
Endrin aldehyde.........................           19.72           19.18
Endosulfan sulfate......................           20.21           20.37
Captafol................................           22.51           21.22
Norfluorazon............................           20.68           22.01
Mirex...................................           22.75           19.79
Methoxychlor............................           22.80           20.68
Endrin ketone...........................           23.00           21.79
Fenarimol...............................           24.53           23.79
cis-Permethrin..........................           25.00           23.59
trans-Permethrin........................           25.62           23.92
PCB-1016................................
PCB-1221................................
PCB-1232................................
PCB-1242................................
PCB-1248................................
PCB-1254................................
PCB-1260 (5 peaks)......................           15.44           14.64
                                                   15.73           15.36
                                                   16.94           16.53
                                                   17.28           18.70
                                                   19.17           19.92
Toxaphene (5 peaks).....................           16.60           16.60
                                                   17.37           17.52
                                                   18.11           17.92
                                                   19.46           18.73
                                                   19.69           19.00
------------------------------------------------------------------------
\1\ Data from EPA Method 1656 (Reference 16).
\2\ Columns: 30-m long x 0.53-mm ID fused-silica capillary; DB-608, 0.83
  [micro]m; and DB-1701, 1.0 [micro]m.
Conditions suggested to meet retention times shown: 150 [deg]C for 0.5
  minute, 150-270 [deg]C at 5 [deg]C/min, and 270 [deg]C until trans-
  Permethrin elutes.
Carrier gas flow rates approximately 7 mL/min.
\3\ Does not elute from DB-1701 column at level tested.
\4\ Not recovered from water at the levels tested.
\5\ Dichlone and Kepone do not elute from the DB-1701 column and should
  be confirmed on DB-5.


                                                             Table 4--QC Acceptance Criteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                            Calibration        Test
                         Analyte                           verification    concentration  Limit for s (%    Range for X     Range for P   Maximum MS/MSD
                                                                (%)        ([micro]g/L)         SD)             (%)             (%)           RPD (%)
--------------------------------------------------------------------------------------------------------------------------------------------------------
Aldrin..................................................          75-125             2.0              25          54-130          42-140              35
alpha-BHC...............................................          69-125             2.0              28          49-130          37-140              36
beta-BHC................................................          75-125             2.0              38          39-130          17-147              44
delta-BHC...............................................          75-125             2.0              43          51-130          19-140              52
gamma-BHC...............................................          75-125             2.0              29          43-130          32-140              39
alpha-Chlordane.........................................          73-125            50.0              24          55-130          45-140              35
gamma-Chlordane.........................................          75-125            50.0              24          55-130          45-140              35
4,4[min]-DDD............................................          75-125            10.0              32          48-130          31-141              39
4,4[min]-DDE............................................          75-125             2.0              30          54-130          30-145              35
4,4[min]-DDT............................................          75-125            10.0              39          46-137          25-160              42
Dieldrin................................................          48-125             2.0              42          58-130          36-146              49
Endosulfan I............................................          75-125             2.0              25          57-141          45-153              28
Endosulfan II...........................................          75-125            10.0              63          22-171           D-202              53
Endosulfan sulfate......................................          70-125            10.0              32          38-132          26-144              38
Endrin..................................................           5-125            10.0              42          51-130          30-147              48
Heptachlor..............................................          75-125             2.0              28          43-130          34-140              43
Heptachlor epoxide......................................          75-125             2.0              22          57-132          37-142              26
Toxaphene...............................................          68-134            50.0              30          56-130          41-140              41
PCB-1016................................................          75-125            50.0              24          61-103          50-140              36
PCB-1221................................................          75-125            50.0              50          44-150          15-178              48
PCB-1232................................................          75-125            50.0              32          28-197          10-215              25
PCB-1242................................................          75-125            50.0              26          50-139          39-150              29
PCB-1248................................................          75-125            50.0              32          58-140          38-158              35
PCB-1254................................................          75-125            50.0              34          44-130          29-140              45
PCB-1260................................................          75-125            50.0              28          37-130           8-140              38
--------------------------------------------------------------------------------------------------------------------------------------------------------
S = Standard deviation of four recovery measurements for the DOC (section 8.2.4).
X = Average of four recovery measurements for the DOC (section 8.2.4).

[[Page 187]]

 
P = Recovery for the LCS (section 8.4.3).
Note: These criteria were developed from data in Table 5 (Reference 2). Where necessary, limits for recovery have been broadened to assure applicability
  to concentrations below those in Table 5.


                          Table 5--Precision and Recovery as Functions of Concentration
----------------------------------------------------------------------------------------------------------------
                                                                              Single analyst
                                                          Recovery, X[min]      precision,          Overall
                        Analyte                             ([micro]g/L)    sr[min] ([micro]g/ precision, S[min]
                                                                                    L)            ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Aldrin.................................................       0.81C + 0.04     0.16(X) - 0.04     0.20(X) - 0.01
alpha-BHC..............................................       0.84C + 0.03     0.13(X) + 0.04     0.23(X) - 0.00
beta-BHC...............................................       0.81C + 0.07     0.22(X) - 0.02     0.33(X) - 0.05
delta-BHC..............................................       0.81C + 0.07     0.18(X) + 0.09     0.25(X) + 0.03
gamma-BHC (Lindane)....................................       0.82C - 0.05     0.12(X) + 0.06     0.22(X) + 0.04
Chlordane..............................................       0.82C - 0.04     0.13(X) + 0.13     0.18(X) + 0.18
4,4[min]-DDD...........................................       0.84C + 0.30     0.20(X) - 0.18     0.27(X) - 0.14
4,4[min]-DDE...........................................       0.85C + 0.14     0.13(X) + 0.06     0.28(X) - 0.09
4,4[min]-DDT...........................................       0.93C - 0.13     0.17(X) + 0.39     0.31(X) - 0.21
Dieldrin...............................................       0.90C + 0.02     0.12(X) + 0.19     0.16(X) + 0.16
Endosulfan I...........................................       0.97C + 0.04     0.10(X) + 0.07     0.18(X) + 0.08
Endosulfan II..........................................       0.93C + 0.34     0.41(X) - 0.65     0.47(X) - 0.20
Endosulfan sulfate.....................................       0.89C - 0.37     0.13(X) + 0.33     0.24(X) + 0.35
Endrin.................................................       0.89C - 0.04     0.20(X) + 0.25     0.24(X) + 0.25
Heptachlor.............................................       0.69C + 0.04     0.06(X) + 0.13     0.16(X) + 0.08
Heptachlor epoxide.....................................       0.89C + 0.10     0.18(X) - 0.11     0.25(X) - 0.08
Toxaphene..............................................       0.80C + 1.74     0.09(X) + 3.20     0.20(X) + 0.22
PCB-1016...............................................       0.81C + 0.50     0.13(X) + 0.15     0.15(X) + 0.45
PCB-1221...............................................       0.96C + 0.65     0.29(X) - 0.76     0.35(X) - 0.62
PCB-1232...............................................       0.91C + 10.8     0.21(X) - 1.93     0.31(X) + 3.50
PCB-1242...............................................       0.93C + 0.70     0.11(X) + 1.40     0.21(X) + 1.52
PCB-1248...............................................       0.97C + 1.06     0.17(X) + 0.41     0.25(X) - 0.37
PCB-1254...............................................       0.76C + 2.07     0.15(X) + 1.66     0.17(X) + 3.62
PCB-1260...............................................       0.66C + 3.76     0.22(X) - 2.37     0.39(X) - 4.86
----------------------------------------------------------------------------------------------------------------
X[min] = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/
  L.


         Table 6--Distribution of Chlorinated Pesticides and PCBs Into Florisil[supreg] Column Fractions
----------------------------------------------------------------------------------------------------------------
                                                                         Percent Recovery by Fraction \1\
                             Analyte                             -----------------------------------------------
                                                                         1               2               3
----------------------------------------------------------------------------------------------------------------
Aldrin..........................................................             100
alpha-BHC.......................................................             100
beta-BHC........................................................              97
delta-BHC.......................................................              98
gamma-BHC (Lindane).............................................             100
Chlordane.......................................................             100
4,4[min]-DDD....................................................              99
4,4[min]-DDE....................................................  ..............              98
4,4[min]-DDT....................................................             100
Dieldrin........................................................               0             100
Endosulfan I....................................................              37              64
Endosulfan II...................................................               0               7              91
Endosulfan sulfate..............................................               0               0             106
Endrin..........................................................               4              96
Endrin aldehyde.................................................               0              68              26
Heptachlor......................................................             100
Heptachlor epoxide..............................................             100
Toxaphene.......................................................              96
PCB-1016........................................................              97
PCB-1221........................................................              97
PCB-1232........................................................              95               4
PCB-1242........................................................              97
PCB-1248........................................................             103
PCB-1254........................................................              90
PCB-1260........................................................  ..............  ..............
----------------------------------------------------------------------------------------------------------------
\1\ Eluant composition:
Fraction 1--6% ethyl ether in hexane.
Fraction 2--15% ethyl ether in hexane.
Fraction 3--50% ethyl ether in hexane.


[[Page 188]]


                Table 7--Suggested Calibration Groups \1\
------------------------------------------------------------------------
                                 Analyte
-------------------------------------------------------------------------
Calibration Group 1:
    Acephate
    Alachlor
    Atrazine
    beta-BHC
    Bromoxynil octanoate
    Captafol
    Diallate
    Endosulfan sulfate
    Endrin
    Isodrin
    Pendimethalin (Prowl)
    trans-Permethrin
Calibration Group 2:
    alpha-BHC
    DCPA
    4,4[min]-DDE
    4,4[min]-DDT
    Dichlone
    Ethalfluralin
    Fenarimol
    Methoxychlor
    Metribuzin
Calibration Group 3:
    gamma-BHC (Lindane)
    gamma-Chlordane
    Endrin ketone
    Heptachlor epoxide
    Isopropalin
    Nitrofen (TOK)
    PCNB
    cis-Permethrin
    Trifluralin
Callibration Group 4:
    Benfluralin
    Chlorobenzilate
    Dieldrin
    Endosulfan I
    Mirex
    Terbacil
    Terbuthylazine
    Triadimefon
 
Calibration Group 5:
    alpha-Chlordane
    Captan
    Chlorothalonil
    4,4[min]-DDD
    Norfluorazon
    Simazine
Calibration Group 6:
    Aldrin
    delta-BHC
    Bromacil
    Butachlor
    Endosulfan II
    Heptachlor
    Kepone
Calibration Group 7:
    Carbophenothion
    Chloroneb
    Chloropropylate
    DBCP
    Dicofol
    Endrin aldehyde
    Etridiazone
    Perthane
    Propachlor
    Propanil
    Propazine
------------------------------------------------------------------------
\1\ The analytes may be organized in other calibration groups, provided
  that there are no coelution problems and that all QC requirements are
  met.

                               22. Figures

[[Page 189]]

[GRAPHIC] [TIFF OMITTED] TR28AU17.010


[[Page 190]]


[GRAPHIC] [TIFF OMITTED] TR28AU17.011

                              23. Glossary

    These definitions and purposes are specific to this method but have 
been conformed to common usage to the extent possible.
    23.1 Units of weight and measure and their abbreviations.
    23.1.1 Symbols.

 [deg]C degrees Celsius
[micro]g microgram

[[Page 191]]

[micro]L microliter
< less than
<= less than or equal to
 greater than
% percent

    23.1.2 Abbreviations (in alphabetical order).

cm centimeter
g gram
hr hour
ID inside diameter
in. inch
L liter
M molar solution--one mole or gram molecular weight of solute in one 
liter of solution
mg milligram
min minute
mL milliliter
mm millimeter
N Normality--one equivalent of solute in one liter of solution
ng nanogram
psia pounds-per-square inch absolute
psig pounds-per-square inch gauge
v/v volume per unit volume
w/v weight per unit volume

    23.2 Definitions and acronyms (in alphabetical order)
    Analyte--A compound or mixture of compounds (e.g., PCBs) tested for 
by this method. The analytes are listed in Tables 1 and 2.
    Analytical batch--The set of samples analyzed on a given instrument 
during a 24-hour period that begins and ends with calibration 
verification (sections 7.8 and 13). See also ``Extraction batch.''
    Blank (method blank; laboratory blank)--An aliquot of reagent water 
that is treated exactly as a sample including exposure to all glassware, 
equipment, solvents, reagents, internal standards, and surrogates that 
are used with samples. The blank is used to determine if analytes or 
interferences are present in the laboratory environment, the reagents, 
or the apparatus.
    Calibration factor (CF)--See section 7.5.1.
    Calibration standard--A solution prepared from stock solutions and/
or a secondary standards and containing the analytes of interest, 
surrogates, and internal standards. This standard is used to model the 
response of the GC instrument against analyte concentration.
    Calibration verification--The process of confirming that the 
response of the analytical system remains within specified limits of the 
calibration.
    Calibration verification standard--The standard (section 6.8.4) used 
to verify calibration (sections 7.8 and 13.6).
    Extraction Batch--A set of up to 20 field samples (not including QC 
samples) started through the extraction process in a given 24-hour 
shift. Each extraction batch of 20 or fewer samples must be accompanied 
by a blank (section 8.5), a laboratory control sample (LCS, section 
8.4), a matrix spike and duplicate (MS/MSD; section 8.3), resulting in a 
minimum of five samples (1 field sample, 1 blank, 1 LCS, 1 MS, and 1 
MSD) and a maximum of 24 samples (20 field samples, 1 blank, 1 LCS, 1 
MS, and 1 MSD) for the batch. If greater than 20 samples are to be 
extracted in a 24-hour shift, the samples must be separated into 
extraction batches of 20 or fewer samples.
    Field Duplicates--Two samples collected at the same time and place 
under identical conditions, and treated identically throughout field and 
laboratory procedures. Results of analyses the field duplicates provide 
an estimate of the precision associated with sample collection, 
preservation, and storage, as well as with laboratory procedures.
    Field blank--An aliquot of reagent water or other reference matrix 
that is placed in a sample container in the field, and treated as a 
sample in all respects, including exposure to sampling site conditions, 
storage, preservation, and all analytical procedures. The purpose of the 
field blank is to determine if the field or sample transporting 
procedures and environments have contaminated the sample. See also 
``Blank.''
    GC--Gas chromatograph or gas chromatography.
    Gel-permeation chromatography (GPC)--A form of liquid chromatography 
in which the analytes are separated based on exclusion from the solid 
phase by size.
    Internal standard--A compound added to an extract or standard 
solution in a known amount and used as a reference for quantitation of 
the analytes of interest and surrogates. Also see Internal standard 
quantitation.
    Internal standard quantitation--A means of determining the 
concentration of an analyte of interest (Tables 1 and 2) by reference to 
a compound not expected to be found in a sample.
    IDC--Initial Demonstration of Capability (section 8.2); four 
aliquots of a reference matrix spiked with the analytes of interest and 
analyzed to establish the ability of the laboratory to generate 
acceptable precision and recovery. An IDC is performed prior to the 
first time this method is used and any time the method or 
instrumentation is modified.
    Laboratory Control Sample (LCS; laboratory fortified blank; section 
8.4)--An aliquot of reagent water spiked with known quantities of the 
analytes of interest and surrogates. The LCS is analyzed exactly like a 
sample. Its purpose is to assure that the results produced by the 
laboratory remain within the limits specified in this method for 
precision and recovery.
    Laboratory Fortified Sample Matrix--See Matrix spike.
    Laboratory reagent blank--See blank.

[[Page 192]]

    Matrix spike (MS) and matrix spike duplicate (MSD) (laboratory 
fortified sample matrix and duplicate)--Two aliquots of an environmental 
sample to which known quantities of the analytes of interest and 
surrogates are added in the laboratory. The MS/MSD are prepared and 
analyzed exactly like a field sample. Their purpose is to quantify any 
additional bias and imprecision caused by the sample matrix. The 
background concentrations of the analytes in the sample matrix must be 
determined in a separate aliquot and the measured values in the MS/MSD 
corrected for background concentrations.
    May--This action, activity, or procedural step is neither required 
nor prohibited.
    May not--This action, activity, or procedural step is prohibited.
    Method detection limit (MDL)--A detection limit determined by the 
procedure at 40 CFR part 136, appendix B. The MDLs determined by EPA are 
listed in Tables 1 and 2. As noted in section 1.6, use the MDLs in 
Tables 1 and 2 in conjunction with current MDL data from the laboratory 
actually analyzing samples to assess the sensitivity of this procedure 
relative to project objectives and regulatory requirements (where 
applicable).
    Minimum level (ML)--The term ``minimum level'' refers to either the 
sample concentration equivalent to the lowest calibration point in a 
method or a multiple of the method detection limit (MDL), whichever is 
higher. Minimum levels may be obtained in several ways: They may be 
published in a method; they may be based on the lowest acceptable 
calibration point used by a laboratory; or they may be calculated by 
multiplying the MDL in a method, or the MDL determined by a laboratory, 
by a factor of 3. For the purposes of NPDES compliance monitoring, EPA 
considers the following terms to be synonymous: ``quantitation limit,'' 
``reporting limit,'' and ``minimum level.''
    MS--Mass spectrometer or mass spectrometry.
    Must--This action, activity, or procedural step is required.
    Preparation blank--See blank.
    Reagent water--Water demonstrated to be free from the analytes of 
interest and potentially interfering substances at the MDLs for the 
analytes in this method.
    Regulatory compliance limit--A limit on the concentration or amount 
of a pollutant or contaminant specified in a nationwide standard, in a 
permit, or otherwise established by a regulatory/control authority.
    Relative standard deviation (RSD)--The standard deviation times 100 
divided by the mean. Also termed ``coefficient of variation.''
    RF--Response factor. See section 7.6.2.
    RPD--Relative percent difference.
    RSD--See relative standard deviation.
    Safety Data Sheet (SDS)--Written information on a chemical's 
toxicity, health hazards, physical properties, fire, and reactivity, 
including storage, spill, and handling precautions that meet the 
requirements of OSHA, 29 CFR 1910.1200(g) and appendix D to Sec.  
1910.1200. United Nations Globally Harmonized System of Classification 
and Labelling of Chemicals (GHS), third revised edition, United Nations, 
2009.
    Should--This action, activity, or procedural step is suggested but 
not required.
    SPE--Solid-phase extraction; a sample extraction or extract cleanup 
technique in which an analyte is selectively removed from a sample or 
extract by passage over or through a material capable of reversibly 
adsorbing the analyte.
    Stock solution--A solution containing an analyte that is prepared 
using a reference material traceable to EPA, the National Institute of 
Science and Technology (NIST), or a source that will attest to the 
purity and authenticity of the reference material.
    Surrogate--A compound unlikely to be found in a sample, which is 
spiked into the sample in a known amount before extraction, and which is 
quantified with the same procedures used to quantify other sample 
components. The purpose of the surrogate is to monitor method 
performance with each sample.

                Method 609--Nitroaromatics and Isophorone

                        1. Scope and Application

    1.1 This method covers the determination of certain nitroaromatics 
and isophorone. The following parameters may be determined by this 
method:

------------------------------------------------------------------------
                   Parameter                     STORET No.    CAS No.
------------------------------------------------------------------------
2,4-Dinitrotoluene............................        34611     121-14-2
2,6-Dinitrotoluene............................        34626     606-20-2
Isophorone....................................        34408      78-59-1
Nitrobenzene..................................        34447      98-95-3
------------------------------------------------------------------------

    1.2 This is a gas chromatographic (GC) method applicable to the 
determination of the compounds listed above in municipal and industrial 
discharges as provided under 40 CFR 136.1. When this method is used to 
analyze unfamiliar samples for any or all of the compounds above, 
compound identifications should be supported by at least one additional 
qualitative technique. This method describes analytical conditions for a 
second gas chromatographic column that can be used to confirm 
measurements made with the primary column. Method 625 provides gas 
chromatograph/mass spectrometer (GC/MS) conditions appropriate for the 
qualitative and quantitative confirmation of results for all of the 
parameters listed above, using the extract produced by this method.

[[Page 193]]

    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 The sample extraction and concentration steps in this method are 
essentially the same as in Methods 606, 608, 611, and 612. Thus, a 
single sample may be extracted to measure the parameters included in the 
scope of each of these methods. When cleanup is required, the 
concentration levels must be high enough to permit selecting aliquots, 
as necessary, to apply appropriate cleanup procedures. The analyst is 
allowed the latitude, under Section 12, to select chromatographic 
conditions appropriate for the simultaneous measurement of combinations 
of these parameters.
    1.5 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is dried and exchanged to hexane during concentration 
to a volume of 10 mL or less. Isophorone and nitrobenzene are measured 
by flame ionization detector gas chromatography (FIDGC). The 
dinitrotoluenes are measured by electron capture detector gas 
chromatography (ECDGC). \2\
    2.2 The method provides a Florisil column cleanup procedure to aid 
in the elimination of interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baseliles in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedure in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \4-6\ for 
the information of the analyst.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of

[[Page 194]]

250 mL of sample. Sample containers must be kept refrigerated at 4 
[deg]C and protected from light during compositing. If the sampler uses 
a peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Chromatographic column--100 mm long x 10 mm ID, with Teflon 
stopcock.
    5.2.4 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.5 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.6 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.7 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.8 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with gas 
chromatograph suitable for on-column injection and all required 
accessories including syringes, analytical columns, gases, detector, and 
strip-chart recorder. A data system is recommended for measuring peak 
areas.
    5.6.1 Column 1--1.2 m long x 2 or 4 mm ID glass, packed with 1.95% 
QF-1/1.5% OV-17 on Gas-Chrom Q (80/100 mesh) or equivalent. This column 
was used to develop the method performance statements given in Section 
14. Guidelines for the use of alternate column packings are provided in 
Section 12.1.
    5.6.2 Column 2--3.0 m long x 2 or 4 mm ID glass, packed with 3% OV-
101 on Gas-Chrom Q (80/100 mesh) or equivalent.
    5.6.3 Detectors--Flame ionization and electron capture detectors. 
The flame ionization detector (FID) is used when determining isophorone 
and nitrobenzene. The electron capture detector (ECD) is used when 
determining the dinitrotoluenes. Both detectors have proven effective in 
the analysis of wastewaters and were used in develop the method 
performance statements in Section 14. Guidelines for the use to 
alternate detectors are provided in Section 12.1.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.3 Sulfuric acid (1 + 1)--Slowly, add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.4 Acetone, hexane, methanol, methylene chloride--Pesticide quality 
or equivalent.
    6.5 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.6 Florisil--PR grade (60/100 mesh). Purchase activated at 1250 
[deg]F and store in dark in glass containers with ground glass stoppers 
or foil-lined screw caps. Before use, activate each batch at least 16 h 
at 200 [deg]C in a foil-covered glass container and allow to cool.
    6.7 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions can be prepared from pure standard materials or 
purchased as certified solutions.
    6.7.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in hexane and dilute to 
volume in a 10-mL volumetric flask. Larger volumes can be used at the 
convenience of the analyst. When compound purity is assayed to be 96% or 
greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.7.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.7.3 Stock standard solutions must be replaced after six months, or 
sooner if comparison with check standards indicates a problem.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatographic operating conditions equivalent to 
those given in

[[Page 195]]

Table 1. The gas chromatographic system can be calibrated using the 
external standard technique (Section 7.2) or the internal standard 
technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with hexane. One of the external standards should be at a concentration 
near, but above, the MDL (Table 1) and the other concentrations should 
correspond to the expected range of concentrations found in real samples 
or should define the working range of the detector.
    7.2.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD) linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flash. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with hexane. One of the standards should be at a 
concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.
    Equation 1.
    [GRAPHIC] [TIFF OMITTED] TC15NO91.110
    
where:

As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

    If the RF value over the working range is a constant (<10% RSD), the 
RF can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.

[[Page 196]]

    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1,5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest in acetone at a concentration of 
20 [micro]g/mL for each dinitrotoluene and 100 [micro]g/mL for 
isophorone and nitrobenzene. The QC check sample concentrate must be 
obtained from the U.S. Environmental Protection Agency, Environmental 
Monitoring and Support Laboratory in Cincinnati, Ohio, if available. If 
not available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Using a pipet, prepare QC check samples at the test 
concentrations shown in Table 2 by adding 1.00 mL of QC check sample 
concentrate to each of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter. Locate and correct the 
source of the problem and repeat the test for all parameters of interest 
beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at the test concentration in Section 8.2.2 or 1 to 5 
times higher than the background concentration determined in Section 
8.3.2, whichever concentration would be larger.
    8.3.1.3 If it is impractical to determile background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none (2) the larger of either 5 times higher than the expected 
background concentration or the test concentration in Section 8.2.2.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100 (A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than the test 
concentration in Section 8.2.2, the analyst must use either the QC 
acceptance criteria in Table 2, or optional QC acceptance criteria 
calculated for the specific spike concentration. To calculate optional 
acceptance criteria for the recovery of a parameter: (1)

[[Page 197]]

Calculate accuracy (X') using the equation in Table 3, substituting the 
spike concentration (T) for C; (2) calculate overall precision (S') 
using the equation in Table 3, substituting X' for X8; (3) calculate the 
range for recovery at the spike concentration as (100 X'/T) 2.44 (100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4. If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of QC program for the laboratory, method accuracy for 
wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \8\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel. Check the pH of the sample with wide-range pH paper 
and adjust to within the range of 5 to 9 with sodium hydroxide solution 
or sulfuric acid.
    10.2 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 
min. with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.

[[Page 198]]

    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.6 Sections 10.7 and 10.8 describe a procedure for exchanging the 
methylene chloride solvent to hexane while concentrating the extract 
volume to 1.0 mL. When it is not necessary to achieve the MDL in Table 
2, the solvent exchange may be made by the addition of 50 mL of hexane 
and concentration to 10 mL as described in Method 606, Sections 10.7 and 
10.8.
    10.7 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.8 Remove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of methylene chloride. A 
5-mL syringe is recommended for this operation. Add 1 to 2 mL of hexane 
and a clean boiling chip to the concentrator tube and attach a two-ball 
micro-Snyder column. Prewet the column by adding about 0.5 mL of hexane 
to the top. Place the micro-K-D apparatus on a hot water bath (60 to 65 
[deg]C) so that the concentrator tube is partially immersed in the hot 
water. Adjust the vertical position of the apparatus and the water 
temperature as required to complete the concentration in 5 to 10 min. At 
the proper rate of distillation the balls of the column will actively 
chatter but the chambers will not flood. When the apparent volume of 
liquid reaches 0.5 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.9 Remove the micro-Snyder column and rinse its lower joint into 
the concentrator tube with a minimum amount of hexane. Adjust the 
extract volume to 1.0 mL. Stopper the concentrator tube and store 
refrigerated if further processing will not be performed immediately. If 
the extract will be stored longer than two days, it should be 
transferred to a Teflon-sealed screw-cap vial. If the sample extract 
requires no further cleanup, proceed with gas chromatographic analysis 
(Section 12). If the sample requires further cleanup, proceed to Section 
11.
    10.10 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use the procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of Section 8.2 can be met using the method as revised 
to incorporate the cleanup procedure.
    11.2 Florisil column cleanup:
    11.2.1 Prepare a slurry of 10 g of activated Florisil in methylene 
chloride/hexane (1 + 9)(V/V) and place the Florisil into a 
chromatographic column. Tap the column to settle the Florisil and add 1 
cm of anhydrous sodium sulfate to the top. Adjust the elution rate to 
about 2 mL/min.
    11.2.2 Just prior to exposure of the sodium sulfate layer to the 
air, quantitatively transfer the sample extract onto the column using an 
additional 2 mL of hexane to complete the transfer. Just prior to 
exposure of the sodium sulfate layer to the air, add 30 mL of methylene 
chloride/hexane (1 + 9)(V/V) and continue the elution of the column. 
Discard the eluate.
    11.2.3 Next, elute the column with 30 mL of acetone/methylene 
chloride (1 + 9)(V/V) into a 500-mL K-D flask equipped with a 10-mL 
concentrator tube. Concentrate the collected fraction as in Sections 
10.6, 10.7, 10.8, and 10.9 including the solvent exchange to 1 mL of 
hexane. This fraction should contain the nitroaromatics and isophorone. 
Analyze by gas chromatography (Section 12).

                         12. Gas Chromatography

    12.1 Isophorone and nitrobenzene are analyzed by injection of a 
portion of the extract into an FIDGC. The dinitrotoluenes are analyzed 
by a separate injection into an ECDGC. Table 1 summarizes the 
recommended operating conditions for the gas chromatograph. Included in 
this table are retention times and MDL that can be achieved under these 
conditions. Examples of the separations achieved by Column 1 are shown 
in Figures 1 and 2. Other packed or capillary (open-tubular) columns, 
chromatographic conditions, or detectors may be used if the requirements 
of Section 8.2 are met.
    12.2 Calibrate the system daily as described in Section 7.

[[Page 199]]

    12.3 If the internal standard calibration procedure is being used, 
the internal standard must be added to the same extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    12.4 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush technique. \9\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, the 
total extract volume, and the resulting peak size in area or peak height 
units.
    12.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    12.6 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    12.7 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.111

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.112

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \10\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 7 x MDL to 1000 x MDL. \10\
    14.3 This method was tested by 18 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 1.0 to 515 [micro]g/L. \11\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Nitroaromatic Compounds and Isophorone in 
Industrial and Municipal Wastewaters,'' EPA 600/ 4-82-024, National 
Technical Information Service, PB82-208398, Springfield, Virginia 22161, 
May 1982.
    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).

[[Page 200]]

    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    8. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    9. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    10. ``Determination of Method Detection Limit and Analytical Curve 
for EPA Method 609--Nitroaromatics and Isophorone,'' Special letter 
report for EPA Contract 68-03-2624, U.S. Environmental Protection 
Agency, Environmental Monitoring and Support Laboratory, Cincinnati, 
Ohio 45268, June 1980.
    11. ``EPA Method Study 19, Method 609 (Nitroaromatics and 
Isophorone),'' EPA 600/4-84-018, National Technical Information Service, 
PB84-176908, Springfield, Virginia 22161, March 1984.

                         Table 1--Chromatographic Conditions and Method Detection Limits
----------------------------------------------------------------------------------------------------------------
                                                             Retention time (min)       Method detection limit
                                                         ----------------------------        ([micro]g/L)
                        Parameter                                                    ---------------------------
                                                             Col. 1        Col. 2         ECDGC         FIDGC
----------------------------------------------------------------------------------------------------------------
Nitrobenzene............................................        3.31          4.31         13.7           3.6
2,6-Dinitrotoluene......................................        3.52          4.75          0.01          -
Isophorone..............................................        4.49          5.72         15.7           5.7
2,4-Dinitrotoluene......................................        5.35          6.54          0.02          -
----------------------------------------------------------------------------------------------------------------
Column 1 conditions: Gas-Chrom Q (80/100 mesh) coated with 1.95% QF-1/1.5% OV-17 packed in a 1.2 m long x 2 mm
  or 4 mm ID glass column. A 2 mm ID column and nitrogen carrier gas at 44 mL/min flow rate were used when
  determining isophorone and nitrobenzene by FIDGC. The column temperature was held isothermal at 85 [deg]C. A 4
  mm ID column and 10% methane/90% argon carrier gas at 44 mL/min flow rate were used when determining the
  dinitrotoluenes by ECDGC. The column temperature was held isothermal at 145 [deg]C.
Column 2 conditions: Gas-Chrom Q (80/100 mesh) coated with 3% OV-101 packed in a 3.0 m long x 2 mm or 4 mm ID
  glass column. A 2 mm ID column and nitrogen carrier gas at 44 mL/min flow rate were used when determining
  isophorone and nitrobenzene by FIDGC. The column temperature was held isothermal at 100 [deg]C. A 4 mm ID
  column and 10% methane/90% argon carrier gas at 44 mL/min flow rate were used when determining the
  dinitrotoluenes by ECDGC. The column temperature was held isothermal at 150 [deg]C.


                                   Table 2--QC Acceptance Criteria--Method 609
----------------------------------------------------------------------------------------------------------------
                                                             Test Conc.
                         Parameter                           ([micro]g/   Limit for s   Range for X   Range for
                                                                 L)      ([micro]g/L)  ([micro]g/L)   P, Ps (%)
----------------------------------------------------------------------------------------------------------------
2,4-Dinitrotoluene........................................           20           5.1  3.6-22.8            6-125
2,6-Dinitrotoluene........................................           20           4.8  3.8-23.0            8-126
Isophorone................................................          100          32.3  8.0-100.0           D-117
Nitrobenzene..............................................          100          33.3  25.7-100.0          6-118
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 609
----------------------------------------------------------------------------------------------------------------
                                                            Accuracy, as      Single analyst        Overall
                       Parameter                            recovery, X'      precision, sr'     precision, S'
                                                            ([micro]g/L)       ([micro]g/L)       ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
2,4-Dinitro-
 toluene...............................................       0.65C + 0.22       0.20X + 0.08         0.37X-0.07
2,6-Dinitro-
 toluene...............................................       0.66C + 0.20       0.19X + 0.06         0.36X-0.00
Isophorone.............................................       0.49C + 2.93       0.28X + 2.77       0.46X + 0.31
Nitrobenzene...........................................       0.60C + 2.00       0.25X + 2.53         0.37X-0.78
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


[[Page 201]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.029


[[Page 202]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.030


[[Page 203]]

              Method 610--Polynuclear Aromatic Hydrocarbons

                        1. Scope and Application

    1.1 This method covers the determination of certain polynuclear 
aromatic hydrocarbons (PAH). The following parameters can be determined 
by this method:

------------------------------------------------------------------------
                  Parameter                    STORET No.      CAS No.
------------------------------------------------------------------------
Acenaphthene................................         34205       83-32-9
Acenaphthylene..............................         34200      208-96-8
Anthracene..................................         34220      120-12-7
Benzo(a)anthracene..........................         34526       56-55-3
Benzo(a)pyrene..............................         34247       50-32-8
Benzo(b)fluoranthene........................         34230      205-99-2
Benzo(ghi)perylene..........................         34521      191-24-2
Benzo(k)fluoranthene........................         34242      207-08-9
Chrysene....................................         34320      218-01-9
Dibenzo(a,h)anthracene......................         34556       53-70-3
Fluoranthene................................         34376      206-44-0
Fluorene....................................         34381       86-73-7
Indeno(1,2,3-cd)pyrene......................         34403      193-39-5
Naphthalene.................................         34696       91-20-3
Phenanthrene................................         34461       85-01-8
Pyrene......................................         34469      129-00-0
------------------------------------------------------------------------

    1.2 This is a chromatographic method applicable to the determination 
of the compounds listed above in municipal and industrial discharges as 
provided under 40 CFR 136.1. When this method is used to analyze 
unfamiliar samples for any or all of the compounds above, compound 
identifications should be supported by at least one additional 
qualitative technique. Method 625 provides gas chromatograph/mass 
spectrometer (GC/MS) conditions appropriate for the qualitative and 
quantitative confirmation of results for many of the parameters listed 
above, using the extract produced by this method.
    1.3 This method provides for both high performance liquid 
chromatographic (HPLC) and gas chromatographic (GC) approaches for the 
determination of PAHs. The gas chromatographic procedure does not 
adequately resolve the following four pairs of compounds: Anthracene and 
phenanthrene; chrysene and benzo(a)anthracene; benzo(b)fluoranthene and 
benzo(k)fluoranthene; and dibenzo(a,h) anthracene and indeno (1,2,3-
cd)pyrene. Unless the purpose for the analysis can be served by 
reporting the sum of an unresolved pair, the liquid chromatographic 
approach must be used for these compounds. The liquid chromatographic 
method does resolve all 16 of the PAHs listed.
    1.4 The method detection limit (MDL, defined in Section 15.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.5 The sample extraction and concentration steps in this method are 
essentially the same as in Methods 606, 608, 609, 611, and 612. Thus, a 
single sample may be extracted to measure the parameters included in the 
scope of each of these methods. When cleanup is required, the 
concentration levels must be high enough to permit selecting aliquots, 
as necessary, to apply appropriate cleanup procedures. Selection of the 
aliquots must be made prior to the solvent exchange steps of this 
method. The analyst is allowed the latitude, under Sections 12 and 13, 
to select chromatographic conditions appropriate for the simultaneous 
measurement of combinations of these parameters.
    1.6 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.7 This method is restricted to use by or under the supervision of 
analysts experienced in the use of HPLC and GC systems and in the 
interpretation of liquid and gas chromatograms. Each analyst must 
demonstrate the ability to generate acceptable results with this method 
using the procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is dried and concentrated to a volume of 10 mL or less. 
The extract is then separated by HPLC or GC. Ultraviolet (UV) and 
fluorescence detectors are used with HPLC to identify and measure the 
PAHs. A flame ionization detector is used with GC. \2\
    2.2 The method provides a silica gel column cleanup procedure to aid 
in the elimination of interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardward that lead to 
discrete artifacts and/or elevated baselines in the chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be

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substituted for the muffle furnace heating. Thorough rinsing with such 
solvents usually eliminates PCB interference. Volumetric ware should not 
be heated in a muffle furnace. After drying and cooling, glassware 
should be sealed and stored in a clean environment to prevent any 
accumulation of dust or other contaminants. Store inverted or capped 
with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedure in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.
    3.3 The extent of interferences that may be encountered using liquid 
chromatographic techniques has not been fully assessed. Although the 
HPLC conditions described allow for a unique resolution of the specific 
PAH compounds covered by this method, other PAH compounds may interfere.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method have not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \4-6\ for 
the information of the analyst.
    4.2 The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: benzo(a)anthracene, benzo(a)pyrene, and dibenzo(a,h)-
anthracene. Primary standards of these toxic compounds should be 
prepared in a hood. A NIOSH/MESA approved toxic gas respirator should be 
worn when the analyst handles high concentrations of these toxic 
compounds.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.4 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.5 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.6 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.7 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.8 Chromatographic column--250 mm long x 10 mm ID, with coarse 
frit filter disc at bottom and Teflon stopcock.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 High performance liquid chromatograph (HPLC)--An analytical 
system complete with column supplies, high pressure syringes, detectors, 
and compatible strip-chart recorder. A data system is recommended for 
measuring peak areas and retention times.
    5.6.1 Gradient pumping system--Constant flow.

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    5.6.2 Reverse phase column--HC-ODS Sil-X, 5 micron particle 
diameter, in a 25 cm x 2.6 mm ID stainless steel column (Perkin Elmer 
No. 089-0716 or equivalent). This column was used to develop the method 
performance statements in Section 15. Guidelines for the use of 
alternate column packings are provided in Section 12.2.
    5.6.3 Detectors--Fluorescence and/or UV detectors. The fluorescence 
detector is used for excitation at 280 nm and emission greater than 389 
nm cutoff (Corning 3-75 or equivalent). Fluorometers should have 
dispersive optics for excitation and can utilize either filter or 
dispersive optics at the emission detector. The UV detector is used at 
254 nm and should be coupled to the fluorescence detector. These 
detectors were used to develop the method performance statements in 
Section 15. Guidelines for the use of alternate detectors are provided 
in Section 12.2.
    5.7 Gas chromatograph--An analytical system complete with 
temperature programmable gas chromatograph suitable for on-column or 
splitless injection and all required accessories including syringes, 
analytical columns, gases, detector, and strip-chart recorder. A data 
system is recommended for measuring peak areas.
    5.7.1 Column--1.8 m long x 2 mm ID glass, packed with 3% OV-17 on 
Chromosorb W-AW-DCMS (100/120 mesh) or equivalent. This column was used 
to develop the retention time data in Table 2. Guidelines for the use of 
alternate column packings are provided in Section 13.3.
    5.7.2 Detector--Flame ionization detector. This detector has proven 
effective in the analysis of wastewaters for the parameters listed in 
the scope (Section 1.1), excluding the four pairs of unresolved 
compounds listed in Section 1.3. Guidelines for the use of alternate 
detectors are provided in Section 13.3.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Cyclohexane, methanol, acetone, methylene chloride, pentane--
Pesticide quality or equivalent.
    6.4 Acetonitrile--HPLC quality, distilled in glass.
    6.5 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.6 Silica gel--100/200 mesh, desiccant, Davison, grade-923 or 
equivalent. Before use, activate for at least 16 h at 130 [deg]C in a 
shallow glass tray, loosely covered with foil.
    6.7 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions can be prepared from pure standard materials or 
purchased as certified solutions.
    6.7.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in acetonitrile and 
dilute to volume in a 10-mL volumetric flask. Larger volumes can be used 
at the convenience of the analyst. When compound purity is assayed to be 
96% or greater, the weight can be used without correction to calculate 
the concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.7.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.7.3 Stock standard solutions must be replaced after six months, or 
sooner if comparison with check standards indicates a problem.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish liquid or gas chromatographic operating conditions 
equivalent to those given in Table 1 or 2. The chromatographic system 
can be calibrated using the external standard technique (Section 7.2) or 
the internal standard technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with acetonitrile. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using injections of 5 to 25 [micro]L for HPLC and 2 to 5 
[micro]L for GC, analyze each calibration standard according to Section 
12 or 13, as appropriate. Tabulate peak height or area responses against 
the mass injected. The results can be used to prepare a calibration 
curve for each compound. Alternatively, if the ratio of response to 
amount injected (calibration factor) is a constant over the working 
range (<10% relative standard deviation, RSD), linearity through the 
origin can be assumed and the average ratio or calibration factor can be 
used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the

[[Page 206]]

compounds of interest. The analyst must further demonstrate that the 
measurement of the internal standard is not affected by method or matrix 
interferences. Because of these limitations, no internal standard can be 
suggested that is applicable to all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with acetonitrile. One of the standards should be 
at a concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using injections of 5 to 25 [micro]L for HPLC and 2 to 5 
[micro]L for GC, analyze each calibration standard according to Section 
12 or 13, as appropriate. Tabulate peak height or area responses against 
concentration for each compound and internal standard. Calculate 
response factors (RF) for each compound using Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.113

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.

    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, the test must 
be repeated using a fresh calibration standard. Alternatively, a new 
calibration curve must be prepared for that compound.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, 12.2, and 13.3) to improve the separations or lower 
the cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at the following concentrations in 
acetonitrile: 100 [micro]g/mL of any

[[Page 207]]

of the six early-eluting PAHs (naphthalene, acenaphthylene, 
acenaphthene, fluorene, phenanthrene, and anthracene); 5 [micro]g/mL of 
benzo(k)fluoranthene; and 10 [micro]g/mL of any of the other PAHs. The 
QC check sample concentrate must be obtained from the U.S. Environmental 
Protection Agency, Environmental Monitoring and Support Laboratory in 
Cincinnati, Ohio, if available. If not available from that source, the 
QC check sample concentrate must be obtained from another external 
source. If not available from either source above, the QC check sample 
concentrate must be prepared by the laboratory using stock standards 
prepared independently from those used for calibration.
    8.2.2 Using a pipet, prepare QC check samples at the test 
concentrations shown in Table 3 by adding 1.00 mL of QC check sample 
concentrate to each of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 3. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter.
    Note: The large number of parameters in Table 3 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when all parameters are analyzed.
    8.2.6 When one or more of the parameters tested fail at least one of 
the acceptance criteria, the analyst must proceed according to Section 
8.2.6.1 or 8.2.6.2.
    8.2.6.1 Locate and correct the source of the problem and repeat the 
test for all parameters of interest beginning with Section 8.2.2.
    8.2.6.2 Beginning with Section 8.2.2, repeat the test only for those 
parameters that failed to meet criteria. Repeated failure, however, will 
confirm a general problem with the measurement system. If this occurs, 
locate and correct the source of the problem and repeat the test for all 
compounds of interest beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at the test concentration in Section 8.2.2 or 1 to 5 
times higher than the background concentration determined in Section 
8.3.2, whichever concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none, (2) the larger of either 5 times higher than the expected 
background concentration or the test concentration in Section 8.2.2.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100 (A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 3. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than the test 
concentration in Section 8.2.2, the analyst must use either the QC 
acceptance criteria in Table 3, or optional QC acceptance criteria 
calculated for the specific spike concentration. To calculate optional 
acceptance criteria for the recovery of a parameter: (1) Calculate 
accuracy (X') using the equation in Table 4, substituting the spike 
concentration (T) for C; (2) calculate overall precision (S') using the 
equation in Table 4, substituting X' for X; (3) calculate the range for 
recovery at the spike concentration as (100 X'/T)2.44(100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter

[[Page 208]]

that failed the critiera must be analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory. If the entire list of parameters in Table 3 must be measured 
in the sample in Section 8.3, the probability that the analysis of a QC 
check standard will be required is high. In this case the QC check 
standard should be routinely analyzed with the spike sample.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
3. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P092sp to P + 
2sp. If P = 90% and sp = 10%, for example, the 
accuracy interval is expressed as 70-110%. Update the accuracy 
assessment for each parameter on a regular basis (e.g. after each five 
to ten new accuracy measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \8\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction. PAHs are known to be light 
sensitive; therefore, samples, extracts, and standards should be stored 
in amber or foil-wrapped bottles in order to minimize photolytic 
decomposition. Fill the sample bottles and, if residual chlorine is 
present, add 80 mg of sodium thiosulfate per liter of sample and mix 
well. EPA Methods 330.4 and 330.5 may be used for measurement of 
residual chlorine. \9\ Field test kits are available for this purpose.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.
    10.2 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 
min. with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.

[[Page 209]]

    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.6 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.7 Remove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of methylene chloride. A 
5-mL syringe is recommended for this operation. Stopper the concentrator 
tube and store refrigerated if further processing will not be performed 
immediately. If the extract will be stored longer than two days, it 
should be transferred to a Teflon-sealed screw-cap vial and protected 
from light. If the sample extract requires no further cleanup, proceed 
with gas or liquid chromatographic analysis (Section 12 or 13). If the 
sample requires further cleanup, proceed to Section 11.
    10.8 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use the procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of Section 8.2 can be met using the methods as revised 
to incorporate the cleanup procedure.
    11.2 Before the silica gel cleanup technique can be utilized, the 
extract solvent must be exchanged to cyclohexane. Add 1 to 10 mL of the 
sample extract (in methylene chloride) and a boiling chip to a clean K-D 
concentrator tube. Add 4 mL of cyclohexane and attach a two-ball micro-
Snyder column. Prewet the column by adding 0.5 mL of methylene chloride 
to the top. Place the micro-K-D apparatus on a boiling (100 [deg]C) 
water bath so that the concentrator tube is partially immersed in the 
hot water. Adjust the vertical position of the apparatus and the water 
temperature as required to complete concentration in 5 to 10 min. At the 
proper rate of distillation the balls of the column will actively 
chatter but the chambers will not flood. When the apparent volume of the 
liquid reaches 0.5 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min. Remove the micro-Snyder column and rinse 
its lower joint into the concentrator tube with a minimum amount of 
cyclohexane. Adjust the extract volume to about 2 mL.
    11.3 Silica gel column cleanup for PAHs:
    11.3.1 Prepare a slurry of 10 g of activiated silica gel in 
methylene chloride and place this into a 10-mm ID chromatographic 
column. Tap the column to settle the silica gel and elute the methylene 
chloride. Add 1 to 2 cm of anhydrous sodium sulfate to the top of the 
silica gel.
    11.3.2 Preelute the column with 40 mL of pentane. The rate for all 
elutions should be about 2 mL/min. Discard the eluate and just prior to 
exposure of the sodium sulfate layer to the air, transfer the 2-mL 
cyclohexane sample extract onto the column using an additional 2 mL 
cyclohexane to complete the transfer. Just prior to exposure of the 
sodium sulfate layer to the air, add 25 mL of pentane and continue the 
elution of the column. Discard this pentane eluate.
    11.3.3 Next, elute the column with 25 mL of methylene chloride/
pentane (4 + 6)(V/V) into a 500-mL K-D flask equipped with a 10-mL 
concentrator tube. Concentrate the collected fraction to less than 10 mL 
as in Section 10.6. When the apparatus is cool, remove the Snyder column 
and rinse the flask and its lower joint with pentane. Proceed with HPLC 
or GC analysis.

               12. High Performance Liquid Chromatography

    12.1 To the extract in the concentrator tube, add 4 mL of 
acetonitrile and a new boiling chip, then attach a two-ball micro-Snyder 
column. Concentrate the solvent as in Section 10.6, except set the water 
bath at 95 to 100 [deg]C. When the apparatus is cool, remove the micro-
Snyder column and rinse its lower joint into the concentrator tube with 
about 0.2 mL of acetonitrile. Adjust the extract volume to 1.0 mL.
    12.2 Table 1 summarizes the recommended operating conditions for the 
HPLC. Included in this table are retention times, capacity factors, and 
MDL that can be achieved under these conditions. The UV detector is 
recommended for the determination of naphthalene, acenaphthylene, 
acenapthene, and

[[Page 210]]

fluorene and the fluorescence detector is recommended for the remaining 
PAHs. Examples of the separations achieved by this HPLC column are shown 
in Figures 1 and 2. Other HPLC columns, chromatographic conditions, or 
detectors may be used if the requirements of Section 8.2 are met.
    12.3 Calibrate the system daily as described in Section 7.
    12.4 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the instrument.
    12.5 Inject 5 to 25 [micro]L of the sample extract or standard into 
the HPLC using a high pressure syringe or a constant volume sample 
injection loop. Record the volume injected to the nearest 0.1 [micro]L, 
and the resulting peak size in area or peak height units. Re-equilibrate 
the HPLC column at the initial gradient conditions for at least 10 min 
between injections.
    12.6 Identify the parameters in the sample by comparing the 
retention time of the peaks in the sample chromatogram with those of the 
peaks in standard chromatograms. The width of the retention time window 
used to make identifications should be based upon measurements of actual 
retention time variations of standards over the course of a day. Three 
times the standard deviation of a retention time for a compound can be 
used to calculate a suggested window size; however, the experience of 
the analyst should weigh heavily in the interpretation of chromatograms.
    12.7 If the response for a peak exceeds the working range of the 
system, dilute the extract with acetonitrile and reanalyze.
    12.8 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                         13. Gas Chromatography

    13.1 The packed column GC procedure will not resolve certain 
isomeric pairs as indicated in Section 1.3 and Table 2. The liquid 
chromatographic procedure (Section 12) must be used for these 
parameters.
    13.2 To achieve maximum sensitivity with this method, the extract 
must be concentrated to 1.0 mL. Add a clean boiling chip to the 
methylene chloride extract in the concentrator tube. Attach a two-ball 
micro-Snyder column. Prewet the micro-Snyder column by adding about 0.5 
mL of methylene chloride to the top. Place the micro-K-D apparatus on a 
hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water. Adjust the vertical position of the 
apparatus and the water temperature as required to complete the 
concentration in 5 to 10 min. At the proper rate of distillation the 
balls will actively chatter but the chambers will not flood. When the 
apparent volume of liquid reaches 0.5 mL, remove the K-D apparatus and 
allow it to drain and cool for at least 10 min. Remove the micro-Snyder 
column and rinse its lower joint into the concentrator tube with a 
minimum amount of methylene chloride. Adjust the final volume to 1.0 mL 
and stopper the concentrator tube.
    13.3 Table 2 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times that were 
obtained under these conditions. An example of the separations achieved 
by this column is shown in Figure 3. Other packed or capillary (open-
tubular) columns, chromatographic conditions, or detectors may be used 
if the requirements of Section 8.2 are met.
    13.4 Calibrate the gas chromatographic system daily as described in 
Section 7.
    13.5 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    13.6 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush technique. \10\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, and 
the resulting peak size in area or peak height units.
    13.7 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    13.8 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    13.9 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            14. Calculations

    14.1 Determine the concentration of individual compounds in the 
sample.
    14.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.

[[Page 211]]

[GRAPHIC] [TIFF OMITTED] TC15NO91.114

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.115

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    14.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         15. Method Performance

    15.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \11\ Similar 
results were achieved using representative wastewaters. MDL for the GC 
approach were not determined. The MDL actually achieved in a given 
analysis will vary depending on instrument sensitivity and matrix 
effects.
    15.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 8 x MDL to 800 x MDL \11\ with the following 
exception: benzo(ghi)perylene recovery at 80 x and 800 x MDL were low 
(35% and 45%, respectively).
    15.3 This method was tested by 16 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 0.1 to 425 [micro]g/L. \12\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 4.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Polynuclear Aromatic Hydrocarbons in 
Industrial and Municipal Wastewaters,'' EPA 600/4-82-025, National 
Technical Information Service, PB82-258799, Springfield, Virginia 22161, 
June 1982.
    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    8. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    9. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    10. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    11. Cole, T., Riggin, R., and Glaser, J. ``Evaluation of Method 
Detection Limits and Analytical Curve for EPA Method 610--PNAs,'' 
International Symposium on Polynuclear Aromatic Hydrocarbons, 5th, 
Battelle's Columbus Laboratories, Columbus, Ohio (1980).
    12. ``EPA Method Study 20, Method 610 (PNA's),'' EPA 600/4-84-063, 
National Technical Information Service, PB84-211614, Springfield, 
Virginia 22161, June 1984.

[[Page 212]]



  Table 1--High Performance Liquid Chromatography Conditions and Method
                            Detection Limits
------------------------------------------------------------------------
                                                                Method
                                        Retention    Column    detection
               Parameter                   time     capacity     limit
                                          (min)      factor   ([micro]g/
                                                      (k')      L) \a\
------------------------------------------------------------------------
Naphthalene...........................       16.6       12.2       1.8
Acenaphthylene........................       18.5       13.7       2.3
Acenaphthene..........................       20.5       15.2       1.8
Fluorene..............................       21.2       15.8       0.21
Phenanthrene..........................       22.1       16.6       0.64
Anthracene............................       23.4       17.6       0.66
Fluoranthene..........................       24.5       18.5       0.21
Pyrene................................       25.4       19.1       0.27
Benzo(a)anthracene....................       28.5       21.6       0.013
Chrysene..............................       29.3       22.2       0.15
Benzo(b)fluoranthene..................       31.6       24.0       0.018
Benzo(k)fluoranthene..................       32.9       25.1       0.017
Benzo(a)pyrene........................       33.9       25.9       0.023
Dibenzo(a,h)anthracene................       35.7       27.4       0.030
Benzo(ghi)perylene....................       36.3       27.8       0.076
Indeno(1,2,3-cd)pyrene................       37.4       28.7       0.043
------------------------------------------------------------------------
HPLC column conditions: Reverse phase HC-ODS Sil-X, 5 micron particle
  size, in a 25 cm x 2.6 mm ID stainless steel column. Isocratic elution
  for 5 min. using acetonitrile/water (4 + 6), then linear gradient
  elution to 100% acetonitrile over 25 min. at 0.5 mL/min flow rate. If
  columns having other internal diameters are used, the flow rate should
  be adjusted to maintain a linear velocity of 2 mm/sec.
\a\ The MDL for naphthalene, acenaphthylene, acenaphthene, and fluorene
  were determined using a UV detector. All others were determined using
  a fluorescence detector.


       Table 2--Gas Chromatographic Conditions and Retention Times
------------------------------------------------------------------------
                                                               Retention
                          Parameter                           time (min)
------------------------------------------------------------------------
Naphthalene.................................................         4.5
Acenaphthylene..............................................        10.4
Acenaphthene................................................        10.8
Fluorene....................................................        12.6
Phenanthrene................................................        15.9
Anthracene..................................................        15.9
Fluoranthene................................................        19.8
Pyrene......................................................        20.6
Benzo(a)anthracene..........................................        24.7
Chrysene....................................................        24.7
Benzo(b)fluoranthene........................................        28.0
Benzo(k)fluoranthene........................................        28.0
Benzo(a)pyrene..............................................        29.4
Dibenzo(a,h)anthracene......................................        36.2
Indeno(1,2,3-cd)pyrene......................................        36.2
Benzo(ghi)perylene..........................................        38.6
------------------------------------------------------------------------
GC Column conditions: Chromosorb W-AW-DCMS (100/120 mesh) coated with 3%
  OV-17 packed in a 1.8 x 2 mm ID glass column with nitrogen carrier gas
  at 40 mL/min. flow rate. Column temperature was held at 100 [deg]C for
  4 min., then programmed at 8 [deg]C/min. to a final hold at 280
  [deg]C.


                                   Table 3--QC Acceptance Criteria--Method 610
----------------------------------------------------------------------------------------------------------------
                                                               Test conc.  Limit for s  Range for X
                          Parameter                            ([micro]g/   ([micro]g/   ([micro]g/   Range for
                                                                   L)           L)           L)       P, Ps (%)
----------------------------------------------------------------------------------------------------------------
Acenaphthene................................................          100         40.3      D-105.7        D-124
Acenaphthylene..............................................          100         45.1   22.1-112.1        D-139
Anthracene..................................................          100         28.7   11.2-112.3        D-126
Benzo(a)anthracene..........................................           10          4.0     3.1-11.6       12-135
Benzo(a)pyrene..............................................           10          4.0     0.2-11.0        D-128
Benzo(b)fluor-anthene.......................................           10          3.1     1.8-13.8        6-150
Benzo(ghi)perylene..........................................           10          2.3       D-10.7        D-116
Benzo(k)fluo-ranthene.......................................            5          2.5        D-7.0        D-159
Chrysene....................................................           10          4.2       D-17.5        D-199
Dibenzo(a,h)an-thracene.....................................           10          2.0     0.3-10.0        D-110
Fluoranthene................................................           10          3.0     2.7-11.1       14-123
Fluorene....................................................          100         43.0        D-119        D-142
Indeno(1,2,3-cd)pyrene......................................           10          3.0     1.2-10.0        D-116
Naphthalene.................................................          100         40.7   21.5-100.0        D-122
Phenanthrene................................................          100         37.7    8.4-133.7        D-155
Pyrene......................................................           10          3.4     1.4-12.1        D-140
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 4. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 4.


[[Page 213]]


                Table 4--Method Accuracy and Precision as Functions of Concentration--Method 610
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                              recovery, X'   precision, sr'   precision, S'
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Acenaphthene....................................................    0.52C + 0.54    0.39X + 0.76    0.53X + 1.32
Acenaphthylene..................................................    0.69C - 1.89    0.36X + 0.29    0.42X + 0.52
Anthracene......................................................    0.63C - 1.26    0.23X + 1.16    0.41X + 0.45
Benzo(a)anthracene..............................................    0.73C + 0.05    0.28X + 0.04    0.34X + 0.02
Benzo(a)pyrene..................................................    0.56C + 0.01    0.38X - 0.01    0.53X - 0.01
Benzo(b)fluoranthene............................................    0.78C + 0.01    0.21X + 0.01    0.38X - 0.00
Benzo(ghi)perylene..............................................    0.44C + 0.30    0.25X + 0.04    0.58X + 0.10
Benzo(k)fluoranthene............................................    0.59C + 0.00    0.44X - 0.00    0.69X + 0.01
Chrysene........................................................    0.77C - 0.18    0.32X - 0.18    0.66X - 0.22
Dibenzo(a,h)anthracene..........................................    0.41C + 0.11    0.24X + 0.02    0.45X + 0.03
Fluoranthene....................................................    0.68C + 0.07    0.22X + 0.06    0.32X + 0.03
Fluorene........................................................    0.56C - 0.52    0.44X - 1.12    0.63X - 0.65
Indeno(1,2,3-cd)pyrene..........................................    0.54C + 0.06    0.29X + 0.02    0.42X + 0.01
Naphthalene.....................................................    0.57C - 0.70    0.39X - 0.18    0.41X + 0.74
Phenanthrene....................................................    0.72C - 0.95    0.29X + 0.05    0.47X - 0.25
Pyrene..........................................................    0.69C - 0.12    0.25X + 0.14   0.42X - 0.00
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.

[GRAPHIC] [TIFF OMITTED] TC02JY92.031


[[Page 214]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.032


[[Page 215]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.033

                         Method 611--Haloethers

                        1. Scope and Application

    1.1 This method covers the determination of certain haloethers. The 
following parameters can be determined by this method:

------------------------------------------------------------------------
                Parameter                   STORET No.        CAS No.
------------------------------------------------------------------------
Bis(2-chloroethyl) ether................           34273        111-44-4
Bis(2-chloroethoxy) methane.............           34278        111-91-1
2, 2[min]-oxybis (1-chloropropane)......           34283        108-60-1
4-Bromophenyl phenyl ether..............           34636        101-55-3
4-Chlorophenyl phenyl ether.............           34641       7005-72-3
------------------------------------------------------------------------

    1.2 This is a gas chromatographic (GC) method applicable to the 
determination of the compounds listed above in municipal and industrial 
discharges as provided under 40 CFR 136.1. When this method is used to 
analyze unfamiliar samples for any or all of the compounds above, 
compound identifications should be supported by at least one additional 
qualitative technique. This method describes analytical conditions for a 
second gas chromatographic column that can be used to confirm 
measurements made with the primary column. Method 625 provides gas 
chromatograph/mass spectrometer (GC/MS) conditions appropriate for the 
qualitative and quantitative confirmation of results for all of the 
parameters listed above, using the extract produced by this method.

[[Page 216]]

    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 The sample extraction and concentration steps in this method are 
essentially the same as in Methods 606, 608, 609, and 612. Thus, a 
single sample may be extracted to measure the parameters included in the 
scope of each of these methods. When cleanup is required, the 
concentration levels must be high enough to permit selecting aliquots, 
as necessary, to apply appropriate cleanup procedures. The analyst is 
allowed the latitude, under Section 12, to select chromatographic 
conditions appropriate for the simultaneous measurement of combinations 
of these parameters.
    1.5 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is dried and exchanged to hexane during concentration 
to a volume of 10 mL or less. The extract is separated by gas 
chromatography and the parameters are then measured with a halide 
specific detector. \2\
    2.2 The method provides a Florisil column cleanup procedure to aid 
in the elimination of interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed be detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such a PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedure in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.
    3.3 Dichlorobenzenes are known to coelute with haloethers under some 
gas chromatographic conditions. If these materials are present together 
in a sample, it may be necessary to analyze the extract with two 
different column packings to completely resolve all of the compounds.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all personnel involved in the chemical analysis. Additional references 
to laboratory safety are available and have been identified \4-6\ for 
the information of the analyst.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene

[[Page 217]]

chloride, and dried before use to minimize contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Chromatographic column--400 mm long x 19 mm ID, with Teflon 
stopcock and coarse frit filter disc at bottom (Kontes K-420540-0224 or 
equivalent).
    5.2.4 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.5 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.6 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.7 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with 
temperature programmable gas chromatograph suitable for on-column 
injection and all required accessories including syringes, analytical 
columns, gases, detector, and strip-chart recorder. A data system is 
recommended for measuring peak areas.
    5.6.1 Column 1--1.8 m long x 2 mm ID glass, packed with 3% SP-1000 
on Supelcoport (100/120 mesh) or equivalent. This column was used to 
develop the method performance statements in Section 14. Guidelines for 
the use of alternate column packings are provided in Section 12.1.
    5.6.2 Column 2--1.8 m long x 2 mm ID glass, packed with 2,6-
diphenylene oxide polymer (60/80 mesh), Tenax, or equivalent.
    5.6.3 Detector--Halide specific detector: electrolytic conductivity 
or microcoulometric. These detectors have proven effective in the 
analysis of wastewaters for the parameters listed in the scope (Section 
1.1). The Hall conductivity detector was used to develop the method 
performance statements in Section 14. Guidelines for the use of 
alternate detectors are provided in Section 12.1. Although less 
selective, an electron capture detector is an acceptable alternative.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Acetone, hexane, methanol, methylene chloride, petroleum ether 
(boiling range 30-60 [deg]C)--Pesticide quality or equivalent.
    6.4 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.5 Florisil--PR Grade (60/100 mesh). Purchase activated at 1250 
[deg]F and store in the dark in glass containers with ground glass 
stoppers or foil-lined screw caps. Before use, activate each batch at 
least 16 h at 130 [deg]C in a foil-covered glass container and allow to 
cool.
    6.6 Ethyl ether--Nanograde, redistilled in glass if necessary.
    6.6.1 Ethyl ether must be shown to be free of peroxides before it is 
used as indicated by EM Laboratories Quant test strips. (Available from 
Scientific Products Co., Cat. No. P1126-8, and other suppliers.)
    6.6.2 Procedures recommended for removal of peroxides are provided 
with the test strips. After cleanup, 20 mL of ethyl alcohol preservative 
must be added to each liter of ether.
    6.7 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions can be prepared from pure standard materials or 
purchased as certified solutions.
    6.7.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in acetone and dilute 
to volume in a 10-mL volumetric flask. Larger volumes can be used at the 
convenience of the analyst. When compound purity is assayed to be 96% or 
greater, the weight can be used without correction to calculate the 
concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.7.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock

[[Page 218]]

standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.
    6.7.3 Stock standard solutions must be replaced after six months, or 
sooner if comparison with check standards indicates a problem.
    6.8 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatographic operating conditions equivalent to 
those given in Table 1. The gas chromatographic system can be calibrated 
using the external standard technique (Section 7.2) or the internal 
standard technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with hexane. One of the external standards should be at a concentration 
near, but above, the MDL (Table 1) and the other concentrations should 
correspond to the expected range of concentrations found in real samples 
or should define the working range of the detector.
    7.2.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD), linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with hexane. One of the standards should be at a 
concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.116

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 The cleanup procedure in Section 11 utilizes Florisil column 
chromatography. Florisil from different batches or sources may vary in 
adsorptive capacity. To standardize the amount of Florisil which is 
used, the use of lauric acid value \7\ is suggested. The referenced 
procedure determines the adsorption from hexane solution of lauric acid 
(mg) per g of Florisil. The amount of Florisil to be used for each 
column is calculated by dividing 110 by this ratio and multiplying by 20 
g.
    7.6 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality

[[Page 219]]

checks are compared with established performance criteria to determine 
if the results of analyses meet the performance characteristics of the 
method. When results of sample spikes indicate atypical method 
performance, a quality control check standard must be analyzed to 
confirm that the measurements were performed in an in-control mode of 
operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at a concentration of 100 
[micro]g/mL in acetone. The QC check sample concentrate must be obtained 
from the U.S. Environmental Protection Agency, Environmental Monitoring 
and Support Laboratory in Cincinnati, Ohio, if available. If not 
available from that source, the QC check sample concentrate must be 
obtained from another external source. If not available from either 
source above, the QC check sample concentrate must be prepared by the 
laboratory using stock standards prepared independently from those used 
for calibration.
    8.2.2 Using a pipet, prepare QC check samples at a concentration of 
100 [micro]g/L by adding 1.00 mL of QC check sample concentrate to each 
of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter. Locate and correct the 
source of the problem and repeat the test for all parameters of interest 
beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1. The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at 100 [micro]g/L or 1 to 5 times higher than the 
background concentration determined in Section 8.3.2, whichever 
concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none (2) the larger of either 5 times higher than the expected 
background concentration or 100 [micro]g/L.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. If necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P)

[[Page 220]]

as 100(A-B)%/T, where T is the known true value of the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\8\ If spiking was performed at a concentration lower than 100 [micro]g/
L, the analyst must use either the QC acceptance criteria in Table 2, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recovery of a parameter: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 3, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T)2.44(100 S'/T)%. \8\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4 If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 m/L of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water. The 
QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P092sp to P + 
2sp. If P = 90% and sp = 10%, for example, the 
accuracy interval is expressed as 70-110%. Update the accuracy 
assessment for each parameter on a regular basis (e.g. after each five 
to ten new accuracy measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \9\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction. Fill the sample bottles and, if 
residual chlorine is present, add 80 mg of sodium thiosulfate per liter 
of sample and mix well. EPA Methods 330.4 and 330.5 may be used for 
measurement of residual chlorine. \10\ Field test kits are available for 
this purpose.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.
    10.2 Add 60 mL methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 min 
with periodic

[[Page 221]]

venting to release excess pressure. Allow the organic layer to separate 
from the water phase for a minimum of 10 min. If the emulsion interface 
between layers is more than one-third the volume of the solvent layer, 
the analyst must employ mechanical techniques to complete the phase 
separation. The optimum technique depends upon the sample, but may 
include stirring, filtration of the emulsion through glass wool, 
centrifugation, or other physical methods. Collect the methylene 
chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.6 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    Note: Some of the haloethers are very volatile and significant 
losses will occur in concentration steps if care is not exercised. It is 
important to maintain a constant gentle evaporation rate and not to 
allow the liquid volume to fall below 1 to 2 mL before removing the K-D 
apparatus from the hot water bath.
    10.7 Momentarily remove the Snyder column, add 50 mL of hexane and a 
new boiling chip, and reattach the Snyder column. Raise the temperature 
of the water bath to 85 to 90 [deg]C. Concentrate the extract as in 
Section 10.6, except use hexane to prewet the column. The elapsed time 
of concentration should be 5 to 10 min.
    10.8 Remove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of hexane. A 5-mL 
syringe is recommended for this operation. Stopper the concentrator tube 
and store refrigerated if further processing will not be performed 
immediately. If the extract will be stored longer than two days, it 
should be transferred to a Teflon-sealed screw-cap vial. If the sample 
extract requires no further cleanup, proceed with gas chromatographic 
analysis (Section 12). If the sample requires further cleanup, proceed 
to Section 11.
    10.9 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use the procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of Section 8.2 can be met using the method as revised 
to incorporate the cleanup procedure.
    11.2 Florisil column cleanup for haloethers:
    11.2.1 Adjust the sample extract volume to 10 mL.
    11.2.2 Place a weight of Florisil (nominally 20 g) predetermined by 
calibration (Section 7.5), into a chromatographic column. Tap the column 
to settle the Florisil and add 1 to 2 cm of anhydrous sodium sulfate to 
the top.
    11.2.3 Preelute the column with 50 to 60 mL of petroleum ether. 
Discard the eluate and just prior to exposure of the sodium sulfate 
layer to the air, quantitatively transfer the sample extract onto the 
column by decantation and subsequent petroleum ether washings. Discard 
the eluate. Just prior to exposure of the sodium sulfate layer to the 
air, begin eluting the column with 300 mL of ethyl ether/petroleum ether 
(6 + 94) (V/V). Adjust the elution rate to approximately 5 mL/min and 
collect the eluate in a 500-mL K-D flask equipped with a 10-mL 
concentrator tube. This fraction should contain all of the haloethers.
    11.2.4 Concentrate the fraction as in Section 10.6, except use 
hexane to prewet the column. When the apparatus is cool, remove the 
Snyder column and rinse the flask and its lower joint into the 
concentrator tube with hexane. Adjust the volume of the cleaned up 
extract to 10 mL with hexane and analyze by gas chromatography (Section 
12).

[[Page 222]]

                         12. Gas Chromatography

    12.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. Examples of the separations 
achieved by Columns 1 and 2 are shown in Figures 1 and 2, respectively. 
Other packed or capillary (open-tubular) columns, chromatographic 
conditions, or detectors may be used if the requirements of Section 8.2 
are met.
    12.2 Calibrate the system daily as described in Section 7.
    12.3 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
thoroughly immediately before injection into the gas chromatrograph.
    12.4 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush technique. \11\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, the 
total extract volume, and the resulting peak size in area or peak height 
units.
    12.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weight heavily in the interpretation of 
chromatograms.
    12.6 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    12.7 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.117

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.118

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \12\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 4 x MDL to 1000 x MDL. \12\
    14.3 This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 1.0 to 626 [micro]/L. \12\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Haloethers in Industrial and Municipal 
Wastewaters,'' EPA 600/4-81-062, National Technical Information Service, 
PB81-232290, Springfield, Virginia 22161, July 1981.

[[Page 223]]

    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constitutents,'' American Society for Testing and Materials, 
Philadelphia.
    4. ``Carcinogens--Working Carcinogens, '' Department of Health, 
Education, and Welfare, Public Health Services, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Mills., P.A. ``Variation of Florisil Activity: Simple Method for 
Measuring Absorbent Capacity and Its Use in Standardizing Florisil 
Columns,'' Journal of the Association of Official Analytical Chemists, 
51, 29 (1968).
    8. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    9. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    10. ``Methods 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric, DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    11. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    12. ``EPA Method Study 21, Method 611, Haloethers,'' EPA 600/4-84-
052, National Technical Information Service, PB84-205939, Springfield, 
Virginia 22161, June 1984.

    Table 1--Chromatographic Conditions and Methods Detection Limits
------------------------------------------------------------------------
                                         Retention time (min)    Method
                                        ---------------------- detection
               Parameters                                        limit
                                          Column 1   Column 2  ([micro]/
                                                                   L)
------------------------------------------------------------------------
Bis(2-chloroisopropyl) ether...........        8.4        9.7        0.8
Bis(2-chloroethyl) ether...............        9.3        9.1        0.3
Bis(2-chloroethoxy) methane............       13.1       10.0        0.5
4-Chlorophenyl ether...................       19.4       15.0        3.9
4-Bromophenyl phenyl ether.............       21.2       16.2        2.3
------------------------------------------------------------------------
Column 1 conditions: Supelcoport (100/120 mesh) coated with 3% SP-1000
  packed in a 1.8 m long x 2 mm ID glass column with helium carrier gas
  at 40 mL/min. flow rate. Column temperature held at 60 [deg]C for 2
  min. after injection then programmed at 8 [deg]C/min. to 230 [deg]C
  and held for 4 min. Under these conditions the retention time for
  Aldrin is 22.6 min.
Column 2 conditions: Tenax-GC (60/80 mesh) packed in a 1.8 m long x 2mm
  ID glass column with helium carrier gas at 40 mL/min. flow rate.
  Column temperature held at 150 [deg]C for 4 min. after injection then
  programmed at 16 [deg]C/min. to 310 [deg]C. Under these conditions the
  retention time for Aldrin is 18.4 min.


                                   Table 2--QC Acceptance Criteria--Method 611
----------------------------------------------------------------------------------------------------------------
                                                              Test conc.                Range for X   Range for
                         Parameter                            ([micro]g/   Limit for s   ([micro]g/     P, Ps
                                                                  L)      ([micro]g/L)       L)        percent
----------------------------------------------------------------------------------------------------------------
Bis (2-chloroethyl)ether...................................          100          26.3   26.3-136.8       11-152
Bis (2-chloroethoxy)methane................................          100          25.7   27.3-115.0       12-128
Bis (2-chloroisopropyl)ether...............................          100          32.7   26.4-147.0        9-165
4-Bromophenyl phenyl ether.................................          100          39.3    7.6-167.5        D-189
4-Chlorophenyl phenyl ether................................          100          30.7   15.4-152.5        D-170
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 611
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                              recovery, X'   precision, sr'   precision, S'
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Bis(2-chloroethyl) ether........................................    0.81C + 0.54    0.19X + 0.28    0.35X + 0,36
Bis(2-chloroethoxy) methane.....................................    0.71C + 0.13    0.20X + 0.15    0.33X + 0.11
Bis(2-chloroisopropyl) ether....................................    0.85C + 1.67    0.20X + 1.05    0.36X + 0.79
4-Bromophenyl phenyl ether......................................    0.85C + 2.55    0.25X + 0.21    0.47X + 0.37

[[Page 224]]

 
4-Chlorophenyl phenyl ether.....................................    0.82C + 1.97    0.18X + 2.13    0.41X + 0.55
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measuremelts of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.

[GRAPHIC] [TIFF OMITTED] TC02JY92.034


[[Page 225]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.035

                  Method 612--Chlorinated Hydrocarbons

                        1. Scope and Application

    1.1 This method covers the determination of certain chlorinated 
hydrocarbons. The following parameters can be determined by this method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
2-Chloronaphthalene..............................     34581      91-58-7
1,2-Dichlorobenzene..............................     34536      95-50-1
1,3-Dichlorobenzene..............................     34566     541-73-1
1,4-Dichlorobenzene..............................     34571     106-46-7
Hexachlorobenzene................................     39700     118-74-1
Hexachlorobutadiene..............................     34391      87-68-3
Hexachlorocyclopentadiene........................     34386      77-47-4
Hexachloroethane.................................     34396      67-72-1

[[Page 226]]

 
1,2,4-Trichlorobenzene...........................     34551     120-82-1
------------------------------------------------------------------------

    1.2 This is a gas chromatographic (GC) method applicable to the 
determination of the compounds listed above in municipal and industrial 
discharges as provided under 40 CFR 136.1. When this method is used to 
analyze unfamiliar samples for any or all of the compounds above, 
compound identifications should be supported by at least one additional 
qualitative technique. This method describes a second gas 
chromatographic column that can be used to confirm measurements made 
with the primary column. Method 625 provides gas chromatograph/mass 
spectrometer (GC/MS) conditions appropriate for the qualitative and 
quantitative confirmation of results for all of the parameters listed 
above, using the extract produced by this method.
    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for each parameter is listed in Table 1. The MDL for a specific 
wastewater may differ from those listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 The sample extraction and concentration steps in this method are 
essentially the same as in Methods 606, 608, 609, and 611. Thus, a 
single sample may be extracted to measure the parameters included in the 
scope of each of these methods. When cleanup is required, the 
concentration levels must be high enough to permit selecting aliquots, 
as necessary, to apply appropriate cleanup procedures. The analyst is 
allowed the latitude, under Section 12, to select chromatographic 
conditions appropriate for the simultaneous measurement of combinations 
of these parameters.
    1.5 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph and in the 
interpretation of gas chromatograms. Each analyst must demonstrate the 
ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is extracted 
with methylene chloride using a separatory funnel. The methylene 
chloride extract is dried and exchanged to hexane during concentration 
to a volume of 10 mL or less. The extract is separated by gas 
chromatography and the parameters are then measured with an electron 
capture detector. \2\
    2.2 The method provides a Florisil column cleanup procedure to aid 
in the elimination of interferences that may be encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated baselines in gas chromatograms. All 
of these materials must be routinely demonstrated to be free from 
interferences under the conditions of the analysis by running laboratory 
reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \3\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by this treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to minimize 
interference problems. Purification of solvents by distillation in all-
glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. The 
cleanup procedure in Section 11 can be used to overcome many of these 
interferences, but unique samples may require additional cleanup 
approaches to achieve the MDL listed in Table 1.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible level 
by whatever means available. The laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method. A reference 
file of material data handling sheets should also be made available to 
all

[[Page 227]]

personnel involved in the chemical analysis. Additional references to 
laboratory safety are available and have been identified \4-6\ for the 
information of the analyst.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1cL or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnel--2-L, with Teflon stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long x 19 mm ID, with coarse frit filter disc.
    5.2.3 Chromatographic column--300 long x 10 mm ID, with Teflon 
stopcock and coarse frit filter disc at bottom.
    5.2.4 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.5 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.6 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.7 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balance--Analytical, capable of accurately weighing 0.0001 g.
    5.6 Gas chromatograph--An analytical system complete with gas 
chromatograph suitable for on-column injection and all required 
accessories including syringes, analytical columns, gases, detector, and 
strip-chart recorder. A data system is recommended for measuring peak 
areas.
    5.6.1 Column 1--1.8 m long x 2 mm ID glass, packed with 1% SP-1000 
on Supelcoport (100/120 mesh) or equivalent. Guidelines for the use of 
alternate column packings are provide in Section 12.1.
    5.6.2 Column 2--1.8 m long x 2 mm ID glass, packed with 1.5% OV-1/
2.4% OV-225 on Supelcoport (80/100 mesh) or equivalent. This column was 
used to develop the method performance statements in Section 14.
    5.6.3 Detector--Electron capture detector. This detector has proven 
effective in the analysis of wastewaters for the parameters listed in 
the scope (Section 1.1), and was used to develop the method performance 
statements in Section 14. Guidelines for the use of alternate detectors 
are provided in Section 12.1.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of the parameters of interest.
    6.2 Acetone, hexane, isooctane, methanol, methylene chloride, 
petroleum ether (boiling range 30 to 60 [deg]C)--Pesticide quality or 
equivalent.
    6.3 Sodium sulfate--(ACS) Granular, anhydrous. Purify heating at 400 
[deg]C for 4 h in a shallow tray.
    6.4 Florisil--PR grade (60/100 mesh). Purchase activated at 1250 
[deg]F and store in the dark in glass containers with ground glass 
stoppers or foil-lined screw caps. Before use, activate each batch at 
least 16 h at 130 [deg]C in a foil-covered glass container and allow to 
cool.
    6.5 Stock standard solution (1.00 [micro]g/[micro]L)--Stock standard 
solutions can be prepared from pure standard materials or purchased as 
certified solutions.
    6.5.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in isooctane and dilute 
to volume in a 120-mL volumetric flask. Larger volumes can be used at 
the convenience of the analyst. When compound purity is assayed to be 
96% or greater, the weight can be used without correction to calculate 
the concentration of the stock standard. Commercially prepared stock 
standards can be used at any concentration if they are certified by the 
manufacturer or by an independent source.
    6.5.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store at 4 [deg]C and protect from light. Stock 
standard solutions should be checked frequently for signs of degradation 
or evaporation, especially just prior to preparing calibration standards 
from them.

[[Page 228]]

    6.5.3 Stock standard solutions must be replaced after six months, or 
sooner if comparision with check standards indicates a problem.
    6.6 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatographic operating conditions equivalent to 
those given in Table 1. The gas chromatographic system can be calibrated 
using the external standard technique (Section 7.2) or the internal 
standard technique (Section 7.3).
    7.2 External standard calibration procedure:
    7.2.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask and diluting to volume 
with isooctane. One of the external standards should be at a 
concentration near, but above, the MDL (Table 1) and the other 
concentrations should correspond to the expected range of concentrations 
found in real samples or should define the working range of the 
detector.
    7.2.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against the mass injected. The results can be used to prepare 
a calibration curve for each compound. Alternatively, if the ratio of 
response to amount injected (calibration factor) is a constant over the 
working range (<10% relative standard deviation, RSD), linearity through 
the origin can be assumed and the average ratio or calibration factor 
can be used in place of a calibration curve.
    7.3 Internal standard calibration procedure--To use this approach, 
the analyst must select one or more internal standards that are similar 
in analytical behavior to the compounds of interest. The analyst must 
further demonstrate that the measurement of the internal standard is not 
affected by method or matrix interferences. Because of these 
limitations, no internal standard can be suggested that is applicable to 
all samples.
    7.3.1 Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding volumes of 
one or more stock standards to a volumetric flask. To each calibration 
standard, add a known constant amount of one or more internal standards, 
and dilute to volume with isooctane. One of the standards should be at a 
concentration near, but above, the MDL and the other concentrations 
should correspond to the expected range of concentrations found in real 
samples or should define the working range of the detector.
    7.3.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standard according to Section 12 and tabulate peak height or area 
responses against concentration for each compound and internal standard. 
Calculate response factors (RF) for each compound using Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.119

                                                              Equation 1

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the parameter to be measured ([micro]g/
          L).

If the RF value over the working range is a constant (<10% RSD), the RF 
can be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to plot a 
calibration curve of response ratios, As/Ais, vs. 
RF.
    7.4 The working calibration curve, calibration factor, or RF must be 
verified on each working day by the measurement of one or more 
calibration standards. If the response for any parameter varies from the 
predicted response by more than 15%, a new 
calibration curve must be prepared for that compound.
    7.5 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When the results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.

[[Page 229]]

    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.4, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such modification is made to the method, 
the analyst is required to repeat the procedure in Section 8.2.
    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples to monitor and evaluate laboratory data 
quality. This procedure is described in Section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing each parameter of interest at the following concentrations in 
acetone: Hexachloro-substituted parameters, 10 [micro]g/mL; any other 
chlorinated hydrocarbon, 100 [micro]g/mL. The QC check sample 
concentrate must be obtained from the U.S. Environmental Protection 
Agency, Environmental Monitoring and Support Laboratory in Cincinnati, 
Ohio, if available. If not available from that source, the QC check 
sample concentrate must be obtained from another external source. If not 
available from either source above, the QC check sample concentrate must 
be prepared by the laboratory using stock standards prepared 
independently from those used for calibration.
    8.2.2 Using a pipet, prepare QC check samples at the test 
concentrations shown in Table 2 by adding 1.00 mL of QC check sample 
concentrate to each of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for each parameter 
using the four results.
    8.2.5 For each parameter compare s and X with the corresponding 
acceptance criteria for precision and accuracy, respectively, found in 
Table 2. If s and X for all parameters of interest meet the acceptance 
criteria, the system performance is acceptable and analysis of actual 
samples can begin. If any individual s exceeds the precision limit or 
any individual X falls outside the range for accuracy, the system 
performance is unacceptable for that parameter.
    Note: The large number of parameters in Table 2 presents a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when all parameters are analyzed.
    8.2.6 When one or more of the parameters tested fail at least one of 
the acceptance criteria, the analyst must proceed according to Section 
8.2.6.1 or 8.2.6.2.
    8.2.6.1 Locate and correct the source of the problem and repeat the 
test for all parameters of interest beginning with Section 8.2.2.
    8.2.6.2 Beginning with Section 8.2.2, repeat the test only for those 
parameters that failed to meet criteria. Repeated failure, however, will 
confirm a general problem with the measurement system. If this occurs, 
locate and correct the source of the problem and repeat the test for all 
compounds of interest beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spike sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of a 
specific parameter in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of a specific parameter in the sample 
is not being checked against a limit specific to that parameter, the 
spike should be at the test concentration in Section 8.2.2 or 1 to 5 
times higher than the background concentration determined in Section 
8.3.2, whichever concentration would be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the spike 
concentration should be (1) the regulatory concentration limit, if any; 
or, if none by (2) the larger of either 5 times higher than the expected 
background concentration or the test concentration in Section 8.2.2.

[[Page 230]]

    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of each parameter. In necessary, prepare a new QC 
check sample concentrate (Section 8.2.1) appropriate for the background 
concentrations in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of each parameter. Calculate each 
percent recovery (P) as 100 (A-B)%/T, where T is the known true value of 
the spike.
    8.3.3 Compare the percent recovery (P) for each parameter with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\7\ If spiking was performed at a concentration lower than the test 
concentration in Section 8.2.2, the analyst must use either the QC 
acceptance criteria in Table 2, or optional QC acceptance criteria 
calculated for the specific spike concentration. To calculate optional 
acceptance criteria for the recovery of a parameter: (1) Calculate 
accuracy (X') using the equation in Table 3, substituting the spike 
concentration (T) for C; (2) calculate overall precision (S') using the 
equation in Table 3, substituting X' for X; (3) calculate the range for 
recovery at the spike concentration as (100 X'/T) 2.44 (100 S'/T)%. \7\
    8.3.4 If any individual P falls outside the designated range for 
recovery, that parameter has failed the acceptance criteria. A check 
standard containing each parameter that failed the criteria must be 
analyzed as described in Section 8.4.
    8.4. If any parameter fails the acceptance criteria for recovery in 
Section 8.3, a QC check standard containing each parameter that failed 
must be prepared and analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the number of parameters being simultaneously tested, 
the complexity of the sample matrix, and the performance of the 
laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Sections 8.2.1 or 8.3.2) to 1 L of reagent water. 
The QC check standard needs only to contain the parameters that failed 
criteria in the test in Section 8.3.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of each parameter. Calculate each percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) for each 
parameter with the corresponding QC acceptance criteria found in Table 
2. Only parameters that failed the test in Section 8.3 need to be 
compared with these criteria. If the recovery of any such parameter 
falls outside the designated range, the laboratory performance for that 
parameter is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for that 
parameter in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the standard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment for each 
parameter on a regular basis (e.g. after each five to ten new accuracy 
measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. When doubt exists over the 
identification of a peak on the chromatogram, confirmatory techniques 
such as gas chromatography with a dissimilar column, specific element 
detector, or mass spectrometer must be used. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevent performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \8\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C from the 
time of collection until extraction.
    9.3 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.

[[Page 231]]

    10.2 Add 60 mL of methylele chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 min 
with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the volume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.3 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.4 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.5 Pour the combined extract through a solvent-rinsed drying 
column containing about 10 cm of anhydrous sodium sulfate, and collect 
the extract in the K-D concentrator. Rinse the Erlenmeyer flask and 
column with 20 to 30 mL of methylene chloride to complete the 
quantitative transfer.
    10.6 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 to 2 mL, remove the K-D apparatus and allow it to 
drain and cool for at least 10 min.
    Note: The dichloribenzenes have a sufficiently high volatility that 
significant losses may occur in concentration steps if care is not 
exercised. It is important to maintain a constant gentle evaporation 
rate and not to allow the liquid volume to fall below 1 to 2 mL before 
removing the K-D apparatus from the hot water bath.
    10.7 Momentarily remove the Snyder column, add 50 mL of hexane and a 
new boiling chip, and reattach the Snyder column. Raise the tempeature 
of the water bath to 85 to 90 [deg]C. Concentrate the extract as in 
Section 10.6, except use hexane to prewet the column. The elapsed time 
of concentration should be 5 to 10 min.
    10.8 Romove the Snyder column and rinse the flask and its lower 
joint into the concentrator tube with 1 to 2 mL of hexane. A 5-mL 
syringe is recommended for this operation. Stopper the concentrator tube 
and store refrigerated if further processing will not be performed 
immediately. If the extract will be stored longer than two days, it 
should be transferred to a Teflon-sealed screw-cap vial. If the sample 
extract requires no further cleanup, proceed with gas chromatographic 
analysis (Section 12). If the sample requires further cleanup, proceed 
to Section 11.
    10.9 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use the procedure below or any other 
appropriate procedure. However, the analyst first must demonstrate that 
the requirements of Section 8.2 can be met using the method as revised 
to incorporate the cleanup procedure.
    11.2 Florisil column cleanup for chlorinated hydrocarbons:
    11.2.1 Adjust the sample extract to 10 mL with hexane.
    11.2.2 Place 12 g of Florisil into a chromatographic column. Tap the 
column to settle the Florisil and add 1 to 2 cm of anhydrous sodium 
sulfate to the top.
    11.2.3 Preelute the column with 100 mL of petroleum ether. Discard 
the eluate and just prior to exposure of the sodium sulfate layer to the 
air, quantitatively transfer the sample extract onto the column by 
decantation and subsequent petroleum ether washings. Discard the eluate. 
Just prior to exposure of the sodium sulfate layer to the air, begin 
eluting the column with 200 mL of petroleum ether and collect the eluate 
in a 500-mL K-D flask equipped with a 10-mL concentrator tube. This 
fraction should contain all of the chlorinated hydrocarbons.
    11.2.4 Concentrate the fraction as in Section 10.6, except use 
hexane to prewet the column. When the apparatus is cool, remove the 
Snyder column and rinse the flask and its lower joint into the 
concentrator tube with hexane. Analyze by gas chromatography (Section 
12).

[[Page 232]]

                         12. Gas Chromatography

    12.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. Examples of the separations 
achieved by Columl 2 are shown in Figures 1 and 2. Other packed or 
capillary (open-tubular) columns, chromatographic conditions, or 
detectors may be used if the requirements of Section 8.2 are met.
    12.2 Calibrate the system daily as described in Section 7.
    12.3 If the internal standard calibration procedure is being used, 
the internal standard must be added to the sample extract and mixed 
throughly immediately before injection into the gas chromatograph.
    12.4 Inject 2 to 5 [micro]L of the sample extract or standard into 
the gas chromatograph using the solvent-flush techlique. \9\ Smaller 
(1.0 [micro]L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 [micro]L, the 
total extract volume, and the resulting peak size in area or peak height 
units.
    12.5 Identify the parameters in the sample by comparing the 
retention times of the peaks in the sample chromatogram with those of 
the peaks in standard chromatograms. The width of the retention time 
window used to make identifications should be based upon measurements of 
actual retention time variations of standards over the course of a day. 
Three times the standard deviation of a retention time for a compound 
can be used to calculate a suggested window size; however, the 
experience of the analyst should weigh heavily in the interpretation of 
chromatograms.
    12.6 If the response for a peak exceeds the working range of the 
system, dilute the extract and reanalyze.
    12.7 If the measurement of the peak response is prevented by the 
presence of interferences, further cleanup is required.

                            13. Calculations

    13.1 Determine the concentration of individual compounds in the 
sample.
    13.1.1 If the external standard calibration procedure is used, 
calculate the amount of material injected from the peak response using 
the calibration curve or calibration factor determined in Section 7.2.2. 
The concentration in the sample can be calculated from Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.120

                                                              Equation 2

where:
A = Amount of material injected (ng).
Vi = Volume of extract injected ([micro]L).
Vt = Volume of total extract ([micro]L).
Vs = Volume of water extracted (mL).

    13.1.2 If the internal standard calibration procedure is used, 
calculate the concentration in the sample using the response factor (RF) 
determined in Section 7.3.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.121

                                                              Equation 3

where:
As = Response for the parameter to be measured.
Ais = Response for the internal standard.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentrations 
listed in Table 1 were obtained using reagent water. \10\ Similar 
results were achieved using representative wastewaters. The MDL actually 
achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method has been tested for linearity of spike recovery 
from reagent water and has been demonstrated to be applicable over the 
concentration range from 4 x MDL to 1000 x MDL. \10\
    14.3 This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 1.0 to 356 [micro]g/L. \11\ Single 
operator precision, overall precision, and method accuracy were found to 
be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of Chlorinated Hydrocarbons In Industrial and 
Municipal Wastewaters, ``EPA 6090/4-84-ABC, National Technical 
Information Service, PBXYZ, Springfield, Virginia, 22161 November 1984.
    3. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American

[[Page 233]]

Society for Testing and Materials, Philadelphia.
    4. ``Carcinogens--Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    5. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    7. Provost, L.P., and Elder, R.S. ``Interpretation of Percent 
Recovery Data,''American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    8. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    9. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    10. ``Development of Detection Limits, EPA Method 612, Chlorinated 
Hydrocarbons,'' Special letter report for EPA Contract 68-03-2625, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268.
    11. ``EPA Method Study Method 612--Chlorinated Hydrocarbons,'' EPA 
600/4-84-039, National Technical Information Service, PB84-187772, 
Springfield, Virginia 22161, May 1984.
    12. ``Method Performance for Hexachlorocyclopentadiene by Method 
612,'' Memorandum from R. Slater, U.S. Environmental Protection Agency, 
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio 45268, 
December 7, 1983.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                     Retention time (min)       Method
                                  --------------------------  detection
            Parameter                                           limit
                                     Column 1     Column 2    ([micro]g/
                                                                  L)
------------------------------------------------------------------------
1,3-Dichlorobenzene..............          4.5          6.8         1.19
Hexachloroethane.................          4.9          8.3         0.03
1,4-Dichlorobenzene..............          5.2          7.6         1.34
1,2-Dichlorobenzene..............          6.6          9.3         1.14
Hexachlorobutadiene..............          7.7         20.0         0.34
1,2,4-Trichlorobenzene...........         15.5         22.3         0.05
Hexachlorocyclopentadiene........           nd     \c\ 16.5         0.40
2-Chloronaphthalene..............      \a\ 2.7      \b\ 3.6         0.94
Hexachlorobenzene................      \a\ 5.6     \b\ 10.1        0.05
------------------------------------------------------------------------
Column 1 conditions: Supelcoport (100/120 mesh) coated with 1% SP-1000
  packed in a 1.8 m x 2 mm ID glass column with 5% methane/95% argon
  carrier gas at 25 mL/min. flow rate. Column temperature held
  isothermal at 65 [deg]C, except where otherwise indicated.
Column 2 conditions: Supelcoport (80/100 mesh) coated with 1.5% OV-1/
  2.4% OV-225 packed in a 1.8 m x 2 mm ID glass column with 5% methane/
  95% argon carrier gas at 25 mL/min. flow rate. Column temperature held
  isothermal at 75 [deg]C, except where otherwise indicated.
nd = Not determined.
\a\ 150 [deg]C column temperature.
\b\ 165 [deg]C column temperature.
\c\ 100 [deg]C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 612
----------------------------------------------------------------------------------------------------------------
                                                                               Limit for
                                                                  Test conc.       s      Range for X  Range for
                            Parameter                             ([micro]g/  ([micro]g/   ([micro]g/    P, Ps
                                                                      L)          L)           L)      (percent)
----------------------------------------------------------------------------------------------------------------
2-Chloronaphthalene.............................................         100        37.3   29.5-126.9      9-148
1,2-Dichlorobenzene.............................................         100        28.3   23.5-145.1      9-160
1,3-Dichlorobenzene.............................................         100        26.4    7.2-138.6      D-150
1,4-Dichlorobenzene.............................................         100        20.8   22.7-126.9     13-137
Hexachlorobenzene...............................................          10         2.4     2.6-14.8     15-159
Hexachlorobutadiene.............................................          10         2.2       D-12.7      D-139
Hexachlorocyclopentadiene.......................................          10         2.5       D-10.4      D-111
Hexachloroethane................................................          10         3.3     2.4-12.3      8-139
1,2,4-Trichlorobenzene..........................................         100        31.6   20.2-133.7      5-149
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
D = Detected; result must be greater than zero.
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


[[Page 234]]


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 612
----------------------------------------------------------------------------------------------------------------
                                                                      Single analyst
               Parameter                Acccuracy, as recovery,       precision, sr'       Overall precision, S'
                                            X' ([micro]g/L)            ([micro]g/L)            ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
2-Chloronaphthalene...................  0.75C + 3.21             0.28X-1.17               0.38X-1.39
1,2-Dichlorobenzene...................  0.85C-0.70               0.22X-2.95               0.41X-3.92
1,3-Dichlorobenzene...................  0.72C + 0.87             0.21X-1.03               0.49X-3.98
1,4-Dichlorobenzene...................  0.72C + 2.80             0.16X-0.48               0.35X-0.57
Hexachlorobenzene.....................  0.87C-0.02               0.14X + 0.07             0.36X-0.19
Hexachlorobutadiene...................  0.61C + 0.03             0.18X + 0.08             0.53X-0.12
Hexachlorocyclopentadiene \a\.........  0.47C                    0.24X                    0.50X
Hexachloroethane......................  0.74C-0.02               0.23X + 0.07             0.36X-0.00
1,2,4-Trichlorobenzene................  0.76C + 0.98             0.23X-0.44               0.40X-1.37
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.
 
\a\ Estimates based upon the performance in a single laboratory. \12\


[[Page 235]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.036


[[Page 236]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.037


[[Page 237]]

             Method 613--2,3,7,8-Tetrachlorodibenzo-p-Dioxin

                        1. Scope and Application

    1.1 This method covers the determination of 2,3,7,8-
tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD). The following parameter may 
be determined by this method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                        No.       GAS No.
------------------------------------------------------------------------
2,3,7,8-TCDD.....................................    34675     1746-01-6
------------------------------------------------------------------------

    1.2 This is a gas chromatographic/mass spectrometer (GC/MS) method 
applicable to the determination of 2,3,7,8-TCDD in municipal and 
industrial discharges as provided under 40 CFR 136.1. Method 625 may be 
used to screen samples for 2,3,7,8-TCDD. When the screening test is 
positive, the final qualitative confirmation and quantification must be 
made using Method 613.
    1.3 The method detection limit (MDL, defined in Section 14.1) \1\ 
for 2,3,7,8-TCDD is listed in Table 1. The MDL for a specific wastewater 
may be different from that listed, depending upon the nature of 
interferences in the sample matrix.
    1.4 Because of the extreme toxicity of this compound, the analyst 
must prevent exposure to himself, of to others, by materials knows or 
believed to contain 2,3,7,8-TCDD. Section 4 of this method contains 
guidelines and protocols that serve as minimum safe-handling standards 
in a limited-access laboratory.
    1.5 Any modification of this method, beyond those expressly 
permitted, shall be considered as a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph/mass spectrometer 
and in the interpretation of mass spectra. Each analyst must demonstrate 
the ability to generate acceptable results with this method using the 
procedure described in Section 8.2.

                          2. Summary of Method

    2.1 A measured volume of sample, approximately 1-L, is spiked with 
an internal standard of labeled 2,3,7,8-TCDD and extracted with 
methylene chloride using a separatory funnel. The methylene chloride 
extract is exchanged to hexane during concentration to a volume of 1.0 
mL or less. The extract is then analyzed by capillary column GC/MS to 
separate and measure 2,3,7,8-TCDD. \2 3\
    2.2 The method provides selected column chromatographic cleanup 
proceudres to aid in the elimination of interferences that may be 
encountered.

                            3. Interferences

    3.1 Method interferences may be caused by contaminants in solvents, 
reagents, glassware, and other sample processing hardware that lead to 
discrete artifacts and/or elevated backgrounds at the masses (m/z) 
monitored. All of these materials must be routinely demonstrated to be 
free from interferences under the conditions of the analysis by running 
laboratory reagent blanks as described in Section 8.1.3.
    3.1.1 Glassware must be scrupulously cleaned. \4\ Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and distilled water. The glassware 
should then be drained dry, and heated in a muffle furnace at 400 [deg]C 
for 15 to 30 min. Some thermally stable materials, such as PCBs, may not 
be eliminated by the treatment. Solvent rinses with acetone and 
pesticide quality hexane may be substituted for the muffle furnace 
heating. Thorough rinsing with such solvents usually eliminates PCB 
interference. Volumetric ware should not be heated in a muffle furnace. 
After drying and cooling, glassware should be sealed and stored in a 
clean environment to prevent any accumulation of dust or other 
contaminants. Store inverted or capped with aluminum foil.
    3.1.2 The use of high purity reagents and solvents helps to 
mininmize interference problems. Purification of solvents by 
distillation in all-glass systems may be required.
    3.2 Matrix interferences may be caused by contaminants that are 
coextracted from the sample. The extent of matrix interferences will 
vary considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. 
2,3,7,8-TCDD is often associated with other interfering chlorinated 
compounds which are at concentrations several magnitudes higher than 
that of 2,3,7,8-TCDD. The cleanup producers in Section 11 can be used to 
overcome many of these interferences, but unique samples may require 
additional cleanup approaches \1 5-7\ to eliminate false positives and 
achieve the MDL listed in Table 1.
    3.3 The primary column, SP-2330 or equivalent, resolves 2,3,7,8-TCDD 
from the other 21 TCDD insomers. Positive results using any other gas 
chromatographic column must be confirmed using the primary column.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to

[[Page 238]]

the lowest possible level by whatever means available. The laboratory is 
responsible for maintaining a current awareness file of OSHA regulations 
regarding the safe handling of the chemicals specified in this method. A 
reference file of material data handling sheets should also be made 
available to all personnel involved in the chemical analysis. Additional 
references to laboratory safety are available and have been identified 
\8-10\ for the information of the analyst. Benzene and 2,3,7,8-TCDD have 
been identified as suspected human or mammalian carcinogens.
    4.2 Each laboratory must develop a strict safety program for 
handling 2,3,7,8-TCDD. The following laboratory practices are 
recommended:
    4.2.1 Contamination of the laboratory will be minimized by 
conducting all manipulations in a hood.
    4.2.2 The effluents of sample splitters for the gas chromatograph 
and roughing pumps on the GC/MS should pass through either a column of 
activated charcoal or be bubbled through a trap containing oil or high-
boiling alcohols.
    4.2.3 Liquid waste should be dissolved in methanol or ethanol and 
irradiated with ultraviolet light with a wavelength greater than 290 nm 
for several days. (Use F 40 BL lamps or equivalent). Analyze liquid 
wastes and dispose of the solutions when 2,3,7,8-TCDD can no longer be 
detected.
    4.3 Dow Chemical U.S.A. has issued the following precautimns 
(revised November 1978) for safe handling of 2,3,7,8-TCDD in the 
laboratory:
    4.3.1 The following statements on safe handling are as complete as 
possible on the basis of available toxicological information. The 
precautions for safe handling and use are necessarily general in nature 
since detailed, specific recommendations can be made only for the 
particular exposure and circumstances of each individual use. Inquiries 
about specific operations or uses may be addressed to the Dow Chemical 
Company. Assistance in evaluating the health hazards of particular plant 
conditions may be obtained from certain consulting laboratories and from 
State Departments of Health or of Labor, many of which have an 
industrial health service. 2,3,7,8-TCDD is extremely toxic to laboratory 
animals. However, it has been handled for years without injury in 
analytical and biological laboratories. Techniques used in handling 
radioactive and infectious materials are applicable to 2,3,7,8,-TCDD.
    4.3.1.1 Protective equipment--Throw-away plastic gloves, apron or 
lab coat, safety glasses, and a lab hood adequate for radioactive work.
    4.3.1.2 Training--Workers must be trained in the proper method of 
removing contaminated gloves and clothing without contacting the 
exterior surfaces.
    4.3.1.3 Personal hygiene--Thorough washing of hands and forearms 
after each manipulation and before breaks (coffee, lunch, and shift).
    4.3.1.4 Confinement--Isolated work area, posted with signs, 
segregated glassware and tools, plastic-backed absorbent paper on 
benchtops.
    4.3.1.5 Waste--Good technique includes minimizing contaminated 
waste. Plastic bag liners should be used in waste cans. Janitors must be 
trained in the safe handling of waste.
    4.3.1.6 Disposal of wastes--2,3,7,8-TCDD decomposes above 800 
[deg]C. Low-level waste such as absorbent paper, tissues, animal 
remains, and plastic gloves may be burned in a good incinerator. Gross 
quantities (milligrams) should be packaged securely and disposed through 
commercial or governmental channels which are capable of handling high-
level radioactive wastes or extremely toxic wastes. Liquids should be 
allowed to evaporate in a good hood and in a disposable container. 
Residues may then be handled as above.
    4.3.1.7 Decontamination--For personal decontamination, use any mild 
soap with plenty of scrubbing action. For decontamination of glassware, 
tools, and surfaces, Chlorothene NU Solvent (Trademark of the Dow 
Chemical Company) is the least toxic solvent shown to be effective. 
Satisfactory cleaning may be accomplished by rinsing with Chlorothene, 
then washing with any detergent and water. Dishwater may be disposed to 
the sewer. It is prudent to minimize solvent wastes because they may 
require special disposal through commercial sources which are expensive.
    4.3.1.8 Laundry--Clothing known to be contaminated should be 
disposed with the precautions described under Section 4.3.1.6. Lab coats 
or other clothing worn in 2,3,7,8-TCDD work areas may be laundered.
    Clothing should be collected in plastic bags. Persons who convey the 
bags and launder the clothing should be advised of the hazard and 
trained in proper handling. The clothing may be put into a washer 
without contact if the launderer knows the problem. The washer should be 
run through a cycle before being used again for other clothing.
    4.3.1.9 Wipe tests--A useful method of determining cleanliness of 
work surfaces and tools is to wipe the surface with a piece of filter 
paper. Extraction and analysis by gas chromatography can achieve a limit 
of sensitivity of 0.1 [micro]g per wipe. Less than 1 [micro]g of 
2,3,7,8-TCDD per sample indicates acceptable cleanliness; anything 
higher warrants further cleaning. More than 10 [micro]g on a wipe sample 
constitutes an acute hazard and requires prompt cleaning before further 
use of the equipment or work space. A high (10 [micro]g)

[[Page 239]]

2,3,7,8-TCDD level indicates that unacceptable work practices have been 
employed in the past.
    4.3.1.10 Inhalation--Any procedure that may produce airborne 
contamination must be done with good ventilation. Gross losses to a 
ventilation system must not be allowed. Handling of the dilute solutions 
normally used in analytical and animal work presents no inhalation 
hazards except in the case of an accident.
    4.3.1.11 Accidents--Remove contaminated clothing immediately, taking 
precautions not to contaminate skin or other articles. Wash exposed skin 
vigorously and repeatedly until medical attention is obtained.

                       5. Apparatus and Materials

    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--1-L or 1-qt, amber glass, fitted with a 
screw cap lined with Teflon. Foil may be substituted for Teflon if the 
sample is not corrosive. If amber bottles are not available, protect 
samples from light. The bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--The sampler must incorporate 
glass sample containers for the collection of a minimum of 250 mL of 
sample. Sample containers must be kept refrigerated at 4 [deg]C and 
protected from light during compositing. If the sampler uses a 
peristaltic pump, a minimum length of compressible silicone rubber 
tubing may be used. Before use, however, the compressible tubing should 
be thoroughly rinsed with methanol, followed by repeated rinsings with 
distilled water to minimize the potential for contamination of the 
sample. An integrating flow meter is required to collect flow 
proportional composites.
    5.1.3 Clearly label all samples as ``POISON'' and ship according to 
U.S. Department of Transportation regulations.
    5.2 Glassware (All specifications are suggested. Catalog numbers are 
included for illustration only.):
    5.2.1 Separatory funnels--2-L and 125-mL, with Teflon stopcock.
    5.2.2 Concentrator tube, Kuderna-Danish--10-mL, graduated (Kontes K-
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. Ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.3 Evaporative flask, Kuderna-Danish--500-mL (Kontes K-570001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.4 Snyder column, Kuderna-Danish--Three-ball macro (Kontes K-
503000-0121 or equivalent).
    5.2.5 Snyder column, Kuderna-Danish--Two-ball micro (Kontes K-
569001-0219 or equivalent).
    5.2.6 Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.7 Chromatographic column--300 mm long x 10 mm ID, with Teflon 
stopcock and coarse frit filter disc at bottom.
    5.2.8 Chromatographic column--400 mm long x 11 mm ID, with Teflon 
stopcock and coarse frit filter disc at bottom.
    5.3 Boiling chips--Approximately 10/40 mesh. Heat to 400 [deg]C for 
30 min or Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 GC/MS system:
    5.5.1 Gas chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph and all required accessories 
including syringes, analytical columns, and gases. The injection port 
must be designed for capillary columns. Either split, splitless, or on-
column injection techniques may be employed, as long as the requirements 
of Section 7.1.1 are achieved.
    5.5.2 Column--60 m long x 0.25 mm ID glass or fused silica, coated 
with SP-2330 (or equivalent) with a film thickness of 0.2 [micro]m. Any 
equivalent column must resolve 2, 3, 7, 8-TCDD from the other 21 TCDD 
isomers. \16\
    5.5.3 Mass spectrometer--Either a low resolution mass spectrometer 
(LRMS) or a high resolution mass spectrometer (HRMS) may be used. The 
mass spectrometer must be equipped with a 70 V (nominal) ion source and 
be capable of aquiring m/z abundance data in real time selected ion 
monitoring (SIM) for groups of four or more masses.
    5.5.4 GC/MS interface--Any GC to MS interface can be used that 
achieves the requirements of Section 7.1.1. GC to MS interfaces 
constructed of all glass or glass-lined materials are recommended. Glass 
surfaces can be deactivated by silanizing with dichlorodimethylsilane. 
To achieve maximum sensitivity, the exit end of the capillary column 
should be placed in the ion source. A short piece of fused silica 
capillary can be used as the interface to overcome problems associated 
with straightening the exit end of glass capillary columns.
    5.5.5 The SIM data acquired during the chromatographic program is 
defined as the Selected Ion Current Profile (SICP). The SICP can be 
acquired under computer control or as a real time analog output. If 
computer control is used, there must be software available to plot the 
SICP and report peak height or area data for any m/z in the SICP between 
specified time or scan number limits.
    5.6 Balance--Analytical, capable of accurately weighing 0.0001 g.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as a water in which an 
interferent is not observed at the MDL of 2, 3, 7, 8-TCDD.

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    6.2 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 mL. Wash the solution with methylene 
chloride and hexane before use.
    6.3 Sodium thiosulfate--(ACS) Granular.
    6.4 Sulfuric acid--Concentrated (ACS, sp. gr. 1.84).
    6.5 Acetone, methylene chloride, hexane, benzene, ortho-xylene, 
tetradecane--Pesticide quality or equivalent.
    6.6 Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400 [deg]C for 4 h in a shallow tray.
    6.7 Alumina--Neutral, 80/200 mesh (Fisher Scientific Co., No. A-540 
or equivalent). Before use, activate for 24 h at 130 [deg]C in a foil-
covered glass container.
    6.8 Silica gel--High purity grade, 100/120 mesh (Fisher Scientific 
Co., No. S-679 or equivalent).
    6.9 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutimns can be prepared from pure standard materials or 
purchased as certified solutions. Acetone should be used as the solvent 
for spiking solutions; ortho-xylene is recommended for calibration 
standards for split injectors; and tetradecane is recommended for 
splitless or on-colum injectors. Analyze stock internal standards to 
verify the absence of native 2,3,7,8-TCDD.
    6.9.1 Prepare stock standard solutions of 2,3,7,8-TCDD (mol wt 320) 
and either \37\C14 2,3,7,8-TCDD (mol wt 328) or 
\13\C112 2,3,7,8-TCDD (mol wt 332) in an isolated area by 
accurately weighing about 0.0100 g of pure material. Dissolve the 
material in pesticide quality solvent and dilute to volume in a 10-mL 
volumetric flask. When compound purity is assayed to be 96% or greater, 
the weight can be used without correction to calculate the concentration 
of the stock standard. Commercially prepared stock standards can be used 
at any concentration if they are certified by the manufacturer or by an 
independent source.
    6.9.2 Transfer the stock standard solutions into Teflon-sealed 
screw-cap bottles. Store in an isolated refrigerator protected from 
light. Stock standard solutions should be checked frequently for signs 
of degradation or evaporation, especially just prior to preparing 
calibration standards or spiking solutions from them.
    6.9.3 Stock standard solutions must be replaced after six months, or 
sooner if comparison with check standards indicates a problem.
    6.10 Internal standard spiking solution (25 ng/mL)--Using stock 
standard solution, prepare a spiking solution in acetone of either \13\ 
Cl12 or \37\ Cl4 2,3,7,8-TCDD at a concentration 
of 25 ng/mL. (See Section 10.2)
    6.11 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Establish gas chromatograhic operating conditions equivalent to 
those given in Table 1 and SIM conditions for the mass spectrometer as 
described in Section 12.2 The GC/MS system must be calibrated using the 
internal standard technique.
    7.1.1 Using stock standards, prepare calibration standards that will 
allow measurement of relative response factors of at least three 
concentration ratios of 2,3,7,8-TCDD to internal standard. Each 
calibration standard must be prepared to contain the internal standard 
at a concentration of 25 ng/mL. If any interferences are contributed by 
the internal standard at m/z 320 and 322, its concentration may be 
reduced in the calibration standards and in the internal standard 
spiking solution (Section 6.10). One of the calibration standards should 
contain 2,3,7,8-TCDD at a concentration near, but above, the MDL and the 
other 2,3,7,8-TCDD concentrations should correspond to the expected 
range of concentrations found in real samples or should define the 
working range of the GC/MS system.
    7.1.2 Using injections of 2 to 5 [micro]L, analyze each calibration 
standardaccording to Section 12 and tabulate peak height or area 
response against the concentration of 2,3,7,8-TCDD and internal 
standard. Calculate response factors (RF) for 2,3,7,8-TCDD using 
Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.122

                                                              Equation 1

where:
As = SIM response for 2,3,7,8-TCDD m/z 320.
Ais = SIM response for the internal standard, m/z 332 for 
          \13\ C12 2,3,7,8-TCDD m/z 328 for \37\ 
          Cl4 2,3,7,8-TCDD.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of 2,3,7,8-TCDD ([micro]g/L).

If the RF value over the working range is a constant (<10% relative 
standard deviation, RSD), the RF can be assumed to be invariant and the 
average RF can be used for calculations. Alternatively, the results can 
be used to plot a calibration curve of response ratios, As/
Ais, vs. RF.
    7.1.3 The working calibration curve or RF must be verified on each 
working day by the measurement of one or more 2,3,7,8-TCDD calibration 
standards. If the response for 2,3,7,8-TCDD varies from the predicted 
response by more than 15%, the test must be 
repeated using a fresh calibration standard. Alternatively, a new 
calibration curve must be prepared.

[[Page 241]]

    7.2 Before using any cleanup procedure, the analyst must process a 
series of calibration standards through the procedure to validate 
elution patterns and the absence of interferences from the reagents.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality control program. The minimum requirements of this program 
consist of an initial demonstration of laboratory capability and an 
ongoing analysis of spiked samples to evaluate and document data 
quality. The laboratory must maintain records to document the quality of 
data that is generated. Ongoing data quality checks are compared with 
established performance criteria to determine if the results of analyses 
meet the performance characteristics of the method. When results of 
sample spikes indicate atypical method performance, a quality control 
check standard must be analyzed to confirm that the measurements were 
performed in an in-control mode of operation.
    8.1.1 The analyst must make an initial, one-time, demonstration of 
the ability to generate acceptable accuracy and precision with this 
method. This ability is established as described in Section 8.2.
    8.1.2 In recognition of advances that are occurring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.5, 11.1, and 12.1) to improve the separations or lower the 
cost of measurements. Each time such a modification is made to the 
method, the analyst is required to repeat the procedure in Section 8.2
    8.1.3 Before processing any samples, the analyst must analyze a 
reagent water blank to demonstrate that interferences from the 
analytical system and glassware are under control. Each time a set of 
samples is extracted or reagents are changed, a reagent water blank must 
be processed as a safeguard against laboratory contamination.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze a 
minimum of 10% of all samples with native 2,3,7,8-TCDD to monitor and 
evaluate laboratory data quality. This procedure is described in Section 
8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
the analyses of quality control check standards that the operation of 
the measurement system is in control. This procedure is described in 
Section 8.4. The frequency of the check standard analyses is equivalent 
to 10% of all samples analyzed but may be reduced if spike recoveries 
from samples (Section 8.3) meet all specified quality control criteria.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.5.
    8.2 To establish the ability to generate acceptable accuracy and 
precision, the analyst must perform the following operations.
    8.2.1 A quality control (QC) check sample concentrate is required 
containing 2,3,7,8-TCDD at a concentration of 0.100 [micro]g/mL in 
acetone. The QC check sample concentrate must be obtained from the U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory in Cincinnati, Ohio, if available. If not available from that 
source, the QC check sample concentrate must be obtained from another 
external source. If not available from either source above, the QC check 
sample concentrate must be prepared by the laboratory using stock 
standards prepared independently from those used for calibration.
    8.2.2 Using a pipet, prepare QC check samples at a concentration of 
0.100 [micro]g/L (100 ng/L) by adding 1.00 mL of QC check sample 
concentrate to each of four 1-L aliquots of reagent water.
    8.2.3 Analyze the well-mixed QC check samples according to the 
method beginning in Section 10.
    8.2.4 Calculate the average recovery (X) in [micro]g/L, and the 
standard deviation of the recovery (s) in [micro]g/L, for 2,3,7,8-TCDD 
using the four results.
    8.2.5 Compare s and (X) with the corresponding acceptance criteria 
for precision and accuracy, respectively, found in Table 2. If s and X 
meet the acceptance criteria, the system performance is acceptable and 
analysis of actual samples can begin. If s exceeds the precision limit 
or X falls outside the range for accuracy, the system performance is 
unacceptable for 2,3,7,8-TCDD. Locate and correct the source of the 
problem and repeat the test beginning with Section 8.2.2.
    8.3 The laboratory must, on an ongoing basis, spike at least 10% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing one to ten samples per month, at least one 
spiked sample per month is required.
    8.3.1 The concentration of the spike in the sample should be 
determined as follows:
    8.3.1.1 If, as in compliance monitoring, the concentration of 
2,3,7,8-TCDD in the sample is being checked against a regulatory 
concentration limit, the spike should be at that limit or 1 to 5 times 
higher than the background concentration determined in Section 8.3.2, 
whichever concentration would be larger.
    8.3.1.2 If the concentration of 2,3,7,8-TCDD in the sample is not 
being checked against a limit specific to that parameter, the spike 
should be at 0.100 [micro]g/L or 1 to 5 times higher than the background 
concentration determined in Section 8.3.2, whichever concentration would 
be larger.
    8.3.1.3 If it is impractical to determine background levels before 
spiking (e.g., maximum holding times will be exceeded), the

[[Page 242]]

spike concentration should be (1) the regulatory concentration limit, if 
any; or, if none (2) the larger of either 5 times higher than the 
expected background concentration or 0.100 [micro]g/L.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of 2,3,7,8-TCDD. If necessary, prepare a new QC check 
sample concentrate (Section 8.2.1) appropriate for the background 
concentration in the sample. Spike a second sample aliquot with 1.0 mL 
of the QC check sample concentrate and analyze it to determine the 
concentration after spiking (A) of 2,3,7,8-TCDD. Calculate percent 
recovery (P) as 100(A-B)%T, where T is the known true value of the 
spike.
    8.3.3 Compare the percent recovery (P) for 2,3,7,8-TCDD with the 
corresponding QC acceptance criteria found in Table 2. These acceptance 
criteria were calculated to include an allowance for error in 
measurement of both the background and spike concentrations, assuming a 
spike to background ratio of 5:1. This error will be accounted for to 
the extent that the analyst's spike to background ratio approaches 5:1. 
\11\ If spiking was performed at a concentration lower than 0.100 
[micro]g/L, the analyst must use either the QC acceptance criteria in 
Table 2, or optional QC acceptance criteria calculated for the specific 
spike concentration. To calculate optional acceptance criteria for the 
recovery of 2,3,7,8-TCDD: (1) Calculate accuracy (X') using the equation 
in Table 3, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 3, 
substituting X' for X; (3) calculate the range for recovery at the spike 
concentration as (100 X'/T)2.44(100 S'/T)%. \11\
    8.3.4 If the recovery of 2,3,7,8-TCDD falls outside the designated 
range for recovery, a check standard must be analyzed as described in 
Section 8.4.
    8.4 If the recovery of 2,3,7,8-TCDD fails the acceptance criteria 
for recovery in Section 8.3, a QC check standard must be prepared and 
analyzed.
    Note: The frequency for the required analysis of a QC check standard 
will depend upon the complexity of the sample matrix and the performance 
of the laboratory.
    8.4.1 Prepare the QC check standard by adding 1.0 mL of QC check 
sample concentrate (Section 8.2.1 or 8.3.2) to 1 L of reagent water.
    8.4.2 Analyze the QC check standard to determine the concentration 
measured (A) of 2,3,7,8-TCDD. Calculate the percent recovery 
(Ps) as 100 (A/T)%, where T is the true value of the standard 
concentration.
    8.4.3 Compare the percent recovery (Ps) with the 
corresponding QC acceptance criteria found in Table 2. If the recovery 
of 2,3,7,8-TCDD falls outside the designated range, the laboratory 
performance is judged to be out of control, and the problem must be 
immediately identified and corrected. The analytical result for 2,3,7,8-
TCDD in the unspiked sample is suspect and may not be reported for 
regulatory compliance purposes.
    8.5 As part of the QC program for the laboratory, method accuracy 
for wastewater samples must be assessed and records must be maintained. 
After the analysis of five spiked wastewater samples as in Section 8.3, 
calculate the average percent recovery (P) and the spandard deviation of 
the percent recovery (sp). Express the accuracy assessment as 
a percent recovery interval from P-2sp to P + 2sp. 
If P = 90% and sp = 10%, for example, the accuracy interval 
is expressed as 70-110%. Update the accuracy assessment on a regular 
basis (e.g. after each five to ten new accuracy measurements).
    8.6 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of the environmental measurements. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples must be collected in glass containers. Conventional 
sampling practices \12\ should be followed, except that the bottle must 
not be prerinsed with sample before collection. Composite samples should 
be collected in refrigerated glass containers in accordance with the 
requirements of the program. Automatic sampling equipment must be as 
free as possible of Tygon tubing and other potential sources of 
contamination.
    9.2 All samples must be iced or refrigerated at 4 [deg]C and 
protected from light from the time of collection until extraction. Fill 
the sample bottles and, if residual chlorine is present, add 80 mg of 
sodium thiosulfate per liter of sample and mix well. EPA Methods 330.4 
and 330.5 may be used for measurement of residual chlorine. \13\ Field 
test kits are available for this purpose.
    9.3 Label all samples and containers ``POISON'' and ship according 
to applicable U.S. Department of Transportation regulations.
    9.4 All samples must be extracted within 7 days of collection and 
completely analyzed within 40 days of extraction. \2\

                          10. Sample Extraction

    Caution: When using this method to analyze for 2,3,7,8-TCDD, all of 
the following operations must be performed in a limited-access 
laboratory with the analyst wearing full

[[Page 243]]

protective covering for all exposed skin surfaces. See Section 4.2.
    10.1 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into a 2-L 
separatory funnel.
    10.2 Add 1.00 mL of internal standard spiking solution to the sample 
in the separatory funnel. If the final extract will be concentrated to a 
fixed volume below 1.00 mL (Section 12.3), only that volume of spiking 
solution should be added to the sample so that the final extract will 
contain 25 ng/mL of internal standard at the time of analysis.
    10.3 Add 60 mL of methylene chloride to the sample bottle, seal, and 
shake 30 s to rinse the inner surface. Transfer the solvent to the 
separatory funnel and extract the sample by shaking the funnel for 2 
min. with periodic venting to release excess pressure. Allow the organic 
layer to separate from the water phase for a minimum of 10 min. If the 
emulsion interface between layers is more than one-third the vmlume of 
the solvent layer, the analyst must employ mechanical techniques to 
complete the phase separation. The optimum technique depends upon the 
sample, but may include stirring, filtration of the emulsion through 
glass wool, centrifugation, or other physical methods. Collect the 
methylene chloride extract in a 250-mL Erlenmeyer flask.
    10.4 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.5 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10-
mL concentrator tube to a 500-mL evaporative flask. Other concentration 
devices or techniques may be used in place of the K-D concentrator if 
the requirements of Section 8.2 are met.
    10.6 Pour the combined extract into the K-D concentrator. Rinse the 
Erlenmeyer flask with 20 to 30 mL of methylele chloride to complete the 
quantitative transfer.
    10.7 Add one or two clean boiling chips to the evaporative flask and 
attach a three-ball Snyder column. Prewet the Snyder column by adding 
about 1 mL of methylene chloride to the top. Place the K-D apparatus on 
a hot water bath (60 to 65 [deg]C) so that the concentrator tube is 
partially immersed in the hot water, and the entire lower rounded 
surface of the flask is bathed with hot vapor. Adjust the vertical 
position of the apparatus and the water temperature as required to 
complete the concentration in 15 to 20 min. At the proper rate of 
distillation the balls of the column will actively chatter but the 
chambers will not flood with condensed solvent. When the apparent volume 
of liquid reaches 1 mL, remove the K-D apparatus and allow it to drain 
and cool for at least 10 min.
    10.8 Momentarily remove the Snyder column, add 50 mL of hexane and a 
new boiling chip, and reattach the Snyder column. Raise the temperature 
of the water bath to 85 to 90 [deg]C. Concentrate the extract as in 
Section 10.7, except use hexane to prewet the column. Remove the Snyder 
column and rinse the flask and its lower joint into the concentrator 
tube with 1 to 2 mL of hexane. A 5-mL syringe is recommended for this 
operation. Set aside the K-D glassware for reuse in Section 10.14.
    10.9 Pour the hexane extract from the concentrator tube into a 125-
mL separatory funnel. Rinse the concentrator tube four times with 10-mL 
aliquots of hexane. Combine all rinses in the 125-mL separatory funnel.
    10.10 Add 50 mL of sodium hydroxide solution to the funnel and shake 
for 30 to 60 s. Discard the aqueous phase.
    10.11 Perform a second wash of the organic layer with 50 mL of 
reagent water. Discard the aqueous phase.
    10.12 Wash the hexane layer with a least two 50-mL aliquots of 
concentrated sulfuric acid. Continue washing the hexane layer with 50-mL 
aliquots of concentrated sulfuric acid until the acid layer remains 
colorless. Discard all acid fractions.
    10.13 Wash the hexane layer with two 50-mL aliquots of reagent 
water. Discard the aqueous phases.
    10.14 Transfer the hexane extract into a 125-mL Erlenmeyer flask 
containing 1 to 2 g of anhydrous sodium sulfate. Swirl the flask for 30 
s and decant the hexane extract into the reassembled K-D apparatus. 
Complete the quantitative transfer with two 10-mL hexane rinses of the 
Erlenmeyer flask.
    10.15 Replace the one or two clean boiling chips and concentrate the 
extract to 6 to 10 mL as in Section 10.8.
    10.16 Add a clean boiling chip to the concentrator tube and attach a 
two-ball micro-Snyder column. Prewet the column by adding about 1 mL of 
hexane to the top. Place the micro-K-D apparatus on the water bath so 
that the concentrator tube is partially immersed in the hot water. 
Adjust the vertical position of the apparatus and the water temperature 
as required to complete the concentration in 5 to 10 min. At the proper 
rate of distillation the balls of the column will actively chatter but 
the chambers will not flood. When the apparent volume of liquid reaches 
about 0.5 mL, remove the K-D apparatus and allow it to drain and cool 
for at least 10 min. Remove the micro-Snyder column and rinse its lower 
joint into the concentrator tube with 0.2 mL of hexane.
    Adjust the extract volume to 1.0 mL with hexane. Stopper the 
concentrator tube and store refrigerated and protected from light if 
further processing will not be performed immediately. If the extract 
will be stored

[[Page 244]]

longer than two days, it should be transferred to a Teflon-sealed screw-
cap vial. If the sample extract requires no further cleanup, proceed 
with GC/MS analysis (Section 12). If the sample requires further 
cleanup, proceed to Section 11.
    10.17 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to a 1000-mL graduated 
cylinder. Record the sample volume to the nearest 5 mL.

                       11. Cleanup and Separation

    11.1 Cleanup procedures may not be necessary for a relatively clean 
sample matrix. If particular circumstances demand the use of a cleanup 
procedure, the analyst may use either procedure below or any other 
appropriate procedure. \1 5-7\ However, the analyst first must 
demonstrate that the requirements of Section 8.2 can be met using the 
method as revised to incorporate the cleanup procedure. Two cleanup 
column options are offered to the analyst in this section. The alumina 
column should be used first to overcome interferences. If background 
problems are still encountered, the silica gel column may be helpful.
    11.2 Alumina column cleanup for 2,3,7,8-TCDD:
    11.2.1 Fill a 300 mm long x 10 mm ID chromatographic column with 
activated alumina to the 150 mm level. Tap the column gently to settle 
the alumina and add 10 mm of anhydrous sodium sulfate to the top.
    11.2.2 Preelute the column with 50 mL of hexane. Adjust the elution 
rate to 1 mL/min. Discard the eluate and just prior to exposure of the 
sodium sulfate layer to the air, quantitatively transfer the 1.0-mL 
sample extract onto the column using two 2-mL portions of hexane to 
complete the transfer.
    11.2.3 Just prior to exposure of the sodium sulfate layer to the 
air, add 50 mL of 3% methylene chloride/95% hexane (V/V) and continue 
the elution of the column. Discard the eluate.
    11.2.4 Next, elute the column with 50 mL of 20% methylene chloride/
80% hexane (V/V) into a 500-mL K-D flask equipped with a 10-mL 
concentrator tube. Concentrate the collected fraction to 1.0 mL as in 
Section 10.16 and analyze by GC/MS (Section 12).
    11.3 Silica gel column cleanup for 2,3,7,8-TCDD:
    11.3.1 Fill a 400 mm long x 11 mm ID chromatmgraphic column with 
silica gel to the 300 mm level. Tap the column gently to settle the 
silica gel and add 10 mm of anhydrous sodium sulfate to the top.
    11.3.2 Preelute the column with 50 mL of 20% benzene/80% hexane (V/
V). Adjust the elution rate to 1 mL/min. Discard the eluate and just 
prior to exposure of the sodium sulfate layer to the air, quantitatively 
transfer the 1.0-mL sample extract onto the column using two 2-mL 
portions of 20% benzene/80% hexane to complete the transfer.
    11.3.3 Just prior to exposure of the sodium sulfate layer to the 
air, add 40 mL of 20% benzene/80% hexane to the column. Collect the 
eluate in a clean 500-mL K-D flask equipped with a 10-mL concentrator 
tube. Concentrate the collected fraction to 1.0 mL as in Section 10.16 
and analyze by GC/MS.

                           12. GC/MS Analysis

    12.1 Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and MDL 
that can be achieved under these conditions. Other capillary columns or 
chromatographic conditions may be used if the requirements of Sections 
5.5.2 and 8.2 are met.
    12.2 Analyze standards and samples with the mass spectrometer 
operating in the selected ion monitoring (SIM) mode using a dwell time 
to give at least seven points per peak. For LRMS, use masses at m/z 320, 
322, and 257 for 2,3,7,8-TCDD and either m/z 328 for \37\Cl4 
2,3,7,8-TCDD or m/z 332 for \13\C12 2,3,7,8-TCDD. For HRMS, 
use masses at m/z 319.8965 and 321.8936 for 2,3,7,8-TCDD and either m/z 
327.8847 for \37\Cl4 2,3,7,8-TCDD or m/z 331.9367 for 
\13\C12 2,3,7,8-TCDD.
    12.3 If lower detection limits are required, the extract may be 
carefully evaporated to dryness under a gentle stream of nitrogen with 
the concentrator tube in a water bath at about 40 [deg]C. Conduct this 
operation immediately before GC/MS analysis. Redissolve the extract in 
the desired final volume of ortho-xylene or tetradecane.
    12.4 Calibrate the system daily as described in Section 7.
    12.5 Inject 2 to 5 [micro]L of the sample extract into the gas 
chromatograph. The volume of calibration standard injected must be 
measured, or be the same as all sample injection volumes.
    12.6 The presence of 2,3,7,8-TCDD is qualitatively confirmed if all 
of the following criteria are achieved:
    12.6.1 The gas chromatographic column must resolve 2,3,7,8-TCDD from 
the other 21 TCDD isomers.
    12.6.2 The masses for native 2,3,7,8-TCDD (LRMS-m/z 320, 322, and 
257 and HRMS-m/z 320 and 322) and labeled 2,3,7,8-TCDD (m/z 328 or 332) 
must exhibit a simultaneous maximum at a retention time that matches 
that of native 2,3,7,8-TCDD in the calibration standard, with the 
performance specifications of the analytical system.
    12.6.3 The chlorine isotope ratio at m/z 320 and m/z 322 must agree 
to within10% of that in the calibration standard.
    12.6.4 The signal of all peaks must be greater than 2.5 times the 
noise level.
    12.7 For quantitation, measure the response of the m/z 320 peak for 
2,3,7,8-TCDD

[[Page 245]]

and the m/z 332 peak for \13\C12 2,3,7,8-TCDD or the m/z 328 
peak for \37\Cl4 2,3,7,8-TCDD.
    12.8 Co-eluting impurities are suspected if all criteria are 
achieved except those in Section 12.6.3. In this case, another SIM 
analysis using masses at m/z 257, 259, 320 and either m/a 328 or m/z 322 
can be performed. The masses at m/z 257 and m/z 259 are indicative of 
the loss of one chlorine and one carbonyl group from 2,3,7,8-TCDD. If 
masses m/z 257 and m/z 259 give a chlorine isotope ratio that agrees to 
within 10% of the same cluster in the calibration 
standards, then the presence of TCDD can be confirmed. Co-eluting DDD, 
DDE, and PCB residues can be confirmed, but will require another 
injection using the appropriate SIM masses or full repetitive mass 
scans. If the response for \37\Cl4 2,3,7,8-TCDD at m/z 328 is 
too large, PCB contamination is suspected and can be confirmed by 
examining the response at both m/z 326 and m/z 328. The 
\37\Cl4 2,3,7,8-TCDD internal standard gives negligible 
response at m/z 326. These pesticide residues can be removed using the 
alumina column cleanup procedure.
    12.9 If broad background interference restricts the sensitivity of 
the GC/MS analysis, the analyst should employ additional cleanup 
procedures and reanalyze by GC/MS.
    12.10 In those circumstances where these procedures do not yield a 
definitive conclusion, the use of high resolution mass spectrometry is 
suggested. \5\

                            13. Calculations

    13.1 Calculate the concentration of 2,3,7,8-TCDD in the sample using 
the response factor (RF) determined in Section 7.1.2 and Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.123

                                                              Equation 2

where:
As = SIM response for 2,3,7,8-TCDD at m/z 320.
Ais = SIM response for the internal standard at m/z 328 or 
          332.
Is = Amount of internal standard added to each extract 
          ([micro]g).
Vo = Volume of water extracted (L).

    13.2 For each sample, calculate the percent recovery of the internal 
standard by comparing the area of the m/z peak measured in the sample to 
the area of the same peak in the calibration standard. If the recovery 
is below 50%, the analyst should review all aspects of his analytical 
technique.
    13.3 Report results in [micro]g/L without correction for recovery 
data. All QC data obtained should be reported with the sample results.

                         14. Method Performance

    14.1 The method detection limit (MDL) is defined as the minimum 
concentration of a substance that can be measured and reported with 99% 
confidence that the value is above zero. \1\ The MDL concentration 
listed in Table 1 was obtained using reagent water. \14\ The MDL 
actually achieved in a given analysis will vary depending on instrument 
sensitivity and matrix effects.
    14.2 This method was tested by 11 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations over the range 0.02 to 0.20 [micro]g/L. \15\ 
Single operator precision, overall precision, and method accuracy were 
found to be directly related to the concentration of the parameter and 
essentially independent of the sample matrix. Linear equations to 
describe these relationships are presented in Table 3.

                               References

    1. 40 CFR part 136, appendix B.
    2. ``Determination of TCDD in Industrial and Municipal 
Wastewaters,'' EPA 600/4-82-028, National Technical Information Service, 
PB82-196882, Springfield, Virginia 22161, April 1982.
    3. Buser, H.R., and Rappe, C. ``High Resolution Gas Chromatography 
of the 22 Tetrachlorodibenzo-p-dioxin Isomers,'' Analytical Chemistry, 
52, 2257 (1980).
    4. ASTM Annual Book of Standards, Part 31, D3694-78. ``Standard 
Practices for Preparation of Sample Containers and for Preservation of 
Organic Constituents,'' American Society for Testing and Materials, 
Philadelphia.
    5. Harless, R. L., Oswald, E. O., and Wilkinson, M. K. ``Sample 
Preparation and Gas Chromatography/Mass Spectrometry Determination of 
2,3,7,8-Tetrachlorodibenzo-p-dioxin,'' Analytical Chemistry, 52, 1239 
(1980).
    6. Lamparski, L. L., and Nestrick, T. J. ``Determination of Tetra-, 
Hepta-, and Octachlorodibenzo-p-dioxin Isomers in Particulate Samples at 
Parts per Trillion Levels,'' Analytical Chemistry, 52, 2045 (1980).
    7. Longhorst, M. L., and Shadoff, L. A. ``Determination of Parts-
per-Trillion Concentrations of Tetra-, Hexa-, and Octachlorodibenzo-p-
dioxins in Human Milk,'' Analytical Chemistry, 52, 2037 (1980).
    8. ``Carcinogens--Working with Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    9. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occuptional Safety and Health Administration, OSHA 2206 
(Revised, January 1976).

[[Page 246]]

    10. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    11. Provost, L. P., and Elder, R. S., ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
used in the equation in Section 8.3.3 is two times the value 1.22 
derived in this report.)
    12. ASTM Annual Book of Standards, Part 31, D3370-76, ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    13. ``Methods, 330.4 (Titrimetric, DPD-FAS) and 330.5 
(Spectrophotometric DPD) for Chlorine, Total Residual,'' Methods for 
Chemical Analysis of Water and Wastes, EPA-600/4-79-020, U.S. 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268, March 1979.
    14. Wong, A.S. et al. ``The Determination of 2,3,7,8-TCDD in 
Industrial and Municipal Wastewaters, Method 613, Part 1--Development 
and Detection Limits,'' G. Choudhay, L. Keith, and C. Ruppe, ed., 
Butterworth Inc., (1983).
    15. ``EPA Method Study 26, Method 613: 2,3,7,8-Tetrachlorodibenzo-p-
dioxin,'' EPA 600/4-84-037, National Technical Information Service, 
PB84-188879, Springfield, Virginia 22161, May 1984.

     Table 1--Chromatographic Conditions and Method Detection Limit
------------------------------------------------------------------------
                                                                Method
                                                   Retention   detection
                    Parameter                         time       limit
                                                     (min)    ([micro]g/
                                                                  L)
------------------------------------------------------------------------
2,3,7,8-TCDD.....................................       13.1       0.002
------------------------------------------------------------------------
Column conditions: SP-2330 coated on a 60 m long x 0.25 mm ID glass
  column with hydrogen carrier gas at 40 cm/sec linear velocity,
  splitless injection using tetradecane. Column temperature held
  isothermal at 200 [deg]C for 1 min, then programmed at 8 [deg]C/min to
  250 [deg]C and held. Use of helium carrier gas will approximately
  double the retention time.


                                   Table 2--QC Acceptance Criteria--Method 613
----------------------------------------------------------------------------------------------------------------
                                                                              Limit for
                                                                 Test conc.       s        Range for X    Range
                           Parameter                             ([micro]g/  ([micro]g/   ([micro]g/L)    for P,
                                                                     L)          L)                       Ps (%)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD...................................................      0.100      0.0276    0.0523-0.1226   45-129
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements, in [micro]g/L (Section 8.2.4).
X = Average recovery for four recovery measurements, in [micro]g/L (Section 8.2.4).
P, Ps = Percent recovery measured (Section 8.3.2, Section 8.4.2).
 
Note: These criteria are based directly upon the method performance data in Table 3. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 3.


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 613
----------------------------------------------------------------------------------------------------------------
                                                         Accuracy, as       Single analyst,
                      Parameter                          recovery, X''      precision, sr''   Overall precision,
                                                         ([micro]g/L)         ([micro]/L)      S'' ([micro]/g/L)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD........................................     0.86C + 0.00145     0.13X + 0.00129     0.19X + 0.00028
----------------------------------------------------------------------------------------------------------------
X' = Expected recovery for one or more measurements. of a sample containing a concentration of C, in [micro]g/L.
sr' = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S' = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.

                    Method 624.1--Purgeables by GC/MS

                        1. Scope and Application

    1.1 This method is for determination of purgeable organic pollutants 
in industrial discharges and other environmental samples by gas 
chromatography combined with mass spectrometry (GC/MS), as provided 
under 40 CFR 136.1. This revision is based on previous protocols 
(References 1--3), on the revision promulgated October 26, 1984, and on 
an interlaboratory method validation study (Reference 4). Although this 
method was validated through an interlaboratory study conducted in the 
early 1980s, the fundamental chemistry principles used in this method 
remain sound and continue to apply.
    1.2 The analytes that may be qualitatively and quantitatively 
determined using this method and their CAS Registry numbers are listed 
in Table 1. The method may be extended to determine the analytes listed 
in Table 2; however, poor purging efficiency or gas chromatography of 
some of these analytes may make quantitative determination difficult. 
For example, an elevated temperature may be required to purge some 
analytes from water. If an elevated temperature is used, calibration and 
all quality control (QC) tests must be performed at the elevated 
temperature. EPA encourages the use of this method to determine 
additional compounds amenable to purge-and-trap GC/MS.
    1.3 The large number of analytes in Tables 1 and 2 of this method 
makes testing difficult if all analytes are determined simultaneously. 
Therefore, it is necessary to determine and perform QC tests for 
``analytes of interest'' only. Analytes of interest are those required 
to be determined by a regulatory/control authority or in a permit, or by 
a client. If a list of analytes is not specified, the

[[Page 247]]

analytes in Table 1 must be determined, at a minimum, and QC testing 
must be performed for these analytes. The analytes in Table 1 and some 
of the analytes in Table 2 have been identified as Toxic Pollutants (40 
CFR 401.15), expanded to a list of Priority Pollutants (40 CFR part 423, 
appendix A).
    1.4 Method detection limits (MDLs; Reference 5) for the analytes in 
Table 1 are listed in that table. These MDLs were determined in reagent 
water (Reference 6). Advances in analytical technology, particularly the 
use of capillary (open-tubular) columns, allowed laboratories to 
routinely achieve MDLs for the analytes in this method that are 2-10 
times lower than those in the version promulgated in 1984. The MDL for a 
specific wastewater may differ from those listed, depending on the 
nature of interferences in the sample matrix.
    1.4.1 EPA has promulgated this method at 40 CFR part 136 for use in 
wastewater compliance monitoring under the National Pollutant Discharge 
Elimination System (NPDES). The data reporting practices described in 
section 13.2 are focused on such monitoring needs and may not be 
relevant to other uses of the method.
    1.4.2 This method includes ``reporting limits'' based on EPA's 
``minimum level'' (ML) concept (see the glossary in section 20). Table 1 
contains MDL values and ML values for many of the analytes. The MDL for 
an analyte in a specific wastewater may differ from that listed in Table 
1, depending upon the nature of interferences in the sample matrix.
    1.5 This method is performance-based. It may be modified to improve 
performance (e.g., to overcome interferences or improve the accuracy of 
results) provided all performance requirements are met.
    1.5.1 Examples of allowed method modifications are described at 40 
CFR 136.6. Other examples of allowed modifications specific to this 
method are described in section 8.1.2.
    1.5.2 Any modification beyond those expressly allowed at 40 CFR 
136.6 or in section 8.1.2 of this method shall be considered a major 
modification that is subject to application and approval of an alternate 
test procedure under 40 CFR 136.4 and 136.5.
    1.5.3 For regulatory compliance, any modification must be 
demonstrated to produce results equivalent or superior to results 
produced by this method when applied to relevant wastewaters (section 
8.3).
    1.6 This method is restricted to use by or under the supervision of 
analysts experienced in the operation of a purge-and-trap system and a 
gas chromatograph/mass spectrometer and in the interpretation of mass 
spectra. Each analyst must demonstrate the ability to generate 
acceptable results with this method using the procedure in section 8.2.
    1.7 Terms and units of measure used in this method are given in the 
glossary at the end of the method.

                          2. Summary of Method

    2.1 A gas is bubbled through a measured volume of water in a 
specially-designed purging chamber. The purgeables are efficiently 
transferred from the aqueous phase to the vapor phase. The vapor is 
swept through a sorbent trap where the purgeables are trapped. After 
purging is completed, the trap is heated and backflushed with the gas to 
desorb the purgeables onto a gas chromatographic column. The column is 
temperature programmed to separate the purgeables which are then 
detected with a mass spectrometer.
    2.2 Different sample sizes in the range of 5-25 mL are allowed in 
order to meet differing sensitivity requirements. Calibration and QC 
samples must have the same volume as field samples.

                            3. Interferences

    3.1 Impurities in the purge gas, organic compounds outgassing from 
the plumbing ahead of the trap, and solvent vapors in the laboratory 
account for the majority of contamination problems. The analytical 
system must be demonstrated to be free from contamination under the 
conditions of the analysis by analyzing blanks initially and with each 
analytical batch (samples analyzed on a given 12-hour shift, to a 
maximum of 20 samples), as described in Section 8.5. Fluoropolymer 
tubing, fittings, and thread sealant should be used to avoid 
contamination.
    3.2 Samples can be contaminated by diffusion of volatile organics 
(particularly fluorocarbons and methylene chloride) through the septum 
seal into the sample during shipment and storage. Protect samples from 
sources of volatiles during collection, shipment, and storage. A reagent 
water field blank carried through sampling and analysis can serve as a 
check on such contamination.
    3.3 Contamination by carry-over can occur whenever high level and 
low level samples are analyzed sequentially. To reduce the potential for 
carry-over, the purging device and sample syringe must be rinsed with 
reagent water between sample analyses. Whenever an unusually 
concentrated sample is encountered, it should be followed by an analysis 
of a blank to check for cross contamination. For samples containing 
large amounts of water-soluble materials, suspended solids, high boiling 
compounds or high purgeable levels, it may be necessary to wash the 
purging device with a detergent solution, rinse it with distilled water, 
and then dry it in a 105 [deg]C oven between analyses. The trap and 
other parts of the system are also subject to contamination; therefore, 
frequent bakeout

[[Page 248]]

and purging of the entire system may be required. Screening samples at 
high dilution may prevent introduction of contaminants into the system.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each reagent used in this 
method has not been precisely defined; however, each chemical compound 
should be treated as a potential health hazard. From this viewpoint, 
exposure to these chemicals must be reduced to the lowest possible 
level. The laboratory is responsible for maintaining a current awareness 
file of OSHA regulations regarding the safe handling of the chemicals 
specified in this method. A reference file of safety data sheets (SDSs, 
OSHA, 29 CFR 1910.1200(g)) should also be made available to all 
personnel involved in sample handling and chemical analysis. Additional 
references to laboratory safety are available and have been identified 
(References 7-9) for the information of the analyst.
    4.2. The following analytes covered by this method have been 
tentatively classified as known or suspected human or mammalian 
carcinogens: Benzene; carbon tetrachloride; chloroform; 1,4-
dichlorobenzene; 1,2-dichloroethane; 1,2-dichloropropane; methylene 
chloride; tetrachloroethylene; trichloroethylene; and vinyl chloride. 
Primary standards of these toxic compounds should be prepared in a 
chemical fume hood, and a NIOSH/MESA approved toxic gas respirator 
should be worn when handling high concentrations of these compounds.
    4.3 This method allows the use of hydrogen as a carrier gas in place 
of helium (Section 5.3.1.2). The laboratory should take the necessary 
precautions in dealing with hydrogen, and should limit hydrogen flow at 
the source to prevent buildup of an explosive mixture of hydrogen in 
air.

                       5. Apparatus and Materials

    Note: Brand names, suppliers, and part numbers are cited for 
illustration purposes only. No endorsement is implied. Equivalent 
performance may be achieved using equipment and materials other than 
those specified here. Demonstration of equivalent performance that meets 
the requirements of this method is the responsibility of the laboratory. 
Suppliers for equipment and materials in this method may be found 
through an on-line search.

    5.1 Sampling equipment for discrete sampling.
    5.1.1 Vial--25- or 40-mL capacity, or larger, with screw cap with a 
hole in the center (Fisher 13075 or equivalent). Unless pre-cleaned, 
detergent wash, rinse with tap and reagent water, and dry at 105  5 [deg]C before use.
    5.1.2 Septum--Fluoropolymer-faced silicone (Fisher 12722 or 
equivalent). Unless pre-cleaned, detergent wash, rinse with tap and 
reagent water, and dry at 105  5 [deg]C for one 
hour before use.
    5.2 Purge-and-trap system--The purge-and-trap system consists of 
three separate pieces of equipment: A purging device, trap, and 
desorber. Several complete systems are commercially available with 
autosamplers. Any system that meets the performance requirements in this 
method may be used.
    5.2.1 The purging device should accept 5- to 25-mL samples with a 
water column at least 3 cm deep. The purge gas must pass though the 
water column as finely divided bubbles. The purge gas must be introduced 
no more than 5 mm from the base of the water column. Purge devices of a 
different volume may be used so long as the performance requirements in 
this method are met.
    5.2.2 The trap should be at least 25 cm long and have an inside 
diameter of at least 0.105 in. The trap should be packed to contain the 
following minimum lengths of adsorbents: 1.0 cm of methyl silicone 
coated packing (section 6.3.2), 15 cm of 2,6-diphenylene oxide polymer 
(section 6.3.1), and 8 cm of silica gel (section 6.3.3). A trap with 
different dimensions and packing materials is acceptable so long as the 
performance requirements in this method are met.
    5.2.3 The desorber should be capable of rapidly heating the trap to 
the temperature necessary to desorb the analytes of interest, and of 
maintaining this temperature during desorption. The trap should not be 
heated higher than the maximum temperature recommended by the 
manufacturer.
    5.2.4 The purge-and-trap system may be assembled as a separate unit 
or coupled to a gas chromatograph.
    5.3 GC/MS system.
    5.3.1 Gas chromatograph (GC)--An analytical system complete with a 
temperature programmable gas chromatograph and all required accessories, 
including syringes and analytical columns. Autosamplers designed for 
purge-and-trap analysis of volatiles also may be used.
    5.3.1.1 Injection port--Volatiles interface, split, splitless, 
temperature programmable split/splitless (PTV), large volume, on-column, 
backflushed, or other.
    5.3.1.2 Carrier gas--Data in the tables in this method were obtained 
using helium carrier gas. If another carrier gas is used, analytical 
conditions may need to be adjusted for optimum performance, and 
calibration and all QC tests must be performed with the alternative 
carrier gas. See Section 4.3 for precautions regarding the use of 
hydrogen as a carrier gas.
    5.3.2 GC column--See the footnote to Table 3. Other columns or 
column systems may be used provided all requirements in this method are 
met.

[[Page 249]]

    5.3.3 Mass spectrometer--Capable of repetitively scanning from 35-
260 Daltons (amu) every 2 seconds or less, utilizing a 70 eV (nominal) 
electron energy in the electron impact ionization mode, and producing a 
mass spectrum which meets all criteria in Table 4 when 50 ng or less of 
4-bromofluorobenzene (BFB) is injected through the GC inlet. If 
acrolein, acrylonitrile, chloromethane, and vinyl chloride are to be 
determined, it may be necessary to scan from below 25 Daltons to measure 
the peaks in the 26-35 Dalton range for reliable identification.
    5.3.4 GC/MS interface--Any GC to MS interface that meets all 
performance requirements in this method may be used.
    5.3.5 Data system--A computer system must be interfaced to the mass 
spectrometer that allows continuous acquisition and storage of mass 
spectra throughout the chromatographic program. The computer must have 
software that allows searching any GC/MS data file for specific m/z's 
(masses) and plotting m/z abundances versus time or scan number. This 
type of plot is defined as an extracted ion current profile (EICP). 
Software must also be available that allows integrating the abundance at 
any EICP between specified time or scan number limits.
    5.4 Syringes--Graduated, 5-25 mL, glass hypodermic with Luerlok tip, 
compatible with the purging device.
    5.5 Micro syringes--Graduated, 25-1000 [micro]L, with 0.006 in. ID 
needle.
    5.6 Syringe valve--Two-way, with Luer ends.
    5.7 Syringe--5 mL, gas-tight with shut-off valve.
    5.8 Bottle--15 mL, screw-cap, with Teflon cap liner.
    5.9 Balance--Analytical, capable of accurately weighing 0.0001 g.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as water in which the 
analytes of interest and interfering compounds are not detected at the 
MDLs of the analytes of interest. It may be generated by passing 
deionized water, distilled water, or tap water through a carbon bed, 
passing the water through a water purifier, or heating the water to 
between 90 and 100 [deg]C while bubbling contaminant-free gas through it 
for approximately 1 hour. While still hot, transfer the water to screw-
cap bottles and seal with a fluoropolymer-lined cap.
    6.2 Sodium thiosulfate--(ACS) Granular.
    6.3 Trap materials.
    6.3.1 2,6-Diphenylene oxide polymer--Tenax, 60/80 mesh, 
chromatographic grade, or equivalent.
    6.3.2 Methyl silicone packing--3% OV-1 on Chromosorb-W, 60/80 mesh, 
or equivalent.
    6.3.3 Silica gel--35/60 mesh, Davison, Grade-15 or equivalent.
    6.3.4 Other trap materials are acceptable if performance 
requirements in this method are met.
    6.4 Methanol--Demonstrated to be free from the target analytes and 
potentially interfering compounds.
    6.5 Stock standard solutions--Stock standard solutions may be 
prepared from pure materials, or purchased as certified solutions. 
Traceability must be to the National Institute of Standards and 
Technology (NIST) or other national or international standard, when 
available. Stock solution concentrations alternative to those below may 
be used. Prepare stock standard solutions in methanol using assayed 
liquids or gases as appropriate. Because some of the compounds in this 
method are known to be toxic, primary dilutions should be prepared in a 
hood, and a NIOSH/MESA approved toxic gas respirator should be worn when 
high concentrations of neat materials are handled. The following 
procedure may be used to prepare standards from neat materials:
    6.5.1 Place about 9.8 mL of methanol in a 10-mL ground-glass-
stoppered volumetric flask. Allow the flask to stand, unstoppered, for 
about 10 minutes or until all alcohol wetted surfaces have dried. Weigh 
the flask to the nearest 0.1 mg.
    6.5.2 Add the assayed reference material.
    6.5.2.1 Liquids--Using a 100 [micro]L syringe, immediately add two 
or more drops of assayed reference material to the flask. Be sure that 
the drops fall directly into the alcohol without contacting the neck of 
the flask. Reweigh, dilute to volume, stopper, then mix by inverting the 
flask several times. Calculate the concentration in [micro]g/[micro]L 
from the net gain in weight.
    6.5.2.2 Gases--To prepare standards for any of compounds that boil 
below 30 [deg]C, fill a 5-mL valved gas-tight syringe with reference 
standard vapor to the 5.0 mL mark. Lower the needle to 5 mm above the 
methanol meniscus. Slowly introduce the vapor above the surface of the 
liquid (the vapor will rapidly dissolve in the methanol). Reweigh, 
dilute to volume, stopper, then mix by inverting the flask several 
times. Calculate the concentration in [micro]g/[micro]L from the net 
gain in weight.
    6.5.3 When compound purity is assayed to be 96% or greater, the 
weight may be used without correction to calculate the concentration of 
the stock standard. Commercially prepared stock standards may be used at 
any concentration if they are certified by the manufacturer or by an 
independent source.
    6.5.4 Prepare fresh standards weekly for the gases and 2-
chloroethylvinyl ether. Unless stated otherwise in this method, store 
non-aqueous standards in fluoropolymer-

[[Page 250]]

lined screw-cap, or heat-sealed, glass containers, in the dark at -20 to 
-10 [deg]C. Store aqueous standards; e.g., the aqueous LCS (section 
8.4.1) in the dark at <=6 [deg]C (but do not freeze) with zero 
headspace; e.g., in VOA vials (section 5.1.1). Standards prepared by the 
laboratory may be stored for up to one month, except when comparison 
with QC check standards indicates that a standard has degraded or become 
more concentrated due to evaporation, or unless the laboratory has data 
on file to prove stability for a longer period. Commercially prepared 
standards may be stored until the expiration date provided by the 
vendor, except when comparison with QC check standards indicates that a 
standard has degraded or become more concentrated due to evaporation, or 
unless the laboratory has data from the vendor on file to prove 
stability for a longer period.
    Note: 2-Chloroethylvinyl ether has been shown to be stable for as 
long as one month if prepared as a separate standard, and the other 
analytes have been shown to be stable for as long as 2 months if stored 
at less than -10 [deg]C with minimal headspace in sealed, miniature 
inert-valved vials.
    6.6 Secondary dilution standards--Using stock solutions, prepare 
secondary dilution standards in methanol that contain the compounds of 
interest, either singly or mixed. Secondary dilution standards should be 
prepared at concentrations such that the aqueous calibration standards 
prepared in section 7.3.2 will bracket the working range of the 
analytical system.
    6.7 Surrogate standard spiking solution--Select a minimum of three 
surrogate compounds from Table 5. The surrogates selected should match 
the purging characteristics of the analytes of interest as closely as 
possible. Prepare a stock standard solution for each surrogate in 
methanol as described in section 6.5, and prepare a solution for spiking 
the surrogates into all blanks, LCSs, and MS/MSDs. Prepare the spiking 
solution such that spiking a small volume will result in a constant 
concentration of the surrogates. For example, add 10 [micro]L of a 
spiking solution containing the surrogates at a concentration of 15 
[micro]g/mL in methanol to a 5-mL aliquot of water to produce a 
concentration of 30 [micro]g/L for each surrogate. Other surrogate 
concentrations may be used. Store per section 6.5.4.
    6.8 BFB standard--Prepare a solution of BFB in methanol as described 
in Sections 6.5 and 6.6. The solution should be prepared such that an 
injection or purging from water will result in introduction of <= 50 ng 
into the GC. BFB may be included in a mixture with the internal 
standards and/or surrogates.
    6.9 Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1 Assemble a purge-and-trap system that meets the specifications 
in Section 5.2. Prior to first use, condition the trap overnight at 180 
[deg]C by backflushing with gas at a flow rate of at least 20 mL/min. 
Condition the trap after each analysis at a temperature and time 
sufficient to prevent detectable concentrations of the analytes or 
contaminants in successive analyses.
    7.2 Connect the purge-and-trap system to the gas chromatograph. The 
gas chromatograph should be operated using temperature and flow rate 
conditions equivalent to those given in the footnotes to Table 3. 
Alternative temperature and flow rate conditions may be used provided 
that performance requirements in this method are met.
    7.3 Internal standard calibration.
    7.3.1 Internal standards.
    7.3.1.1 Select three or more internal standards similar in 
chromatographic behavior to the compounds of interest. Suggested 
internal standards are listed in Table 5. Use the base peak m/z as the 
primary m/z for quantification of the standards. If interferences are 
found at the base peak, use one of the next two most intense m/z's for 
quantitation. Demonstrate that measurements of the internal standards 
are not affected by method or matrix interferences.
    7.3.1.2 To assure accurate analyte identification, particularly when 
selected ion monitoring (SIM) is used, it may be advantageous to include 
more internal standards than those suggested in Section 7.3.1.1. An 
analyte will be located most accurately if its retention time relative 
to an internal standard is in the range of 0.8 to 1.2.
    7.3.1.3 Prepare a stock standard solution for each internal standard 
in methanol as described in Section 6.5, and prepare a solution for 
spiking the internal standards into all blanks, LCSs, and MS/MSDs. 
Prepare the spiking solution such that spiking a small volume will 
result in a constant concentration of the internal standards. For 
example, add 10 [micro]L of a spiking solution containing the internal 
standards at a concentration of 15 [micro]g/mL in methanol to a 5-mL 
aliquot of water to produce a concentration of 30 [micro]g/L for each 
internal standard. Other concentrations may be used. The internal 
standard solution and the surrogate standard spiking solution (Section 
6.7) may be combined, if desired. Store per section 6.5.4.
    7.3.2 Calibration.
    7.3.2.1 Calibration standards.
    7.3.2.1.1 Prepare calibration standards at a minimum of five 
concentration levels for each analyte of interest by adding appropriate 
volumes of one or more stock standards to a fixed volume (e.g., 40 mL) 
of reagent water in volumetric glassware. Fewer levels may be necessary 
for some analytes based on the sensitivity of the MS, but no

[[Page 251]]

fewer than 3 levels may be used, and only the highest or lowest point(s) 
may be dropped from the calibration. One of the calibration standards 
should be at a concentration at or below the ML or as specified by a 
regulatory/control authority or in a permit. The ML value may be rounded 
to a whole number that is more convenient for preparing the standard, 
but must not exceed the ML values listed in Table 1 for those analytes 
which list ML values. Alternatively, the laboratory may establish the ML 
for each analyte based on the concentration of the lowest calibration 
standard in a series of standards produced in the laboratory or obtained 
from a commercial vendor, again, provided that the ML value does not 
exceed the MLs in Table 1, and provided that the resulting calibration 
meets the acceptance criteria in Section 7.3.4, based on the RSD, RSE, 
or R\2\. The concentrations of the higher standards should correspond to 
the expected range of concentrations found in real samples, or should 
define the working range of the GC/MS system for full-scan and/or SIM 
operation, as appropriate. A minimum of six concentration levels is 
required for a second order, non-linear (e.g., quadratic; ax\2\ + bx + c 
= 0) calibration. Calibrations higher than second order are not allowed.
    7.3.2.1.2 To each calibration standard or standard mixture, add a 
known constant volume of the internal standard spiking solution (section 
7.3.1.3) and surrogate standard spiking solution (section 6.7) or the 
combined internal standard solution and surrogate spiking solution 
(section 7.3.1.3). Aqueous standards may be stored up to 24 hours, if 
held in sealed vials with zero headspace. If not so stored, they must be 
discarded after one hour.
    7.3.2.2 Prior to analysis of the calibration standards, analyze the 
BFB standard (section 6.8) and adjust the scan rate of the MS to produce 
a minimum of 5 mass spectra across the BFB GC peak, but do not exceed 2 
seconds per scan. Adjust instrument conditions until the BFB criteria in 
Table 4 are met. Once the scan conditions are established, they must be 
used for analyses of all standards, blanks, and samples.

    Note: The BFB spectrum may be evaluated by summing the intensities 
of the m/z's across the GC peak, subtracting the background at each m/z 
in a region of the chromatogram within 20 scans of but not including any 
part of the BFB peak. The BFB spectrum may also be evaluated by fitting 
a Gaussian to each m/z and using the intensity at the maximum for each 
Gaussian, or by integrating the area at each m/z and using the 
integrated areas. Other means may be used for evaluation of the BFB 
spectrum so long as the spectrum is not distorted to meet the criteria 
in Table 4.
    7.3.2.3 Analyze the mid-point standard and enter or review the 
retention time, relative retention time, mass spectrum, and quantitation 
m/z in the data system for each analyte of interest, surrogate, and 
internal standard. If additional analytes (Table 2) are to be 
quantified, include these analytes in the standard. The mass spectrum 
for each analyte must be comprised of a minimum of 2 m/z's; 3 to 5 m/z's 
assure more reliable analyte identification. Suggested quantitation m/
z's are shown in Table 6 as the primary m/z. For analytes in Table 6 
that do not have a secondary m/z, acquire a mass spectrum and enter one 
or more secondary m/z's for more reliable identification. If an 
interference occurs at the primary m/z, use one of the secondary m/z's 
or an alternative m/z. A single m/z only is required for quantitation.
    7.3.2.4 For SIM operation, determine the analytes in each 
descriptor, the quantitation m/z for each analyte (the quantitation m/z 
can be the same as for full-scan operation; Section 7.3.2.3), the dwell 
time on each m/z for each analyte, and the beginning and ending 
retention time for each descriptor. Analyze the verification standard in 
scan mode to verify m/z's and establish retention times for the 
analytes. There must be a minimum of two m/z's for each analyte to 
assure analyte identification. To maintain sensitivity, the number of m/
z's in a descriptor should be limited. For example, for a descriptor 
with 10 m/z's and a chromatographic peak width of 5 sec, a dwell time of 
100 ms at each m/z would result in a scan time of 1 second and provide 5 
scans across the GC peak. The quantitation m/z will usually be the most 
intense peak in the mass spectrum. The quantitation m/z and dwell time 
may be optimized for each analyte. The acquisition table used for SIM 
must take into account the mass defect (usually less than 0.2 Dalton) 
that can occur at each m/z monitored. Refer to the footnotes to Table 3 
for establishing operating conditions and to section 7.3.2.2 for 
establishing scan conditions.
    7.3.2.5 For combined scan and SIM operation, set up the scan 
segments and descriptors to meet requirements in sections 7.3.2.2-
7.3.2.4. Analyze unfamiliar samples in the scan mode to assure that the 
analytes of interest are determined.
    7.3.3 Analyze each calibration standard according to Section 10 and 
tabulate the area at the quantitation m/z against concentration for each 
analyte of interest, surrogate, and internal standard. Calculate the 
response factor (RF) for each compound at each concentration using 
Equation 1.

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[GRAPHIC] [TIFF OMITTED] TR28AU17.012

Where:

As = Area of the characteristic m/z for the analyte to be 
          measured.
Ais = Area of the characteristic m/z for the internal 
          standard.
Cis = Concentration of the internal standard ([micro]g/L).
Cs = Concentration of the analyte to be measured ([micro]g/
          L).

    7.3.4 Calculate the mean (average) and relative standard deviation 
(RSD) of the response factors. If the RSD is less than 35%, the RF can 
be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to fit a linear or 
quadratic regression of response ratios, As/Ais, 
vs. concentration ratios Cs/Cis. If used, the regression must be 
weighted inversely proportional to concentration (1/C). The coefficient 
of determination (R\2\) of the weighted regression must be greater than 
0.920 (this value roughly corresponds to the RSD limit of 35%). 
Alternatively, the relative standard error (Reference 10) may be used as 
an acceptance criterion. As with the RSD, the RSE must be less than 35%. 
If an RSE less than 35% cannot be achieved for a quadratic regression, 
system performance is unacceptable, and the system must be adjusted and 
re-calibrated.
    Note: Using capillary columns and current instrumentation, it is 
quite likely that a laboratory can calibrate the target analytes in this 
method and achieve a linearity metric (either RSD or RSE) well below 
35%. Therefore, laboratories are permitted to use more stringent 
acceptance criteria for calibration than described here, for example, to 
harmonize their application of this method with those from other 
sources.
    7.4 Calibration verification--Because the analytical system is 
calibrated by purge of the analytes from water, calibration verification 
is performed using the laboratory control sample (LCS). See section 8.4 
for requirements for calibration verification using the LCS, and the 
Glossary for further definition.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability and 
ongoing analysis of spiked samples and blanks to evaluate and document 
data quality (40 CFR 136.7). The laboratory must maintain records to 
document the quality of data generated. Results of ongoing performance 
tests are compared with established QC acceptance criteria to determine 
if the results of analyses meet performance requirements of this method. 
When results of spiked samples do not meet the QC acceptance criteria in 
this method, a quality control check sample (laboratory control sample; 
LCS) must be analyzed to confirm that the measurements were performed in 
an in-control mode of operation. A laboratory may develop its own 
performance criteria (as QC acceptance criteria), provided such criteria 
are as or more restrictive than the criteria in this method.
    8.1.1 The laboratory must make an initial demonstration of 
capability (DOC) to generate acceptable precision and recovery with this 
method. This demonstration is detailed in Section 8.2. On a continuing 
basis, the laboratory must repeat demonstration of capability (DOC) at 
least annually.
    8.1.2 In recognition of advances that are occurring in analytical 
technology, and to overcome matrix interferences, the laboratory is 
permitted certain options (section 1.5 and 40 CFR 136.6(b)) to improve 
separations or lower the costs of measurements. These options may 
include an alternative purge-and-trap device, and changes in both column 
and type of mass spectrometer (see 40 CFR 136.6(b)(4)(xvi)). Alternative 
determinative techniques, such as substitution of spectroscopic or 
immunoassay techniques, and changes that degrade method performance, are 
not allowed. If an analytical technique other than GC/MS is used, that 
technique must have a specificity equal to or greater than the 
specificity of GC/MS for the analytes of interest. The laboratory is 
also encouraged to participate in inter-comparison and performance 
evaluation studies (see section 8.8).
    8.1.2.1 Each time a modification is made to this method, the 
laboratory is required to repeat the procedure in section 8.2. If the 
detection limit of the method will be affected by the change, the 
laboratory must demonstrate that the MDLs (40 CFR part 136, appendix B) 
are lower than one-third the regulatory compliance limit or the MDLs in 
this method, whichever are greater. If calibration will be affected by 
the change, the instrument must be recalibrated per section 7. Once the 
modification is demonstrated to produce results equivalent or superior 
to results produced by this method, that modification may be used 
routinely thereafter, so long as the other requirements in this method 
are met (e.g., matrix spike/matrix spike

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duplicate recovery and relative percent difference).
    8.1.2.1.1 If a modification is to be applied to a specific 
discharge, the laboratory must prepare and analyze matrix spike/matrix 
spike duplicate (MS/MSD) samples (Section 8.3) and LCS samples (section 
8.4). The laboratory must include internal standards and surrogates 
(section 8.7) in each of the samples. The MS/MSD and LCS samples must be 
fortified with the analytes of interest (section 1.3.). If the 
modification is for nationwide use, MS/MSD samples must be prepared from 
a minimum of nine different discharges (See section 8.1.2.1.2), and all 
QC acceptance criteria in this method must be met. This evaluation only 
needs to be performed once, other than for the routine QC required by 
this method (for example it could be performed by the vendor of the 
alternative materials) but any laboratory using that specific material 
must have the results of the study available. This includes a full data 
package with the raw data that will allow an independent reviewer to 
verify each determination and calculation performed by the laboratory 
(see section 8.1.2.2.5, items (a)-(l)).
    8.1.2.1.2 Sample matrices on which MS/MSD tests must be performed 
for nationwide use of an allowed modification:
    (a) Effluent from a publicly owned treatment works (POTW).
    (b) ASTM D5905 Standard Specification for Substitute Wastewater.
    (c) Sewage sludge, if sewage sludge will be in the permit.
    (d) ASTM D1141 Standard Specification for Substitute Ocean Water, if 
ocean water will be in the permit.
    (e) Untreated and treated wastewaters up to a total of nine matrix 
types (see https://www.epa.gov/eg/industrial-effluent-guidelines for a 
list of industrial categories with existing effluent guidelines).
    (i) At least one of the above wastewater matrix types must have at 
least one of the following characteristics:
    (A) Total suspended solids greater than 40 mg/L.
    (B) Total dissolved solids greater than 100 mg/L.
    (C) Oil and grease greater than 20 mg/L.
    (D) NaCl greater than 120 mg/L.
    (E) CaCO3 greater than 140 mg/L.
    (ii) Results of MS/MSD tests must meet QC acceptance criteria in 
section 8.3.
    (f) A proficiency testing (PT) sample from a recognized provider, in 
addition to tests of the nine matrices (section 8.1.2.1.1).
    8.1.2.2 The laboratory is required to maintain records of 
modifications made to this method. These records include the following, 
at a minimum:
    8.1.2.2.1 The names, titles, and business street addresses, 
telephone numbers, and email addresses of the analyst(s) that performed 
the analyses and modification, and of the quality control officer that 
witnessed and will verify the analyses and modifications.
    8.1.2.2.2 A list of analytes, by name and CAS Registry Number.
    8.1.2.2.3 A narrative stating reason(s) for the modifications.
    8.1.2.2.4 Results from all quality control (QC) tests comparing the 
modified method to this method, including:
    (a) Calibration (section 7).
    (b) Calibration verification/LCS (section 8.4).
    (c) Initial demonstration of capability (section 8.2).
    (d) Analysis of blanks (section 8.5).
    (e) Matrix spike/matrix spike duplicate analysis (section 8.3).
    (f) Laboratory control sample analysis (section 8.4).
    8.1.2.2.5 Data that will allow an independent reviewer to validate 
each determination by tracing the instrument output (peak height, area, 
or other signal) to the final result. These data are to include:
    (a) Sample numbers and other identifiers.
    (b) Analysis dates and times.
    (c) Analysis sequence/run chronology.
    (d) Sample volume (Section 10).
    (e) Sample dilution (Section 13.2).
    (f) Instrument and operating conditions.
    (g) Column (dimensions, material, etc).
    (h) Operating conditions (temperature program, flow rate, etc).
    (i) Detector (type, operating conditions, etc).
    (j) Chromatograms, mass spectra, and other recordings of raw data.
    (k) Quantitation reports, data system outputs, and other data to 
link the raw data to the results reported.
    (l) A written Standard Operating Procedure (SOP).
    8.1.2.2.6 Each individual laboratory wishing to use a given 
modification must perform the start-up tests in section 8.1.2 (e.g., 
DOC, MDL), with the modification as an integral part of this method 
prior to applying the modification to specific discharges. Results of 
the DOC must meet the QC acceptance criteria in Table 7 for the analytes 
of interest (section 1.3), and the MDLs must be equal to or lower than 
the MDLs in Table3 for the analytes of interest
    8.1.3 Before analyzing samples, the laboratory must analyze a blank 
to demonstrate that interferences from the analytical system, labware, 
and reagents are under control. Each time a batch of samples is analyzed 
or reagents are changed, a blank must be analyzed as a safeguard against 
laboratory contamination. Requirements for the blank are given in 
section 8.5.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze 
samples to monitor

[[Page 254]]

and evaluate method and laboratory performance on the sample matrix. The 
procedure for spiking and analysis is given in section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
analysis of a quality control check sample (laboratory control sample, 
LCS; on-going precision and recovery sample, OPR) that the measurement 
system is in control. This procedure is given in section 8.4.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is given in 
section 8.8.
    8.1.7 The large number of analytes tested in performance tests in 
this method present a substantial probability that one or more will fail 
acceptance criteria when many analytes are tested simultaneously, and a 
re-test is allowed if this situation should occur. If, however, 
continued re-testing results in further repeated failures, the 
laboratory must document and report the failures (e.g., as qualifiers on 
results), unless the failures are not required to be reported as 
determined by the regulatory/control authority. Results associated with 
a QC failure for an analyte regulated in a discharge cannot be used to 
demonstrate regulatory compliance. QC failures do not relieve a 
discharger or permittee of reporting timely results.
    8.2 Initial demonstration of capability (DOC)--To establish the 
ability to generate acceptable recovery and precision, the laboratory 
must perform the DOC in sections 8.2.1 through 8.2.6 for the analytes of 
interest. The laboratory must also establish MDLs for the analytes of 
interest using the MDL procedure at 40 CFR part 136, appendix B. The 
laboratory's MDLs must be equal to or lower than those listed in Table 1 
for those analytes which list MDL values, or lower than one-third the 
regulatory compliance limit, whichever is greater. For MDLs not listed 
in Table 1, the laboratory must determine the MDLs using the MDL 
procedure at 40 CFR part 136, appendix B under the same conditions used 
to determine the MDLs for the analytes listed in Table 1. All procedures 
used in the analysis must be included in the DOC.
    8.2.1 For the DOC, a QC check sample concentrate (LCS concentrate) 
containing each analyte of interest (section 1.3) is prepared in 
methanol. The QC check sample concentrate must be prepared independently 
from those used for calibration, but may be from the same source as the 
second-source standard used for calibration verification/LCS (sections 
7.4 and 8.4). The concentrate should produce concentrations of the 
analytes of interest in water at the mid-point of the calibration range, 
and may be at the same concentration as the LCS (section 8.4).
    Note: QC check sample concentrates are no longer available from EPA.
    8.2.2 Using a pipet or micro-syringe, prepare four LCSs by adding an 
appropriate volume of the concentrate to each of four aliquots of 
reagent water. The volume of reagent water must be the same as the 
volume that will be used for the sample, blank (section 8.5), and MS/MSD 
(section 8.3). A volume of 5 mL and a concentration of 20 [micro]g/L 
were used to develop the QC acceptance criteria in Table 7. An 
alternative volume and sample concentration may be used, provided that 
all QC tests are performed and all QC acceptance criteria in this method 
are met. Also add an aliquot of the surrogate spiking solution (section 
6.7) and internal standard spiking solution (section 7.3.1.3) to the 
reagent-water aliquots.
    8.2.3 Analyze the four LCSs according to the method beginning in 
section 10.
    8.2.4 Calculate the average percent recovery (X) and the standard 
deviation of the percent recovery (s) for each analyte using the four 
results.
    8.2.5 For each analyte, compare s and X with the corresponding 
acceptance criteria for precision and recovery in Table 7. For analytes 
in Tables 1 and 2 not listed in Table 7, DOC QC acceptance criteria must 
be developed by the laboratory. EPA has provided guidance for 
development of QC acceptance criteria (References 11 and 12). 
Alternatively, acceptance criteria for analytes not listed in Table 7 
may be based on laboratory control charts. If s and X for all analytes 
of interest meet the acceptance criteria, system performance is 
acceptable and analysis of blanks and samples may begin. If any 
individual s exceeds the precision limit or any individual X falls 
outside the range for recovery, system performance is unacceptable for 
that analyte.
    Note: The large number of analytes in Tables 1 and 2 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when many or all analytes are determined 
simultaneously. Therefore, the analyst is permitted to conduct a ``re-
test'' as described in section 8.2.6.
    8.2.6 When one or more of the analytes tested fail at least one of 
the acceptance criteria, repeat the test for only the analytes that 
failed. If results for these analytes pass, system performance is 
acceptable and analysis of samples and blanks may proceed. If one or 
more of the analytes again fail, system performance is unacceptable for 
the analytes that failed the acceptance criteria. Correct the problem 
and repeat the test (section 8.2). See section 8.1.7 for disposition of 
repeated failures.
    Note: To maintain the validity of the test and re-test, system 
maintenance and/or adjustment is not permitted between this pair of 
tests.
    8.3 Matrix spike and matrix spike duplicate (MS/MSD)--The purpose of 
the MS/MSD

[[Page 255]]

requirement is to provide data that demonstrate the effectiveness of the 
method as applied to the samples in question by a given laboratory, and 
both the data user (discharger, permittee, regulated entity, regulatory/
control authority, customer, other) and the laboratory share 
responsibility for provision of such data. The data user should identify 
the sample and the analytes of interest (section 1.3) to be spiked and 
provide sufficient sample volume to perform MS/MSD analyses. The 
laboratory must, on an ongoing basis, spike at least 5% of the samples 
in duplicate from each discharge being monitored to assess accuracy 
(recovery and precision). If direction cannot be obtained from the data 
user, the laboratory must spike at least one sample in duplicate per 
extraction batch of up to 20 samples with the analytes in Table 1. 
Spiked sample results should be reported only to the data user whose 
sample was spiked, or as requested or required by a regulatory/control 
authority, or in a permit.
    8.3.1 If, as in compliance monitoring, the concentration of a 
specific analyte will be checked against a regulatory concentration 
limit, the concentration of the spike should be at that limit; 
otherwise, the concentration of the spike should be one to five times 
higher than the background concentration determined in section 8.3.2, at 
or near the mid-point of the calibration range, or at the concentration 
in the LCS (section 8.4) whichever concentration would be larger.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of the each analyte of interest. If necessary, prepare 
a new check sample concentrate (section 8.2.1) appropriate for the 
background concentration. Spike and analyze two additional sample 
aliquots, and determine the concentration after spiking (A1 
and A2) of each analyte. Calculate the percent recoveries 
(P1 and P2) as 100 (A1-B)/T and 100 
(A2-B)/T, where T is the known true value of the spike. Also 
calculate the relative percent difference (RPD) between the 
concentrations (A1 and A2) as 200 
A1-A2/(A1 + 
A2). If necessary, adjust the concentrations used to 
calculate the RPD to account for differences in the volumes of the 
spiked aliquots.
    8.3.3 Compare the percent recoveries (P1 and 
P2) and the RPD for each analyte in the MS/MSD aliquots with 
the corresponding QC acceptance criteria in Table 7. A laboratory may 
develop and apply QC acceptance criteria more restrictive than the 
criteria in Table 7, if desired.
    8.3.3.1 If any individual P falls outside the designated range for 
recovery in either aliquot, or the RPD limit is exceeded, the result for 
the analyte in the unspiked sample is suspect. See Section 8.1.7 for 
disposition of failures.
    8.3.3.2 The acceptance criteria in Table 7 were calculated to 
include an allowance for error in measurement of both the background and 
spike concentrations, assuming a spike to background ratio of 5:1. This 
error will be accounted for to the extent that the spike to background 
ratio approaches 5:1 (Reference 13) and is applied to spike 
concentrations of 20 [micro]g/L and higher. If spiking is performed at a 
concentration lower than 20 [micro]g/L, the laboratory must use the QC 
acceptance criteria in Table 7, the optional QC acceptance criteria 
calculated for the specific spike concentration in Table 8, or optional 
in-house criteria (Section 8.3.4). To use the acceptance criteria in 
Table 8: (1) Calculate recovery (X') using the equation in Table 8, 
substituting the spike concentration (T) for C; (2) Calculate overall 
precision (S') using the equation in Table 8, substituting X' for X; (3) 
Calculate the range for recovery at the spike concentration as (100 X'/
T)  2.44(100 S'/T)% (Reference 4). For analytes of 
interest in Tables 1 and 2 not listed in Table 7, QC acceptance criteria 
must be developed by the laboratory. EPA has provided guidance for 
development of QC acceptance criteria (References 11 and 12). 
Alternatively, acceptance criteria may be based on laboratory control 
charts. In-house LCS QC acceptance criteria must be updated at least 
every two years.
    8.3.4 After analysis of a minimum of 20 MS/MSD samples for each 
target analyte and surrogate, and if the laboratory chooses to develop 
and apply in-house QC limits, the laboratory should calculate and apply 
in-house QC limits for recovery and RPD of future MS/MSD samples 
(section 8.3). The QC limits for recovery are calculated as the mean 
observed recovery  3 standard deviations, and the 
upper QC limit for RPD is calculated as the mean RPD plus 3 standard 
deviations of the RPDs. The in-house QC limits must be updated at least 
every two years and re-established after any major change in the 
analytical instrumentation or process. If in-house QC limits are 
developed, at least 80% of the analytes tested in the MS/MSD must have 
in-house QC acceptance criteria that are tighter than those in Table 7 
and the remaining analytes (those other than the analytes included in 
the 80%) must meet the acceptance criteria in Table 7. If an in-house QC 
limit for the RPD is greater than the limit in Table 7, then the limit 
in Table 7 must be used. Similarly, if an in-house lower limit for 
recovery is below the lower limit in Table 7, then the lower limit in 
Table 7 must be used, and if an in-house upper limit for recovery is 
above the upper limit in Table 7, then the upper limit in Table 7 must 
be used.
    8.4 Calibration verification/laboratory control sample (LCS)--The 
working calibration curve or RF must be verified immediately after 
calibration and at the beginning of each 12-hour shift by the 
measurement of an LCS. The LCS must be from a source different from the 
source used for

[[Page 256]]

calibration (section 7.3.2.1), but may be the same as the sample 
prepared for the DOC (section 8.2.1).
    Note: The 12-hour shift begins after analysis of BFB, the LCS, and 
the blank, and ends 12 hours later. BFB, the LCS, and blank are outside 
of the 12-hour shift (Section 11.4). The MS and MSD are treated as 
samples and are analyzed within the 12-hour shift.
    8.4.1 Prepare the LCS by adding QC check sample concentrate (section 
8.2.1) to reagent water. Include all analytes of interest (Section 1.3) 
in the LCS. The volume of reagent water must be the same as the volume 
used for the sample, blank (Section 8.5), and MS/MSD (section 8.3). Also 
add an aliquot of the surrogate solution (Section 6.7) and internal 
standard solution (section 7.3.1.3). The concentration of the analytes 
in reagent water should be the same as the concentration in the DOC 
(section 8.2.2).
    8.4.2 Analyze the LCS prior to analysis of field samples in the 
batch of samples analyzed during the 12-hour shift (see the Note at 
section 8.4). Determine the concentration (A) of each analyte. Calculate 
the percent recovery (Q) as 100 (A/T) %, where T is the true value of 
the concentration in the LCS.
    8.4.3 Compare the percent recovery (Q) for each analyte with its 
corresponding QC acceptance criterion in Table 7. For analytes of 
interest in Tables 1 and 2 not listed in Table 7, use the QC acceptance 
criteria developed for the LCS (section 8.4.5). If the recoveries for 
all analytes of interest fall within their respective QC acceptance 
criteria, analysis of blanks and field samples may proceed. If any 
individual Q falls outside the range, proceed according to section 
8.4.4.
    Note: The large number of analytes in Tables 1--2 present a 
substantial probability that one or more will fail the acceptance 
criteria when all analytes are tested simultaneously. Because a re-test 
is allowed in event of failure (sections 8.1.7 and 8.4.3), it may be 
prudent to analyze two LCSs together and evaluate results of the second 
analysis against the QC acceptance criteria only if an analyte fails the 
first test.
    8.4.4 Repeat the test only for those analytes that failed to meet 
the acceptance criteria (Q). If these analytes now pass, system 
performance is acceptable and analysis of blanks and samples may 
proceed. Repeated failure, however, will confirm a general problem with 
the measurement system. If this occurs, repeat the test (section 8.4.2). 
using a fresh LCS (section 8.2.2) or an LCS prepared with a fresh QC 
check sample concentrate (section 8.2.1), or perform and document system 
repair. Subsequent to repair, repeat the calibration verification/LCS 
test (section 8.4). If the acceptance criteria for Q cannot be met, re-
calibrate the instrument (section 7). See section 8.1.7 for disposition 
of repeated failures.
    Note: To maintain the validity of the test and re-test, system 
maintenance and/or adjustment is not permitted between the pair of 
tests.
    8.4.5 After analysis of 20 LCS samples, and if the laboratory 
chooses to develop and apply in-house QC limits, the laboratory should 
calculate and apply in-house QC limits for recovery to future LCS 
samples (section 8.4). Limits for recovery in the LCS calculated as the 
mean recovery 3 standard deviations. A minimum of 
80% of the analytes tested for in the LCS must have QC acceptance 
criteria tighter than those in Table 7, and the remaining analytes 
(those other than the analytes included in the 80%) must meet the 
acceptance criteria in Table 7. If an in-house lower limit for recovery 
is lower than the lower limit in Table 7, the lower limit in Table 7 
must be used, and if an in-house upper limit for recovery is higher than 
the upper limit in Table 7, the upper limit in Table 7 must be used. 
Many of the analytes and surrogates do not have acceptance criteria. The 
laboratory should use 60-140% as interim acceptance criteria for 
recoveries of spiked analytes that do not have recovery limits specified 
in Table 7, and least 80% of the analytes should meet the 60-140% 
interim criteria until in-house LCS limits are developed. Alternatively, 
acceptance criteria for analytes that do not have recovery limits in 
Table 7 may be based on laboratory control charts. In-house QC 
acceptance criteria must be updated at least every two years.
    8.5 Blank--A blank must be analyzed prior to each 12-hour shift to 
demonstrate freedom from contamination. A blank must also be analyzed 
after a sample containing a high concentration of an analyte or 
potentially interfering compound to demonstrate freedom from carry-over.
    8.5.1 Spike the internal standards and surrogates into the blank. 
Analyze the blank immediately after analysis of the LCS (Section 8.4) 
and prior to analysis of the MS/MSD and samples to demonstrate freedom 
from contamination.
    8.5.2 If any analyte of interest is found in the blank: At a 
concentration greater than the MDL for the analyte, at a concentration 
greater than one-third the regulatory compliance limit, or at a 
concentration greater than one-tenth the concentration in a sample 
analyzed during the 12-hour shift (section 8.4), whichever is greater; 
analysis of samples must be halted and samples affected by the blank 
must be re-analyzed. If, however, continued re-testing results in 
repeated blank contamination, the laboratory must document and report 
the failures (e.g., as qualifiers on results), unless the failures are 
not required to be reported as determined by the regulatory/control 
authority. Results associated with blank contamination for an analyte 
regulated in a discharge cannot be used to demonstrate regulatory 
compliance.

[[Page 257]]

QC failures do not relieve a discharger or permittee of reporting timely 
results.
    8.6 Surrogate recoveries--The laboratory must evaluate surrogate 
recovery data in each sample against its in-house surrogate recovery 
limits for surrogates that do not have acceptance criteria in Table 7. 
The laboratory may use 60-140% as interim acceptance criteria for 
recoveries for surrogates not listed in Table 5. At least 80% of the 
surrogates must meet the 60-140% interim criteria until in-house limits 
are developed. Alternatively, surrogate recovery limits may be developed 
from laboratory control charts.
    8.6.1 Spike the surrogates into all samples, blanks, LCSs, and MS/
MSDs. Compare surrogate recoveries against the QC acceptance criteria in 
Table 7. For surrogates in Table 5 without QC acceptance criteria in 
Table 7, and for other surrogates that may be used by the laboratory, 
limits must be developed by the laboratory. EPA has provided guidance 
for development of QC acceptance criteria (References 11 and 12). 
Alternatively, surrogate recovery limits may be developed from 
laboratory control charts. In-house QC acceptance criteria must be 
updated at least every two years.
    8.6.2 If any recovery fails its criteria, attempt to find and 
correct the cause of the failure. See section 8.1.7 for disposition of 
failures.
    8.7 Internal standard responses.
    8.7.1 Calibration verification/LCS--The responses (GC peak heights 
or areas) of the internal standards in the calibration verification/LCS 
must be within 50% to 200% (1/2 to 2x) of their respective responses in 
the mid-point calibration standard. If they are not, repeat the LCS test 
using a fresh QC check sample (section 8.4.1) or perform and document 
system repair. Subsequent to repair, repeat the calibration 
verification/LCS test (section 8.4). If the responses are still not 
within 50% to 200%, re-calibrate the instrument (section 7) and repeat 
the calibration verification/LCS test.
    8.7.2 Samples, blanks, and MS/MSDs--The responses (GC peak heights 
or areas) of each internal standard in each sample, blank, and MS/MSD 
must be within 50% to 200% (1/2 to 2x) of its respective response in the 
mid-point calibration standard. If, as a group, all internal standards 
are not within this range, perform and document system repair, repeat 
the calibration verification/LCS test (section 8.4), and re-analyze the 
affected samples. If a single internal standard is not within the 50% to 
200% range, use an alternative internal standard for quantitation of the 
analyte referenced to the affected internal standard. It may be 
necessary to use the data system to calculate a new response factor from 
calibration data for the alternative internal standard/analyte pair. If 
an internal standard fails the 50-200% criteria and no analytes are 
detected in the sample, ignore the failure or report it if required by 
the regulatory/control authority.
    8.8 As part of the QC program for the laboratory, control charts or 
statements of accuracy for wastewater samples must be assessed and 
records maintained periodically (see 40 CFR 136.7(c)(1)(viii)). After 
analysis of five or more spiked wastewater samples as in section 8.3, 
calculate the average percent recovery (PX) and the standard 
deviation of the percent recovery (sp). Express the accuracy assessment 
as a percent interval from PX-2sp to PX 
+ 2sp. For example, if PX = 90% and sp = 10%, the 
accuracy interval is expressed as 70-110%. Update the accuracy 
assessment for each analyte on a regular basis (e.g., after each 5-10 
new accuracy measurements). If desired, statements of accuracy for 
laboratory performance, independent of performance on samples, may be 
developed using LCSs.
    8.9 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of environmental measurements. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Collect the sample as a grab sample in a glass container having 
a total volume of at least 25 mL. Fill the sample bottle just to 
overflowing in such a manner that no air bubbles pass through the sample 
as the bottle is being filled. Seal the bottle so that no air bubbles 
are entrapped in it. If needed, collect additional sample(s) for the MS/
MSD (section 8.3).
    9.2 Ice or refrigerate samples at <=6 [deg]C from the time of 
collection until analysis, but do not freeze. If residual chlorine is 
present, add sodium thiosulfate preservative (10 mg/40 mL is sufficient 
for up to 5 ppm Cl2) to the empty sample bottle just prior to 
shipping to the sampling site. Any method suitable for field use may be 
employed to test for residual chlorine (Reference 14). Field test kits 
are also available for this purpose. If sodium thiosulfate interferes in 
the determination of the analytes, an alternative preservative (e.g., 
ascorbic acid or sodium sulfite) may be used. If preservative has been 
added, shake the sample vigorously for one minute. Maintain the hermetic 
seal on the sample bottle until time of analysis.
    9.3 If acrolein is to be determined, analyze the sample within 3 
days. To extend the holding time to 14 days, acidify a separate sample 
to pH 4-5 with HCl using the procedure in section 9.7.
    9.4 Experimental evidence indicates that some aromatic compounds, 
notably benzene,

[[Page 258]]

toluene, and ethyl benzene are susceptible to rapid biological 
degradation under certain environmental conditions (Reference 3). 
Refrigeration alone may not be adequate to preserve these compounds in 
wastewaters for more than seven days. To extend the holding time for 
aromatic compounds to 14 days, acidify the sample to approximately pH 2 
using the procedure in section 9.7.
    9.5 If halocarbons are to be determined, either use the acidified 
aromatics sample in section 9.4 or acidify a separate sample to a pH of 
about 2 using the procedure in section 9.7.
    9.6 The ethers listed in Table 2 are prone to hydrolysis at pH 2 
when a heated purge is used. Aqueous samples should not be acid 
preserved if these ethers are of interest, or if the alcohols they would 
form upon hydrolysis are of interest and the ethers are anticipated to 
present.
    9.7 Sample acidification--Collect about 500 mL of sample in a clean 
container and adjust the pH of the sample to 4-5 for acrolein (section 
9.3), or to about 2 for the aromatic compounds (section 9.4) by adding 
1+1 HCl while swirling or stirring. Check the pH with narrow range pH 
paper. Fill a sample container as described in section 9.1. 
Alternatively, fill a precleaned vial (section 5.1.1) that contains 
approximately 0.25 mL of 1+1 HCl with sample as in section 9.1. If 
preserved using this alternative procedure, the pH of the sample can be 
verified to be <2 after some of the sample is removed for analysis. 
Acidification will destroy 2-chloroethylvinyl ether; therefore, 
determine 2-chloroethylvinyl ether from the unacidified sample.
    9.8 All samples must be analyzed within 14 days of collection 
(Reference 3), unless specified otherwise in sections 9.3-9.7.

                10. Sample Purging and Gas Chromatography

    10.1 The footnote to Table 3 gives the suggested GC column and 
operating conditions MDLs and MLs for many of the analytes are given in 
Table 1. Retention times for many of the analytes are given in Table 3. 
Sections 10.2 through 10.7 suggest procedures that may be used with a 
manual purge-and-trap system. Auto-samplers and other columns or 
chromatographic conditions may be used if requirements in this method 
are met. Prior to performing analyses, and between analyses, it may be 
necessary to bake the purge-and-trap and GC systems (section 3.3).
    10.2 Attach the trap inlet to the purging device, and set the purge-
and-trap system to purge. Open the syringe valve located on the purging 
device sample introduction needle.
    10.3 Allow the sample to come to ambient temperature prior to 
pouring an aliquot into the syringe. Remove the plunger from a syringe 
and attach a closed syringe valve. Open the sample bottle (or standard) 
and carefully pour the sample into the syringe barrel to just short of 
overflowing. Replace the syringe plunger and compress the sample. Open 
the syringe valve and vent any residual air while adjusting the sample 
volume. Since this process of taking an aliquot destroys the validity of 
the sample for future analysis, the analyst should fill a second syringe 
at this time to protect against possible loss of data. Add the surrogate 
spiking solution (section 6.7) and internal standard spiking solution 
(section 7.3.1.3) through the valve bore, then close the valve. The 
surrogate and internal standards may be mixed and added as a single 
spiking solution. Autosamplers designed for purge-and-trap analysis of 
volatiles also may be used.
    10.4 Attach the syringe valve assembly to the syringe valve on the 
purging device. Open the syringe valve and inject the sample into the 
purging chamber.
    10.5 Close both valves and purge the sample at a temperature, flow 
rate, and duration sufficient to purge the less-volatile analytes onto 
the trap, yet short enough to prevent blowing the more-volatile analytes 
through the trap. The temperature, flow rate, and time should be 
determined by test. The same purge temperature, flow rate, and purge 
time must be used for all calibration, QC, and field samples.
    10.6 After the purge, set the purge-and-trap system to the desorb 
mode, and begin the temperature program of the gas chromatograph. 
Introduce the trapped materials to the GC column by rapidly heating the 
trap to the desorb temperature while backflushing the trap with carrier 
gas at the flow rate and for the time necessary to desorb the analytes 
of interest. The optimum temperature, flow rate, and time should be 
determined by test. The same temperature, desorb time, and flow rate 
must be used for all calibration, QC, and field samples. If heating of 
the trap does not result in sharp peaks for the early eluting analytes, 
the GC column may be used as a secondary trap by cooling to an ambient 
or subambient temperature. To avoid carry-over and interferences, 
maintain the trap at the desorb temperature and flow rate until the 
analytes, interfering compounds, and excess water are desorbed. The 
optimum conditions should be determined by test.
    10.7 Start MS data acquisition at the start of the desorb cycle and 
stop data collection when the analytes of interest, potentially 
interfering compounds, and water have eluted (see the footnote to Table 
3 for conditions).
    10.8 Cool the trap to the purge temperature and return the trap to 
the purge mode. When the trap is cool, the next sample can be analyzed.

                          11. Performance Tests

    11.1 At the beginning of each 12-hour shift during which standards 
or samples will be

[[Page 259]]

analyzed, perform the tests in sections 11.2-11.3 to verify system 
performance. Use the instrument operating conditions in the footnotes to 
Table 3 for these performance tests. Alternative conditions may be used 
so as long as all QC requirements are met.
    11.2 BFB--Inject 50 ng of BFB solution directly on the column. 
Alternatively, add BFB to reagent water or an aqueous standard such that 
50 ng or less of BFB will be introduced into the GC. Analyze according 
to section 10. Confirm that all criteria in section 7.3.2.2 and Table 4 
are met. If all criteria are not met, perform system repair, retune the 
mass spectrometer, and repeat the test until all criteria are met.
    11.3 Verify calibration with the LCS (section 8.4) after the 
criteria for BFB are met (Reference 15) and prior to analysis of a blank 
or sample. After verification, analyze a blank (section 8.5) to 
demonstrate freedom from contamination and carry-over at the MDL. Tests 
for BFB, the LCS, and the blank are outside of the 12-hour shift, and 
the 12-hour shift includes samples and matrix spikes and matrix spike 
duplicates (section 8.4). The total time for analysis of BFB, the LCS, 
the blank, and the 12-hour shift must not exceed 14 hours.

                     12. Qualitative Identification

    12.1 Identification is accomplished by comparison of results from 
analysis of a sample or blank with data stored in the GC/MS data system 
(section 7.3.2.3). Identification of an analyte is confirmed per 
sections 12.1.1 through 12.1.4.
    12.1.1 The signals for the quantitation and secondary m/z's stored 
in the data system (section 7.3.2.3) for each analyte of interest must 
be present and must maximize within the same two consecutive scans.
    12.1.2 The retention time for the analyte should be within  10 seconds of the analyte in the LCS run at the 
beginning of the shift (section 8.4).
    Note: Retention time windows other than  10 
seconds may be appropriate depending on the performance of the gas 
chromatograph or observed retention time drifts due to certain types of 
matrix effects. Relative retention time (RRT) may be used as an 
alternative to absolute retention times if retention time drift is a 
concern. RRT is a unitless quantity (see section 20.2), although some 
procedures refer to ``RRT units'' in providing the specification for the 
agreement between the RRT values in the sample and the LCS or other 
standard. When significant retention time drifts are observed, dilutions 
or spiked samples may help the analyst determine the effects of the 
matrix on elution of the target analytes and to assist in qualitative 
identification.
    12.1.3 Either the background corrected EICP areas, or the corrected 
relative intensities of the mass spectral peaks at the GC peak maximum, 
must agree within 50% to 200% (\1/2\ to 2 times) for the quantitation 
and secondary m/z's in the reference mass spectrum stored in the data 
system (section 7.3.2.3), or from a reference library. For example, if a 
peak has an intensity of 20% relative to the base peak, the analyte is 
identified if the intensity of the peak in the sample is in the range of 
10% to 40% of the base peak.
    12.1.4 If the acquired mass spectrum is contaminated, or if 
identification is ambiguous, an experienced spectrometrist (section 1.6) 
must determine the presence or absence of the compound.
    12.2 Structural isomers that produce very similar mass spectra 
should be identified as individual isomers if they have sufficiently 
different gas chromatographic retention times. Sufficient gas 
chromatographic resolution is achieved if the height of the valley 
between two isomer peaks is less than 50% of the average of the two peak 
heights. Otherwise, structural isomers are identified as isomeric pairs. 
The resolution should be verified on the mid-point concentration of the 
initial calibration as well as the laboratory designated continuing 
calibration verification level if closely eluting isomers are to be 
reported.

                            13. Calculations

    13.1 When an analyte has been identified, quantitation of that 
analyte is based on the integrated abundance from the EICP of the 
primary characteristic m/z in Table 5 or 6. Calculate the concentration 
using the response factor (RF) determined in section 7.3.3 and Equation 
2. If a calibration curve was used, calculate the concentration using 
the regression equation for the curve. If the concentration of an 
analyte exceeds the calibration range, dilute the sample by the minimum 
amount to bring the concentration into the calibration range, and re-
analyze. Determine a dilution factor (DF) from the amount of the 
dilution. For example, if the extract is diluted by a factor of 2, DF = 
2.
[GRAPHIC] [TIFF OMITTED] TR28AU17.013


[[Page 260]]


Where:

Cs = Concentration of the analyte in the sample, and the 
          other terms are as defined in Section 7.3.3.

    13.2 Reporting of results
    As noted in section 1.4.1, EPA has promulgated this method at 40 CFR 
part 136 for use in wastewater compliance monitoring under the National 
Pollutant Discharge Elimination System (NPDES). The data reporting 
practices described here are focused on such monitoring needs and may 
not be relevant to other uses of this method.
    13.2.1 Report results for wastewater samples in [micro]g/L without 
correction for recovery. (Other units may be used if required by a 
permit.) Report all QC data with the sample results.
    13.2.2 Reporting level. Unless otherwise specified in by a 
regulatory authority or in a discharge permit, results for analytes that 
meet the identification criteria are reported down to the concentration 
of the ML established by the laboratory through calibration of the 
instrument (see section 7.3.2 and the glossary for the derivation of the 
ML). EPA considers the terms ``reporting limit,'' ``limit of 
quantitation,'' ``quantitation limit,'' and ``minimum level'' to be 
synonymous.
    13.2.2.1 Report a result for each analyte in each field sample or QC 
standard at or above the ML to 3 significant figures. Report a result 
for each analyte found in each field sample or QC standard below the ML 
as ``12, are hazardous and must 
be handled and disposed of as hazardous waste, or neutralized and 
disposed of in accordance with all federal, state, and local 
regulations. It is the laboratory's responsibility to comply with all 
federal, state, and local regulations governing waste management, 
particularly the hazardous waste identification rules and land disposal 
restrictions. The laboratory using this method has the responsibility to 
protect the air, water, and land by minimizing and controlling all 
releases from fume hoods and bench operations. Compliance is also 
required with any sewage discharge permits and regulations. For further 
information on waste management, see ``The Waste Management Manual for 
Laboratory Personnel,'' also available from the American Chemical 
Society at the address in Section 15.3.
    16.3 Many analytes in this method decompose above 500 [deg]C. Low-
level waste such as absorbent paper, tissues, and plastic gloves may be 
burned in an appropriate incinerator. Gross quantities of neat or highly 
concentrated solutions of toxic or hazardous chemicals should be 
packaged securely and disposed of through commercial or governmental 
channels that are capable of handling these types of wastes.
    16.4 For further information on waste management, consult ``Waste 
Management Manual for Laboratory Personnel and Less is Better-Laboratory 
Chemical Management for Waste Reduction,'' available from the American 
Chemical Society's Department of Government Relations and Science 
Policy, 1155 16th Street NW., Washington, DC 20036, 202-872-4477.

                             17. References

    1. Bellar, T.A. and Lichtenberg, J.J. ``Determining Volatile 
Organics at Microgram-per-Litre Levels by Gas Chromatography,'' Journal 
American Water Works Association, 66: 739 (1974).
    2. ``Sampling and Analysis Procedures for Screening of Industrial 
Effluents for Priority Pollutants,'' U.S. Environmental Protection 
Agency, Environmental Monitoring and Support Laboratory, Cincinnati, 
Ohio 45268, March 1977, Revised April 1977.
    3. Bellar, T.A. and Lichtenberg, J.J. ``Semi-Automated Headspace 
Analysis of Drinking Waters and Industrial Waters for Purgeable Volatile 
Organic Compounds,'' Measurement of Organic Pollutants in Water and 
Wastewater, C.E. Van Hall, editor, American Society for Testing and 
Materials, Philadelphia, PA. Special Technical Publication 686, 1978.
    4. ``EPA Method Study 29 EPA Method 624-Purgeables,'' EPA 600/4-84-
054, National Technical Information Service, PB84-209915, Springfield, 
Virginia 22161, June 1984.
    5. 40 CFR part 136, appendix B.
    6. ``Method Detection Limit for Methods 624 and 625,'' Olynyk, P., 
Budde, W.L., and Eichelberger, J.W. Unpublished report, May 14, 1980.
    7. ``Carcinogens-Working With Carcinogens,'' Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, August 1977.
    8. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR 
part 1910), Occupational Safety and Health Administration, OSHA 2206 
(Revised, January 1976).
    9. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety, 7th Edition, 2003.
    10. 40 CFR 136.6(b)(5)(x).
    11. 40 CFR 136.6(b)(2)(i).
    12. Protocol for EPA Approval of New Methods for Organic and 
Inorganic Analytes in Wastewater and Drinking Water (EPA-821-B-98-003) 
March 1999.
    13. Provost, L.P. and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15, 58-63 (1983).
    14. 40 CFR 136.3(a), Table IB, Chlorine--Total residual.
    15. Budde, W.L. and Eichelberger, J.W. ``Performance Tests for the 
Evaluation of Computerized Gas Chromatography/Mass Spectrometry 
Equipment and Laboratories,'' EPA-600/4-80-025, U.S. Environmental 
Protection Agency, Environmental Monitoring and Support Laboratory, 
Cincinnati, Ohio 45268, April 1980.
    16. ``Method Performance Data for Method 624,'' Memorandum from R. 
Slater and T. Pressley, U.S. Environmental Protection Agency, 
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio 45268, 
January 17, 1984.

                               18. Tables

[[Page 262]]



                                             Table 1--Purgeables \1\
----------------------------------------------------------------------------------------------------------------
                                                                   CAS Registry   MDL ([micro]g/   ML ([micro]g/
                             Analyte                                    No.           L) \2\          L) \3\
----------------------------------------------------------------------------------------------------------------
Acrolein........................................................        107-02-8
Acrylonitrile...................................................        107-13-1
Benzene.........................................................         71-43-2             4.4            13.2
Bromodichloromethane............................................         75-27-4             2.2             6.6
Bromoform.......................................................         75-25-2             4.7            14.1
Bromomethane....................................................         74-83-9
Carbon tetrachloride............................................         56-23-5             2.8             8.4
Chlorobenzene...................................................        108-90-7             6.0            18.0
Chloroethane....................................................         75-00-3
2-Chloroethylvinyl ether........................................        110-75-8
Chloroform......................................................         67-66-3             1.6             4.8
Chloromethane...................................................         74-87-3
Dibromochloromethane............................................        124-48-1             3.1             9.3
1,2-Dichlorobenzene.............................................         95-50-1
1,3-Dichlorobenzene.............................................        541-73-1
1,4-Dichlorobenzene.............................................        106-46-7
1,1-Dichloroethane..............................................         75-34-3             4.7            14.1
1,2-Dichloroethane..............................................        107-06-2             2.8             8.4
1,1-Dichloroethene..............................................         75-35-4             2.8             8.4
trans-1,2-Dichloroethene........................................        156-60-5             1.6             4.8
1,2-Dichloropropane.............................................         78-87-5             6.0            18.0
cis-1,3-Dichloropropene.........................................      10061-01-5             5.0            15.0
trans-1,3-Dichloropropene.......................................      10061-02-6
Ethyl benzene...................................................        100-41-4             7.2            21.6
Methylene chloride..............................................         75-09-2             2.8             8.4
1,1,2,2-Tetrachloroethane.......................................         79-34-5             6.9            20.7
Tetrachloroethene...............................................        127-18-4             4.1            12.3
Toluene.........................................................        108-88-3             6.0            18.0
1,1,1-Trichloroethane...........................................         71-55-6             3.8            11.4
1,1,2-Trichloroethane...........................................         79-00-5             5.0            15.0
Trichloroethene.................................................         79-01-6             1.9             5.7
Vinyl chloride..................................................         75-01-4  ..............
----------------------------------------------------------------------------------------------------------------
\1\ All the analytes in this table are Priority Pollutants (40 CFR part 423, appendix A).
\2\ MDL values from the 1984 promulgated version of Method 624.
\3\ ML = Minimum Level--see Glossary for definition and derivation.


                     Table 2--Additional Purgeables
------------------------------------------------------------------------
                         Analyte                           CAS Registry
------------------------------------------------------------------------
Acetone \1\.............................................         67-64-1
Acetonitrile \2\........................................         75-05-8
Acrolein................................................        107-02-8
Acrylonitrile...........................................        107-13-1
Allyl alcohol \1\.......................................        107-18-6
Allyl chloride..........................................        107-05-1
t-Amyl ethyl ether (TAEE)...............................        919-94-8
t-Amyl methyl ether (TAME)..............................         994-058
Benzyl chloride.........................................        100-44-7
Bromoacetone \2\........................................        598-31-2
Bromobenzene............................................        108-86-1
Bromochloromethane......................................         74-97-5
1,3-Butadiene...........................................        106-99-0
n-Butanol \1\...........................................         71-36-3
2-Butanone (MEK) \1 2\..................................         78-93-3
t-Butyl alcohol (TBA)...................................         75-65-0
n-Butylbenzene..........................................        104-51-8
sec-Butylbenzene........................................        135-98-8
t-Butylbenzene..........................................         98-06-6
t-Butyl ethyl ether (ETBE)..............................        637-92-3
Carbon disulfide........................................         75-15-0
Chloral hydrate \2\.....................................        302-17-0
Chloroacetonitrile \1\..................................        107-14-2
1-Chlorobutane..........................................        109-69-3
Chlorodifluoromethane...................................         75-45-6
2-Chloroethanol \2\.....................................        107-07-3
bis (2-Chloroethyl) sulfide \2\.........................        505-60-2
1-Chlorohexanone........................................      20261-68-1
Chloroprene (2-chloro-1,3-butadiene)....................        126-99-8
3-Chloropropene.........................................        107-05-1
3-Chloropropionitrile...................................        542-76-7
2-Chlorotoluene.........................................         95-49-8
4-Chlorotoluene.........................................        106-43-4
Crotonaldehyde \1 2\....................................        123-73-9
Cyclohexanone...........................................        108-94-1
1,2-Dibromo-3-chloropropane.............................         96-12-8
1,2-Dibromoethane.......................................        106-93-4
Dibromomethane..........................................         74-95-3
cis-1,4-Dichloro-2-butene...............................       1476-11-5
trans-1,4-Dichloro-2-butene.............................        110-57-6
cis-1,2-Dichloroethene..................................        156-59-2
Dichlorodifluoromethane.................................         75-71-8
1,3-Dichloropropane.....................................        142-28-9
2,2-Dichloropropane.....................................        590-20-7
1,3-Dichloro-2-propanol \2\.............................         96-23-1
1,1-Dichloropropene.....................................        563-58-6
cis-1,3-Dichloropropene.................................      10061-01-5
1:2,3:4-Diepoxybutane...................................       1464-53-5
Diethyl ether...........................................         60-29-7
Diisopropyl ether (DIPE)................................        108-20-3
1,4-Dioxane \2\.........................................        123-91-1
Epichlorohydrin \2\.....................................        106-89-8
Ethanol \2\.............................................         64-17-5
Ethyl acetate \2\.......................................        141-78-6
Ethyl methacrylate......................................         97-63-2
Ethylene oxide \2\......................................         75-21-8
Hexachlorobutadiene.....................................         87-63-3
Hexachloroethane........................................         67-72-1
2-Hexanone \2\..........................................        591-78-6
Iodomethane.............................................         74-88-4
Isobutyl alcohol \1\....................................         78-83-1
Isopropylbenzene........................................         98-82-8

[[Page 263]]

 
p-Isopropyltoluene......................................         99-87-6
Methacrylonitrile \2\...................................        126-98-7
Methanol \2\............................................         67-56-1
Malonitrile \2\.........................................        109-77-3
Methyl acetate..........................................         79-20-9
Methyl acrylate.........................................         96-33-3
Methyl cyclohexane......................................        108-87-2
Methyl iodide...........................................         74-88-4
Methyl methacrylate.....................................         78-83-1
4-Methyl-2-pentanone (MIBK) \2\.........................        108-10-1
Methyl-t-butyl ether (MTBE).............................       1634-04-4
Naphthalene.............................................         91-20-3
Nitrobenzene............................................         98-95-3
N-Nitroso-di-n-butylamine \2\...........................        924-16-3
2-Nitropropane..........................................         79-46-9
Paraldehyde \2\.........................................        123-63-7
Pentachloroethane \2\...................................         76-01-7
Pentafluorobenzene......................................        363-72-4
2-Pentanone \2\.........................................        107-19-7
2-Picoline \2\..........................................        109-06-8
1-Propanol \1\..........................................         71-23-8
2-Propanol \1\..........................................         67-63-0
Propargyl alcohol \2\...................................        107-19-7
beta-Propiolactone \2\..................................         57-58-8
Propionitrile (ethyl cyanide) \1\.......................        107-12-0
n-Propylamine...........................................        107-10-8
n-Propylbenzene.........................................        103-65-1
Pyridine \2\............................................        110-86-1
Styrene.................................................        100-42-5
1,1,1,2-Tetrachloroethane...............................        630-20-6
Tetrahydrofuran.........................................        109-99-9
o-Toluidine \2\.........................................         95-53-4
1,2,3-Trichlorobenzene..................................         87-61-6
Trichlorofluoromethane..................................         75-69-4
1,2,3-Trichloropropane..................................         96-18-4
1,2,3-Trimethylbenzene..................................        526-73-8
1,2,4-Trimethylbenzene..................................         95-63-6
1,3,5-Trimethylbenzene..................................        108-67-8
Vinyl acetate...........................................        108-05-4
m-Xylene \3\............................................        108-38-3
o-Xylene \3\............................................         95-47-6
p-Xylene \3\............................................        106-42-3
m+o-Xylene \3\..........................................     179601-22-0
m+p-Xylene \3\..........................................     179601-23-1
o+p-Xylene \3\..........................................     136777-61-2
------------------------------------------------------------------------
\1\ Determined at a purge temperature of 80 [deg]C.
\2\ May be detectable at a purge temperature of 80 [deg]C.
\3\ Determined in combination separated by GC column. Most GC columns
  will resolve o-xylene from m+p-xylene. Report using the CAS number for
  the individual xylene or the combination, as determined.


                    Table 3--Example Retention Times
------------------------------------------------------------------------
                                                          Retention time
                         Analyte                               (min)
------------------------------------------------------------------------
Chloromethane...........................................            3.68
Vinyl chloride..........................................            3.92
Bromomethane............................................            4.50
Chloroethane............................................            4.65
Trichlorofluoromethane..................................            5.25
Diethyl ether...........................................            5.88
Acrolein................................................            6.12
1,1-Dichloroethene......................................            6.30
Acetone.................................................            6.40
Iodomethane.............................................            6.58
Carbon disulfide........................................            6.72
3-Chloropropene.........................................            6.98
Methylene chloride......................................            7.22
Acrylonitrile...........................................            7.63
trans-1,2-Dichloroethene................................            7.73
1,1-Dichloroethane......................................            8.45
Vinyl acetate...........................................            8.55
Allyl alcohol...........................................            8.58
2-Chloro-1,3-butadiene..................................            8.65
Methyl ethyl ketone.....................................            9.50
cis-1,2-Dichloroethene..................................            9.50
Ethyl cyanide...........................................            9.57
Methacrylonitrile.......................................            9.83
Chloroform..............................................           10.05
1,1,1-Trichloroethane...................................           10.37
Carbon tetrachloride....................................           10.70
Isobutanol..............................................           10.77
Benzene.................................................           10.98
1,2-Dichloroethane......................................           11.00
Crotonaldehyde..........................................           11.45
Trichloroethene.........................................           12.08
1,2-Dichloropropane.....................................           12.37
Methyl methacrylate.....................................           12.55
p-Dioxane...............................................           12.63
Dibromomethane..........................................           12.65
Bromodichloromethane....................................           12.95
Chloroacetonitrile......................................           13.27
2-Chloroethylvinyl ether................................           13.45
cis-1,3-Dichloropropene.................................           13.65
4-Methyl-2-pentanone....................................           13.83
Toluene.................................................           14.18
trans-1,3-Dichloropropene...............................           14.57
Ethyl methacrylate......................................           14.70
1,1,2-Trichloroethane...................................           14.93
1,3-Dichloropropane.....................................           15.18
Tetrachloroethene.......................................           15.22
2-Hexanone..............................................           15.30
Dibromochloromethane....................................           15.68
1,2-Dibromoethane.......................................           15.90
Chlorobenzene...........................................           16.78
Ethylbenzene............................................           16.82
1,1,1,2-Tetrachloroethane...............................           16.87
m+p-Xylene..............................................           17.08
o-Xylene................................................           17.82
Bromoform...............................................           18.27
Bromofluorobenzene......................................           18.80
1,1,2,2-Tetrachloroethane...............................           18.98
1,2,3-Trichloropropane..................................           19.08
trans-1,4-Dichloro-2-butene.............................           19.12
------------------------------------------------------------------------
Column: 75 m x 0.53 mm ID x 3.0 [micro]m wide-bore DB-624
Conditions: 40 [deg]C for 4 min, 9 [deg]C/min to 200 [deg]C, 20 [deg]C/
  min (or higher) to 250 [deg]C, hold for 20 min at 250 [deg]C to remove
  water.
Carrier gas flow rate: 6-7 mL/min at 40 [deg]C.
Inlet split ratio: 3:1.
Interface split ratio: 7:2.


               Table 4--BFB Key m/z Abundance Criteria \1\
------------------------------------------------------------------------
                    m/z                          Abundance criteria
------------------------------------------------------------------------
50........................................  15-40% of m/z 95.
75........................................  30-60% of m/z 95.
95........................................  Base Peak, 100% Relative
                                             Abundance.
96........................................  5-9% of m/z 95.
173.......................................  <2% of m/z 174.
174.......................................  50% of m/z 95.
175.......................................  5-9% of m/z 174.
176.......................................  95% but <101% of
                                             m/z 174.

[[Page 264]]

 
177.......................................  5-9% of m/z 176.
------------------------------------------------------------------------
\1\ Abundance criteria are for a quadrupole mass spectrometer.
  Alternative tuning criteria from other published EPA reference methods
  may be used, provided method performance is not adversely affected.
  Alternative tuning criteria specified by an instrument manufacturer
  may also be used for another type of mass spectrometer, or for an
  alternative carrier gas, provided method performance is not adversely
  affected.


                               Table 5--Suggested Surrogate and Internal Standards
----------------------------------------------------------------------------------------------------------------
                                                                  Retention time                   Secondary m/
                             Analyte                                 (min) \1\      Primary m/z         z's
----------------------------------------------------------------------------------------------------------------
Benzene-d6......................................................           10.95              84
4-Bromofluorobenzene............................................           18.80              95        174, 176
Bromochloromethane..............................................            9.88             128     49, 130, 51
2-Bromo-1-chloropropane.........................................           14.80              77         79, 156
2-Butanone-d5...................................................            9.33              77
Chloroethane-d5.................................................            4.63              71
Chloroform-\13\C................................................           10.00              86
1,2-Dichlorobenzene-d4..........................................  ..............             152
1,4-Dichlorobutane..............................................           18.57              55          90, 92
1,2-Dichloroethane-d4...........................................           10.88             102
1,1-Dichloroethene-d2...........................................            6.30              65
1,2-Dichloropropane-d6..........................................           12.27              67
trans-1,3-Dichloropropene-d4....................................           14.50              79
1,4-Difluorobenzene.............................................  ..............             114          63, 88
Ethylbenzene-d10................................................           16.77              98
Fluorobenzene...................................................  ..............              96              70
2-Hexanone-d5...................................................           15.30              63
Pentafluorobenzene..............................................  ..............             168
1,1,2,2-Tetrachloroethane-d2....................................           18.93              84
Toluene-d8......................................................           14.13             100
Vinyl chloride-d3...............................................            3.87              65
----------------------------------------------------------------------------------------------------------------
\1\ For chromatographic conditions, see the footnote to Table 3.


          Table 6--Characteristic m/z's for Purgeable Organics
------------------------------------------------------------------------
              Analyte                 Primary m/z      Secondary m/z's
------------------------------------------------------------------------
Acrolein..........................              56  55 and 58.
Acrylonitrile.....................              53  52 and 51.
Chloromethane.....................              50  52.
Bromomethane......................              94  96.
Vinyl chloride....................              62  64.
Chloroethane......................              64  66.
Methylene chloride................              84  49, 51, and 86.
Trichlorofluoromethane............             101  103.
1,1-Dichloroethene................              96  61 and 98.
1,1-Dichloroethane................              63  65, 83, 85, 98, and
                                                     100.
trans-1,2-Dichloroethene..........              96  61 and 98.
Chloroform........................              83  85.
1,2-Dichloroethane................              98  62, 64, and 100.
1,1,1-Trichloroethane.............              97  99, 117, and 119.
Carbon tetrachloride..............             117  119 and 121.
Bromodichloromethane..............              83  127, 85, and 129.
1,2-Dichloropropane...............              63  112, 65, and 114.
trans-1,3-Dichloropropene.........              75  77.
Trichloroethene...................             130  95, 97, and 132.
Benzene...........................              78
Dibromochloromethane..............             127  129, 208, and 206.
1,1,2-Trichloroethane.............              97  83, 85, 99, 132, and
                                                     134.
cis-1,3-Dichloropropene...........              75  77.
2-Chloroethylvinyl ether..........             106  63 and 65.
Bromoform.........................             173  171, 175, 250, 252,
                                                     254, and 256.
1,1,2,2-Tetrachloroethane.........             168  83, 85, 131, 133,
                                                     and 166.
Tetrachloroethene.................             164  129, 131, and 166.
Toluene...........................              92  91.
Chlorobenzene.....................             112  114.

[[Page 265]]

 
Ethyl benzene.....................             106  91.
1,3-Dichlorobenzene...............             146  148 and 111.
1,2-Dichlorobenzene...............             146  148 and 111.
1,4-Dichlorobenzene...............             146  148 and 111.
------------------------------------------------------------------------


                 Table 7--LCS (Q), DOC (s and X), and MS/MSD (P and RPD) Acceptance Criteria \1\
----------------------------------------------------------------------------------------------------------------
                                    Range for Q     Limit for s     Range for X    Range for P1,
             Analyte                    (%)             (%)             (%)           P2 (%)       Limit for RPD
----------------------------------------------------------------------------------------------------------------
Acrolein........................          60-140              30          50-150          40-160              60
Acrylonitrile...................          60-140              30          50-150          40-160              60
Benzene.........................          65-135              33          75-125          37-151              61
Benzene-d6......................  ..............  ..............  ..............
Bromodichloromethane............          65-135              34          50-140          35-155              56
Bromoform.......................          70-130              25          57-156          45-169              42
Bromomethane....................          15-185              90           D-206           D-242              61
2-Butanone-d5...................  ..............  ..............  ..............
Carbon tetrachloride............          70-130              26          65-125          70-140              41
Chlorobenzene...................          65-135              29          82-137          37-160              53
Chloroethane....................          40-160              47          42-202          14-230              78
Chloroethane-d5.................  ..............  ..............  ..............
2-Chloroethylvinyl ether........           D-225             130           D-252           D-305              71
Chloroform......................          70-135              32          68-121          51-138              54
Chloroform-\13\C................  ..............  ..............  ..............
Chloromethane...................           D-205             472           D-230           D-273              60
Dibromochloromethane............          70-135              30          69-133          53-149              50
1,2-Dichlorobenzene.............          65-135              31          59-174          18-190              57
1,2-Dichlorobenzene-d4..........  ..............  ..............  ..............
1,3-Dichlorobenzene.............          70-130              24          75-144          59-156              43
1,4-Dichlorobenzene.............          65-135              31          59-174          18-190              57
1,1-Dichloroethane..............          70-130              24          71-143          59-155              40
1,2-Dichloroethane..............          70-130              29          72-137          49-155              49
1,2-Dichloroethane-d4...........  ..............  ..............  ..............
1,1-Dichloroethene..............          50-150              40          19-212           D-234              32
1,1-Dichloroethene-d2...........  ..............  ..............  ..............
trans-1,2-Dichloroethene........          70-130              27          68-143          54-156              45
1,2-Dichloropropane.............          35-165              69          19-181           D-210              55
1,2-Dichloropropane-d6..........  ..............  ..............  ..............
cis-1,3-Dichloropropene.........          25-175              79           5-195           D-227              58
trans-1,3-Dichloropropene.......          50-150              52          38-162          17-183              86
trans-1,3-Dichloropropene-d4....  ..............  ..............  ..............
Ethyl benzene...................          60-140              34          75-134          37-162              63
2-Hexanone-d5...................  ..............  ..............  ..............
Methylene chloride..............          60-140             192           D-205           D-221              28
1,1,2,2-Tetrachloroethane.......          60-140              36          68-136          46-157              61
1,1,2,2-Tetrachloroethane-d2....  ..............  ..............  ..............
Tetrachloroethene...............          70-130              23          65-133          64-148              39
Toluene.........................          70-130              22          75-134          47-150              41
Toluene-d8......................  ..............  ..............  ..............
1,1,1-Trichloroethane...........          70-130              21          69-151          52-162              36
1,1,2-Trichloroethane...........          70-130              27          75-136          52-150              45
Trichloroethene.................          65-135              29          75-138          70-157              48
Trichlorofluoromethane..........          50-150              50          45-158          17-181              84
Vinyl chloride..................           5-195             100           D-218           D-251              66
Vinyl chloride-d3...............  ..............  ..............  ..............  ..............
----------------------------------------------------------------------------------------------------------------
\1\ Criteria were calculated using an LCS concentration of 20 [micro]g/L.
Q = Percent recovery in calibration verification/LCS (section 8.4).
s = Standard deviation of percent recovery for four recovery measurements (section 8.2.4).
X = Average percent recovery for four recovery measurements (section 8.2.4).
P = Percent recovery for the MS or MSD (section 8.3.3).
D = Detected; result must be greater than zero.
Notes:
1. Criteria for pollutants are based upon the method performance data in Reference 4. Where necessary, limits
  have been broadened to assure applicability to concentrations below those used to develop Table 7.
2. Criteria for surrogates are from EPA CLP SOM01.2D.


[[Page 266]]


                          Table 8--Recovery and Precision as Functions of Concentration
----------------------------------------------------------------------------------------------------------------
                                                                                  Single analyst      Overall
                                                                     Recovery,      precision,      precision,
                             Analyte                                  X[min]          sr[min]         S[min]
                                                                   ([micro]g/L)    ([micro]g/L)    ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Benzene.........................................................      0.93C+2.00    20.26 X-1.74     0.25 X-1.33
Bromodichloromethane............................................      1.03C-1.58     0.15 X+0.59     0.20 X+1.13
Bromoform.......................................................      1.18C-2.35     0.12 X+0.36     0.17 X+1.38
Bromomethane \a\................................................           1.00C          0.43 X          0.58 X
Carbon tetrachloride............................................      1.10C-1.68     0.12 X+0.25     0.11 X+0.37
Chlorobenzene...................................................      0.98C+2.28     0.16 X-0.09     0.26 X-1.92
Chloroethane....................................................      1.18C+0.81     0.14 X+2.78     0.29 X+1.75
2-Chloroethylvinyl ether \a\....................................           1.00C          0.62 X          0.84 X
Chloroform......................................................      0.93C+0.33     0.16 X+0.22     0.18 X+0.16
Chloromethane...................................................      1.03C+0.81     0.37 X+2.14     0.58 X+0.43
Dibromochloromethane............................................      1.01C-0.03     0.17 X-0.18     0.17 X+0.49
1,2-Dichlorobenzene \b\.........................................      0.94C+4.47     0.22 X-1.45     0.30 X-1.20
1,3-Dichlorobenzene.............................................      1.06C+1.68     0.14 X-0.48     0.18 X-0.82
1,4-Dichlorobenzene \b\.........................................      0.94C+4.47     0.22 X-1.45     0.30 X-1.20
1,1-Dichloroethane..............................................      1.05C+0.36     0.13 X-0.05     0.16 X+0.47
1,2-Dichloroethane..............................................      1.02C+0.45     0.17 X-0.32     0.21 X-0.38
1,1-Dichloroethene..............................................      1.12C+0.61     0.17 X+1.06     0.43 X-0.22
trans-1,2,-Dichloroethene.......................................      1.05C+0.03    0.14 X-+0.09    0.19 X-+0.17
1,2-Dichloropropane \a\.........................................           1.00C          0.33 X          0.45 X
cis-1,3-Dichloropropene \a\.....................................           1.00C          0.38 X          0.52 X
trans-1,3-Dichloropropene \a\...................................           1.00C          0.25 X          0.34 X
Ethyl benzene...................................................      0.98C+2.48     0.14 X+1.00     0.26 X-1.72
Methylene chloride..............................................      0.87C+1.88     0.15 X+1.07     0.32 X+4.00
1,1,2,2-Tetrachloroethane.......................................      0.93C+1.76     0.16 X+0.69     0.20 X+0.41
Tetrachloroethene...............................................      1.06C+0.60     0.13 X-0.18     0.16 X-0.45
Toluene.........................................................      0.98C+2.03     0.15 X-0.71     0.22 X-1.71
1,1,1-Trichloroethane...........................................      1.06C+0.73     0.12 X-0.15     0.21 X-0.39
1,1,2-Trichloroethane...........................................      0.95C+1.71     0.14 X+0.02     0.18 X+0.00
Trichloroethene.................................................      1.04C+2.27     0.13 X+0.36     0.12 X+0.59
Trichlorofluoromethane..........................................      0.99C+0.39     0.33 X-1.48     0.34 X-0.39
Vinyl chloride..................................................           1.00C          0.48 X          0.65 X
----------------------------------------------------------------------------------------------------------------
X[min] = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/
  L.
Sr[min] = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S[min] = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.
\a\ Estimates based upon the performance in a single laboratory (References 4 and 16).
\b\ Due to coelutions, performance statements for these isomers are based upon the sums of their concentrations.

                              19. Glossary

    These definitions and purposes are specific to this method, but have 
been conformed to common usage to the extent possible.
    19.1 Units of weight and measure and their abbreviations.
    19.1.1 Symbols.
 [deg]C degrees Celsius
[micro]g microgram
[micro]L microliter
< less than
 greater than
% percent
    19.1.2 Abbreviations (in alphabetical order).
cm centimeter
g gram
h hour
ID inside diameter
in. inch
L liter
m mass
mg milligram
min minute
mL milliliter
mm millimeter
ms millisecond
m/z mass-to-charge ratio
N normal; gram molecular weight of solute divided by hydrogen equivalent 
of solute, per liter of solution
ng nanogram
pg picogram
ppb part-per-billion
ppm part-per-million
ppt part-per-trillion
psig pounds-per-square inch gauge
v/v volume per unit volume
w/v weight per unit volume
    19.2 Definitions and acronyms (in alphabetical order).
    Analyte--A compound tested for by this method. The analytes are 
listed in Tables 1 and 2.
    Analyte of interest--An analyte of interest is an analyte required 
to be determined by a regulatory/control authority or in a permit, or by 
a client.
    Analytical batch--The set of samples analyzed on a given instrument 
during a 12-hour period that begins with analysis of a calibration 
verification/LCS. See section 8.4.

[[Page 267]]

    Blank--An aliquot of reagent water that is treated exactly as a 
sample including exposure to all glassware, equipment, solvents, 
reagents, internal standards, and surrogates that are used with samples. 
The blank is used to determine if analytes or interferences are present 
in the laboratory environment, the reagents, or the apparatus. See 
section 8.5.
    Calibration--The process of determining the relationship between the 
output or response of a measuring instrument and the value of an input 
standard. Historically, EPA has referred to a multi-point calibration as 
the ``initial calibration,'' to differentiate it from a single-point 
calibration verification.
    Calibration standard--A solution prepared from stock solutions and/
or a secondary standards and containing the analytes of interest, 
surrogates, and internal standards. The calibration standard is used to 
calibrate the response of the GC/MS instrument against analyte 
concentration.
    Calibration verification standard--The laboratory control sample 
(LCS) used to verify calibration. See Section 8.4.
    Descriptor--In SIM, the beginning and ending retention times for the 
RT window, the m/z's sampled in the RT window, and the dwell time at 
each m/z.
    Extracted ion current profile (EICP)--The line described by the 
signal at a given m/z.
    Field duplicates--Two samples collected at the same time and place 
under identical conditions, and treated identically throughout field and 
laboratory procedures. Results of analyses of field duplicates provide 
an estimate of the precision associated with sample collection, 
preservation, and storage, as well as with laboratory procedures.
    Field blank--An aliquot of reagent water or other reference matrix 
that is placed in a sample container in the field, and treated as a 
sample in all respects, including exposure to sampling site conditions, 
storage, preservation, and all analytical procedures. The purpose of the 
field blank is to determine if the field or sample transporting 
procedures and environments have contaminated the sample.
    GC--Gas chromatograph or gas chromatography.
    Internal standard--A compound added to a sample in a known amount 
and used as a reference for quantitation of the analytes of interest and 
surrogates. Internal standards are listed in Table 5. Also see Internal 
standard quantitation.
    Internal standard quantitation--A means of determining the 
concentration of an analyte of interest (Tables 1 and 2) by reference to 
a compound added to a sample and not expected to be found in the sample.
    DOC--Initial demonstration of capability (DOC; section 8.2); four 
aliquots of reagent water spiked with the analytes of interest and 
analyzed to establish the ability of the laboratory to generate 
acceptable precision and recovery. A DOC is performed prior to the first 
time this method is used and any time the method or instrumentation is 
modified.
    Laboratory control sample (LCS; laboratory fortified blank (LFB); 
on-going precision and recovery sample; OPR)--An aliquot of reagent 
water spiked with known quantities of the analytes of interest and 
surrogates. The LCS is analyzed exactly like a sample. Its purpose is to 
assure that the results produced by the laboratory remain within the 
limits specified in this method for precision and recovery. In this 
method, the LCS is synonymous with a calibration verification sample 
(See sections 7.4 and 8.4).
    Laboratory fortified sample matrix--See Matrix spike.
    Laboratory reagent blank--See Blank.
    Matrix spike (MS) and matrix spike duplicate (MSD) (laboratory 
fortified sample matrix and duplicate)--Two aliquots of an environmental 
sample to which known quantities of the analytes of interest and 
surrogates are added in the laboratory. The MS/MSD are prepared and 
analyzed exactly like a field sample. Their purpose is to quantify any 
additional bias and imprecision caused by the sample matrix. The 
background concentrations of the analytes in the sample matrix must be 
determined in a separate aliquot and the measured values in the MS/MSD 
corrected for background concentrations.
    May--This action, activity, or procedural step is neither required 
nor prohibited.
    May not--This action, activity, or procedural step is prohibited.
    Method blank (laboratory reagent blank)--See Blank.
    Method detection limit (MDL)--A detection limit determined by the 
procedure at 40 CFR part 136, appendix B. The MDLs determined by EPA in 
the original version of the method are listed in Table 1. As noted in 
Sec. 1.4, use the MDLs in Table 1 in conjunction with current MDL data 
from the laboratory actually analyzing samples to assess the sensitivity 
of this procedure relative to project objectives and regulatory 
requirements (where applicable).
    Minimum level (ML)--The term ``minimum level'' refers to either the 
sample concentration equivalent to the lowest calibration point in a 
method or a multiple of the method detection limit (MDL), whichever is 
higher. Minimum levels may be obtained in several ways: They may be 
published in a method; they may be based on the lowest acceptable 
calibration point used by a laboratory; or they may be calculated by 
multiplying the MDL in a method, or the MDL determined by a laboratory, 
by a factor of 3. For the purposes of NPDES compliance monitoring, EPA 
considers the following terms to

[[Page 268]]

be synonymous: ``quantitation limit,'' ``reporting limit,'' and 
``minimum level.''
    MS--Mass spectrometer or mass spectrometry.
    Must--This action, activity, or procedural step is required.
    m/z--The ratio of the mass of an ion (m) detected in the mass 
spectrometer to the charge (z) of that ion.
    Quality control sample (QCS)--A sample containing analytes of 
interest at known concentrations. The QCS is obtained from a source 
external to the laboratory or is prepared from standards obtained from a 
different source than the calibration standards.
    The purpose is to check laboratory performance using test materials 
that have been prepared independent of the normal preparation process.
    Reagent water--Water demonstrated to be free from the analytes of 
interest and potentially interfering substances at the MDLs for the 
analytes in this method.
    Regulatory compliance limit (or regulatory concentration limit)--A 
limit on the concentration or amount of a pollutant or contaminant 
specified in a nationwide standard, in a permit, or otherwise 
established by a regulatory/control authority.
    Relative retention time (RRT)--The ratio of the retention time of an 
analyte to the retention time of its associated internal standard. RRT 
compensates for small changes in the GC temperature program that can 
affect the absolute retention times of the analyte and internal 
standard. RRT is a unitless quantity.
    Relative standard deviation (RSD)--The standard deviation times 100 
divided by the mean. Also termed ``coefficient of variation.''
    RF--Response factor. See section 7.3.3.
    RSD--See relative standard deviation.
    Safety Data Sheet (SDS)--Written information on a chemical's 
toxicity, health hazards, physical properties, fire, and reactivity, 
including storage, spill, and handling precautions that meet the 
requirements of OSHA, 29 CFR 1910.1200(g) and appendix D to Sec.  
1910.1200. United Nations Globally Harmonized System of Classification 
and Labelling of Chemicals (GHS), third revised edition, United Nations, 
2009.
    Selected Ion Monitoring (SIM)--An MS technique in which a few m/z's 
are monitored. When used with gas chromatography, the m/z's monitored 
are usually changed periodically throughout the chromatographic run to 
correlate with the characteristic m/z's for the analytes, surrogates, 
and internal standards as they elute from the chromatographic column. 
The technique is often used to increase sensitivity and minimize 
interferences.
    Signal-to-noise ratio (S/N)--The height of the signal as measured 
from the mean (average) of the noise to the peak maximum divided by the 
width of the noise.
    SIM--See Selection Ion Monitoring.
    Should--This action, activity, or procedural step is suggested but 
not required.
    Stock solution--A solution containing an analyte that is prepared 
using a reference material traceable to EPA, the National Institute of 
Science and Technology (NIST), or a source that will attest to the 
purity and authenticity of the reference material.
    Surrogate--A compound unlikely to be found in a sample, and which is 
spiked into sample in a known amount before purge-and-trap. The 
surrogate is quantitated with the same procedures used to quantitate the 
analytes of interest. The purpose of the surrogate is to monitor method 
performance with each sample.
    VOA--Volatile organic analysis: e.g., the analysis performed by this 
method.

             Method 625.1--Base/Neutrals and Acids by GC/MS

                        1. Scope and Application

    1.1 This method is for determination of semivolatile organic 
pollutants in industrial discharges and other environmental samples by 
gas chromatography combined with mass spectrometry (GC/MS), as provided 
under 40 CFR 136.1. This revision is based on a previous protocol 
(Reference 1), on the basic revision promulgated October 26, 1984, and 
on an interlaboratory method validation study (Reference 2). Although 
this method was validated through an interlaboratory study conducted in 
the early 1980s, the fundamental chemistry principles used in this 
method remain sound and continue to apply.
    1.2 The analytes that may be qualitatively and quantitatively 
determined using this method and their CAS Registry numbers are listed 
in Tables 1 and 2. The method may be extended to determine the analytes 
listed in Table 3; however, extraction or gas chromatography of some of 
these analytes may make quantitative determination difficult. For 
example, benzidine is subject to oxidative losses during extraction and/
or solvent concentration. Under the alkaline conditions of the 
extraction, alpha-BHC, gamma-BHC, endosulfan I and II, and endrin are 
subject to decomposition. Hexachlorocyclopentadiene is subject to 
thermal decomposition in the inlet of the gas chromatograph, chemical 
reaction in acetone solution, and photochemical decomposition. N-
nitrosodiphenylamine and other nitrosoamines may decompose in the gas 
chromatographic inlet. The sample may be extracted at neutral pH if 
necessary to overcome these or other decomposition problems that could 
occur at alkaline or acidic pH. EPA also has provided other methods 
(e.g., Method 607--Nitrosamines) that may be used for determination of 
some of these analytes.

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EPA encourages use of Method 625.1 to determine additional compounds 
amenable to extraction and GC/MS.
    1.3 The large number of analytes in Tables 1-3 of this method makes 
testing difficult if all analytes are determined simultaneously. 
Therefore, it is necessary to determine and perform quality control (QC) 
tests for the ``analytes of interest'' only. Analytes of interest are 
those required to be determined by a regulatory/control authority or in 
a permit, or by a client. If a list of analytes is not specified, the 
analytes in Tables 1 and 2 must be determined, at a minimum, and QC 
testing must be performed for these analytes. The analytes in Tables 1 
and 2, and some of the analytes in Table 3 have been identified as Toxic 
Pollutants (40 CFR 401.15), expanded to a list of Priority Pollutants 
(40 CFR part 423, appendix A).
    1.4 In this revision to Method 625, the pesticides and 
polychlorinated biphenyls (PCBs) have been moved from Table 1 to Table 3 
(Additional Analytes) to distinguish these analytes from the analytes 
required in quality control tests (Tables 1 and 2). QC acceptance 
criteria for pesticides and PCBs have been retained in Table 6 and may 
continue to be applied if desired, or if requested or required by a 
regulatory/control authority or in a permit. Method 608.3 should be used 
for determination of pesticides and PCBs. However, if pesticides and/or 
PCBs are to be determined, an additional sample must be collected and 
extracted using the pH adjustment and extraction procedures specified in 
Method 608.3. Method 1668C may be useful for determination of PCBs as 
individual chlorinated biphenyl congeners, and Method 1699 may be useful 
for determination of pesticides. At the time of writing of this 
revision, Methods 1668C and 1699 had not been approved for use at 40 CFR 
part 136. The screening procedure for 2,3,7,8-tetrachlorodibenzo-p-
dioxin (2,3,7,8-TCDD) contained in the version of Method 625 promulgated 
October 26, 1984 has been replaced with procedures for selected ion 
monitoring (SIM), and 2,3,7,8-TCDD may be determined using the SIM 
procedures. However, EPA Method 613 or 1613B should be used for analyte-
specific determination of 2,3,7,8-TCDD because of the focus of these 
methods on this compound. Methods 613 and 1613B are approved for use at 
40 CFR part 136.
    1.5 Method detection limits (MDLs; Reference 3) for the analytes in 
Tables 1, 2, and 3 are listed in those tables. These MDLs were 
determined in reagent water (Reference 4). Advances in analytical 
technology, particularly the use of capillary (open-tubular) columns, 
allowed laboratories to routinely achieve MDLs for the analytes in this 
method that are 2-10 times lower than those in the version promulgated 
in 1984. The MDL for an analyte in a specific wastewater may differ from 
those listed, depending upon the nature of interferences in the sample 
matrix.
    1.5.1 EPA has promulgated this method at 40 CFR part 136 for use in 
wastewater compliance monitoring under the National Pollutant Discharge 
Elimination System (NPDES). The data reporting practices described in 
section 15.2 are focused on such monitoring needs and may not be 
relevant to other uses of the method.
    1.5.2 This method includes ``reporting limits'' based on EPA's 
``minimum level'' (ML) concept (see the glossary in section 22). Tables 
1, 2, and 3 contain MDL values and ML values for many of the analytes.
    1.6 This method is performance-based. It may be modified to improve 
performance (e.g., to overcome interferences or improve the accuracy of 
results) provided all performance requirements are met.
    1.6.1 Examples of allowed method modifications are described at 40 
CFR 136.6. Other examples of allowed modifications specific to this 
method, including solid-phase extraction (SPE) are described in section 
8.1.2.
    1.6.2 Any modification beyond those expressly permitted at 40 CFR 
136.6 or in section 8.1.2 of this method shall be considered a major 
modification subject to application and approval of an alternate test 
procedure under 40 CFR 136.4 and 136.5.
    1.6.3 For regulatory compliance, any modification must be 
demonstrated to produce results equivalent or superior to results 
produced by this method when applied to relevant wastewaters (section 
8.3).
    1.7 This method is restricted to use by or under the supervision of 
analysts experienced in the use of a gas chromatograph/mass spectrometer 
and in the interpretation of mass spectra. Each laboratory that uses 
this method must demonstrate the ability to generate acceptable results 
using the procedure in Section 8.2.
    1.8 Terms and units of measure used in this method are given in the 
glossary at the end of the method.

                          2. Summary of Method

    2.1 A measured volume of sample, sufficient to meet an MDL or 
reporting limit, is serially extracted with methylene chloride at pH 11-
13 and again at a pH less than 2 using a separatory funnel or continuous 
liquid/liquid extractor.
    2.2 The extract is concentrated to a volume necessary to meet the 
required compliance or detection limit, and analyzed by GC/MS. 
Qualitative identification of an analyte in the extract is performed 
using the retention time and the relative abundance of two or more 
characteristic masses (m/z's). Quantitative analysis is performed using 
the internal standard technique with a single characteristic m/z.

[[Page 270]]

                   3. Contamination and Interferences

    3.1 Solvents, reagents, glassware, and other sample processing 
labware may yield artifacts, elevated baselines, or matrix interferences 
causing misinterpretation of chromatograms and mass spectra. All 
materials used in the analysis must be demonstrated to be free from 
contamination and interferences by analyzing blanks initially and with 
each extraction batch (samples started through the extraction process in 
a given 24-hour period, to a maximum of 20 samples--see Glossary for 
detailed definition), as described in Section 8.5. Specific selection of 
reagents and purification of solvents by distillation in all-glass 
systems may be required. Where possible, labware is cleaned by 
extraction or solvent rinse, or baking in a kiln or oven.
    3.2 Glassware must be scrupulously cleaned (Reference 5). Clean all 
glassware as soon as possible after use by rinsing with the last solvent 
used in it. Solvent rinsing should be followed by detergent washing with 
hot water, and rinses with tap water and reagent water. The glassware 
should then be drained dry, and heated at 400 [deg]C for 15-30 minutes. 
Some thermally stable materials, such as PCBs, may require higher 
temperatures and longer baking times for removal. Solvent rinses with 
pesticide quality acetone, hexane, or other solvents may be substituted 
for heating. Do not heat volumetric labware above 90 [deg]C. After 
drying and cooling, store inverted or capped with solvent-rinsed or 
baked aluminum foil in a clean environment to prevent accumulation of 
dust or other contaminants.
    3.3 Matrix interferences may be caused by contaminants co-extracted 
from the sample. The extent of matrix interferences will vary 
considerably from source to source, depending upon the nature and 
diversity of the industrial complex or municipality being sampled. 
Interferences extracted from samples high in total organic carbon (TOC) 
may result in elevated baselines, or by enhancing or suppressing a 
signal at or near the retention time of an analyte of interest. Analyses 
of the matrix spike and duplicate (section 8.3) may be useful in 
identifying matrix interferences, and gel permeation chromatography 
(GPC; Section 11.1) and sulfur removal (section 11.2) may aid in 
eliminating these interferences. EPA has provided guidance that may aid 
in overcoming matrix interferences (Reference 6).
    3.4 In samples that contain an inordinate number of interferences, 
the use of chemical ionization (CI) or triple quadrupole (MRM) mass 
spectrometry may make identification easier. Tables 4 and 5 give 
characteristic CI and MRM m/z's for many of the analytes covered by this 
method. The use of CI or MRM mass spectrometry may be utilized to 
support electron ionization (EI) mass spectrometry or as a primary 
method for identification and quantification. While the use of these 
enhanced techniques is encouraged, it is not required.

                                4. Safety

    4.1 Hazards associated with each reagent used in this method have 
not been precisely defined; however, each chemical compound should be 
treated as a potential health hazard. From this viewpoint, exposure to 
these chemicals must be reduced to the lowest possible level by whatever 
means available. The laboratory is responsible for maintaining a current 
awareness file of OSHA regulations regarding the safe handling of the 
chemicals specified in this method. A reference file of safety data 
sheets (SDSs, OSHA, 29 CFR 1910.1200(g)) should also be made available 
to all personnel involved in sample handling and chemical analysis. 
Additional references to laboratory safety are available and have been 
identified (References 7-9) for the information of the analyst.
    4.2 The following analytes covered by this method have been 
tentatively classified as known or suspected human or mammalian 
carcinogens: Benzo(a)anthracene, benzidine, 3,3[min]-dichlorobenzidine, 
benzo(a)pyrene, alpha-BHC, beta-BHC, delta-BHC, gamma-BHC, Dibenz(a,h)-
anthracene, N-nitrosodimethylamine, 4,4[min]-DDT, and PCBs. Other 
compounds in Table 3 may also be toxic. Primary standards of toxic 
compounds should be prepared in a chemical fume hood, and a NIOSH/MESA 
approved toxic gas respirator should be worn when handling high 
concentrations of these compounds.
    4.3 This method allows the use of hydrogen as a carrier gas in place 
of helium (section 5.6.1.2). The laboratory should take the necessary 
precautions in dealing with hydrogen, and should limit hydrogen flow at 
the source to prevent buildup of an explosive mixture of hydrogen in 
air.

                       5. Apparatus and Materials

    Note: Brand names, suppliers, and part numbers are for illustration 
purposes only. No endorsement is implied. Equivalent performance may be 
achieved using equipment and materials other than those specified here. 
Demonstrating that the equipment and supplies used in the laboratory 
achieves the required performance is the responsibility of the 
laboratory. Suppliers for equipment and materials in this method may be 
found through an on-line search. Please do not contact EPA for supplier 
information.
    5.1 Sampling equipment, for discrete or composite sampling.
    5.1.1 Grab sample bottle--amber glass bottle large enough to contain 
the necessary sample volume, fitted with a fluoropolymer-lined screw 
cap. Foil may be substituted for fluoropolymer if the sample is not 
corrosive.

[[Page 271]]

If amber bottles are not available, protect samples from light. Unless 
pre-cleaned, the bottle and cap liner must be washed, rinsed with 
acetone or methylene chloride, and dried before use to minimize 
contamination.
    5.1.2 Automatic sampler (optional)--the sampler must incorporate a 
pre-cleaned glass sample container. Samples must be kept refrigerated at 
<=6 [deg]C and protected from light during compositing. If the sampler 
uses a peristaltic pump, a minimum length of compressible silicone 
rubber tubing may be used. Before use, however, rinse the compressible 
tubing with methanol, followed by repeated rinsing with reagent water, 
to minimize the potential for sample contamination. An integrating flow 
meter is required to collect flow-proportioned composites.
    5.2 Glassware.
    5.2.1 Separatory funnel--Size appropriate to hold sample volume and 
extraction solvent volume, and equipped with fluoropolymer stopcock.
    5.2.2 Drying column--Chromatographic column, approximately 400 mm 
long by 19 mm ID, with coarse frit, or equivalent, sufficient to hold 15 
g of anhydrous sodium sulfate.
    5.2.3 Concentrator tube, Kuderna-Danish--10 mL, graduated (Kontes 
570050-1025 or equivalent). Calibration must be checked at the volumes 
employed in the test. A ground glass stopper is used to prevent 
evaporation of extracts.
    5.2.4 Evaporative flask, Kuderna-Danish--500 mL (Kontes 57001-0500 
or equivalent). Attach to concentrator tube with springs.
    Note: Use of a solvent recovery system with the K-D or other solvent 
evaporation apparatus is strongly recommended.
    5.2.5 Snyder column, Kuderna-Danish--Three-ball macro (Kontes 
503000-0121 or equivalent).
    5.2.6 Snyder column, Kuderna-Danish--Two-ball micro (Kontes 569001-
0219 or equivalent).
    5.2.7 Vials--10-15 mL, amber glass, with Teflon-lined screw cap.
    5.2.8 Continuous liquid-liquid extractor--Equipped with 
fluoropolymer or glass connecting joints and stopcocks requiring no 
lubrication. (Hershberg-Wolf Extractor, Ace Glass Company, Vineland, NJ, 
P/N 6848-20, or equivalent.)
    5.2.9 In addition to the glassware listed above, the laboratory 
should be equipped with all necessary pipets, volumetric flasks, 
beakers, and other glassware listed in this method and necessary to 
perform analyses successfully.
    5.3 Boiling chips--Approximately 10/40 mesh, glass, silicon carbide, 
or equivalent. Heat to 400 [deg]C for 30 minutes, or solvent rinse or 
Soxhlet extract with methylene chloride.
    5.4 Water bath--Heated, with concentric ring cover, capable of 
temperature control (2 [deg]C). The bath should be 
used in a hood.
    5.5 Balances.
    5.5.1 Analytical, capable of accurately weighing 0.1 mg.
    5.5.2 Top loading, capable of accurately weighing 10 mg.
    5.6 GC/MS system.
    5.6.1 Gas chromatograph (GC)--An analytical system complete with a 
temperature programmable gas chromatograph and all required accessories, 
including syringes and analytical columns.
    5.6.1.1 Injection port--Can be split, splitless, temperature 
programmable vaporization split/splitless (PTV), solvent-purge, large-
volume, on-column, backflushed, or other. An autosampler is highly 
recommended because it injects volumes more precisely than volumes 
injected manually.
    5.6.1.2 Carrier gas--Helium or hydrogen. Data in the tables in this 
method were obtained using helium carrier gas. If hydrogen is used, 
analytical conditions may need to be adjusted for optimum performance, 
and calibration and all QC tests must be performed with hydrogen carrier 
gas. See Section 4.3 for precautions regarding the use of hydrogen as a 
carrier gas.
    5.6.2 GC column--See the footnotes to Tables 4 and 5. Other columns 
or column systems may be used provided all requirements in this method 
are met.
    5.6.3 Mass spectrometer--Capable of repetitively scanning from 35-
450 Daltons (amu) every two seconds or less, utilizing a 70 eV (nominal) 
electron energy in the electron impact ionization mode, and producing a 
mass spectrum which meets all the criteria in Table 9A or 9B when 50 ng 
or less of decafluorotriphenyl phosphine (DFTPP; CAS 5074-71-5; 
bis(pentafluorophenyl) phenyl phosphine) is injected into the GC.
    5.6.4 GC/MS interface--Any GC to MS interface that meets all 
performance requirements in this method may be used.
    5.6.5 Data system--A computer system must be interfaced to the mass 
spectrometer that allows the continuous acquisition and storage of mass 
spectra acquired throughout the chromatographic program. The computer 
must have software that allows searching any GC/MS data file for 
specific m/z's (masses) and plotting m/z abundances versus time or scan 
number. This type of plot is defined as an extracted ion current profile 
(EICP). Software must also be available that allows integrating the 
abundance at any EICP between specified time or scan number limits.
    5.7 Automated gel permeation chromatograph (GPC).
    5.7.1 GPC column--150-700 mm long x 21-25 mm ID, packed with 70 g of 
SX-3 Biobeads; Bio-Rad Labs, or equivalent.
    5.7.2 Pump, injection valve, UV detector, and other apparatus 
necessary to meet the requirements in this method.

[[Page 272]]

    5.8 Nitrogen evaporation device--Equipped with a water bath than can 
be maintained at 30-45 [deg]C; N-Evap, Organomation Associates, or 
equivalent.
    5.9 Muffle furnace or kiln--Capable of baking glassware or sodium 
sulfate in the range of 400-450 [deg]C.

                               6. Reagents

    6.1 Reagent water--Reagent water is defined as water in which the 
analytes of interest and interfering compounds are not detected at the 
MDLs of the analytes of interest.
    6.2 Sodium hydroxide solution (10 N)--Dissolve 40 g of NaOH (ACS) in 
reagent water and dilute to 100 mL.
    6.3 Sodium thiosulfate--(ACS) granular.
    6.4 Sulfuric acid (1+1)--Slowly add 50 mL of 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.5 Acetone, methanol, methylene chloride, 2-propanol--High purity 
pesticide quality, or equivalent, demonstrated to be free of the 
analytes of interest and interferences (Section 3). Purification of 
solvents by distillation in all-glass systems may be required.
    6.6 Sodium sulfate--(ACS) granular, anhydrous, rinsed or Soxhlet 
extracted with methylene chloride (20 mL/g), baked in a shallow tray at 
450 [deg]C for one hour minimum, cooled in a desiccator, and stored in a 
pre-cleaned glass bottle with screw cap that prevents moisture from 
entering.
    6.7 Stock standard solutions (1.00 [micro]g/[micro]L)--Stock 
standard solutions may be prepared from pure materials, or purchased as 
certified solutions. Traceability must be to the National Institute of 
Standards and Technology (NIST) or other national or international 
standard, when available. Stock solution concentrations alternate to 
those below may be used. Because of the toxicity of some of the 
compounds, primary dilutions should be prepared in a hood, and a NIOSH/
MESA approved toxic gas respirator should be worn when high 
concentrations of neat materials are handled. The following procedure 
may be used to prepare standards from neat materials.
    6.7.1 Prepare stock standard solutions by accurately weighing about 
0.0100 g of pure material. Dissolve the material in pesticide quality 
methanol or other suitable solvent and dilute to volume in a 10-mL 
volumetric flask. Larger volumes may be used at the convenience of the 
laboratory. When compound purity is assayed to be 96% or greater, the 
weight may be used without correction to calculate the concentration of 
the stock standard. Commercially prepared stock standards may be used at 
any concentration if they are certified by the manufacturer or by an 
independent source.
    6.7.2 Unless stated otherwise in this method, store non-aqueous 
standards in fluoropolymer-lined screw-cap, or heat-sealed, glass 
containers, in the dark at -20 to -10 [deg]C. Store aqueous standards; 
e.g., the aqueous LCS (section 8.4.1), in the dark at <= 6 [deg]C, but 
do not freeze. Standards prepared by the laboratory may be stored for up 
to one year, except when comparison with QC check standards indicates 
that a standard has degraded or become more concentrated due to 
evaporation, or unless the laboratory has data on file to prove 
stability for a longer period. Commercially prepared standards may be 
stored until the expiration date provided by the vendor, except when 
comparison with QC check standards indicates that a standard has 
degraded or become more concentrated due to evaporation, or unless the 
laboratory has data from the vendor on file to prove stability for a 
longer period.
    6.8 Surrogate standard spiking solution.
    6.8.1 Select a minimum of three surrogate compounds from Table 8 
that most closely match the recovery of the analytes of interest. For 
example, if all analytes tested are considered acids, use surrogates 
that have similar chemical attributes. Other compounds may be used as 
surrogates so long as they do not interfere in the analysis. If only one 
or two analytes are determined, one or two surrogates may be used.
    6.8.2 Prepare a solution containing each selected surrogate such 
that the concentration in the sample would match the concentration in 
the mid-point calibration standard. For example, if the midpoint of the 
calibration is 100 [micro]g/L, prepare the spiking solution at a 
concentration of 100 [micro]g/mL in methanol. Addition of 1.00 mL of 
this solution to 1000 mL of sample will produce a concentration of 100 
[micro]g/L of the surrogate. Alternate volumes and concentrations 
appropriate to the response of the GC/MS instrument or for selective ion 
monitoring (SIM) may be used, if desired. Store per section 6.7.2.
    6.9 Internal standard spiking solution.
    6.9.1 Select three or more internal standards similar in 
chromatographic behavior to the analytes of interest. Internal standards 
are listed in Table 8. Suggested internal standards are: 1,4-
dichlorobenzene-d4; naphthalene-d8; acenaphthene-
d10; phenanthrene-d10; chrysene-d12; 
and perylene-d12. The laboratory must demonstrate that 
measurement of the internal standards is not affected by method or 
matrix interferences (see also section 7.3.4).
    6.9.2 Prepare the internal standards at a concentration of 10 mg/mL 
in methylene chloride or other suitable solvent. When 10 [micro]L of 
this solution is spiked into a 1-mL extract, the concentration of the 
internal standards will be 100 [micro]g/mL. A lower concentration 
appropriate to the response of the GC/MS instrument or for SIM may be 
used, if desired. Store per section 6.7.3.

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    6.9.3 To assure accurate analyte identification, particularly when 
SIM is used, it may be advantageous to include more internal standards 
than those suggested in section 6.9.1. An analyte will be located most 
accurately if its retention time relative to an internal standard is in 
the range of 0.8 to 1.2.
    6.10 DFTPP standard--Prepare a solution of DFTPP in methanol or 
other suitable solvent such that 50 ng or less will be injected (see 
section 13.2). An alternative concentration may be used to compensate 
for specific injection volumes or to assure that the operating range of 
the instrument is not exceeded, so long as the total injected is 50 ng 
or less. Include benzidine and pentachlorophenol in this solution such 
that <=100 ng of benzidine and <=50 ng of pentachlorophenol will be 
injected.
    6.11 Quality control check sample concentrate--See section 8.2.1.
    6.12 GPC calibration solution.
    6.12.1 Prepare a methylene chloride solution to contain corn oil, 
bis(2-ethylhexyl) phthalate (BEHP), perylene, and sulfur at the 
concentrations in section 6.12.2, or at concentrations appropriate to 
the response of the detector.
    Note: Sulfur does not readily dissolve in methylene chloride, but is 
soluble in warm corn oil. The following procedure is suggested for 
preparation of the solution.
    6.12.2 Weigh 8 mg sulfur and 2.5 g corn oil into a 100-mL volumetric 
flask and warm to dissolve the sulfur. Separately weigh 100 mg BEHP, 20 
mg pentachlorophenol, and 2 mg perylene and add to flask. Bring to 
volume with methylene chloride and mix thoroughly.
    6.12.3 Store the solution in an amber glass bottle with a 
fluoropolymer-lined screw cap at 0-6 [deg]C. Protect from light. 
Refrigeration may cause the corn oil to precipitate. Before use, allow 
the solution to stand at room temperature until the corn oil dissolves, 
or warm slightly to aid in dissolution. Replace the solution every year, 
or more frequently if the response of a component changes.
    6.13 Sulfur removal--Copper foil or powder (bright, non-oxidized), 
or tetrabutylammonium sulfite (TBA sulfite).
    6.13.1 Copper foil, or powder--Fisher, Alfa Aesar 42455-18, 625 
mesh, or equivalent. Cut copper foil into approximately 1-cm squares. 
Copper must be activated before it may be used, as described below:
    6.13.1.1 Place the quantity of copper needed for sulfur removal 
(section 11.2.1.3) in a ground-glass-stoppered Erlenmeyer flask or 
bottle. Cover the foil or powder with methanol.
    6.13.1.2 Add HCl dropwise (0.5-1.0 mL) while swirling, until the 
copper brightens.
    6.13.1.3 Pour off the methanol/HCl and rinse 3 times with reagent 
water to remove all traces of acid, then 3 times with acetone, then 3 
times with hexane.
    6.13.1.4 For copper foil, cover with hexane after the final rinse. 
Store in a stoppered flask under nitrogen until used. For the powder, 
dry on a rotary evaporator or under a stream of nitrogen. Store in a 
stoppered flask under nitrogen until used. Inspect the copper foil or 
powder before each use. It must have a bright, non-oxidized appearance 
to be effective. Copper foil or powder that has oxidized may be 
reactivated using the procedure described above.
    6.13.2 Tetrabutylammonium sodium sulfite (TBA sodium sulfite).
    6.13.2.1 Tetrabutylammonium hydrogen sulfate, 
[CH3(CH2)3]4NHSO4.

    6.13.2.2 Sodium sulfite, Na2SO3.
    6.13.2.3 Dissolve approximately 3 g tetrabutylammonium hydrogen 
sulfate in 100 mL of reagent water in an amber bottle with 
fluoropolymer-lined screw cap. Extract with three 20-mL portions of 
hexane and discard the hexane extracts.
    6.13.2.4 Add 25 g sodium sulfite to produce a saturated solution. 
Store at room temperature. Replace after 1 month.
    6.14 DDT and endrin decomposition (breakdown) solution--Prepare a 
solution containing endrin at a concentration of 1 [micro]g/mL and 
4,4[min]-DDT at a concentration of 2 [micro]g/mL, in isooctane or 
hexane. A 1-[micro]L injection of this standard will contain 1 nanogram 
(ng) of endrin and 2 ng of DDT. The concentration of the solution may be 
adjusted by the laboratory to accommodate other injection volumes such 
that the same masses of the two analytes are introduced into the 
instrument.

                             7. Calibration

    7.1 Establish operating conditions equivalent to those in the 
footnote to Table 4 or 5 for the base/neutral or acid fraction, 
respectively. If a combined base/neutral/acid fraction will be analyzed, 
use the conditions in the footnote to Table 4. Alternative temperature 
program and flow rate conditions may be used. It is necessary to 
calibrate the GC/MS for the analytes of interest (Section 1.3) only.
    7.2 Internal standard calibration.
    7.2.1 Prepare calibration standards for the analytes of interest and 
surrogates at a minimum of five concentration levels by adding 
appropriate volumes of one or more stock standards to volumetric flasks. 
One of the calibration standards should be at a concentration at or 
below the ML specified in Table 1, 2, or 3, or as specified by a 
regulatory/control authority or in a permit. The ML value may be rounded 
to a whole number that is more convenient for preparing the standard, 
but must not exceed the ML in Table 1, 2, or 3 for those analytes which 
list ML values. Alternatively, the laboratory may establish a laboratory 
ML for each analyte based on the concentration in a

[[Page 274]]

nominal whole-volume sample that is equivalent to the concentration of 
the lowest calibration standard in a series of standards produced in the 
laboratory or obtained from a commercial vendor. The laboratory's ML 
must not exceed the ML in Table 1, 2, or 3, and the resulting 
calibration must meet the acceptance criteria in Section 7.2.3, based on 
the RSD, RSE, or R\2\. The concentrations of the other calibration 
standards should correspond to the expected range of concentrations 
found in real samples or should define the working range of the GC/MS 
system for full-scan and/or SIM operation, as appropriate. A minimum of 
six concentration levels is required for a second order, non-linear 
(e.g., quadratic; ax\2\ + bx + c = 0) calibration (section 7.2.3). 
Calibrations higher than second order are not allowed. To each 
calibration standard or standard mixture, add a known constant volume of 
the internal standard solution (section 6.9), and dilute to volume with 
methylene chloride.
    Note: The large number of analytes in Tables 1 through 3 may not be 
soluble or stable in a single solution; multiple solutions may be 
required if a large number of analytes are to be determined 
simultaneously.
    7.2.1.1 Prior to analysis of the calibration standards, inject the 
DFTPP standard (Section 6.10) and adjust the scan rate of the mass 
spectrometer to produce a minimum of 5 mass spectra across the DFTPP GC 
peak. Adjust instrument conditions until the DFTPP criteria in Table 9A 
or 9B are met. Calculate peak tailing factors for benzidine and 
pentachlorophenol. Calculation of the tailing factor is illustrated in 
Figure 1. The tailing factor for benzidine and pentachlorophenol must be 
<2; otherwise, adjust instrument conditions and either replace the 
column or break off a short section of the front end of the column, and 
repeat the test. Once the scan conditions are established, they must be 
used for analyses of all standards, blanks, and samples.
    Note: The DFTPP spectrum may be evaluated by summing the intensities 
of the m/z's across the GC peak, subtracting the background at each m/z 
in a region of the chromatogram within 20 scans of but not including any 
part of, the DFTPP peak. The DFTPP spectrum may also be evaluated by 
fitting a Gaussian to each m/z and using the intensity at the maximum 
for each Gaussian or by integrating the area at each m/z and using the 
integrated areas. Other means may be used for evaluation of the DFTPP 
spectrum so long as the spectrum is not distorted to meet the criteria 
in Table 9A or 9B.
    7.2.1.2 Analyze the mid-point combined base/neutral and acid 
calibration standard and enter or review the retention time, relative 
retention time, mass spectrum, and quantitation m/z in the data system 
for each analyte of interest, surrogate, and internal standard. If 
additional analytes (Table 3) are to be quantified, include these 
analytes in the standard. The mass spectrum for each analyte must be 
comprised of a minimum of 2 m/z's (Tables 4 and 5); 3 to 5 m/z's assure 
more reliable analyte identification. Suggested quantitation m/z's are 
shown in Tables 4 and 5 as the primary m/z. If an interference occurs at 
the primary m/z, use one of the secondary m/z's or an alternate m/z. A 
single m/z only is required for quantitation.
    7.2.1.3 For SIM operation, determine the analytes in each 
descriptor, the quantitation m/z for each analyte (the quantitation m/z 
can be the same as for full-scan operation; section 7.2.1.2), the dwell 
time on each m/z for each analyte, and the beginning and ending 
retention time for each descriptor. Analyze the verification standard in 
scan mode to verify m/z's and establish retention times for the 
analytes. There must be a minimum of two m/z's for each analyte to 
assure analyte identification. To maintain sensitivity, the number of m/
z's in a descriptor should be limited. For example, for a descriptor 
with 10 m/z's and a chromatographic peak width of 5 sec, a dwell time of 
100 ms at each m/z would result in a scan time of 1 second and provide 5 
scans across the GC peak. The quantitation m/z will usually be the most 
intense peak in the mass spectrum. The quantitation m/z and dwell time 
may be optimized for each analyte. The acquisition table used for SIM 
must take into account the mass defect (usually less than 0.2 Dalton) 
that can occur at each m/z monitored. Refer to the footnotes to Table 4 
or 5 for establishing operating conditions and to section 7.2.1.1 for 
establishing scan conditions.
    7.2.1.4 For combined scan and SIM operation, set up the scan 
segments and descriptors to meet requirements in sections 7.2.1.1-
7.2.1.3. Analyze unfamiliar samples in the scan mode to assure that the 
analytes of interest are determined.
    7.2.2 Analyze each calibration standard according to section 12 and 
tabulate the area at the quantitation m/z against concentration for each 
analyte of interest, surrogate, and internal standard. If an 
interference is encountered, use a secondary m/z (Table 4 or 5) for 
quantitation. Calculate a response factor (RF) for each analyte of 
interest at each concentration using Equation 1.

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[GRAPHIC] [TIFF OMITTED] TR28AU17.014

where:

As = Area of the characteristic m/z for the analyte of 
          interest or surrogate.
Ais = Area of the characteristic m/z for the internal 
          standard.
Cis = Concentration of the internal standard ([micro]g/mL).
Cs = Concentration of the analyte of interest or surrogate 
          ([micro]g/mL).

    7.2. Calculate the mean (average) and relative standard deviation 
(RSD) of the responses factors. If the RSD is less than 35%, the RF can 
be assumed to be invariant and the average RF can be used for 
calculations. Alternatively, the results can be used to fit a linear or 
quadratic regression of response ratios, As/Ais, vs. concentration 
ratios Cs/Cis. If used, the regression must be weighted inversely 
proportional to concentration. The coefficient of determination (R\2\; 
Reference 10) of the weighted regression must be greater than 0.920 
(this value roughly corresponds to the RSD limit of 35%). Alternatively, 
the relative standard error (Reference 11) may be used as an acceptance 
criterion. As with the RSD, the RSE must be less than 35%. If an RSE 
less than 35% cannot be achieved for a quadratic regression, system 
performance is unacceptable and the system must be adjusted and re-
calibrated.
    Note: Using capillary columns and current instrumentation, it is 
quite likely that a laboratory can calibrate the target analytes in this 
method and achieve a linearity metric (either RSD or RSE) well below 
35%. Therefore, laboratories are permitted to use more stringent 
acceptance criteria for calibration than described here, for example, to 
harmonize their application of this method with those from other 
sources.
    7.3 Calibration verification--The RF or calibration curve must be 
verified immediately after calibration and at the beginning of each 12-
hour shift, by analysis of a standard at or near the concentration of 
the mid-point calibration standard (section 7.2.1). The standard(s) must 
be obtained from a second manufacturer or a manufacturer's batch 
prepared independently from the batch used for calibration. Traceability 
must be to a national standard, when available. Include the surrogates 
(section 6.8) in this solution. It is necessary to verify calibration 
for the analytes of interest (section 1.3) only.
    Note: The 12-hour shift begins after the DFTPP (section 13.1) and 
DDT/endrin tests (if DDT and endrin are to be determined), and after 
analysis of the calibration verification standard. The 12-hour shift 
ends 12 hours later. The DFTPP, DDT/endrin, and calibration verification 
tests are outside of the 12-hour shift.
    7.3.1 Analyze the calibration verification standard(s) beginning in 
section 12. Calculate the percent recovery of each analyte. Compare the 
recoveries for the analytes of interest against the acceptance criteria 
for recovery (Q) in Table 6, and the recoveries for the surrogates 
against the acceptance criteria in Table 8. If recovery of the analytes 
of interest and surrogates meet acceptance criteria, system performance 
is acceptable and analysis of samples may continue. If any individual 
recovery is outside its limit, system performance is unacceptable for 
that analyte.
    Note: The large number of analytes in Tables 6 and 8 present a 
substantial probability that one or more will fail acceptance criteria 
when all analytes are tested simultaneously.
    7.3.2 When one or more analytes fail acceptance criteria, analyze a 
second aliquot of the calibration verification standard and compare ONLY 
those analytes that failed the first test (section 7.3.1) with their 
respective acceptance criteria. If these analytes now pass, system 
performance is acceptable and analysis of samples may continue. A repeat 
failure of any analyte that failed the first test, however, will confirm 
a general problem with the measurement system. If this occurs, repair 
the system (section 7.2.1.1) and repeat the test (section 7.3.1), or 
prepare a fresh calibration standard and repeat the test. If calibration 
cannot be verified after maintenance or injection of the fresh 
calibration standard, re-calibrate the instrument.
    Note: If it is necessary to perform a repeat verification test 
frequently; i.e., perform two tests in order to pass, it may be prudent 
to perform two injections in succession and review the results, rather 
than perform one injection, review the results, then perform the second 
injection if results from the first injection fail. To maintain the 
validity of the test and re-test, system maintenance and/or adjustment 
is not permitted between the injections.
    7.3.3 Many of the analytes in Table 3 do not have QC acceptance 
criteria in Table 6, and some of the surrogates in Table 8 do not have 
acceptance criteria. If calibration is to be verified and other QC tests 
are to be performed for these analytes, acceptance criteria must be 
developed and applied. EPA has provided guidance for development of QC 
acceptance criteria (References 12 and 13). Alternatively, analytes that 
do not have acceptance criteria in Table 6 or Table 8 may

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be based on laboratory control charts, or 60 to 140% may be used.
    7.3.4 Internal standard responses--Verify that detector sensitivity 
has not changed by comparing the response of each internal standard in 
the calibration verification standard (section 7.3) to the response of 
the respective internal standard in the midpoint calibration standard 
(section 7.2.1). The peak areas or heights of the internal standards in 
the calibration verification standard must be within 50% to 200% (1/2 to 
2x) of their respective peak areas or heights in the mid-point 
calibration standard. If not, repeat the calibration verification test 
using a fresh calibration verification standard (7.3), or perform and 
document system repair. Subsequent to repair, repeat the calibration 
verification test (section 7.3.1). If the responses are still not within 
50% to 200%, re-calibrate the instrument (section 7.2.2) and repeat the 
calibration verification test.

                           8. Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability and 
ongoing analysis of spiked samples and blanks to evaluate and document 
data quality (40 CFR 136.7). The laboratory must maintain records to 
document the quality of data generated. Results of ongoing performance 
tests are compared with established QC acceptance criteria to determine 
if the results of analyses meet performance requirements of this method. 
When results of spiked samples do not meet the QC acceptance criteria in 
this method, a quality control check sample (laboratory control sample; 
LCS) must be analyzed to confirm that the measurements were performed in 
an in-control mode of operation. A laboratory may develop its own 
performance criteria (as QC acceptance criteria), provided such criteria 
are as or more restrictive than the criteria in this method.
    8.1.1 The laboratory must make an initial demonstration of 
capability (DOC) to generate acceptable precision and recovery with this 
method. This demonstration is detailed in Section 8.2.
    8.1.2 In recognition of advances that are occurring in analytical 
technology, and to overcome matrix interferences, the laboratory is 
permitted certain options (section 1.6 and 40 CFR 136.6(b)) to improve 
separations or lower the costs of measurements. These options may 
include alternate extraction, concentration, and cleanup procedures 
(e.g., solid-phase extraction; rotary-evaporator concentration; column 
chromatography cleanup), changes in column and type of mass spectrometer 
(40 CFR 136.6(b)(4)(xvi)). Alternate determinative techniques, such as 
substitution of spectroscopic or immunoassay techniques, and changes 
that degrade method performance, are not allowed. If an analytical 
technique other than GC/MS is used, that technique must have a 
specificity equal to or greater than the specificity of GC/MS for the 
analytes of interest. The laboratory is also encouraged to participate 
in inter-comparison and performance evaluation studies (see section 
8.10).
    8.1.2.1 Each time a modification is made to this method, the 
laboratory is required to repeat the procedure in section 8.2. If the 
detection limit of the method will be affected by the change, the 
laboratory must demonstrate that the MDLs (40 CFR part 136, appendix B) 
are lower than one-third the regulatory compliance limit or the MDLs in 
this method, whichever are greater. If calibration will be affected by 
the change, the instrument must be recalibrated per section 7. Once the 
modification is demonstrated to produce results equivalent or superior 
to results produced by this method, that modification may be used 
routinely thereafter, so long as the other requirements in this method 
are met (e.g., matrix spike/matrix spike duplicate recovery and relative 
percent difference).
    8.1.2.1.1 If SPE, or another allowed method modification, is to be 
applied to a specific discharge, the laboratory must prepare and analyze 
matrix spike/matrix spike duplicate (MS/MSD) samples (section 8.3) and 
LCS samples (section 8.4). The laboratory must include surrogates 
(section 8.7) in each of the samples. The MS/MSD and LCS samples must be 
fortified with the analytes of interest (Section 1.3). If the 
modification is for nationwide use, MS/MSD samples must be prepared from 
a minimum of nine different discharges (See section 8.1.2.1.2), and all 
QC acceptance criteria in this method must be met. This evaluation only 
needs to be performed once other than for the routine QC required by 
this method (for example it could be performed by the vendor of the SPE 
materials) but any laboratory using that specific material must have the 
results of the study available. This includes a full data package with 
the raw data that will allow an independent reviewer to verify each 
determination and calculation performed by the laboratory (see section 
8.1.2.2.5, items (a)-(q)).
    8.1.2.1.2 Sample matrices on which MS/MSD tests must be performed 
for nationwide use of an allowed modification:
    (a) Effluent from a POTW.
    (b) ASTM D5905 Standard Specification for Substitute Wastewater.
    (c) Sewage sludge, if sewage sludge will be in the permit.
    (d) ASTM D1141 Standard Specification for Substitute Ocean Water, if 
ocean water will be in the permit.
    (e) Untreated and treated wastewaters up to a total of nine matrix 
types (see https://www.epa.gov/eg/industrial-effluent-guidelines

[[Page 277]]

for a list of industrial categories with existing effluent guidelines).
    (i) At least one of the above wastewater matrix types must have at 
least one of the following characteristics:
    (A) Total suspended solids greater than 40 mg/L.
    (B) Total dissolved solids greater than 100 mg/L.
    (C) Oil and grease greater than 20 mg/L.
    (D) NaCl greater than 120 mg/L.
    (E) CaCO3 greater than 140 mg/L.
    (ii) Results of MS/MSD tests must meet QC acceptance criteria in 
Section 8.3.
    (f) A proficiency testing (PT) sample from a recognized provider, in 
addition to tests of the nine matrices (section 8.1.2.1.1).
    8.1.2.2 The laboratory is required to maintain records of 
modifications made to this method. These records include the following, 
at a minimum:
    8.1.2.2.1 The names, titles, and business street addresses, 
telephone numbers, and email addresses, of the analyst(s) that performed 
the analyses and modification, and of the quality control officer that 
witnessed and will verify the analyses and modifications.
    8.1.2.2.2 A list of analytes, by name and CAS Registry Number.
    8.1.2.2.3 A narrative stating reason(s) for the modifications.
    8.1.2.2.4 Results from all quality control (QC) tests comparing the 
modified method to this method, including:
    (a) Calibration (section 7).
    (b) Calibration verification (section 7).
    (c) Initial demonstration of capability (section 8.2).
    (d) Analysis of blanks (section 8.5).
    (e) Matrix spike/matrix spike duplicate analysis (section 8.3).
    (f) Laboratory control sample analysis (section 8.4).
    8.1.2.2.5 Data that will allow an independent reviewer to validate 
each determination by tracing the instrument output (peak height, area, 
or other signal) to the final result. These data are to include:
    (a) Sample numbers and other identifiers.
    (b) Extraction dates.
    (c) Analysis dates and times.
    (d) Analysis sequence/run chronology.
    (e) Sample weight or volume (ssection 10).
    (f) Extract volume prior to each cleanup step (sections 10 and 11).
    (g) Extract volume after each cleanup step (section 11).
    (h) Final extract volume prior to injection (sections 10 and 12).
    (i) Injection volume (section 12.2.3).
    (j) Sample or extract dilution (section 12.2.3.2).
    (k) Instrument and operating conditions.
    (l) Column (dimensions, material, etc).
    (m) Operating conditions (temperature program, flow rate, etc).
    (n) Detector (type, operating conditions, etc).
    (o) Chromatograms, mass spectra, and other recordings of raw data.
    (p) Quantitation reports, data system outputs, and other data to 
link the raw data to the results reported.
    (q) A written Standard Operating Procedure (SOP).
    8.1.2.2.6 Each individual laboratory wishing to use a given 
modification must perform the start-up tests in section 8.1.2 (e.g., 
DOC, MDL), with the modification as an integral part of this method 
prior to applying the modification to specific discharges. Results of 
the DOC must meet the QC acceptance criteria in Table 6 for the analytes 
of interest (section 1.3), and the MDLs must be equal to or lower than 
the MDLs in Tables 1, 2, or 3 for the analytes of interest.
    8.1.3 Before analyzing samples, the laboratory must analyze a blank 
to demonstrate that interferences from the analytical system, labware, 
and reagents, are under control. Each time a batch of samples is 
extracted or reagents are changed, a blank must be extracted and 
analyzed as a safeguard against laboratory contamination. Requirements 
for the blank are given in section 8.5.
    8.1.4 The laboratory must, on an ongoing basis, spike and analyze to 
monitor and evaluate method and laboratory performance on the sample 
matrix. The procedure for spiking and analysis is given in section 8.3.
    8.1.5 The laboratory must, on an ongoing basis, demonstrate through 
analysis of a quality control check sample (laboratory control sample, 
LCS; on-going precision and recovery sample, OPR) that the measurement 
system is in control. This procedure is given in section 8.4.
    8.1.6 The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is given in 
section 8.9.
    8.1.7 The large number of analytes tested in performance tests in 
this method present a substantial probability that one or more will fail 
acceptance criteria when many analytes are tested simultaneously, and a 
re-test is allowed if this situation should occur. If, however, 
continued re-testing results in further repeated failures, the 
laboratory must document and report the failures (e.g., as qualifiers on 
results), unless the failures are not required to be reported as 
determined by the regulatory/control authority. Results associated with 
a QC failure for an analyte regulated in a discharge cannot be used to 
demonstrate regulatory compliance. QC failures do not relieve a 
discharger or permittee of reporting timely results.
    8.2 Initial demonstration of capability (DOC)--To establish the 
ability to generate acceptable recovery and precision, the laboratory 
must perform the DOC in sections

[[Page 278]]

8.2.1 through 8.2.6 for the analytes of interest. The laboratory must 
also establish MDLs for the analytes of interest using the MDL procedure 
at 40 CFR part 136, appendix B. The laboratory's MDLs must be equal to 
or lower than those listed in Tables 1, 2, or 3 or lower than one third 
the regulatory compliance limit, whichever is greater. For MDLs not 
listed in Tables 4 and 5, the laboratory must determine the MDLs using 
the MDL procedure at 40 CFR part 136, appendix B under the same 
conditions used to determine the MDLs for the analytes listed in Tables 
1, 2, and 3. All procedures used in the analysis, including cleanup 
procedures, must be included in the DOC.
    8.2.1 For the DOC, a QC check sample concentrate (LCS concentrate) 
containing each analyte of interest (section 1.3) is prepared in a 
water-miscible solvent. The QC check sample concentrate must be prepared 
independently from those used for calibration, but may be from the same 
source as the second-source standard used for calibration verification 
(Section 7.3). The concentrate should produce concentrations of the 
analytes of interest in water at the mid-point of the calibration range, 
and may be at the same concentration as the LCS (section 8.4). Multiple 
solutions may be required.
    Note: QC check sample concentrates are no longer available from EPA.
    8.2.2 Using a pipet or micro-syringe, prepare four LCSs by adding an 
appropriate volume of the concentrate to each of four aliquots of 
reagent water, and mix well. The volume of reagent water must be the 
same as the volume that will be used for the sample, blank (section 
8.5), and MS/MSD (section 8.3). A volume of 1-L and a concentration of 
100 [micro]g/L were used to develop the QC acceptance criteria in Table 
6. Also add an aliquot of the surrogate spiking solution (section 6.8) 
to the reagent-water aliquots.
    8.2.3 Extract and analyze the four LCSs according to the method 
beginning in Section 10.
    8.2.4 Calculate the average percent recovery (X) and the standard 
deviation of the percent recovery (s) for each analyte using the four 
results.
    8.2.5 For each analyte, compare s and (X) with the corresponding 
acceptance criteria for precision and recovery in Table 6. For analytes 
in Table 3 not listed in Table 6, DOC QC acceptance criteria must be 
developed by the laboratory. EPA has provided guidance for development 
of QC acceptance criteria (References 12 and 13). Alternatively, 
acceptance criteria for analytes not listed in Table 6 may be based on 
laboratory control charts. If s and (X) for all analytes of interest 
meet the acceptance criteria, system performance is acceptable and 
analysis of blanks and samples may begin. If any individual s exceeds 
the precision limit or any individual (X) falls outside the range for 
recovery, system performance is unacceptable for that analyte.
    Note: The large number of analytes in Tables 1-3 present a 
substantial probability that one or more will fail at least one of the 
acceptance criteria when many or all analytes are determined 
simultaneously. Therefore, the analyst is permitted to conduct a ``re-
test'' as described in section 8.2.6.
    8.2.6 When one or more of the analytes tested fail at least one of 
the acceptance criteria, repeat the test for only the analytes that 
failed. If results for these analytes pass, system performance is 
acceptable and analysis of samples and blanks may proceed. If one or 
more of the analytes again fail, system performance is unacceptable for 
the analytes that failed the acceptance criteria. Correct the problem 
and repeat the test (section 8.2). See section 8.1.7 for disposition of 
repeated failures.
    Note: To maintain the validity of the test and re-test, system 
maintenance and/or adjustment is not permitted between this pair of 
tests.
    8.3 Matrix spike and matrix spike duplicate (MS/MSD)--The purpose of 
the MS/MSD requirement is to provide data that demonstrate the 
effectiveness of the method as applied to the samples in question by a 
given laboratory, and both the data user (discharger, permittee, 
regulated entity, regulatory/control authority, customer, other) and the 
laboratory share responsibility for provision of such data. The data 
user should identify the sample and the analytes of interest (section 
1.3) to be spiked and provide sufficient sample volume to perform MS/MSD 
analyses. The laboratory must, on an ongoing basis, spike at least 5% of 
the samples in duplicate from each discharge being monitored to assess 
accuracy (recovery and precision). If direction cannot be obtained from 
the data user, the laboratory must spike at least one sample in 
duplicate per extraction batch of up to 20 samples with the analytes in 
Table 1. Spiked sample results should be reported only to the data user 
whose sample was spiked, or as requested or required by a regulatory/
control authority, or in a permit.
    8.3.1 If, as in compliance monitoring, the concentration of a 
specific analyte will be checked against a regulatory concentration 
limit, the concentration of the spike should be at that limit; 
otherwise, the concentration of the spike should be one to five times 
higher than the background concentration determined in section 8.3.2, at 
or near the midpoint of the calibration range, or at the concentration 
in the LCS (section 8.4) whichever concentration would be larger.
    8.3.2 Analyze one sample aliquot to determine the background 
concentration (B) of the each analyte of interest. If necessary, prepare 
a new check sample concentrate (section 8.2.1) appropriate for the 
background

[[Page 279]]

concentration. Spike and analyze two additional sample aliquots, and 
determine the concentration after spiking (A1 and 
A2) of each analyte. Calculate the percent recoveries 
(P1 and P2) as 100 (A1 - B)/T and 100 
(A2 - B)/T, where T is the known true value of the spike. 
Also calculate the relative percent difference (RPD) between the 
concentrations (A1 and A2) as 200 
[verbar]A1 - A2[verbar]/(A1 + 
A2). If necessary, adjust the concentrations used to 
calculate the RPD to account for differences in the volumes of the 
spiked aliquots.
    8.3.3 Compare the percent recoveries (P1 and 
P2) and the RPD for each analyte in the MS/MSD aliquots with 
the corresponding QC acceptance criteria in Table 6. A laboratory may 
develop and apply QC acceptance criteria more restrictive than the 
criteria in Table 6, if desired.
    8.3.3.1 If any individual P falls outside the designated range for 
recovery in either aliquot, or the RPD limit is exceeded, the result for 
the analyte in the unspiked sample is suspect. See Section 8.1.7 for 
disposition of failures.
    8.3.3.2 The acceptance criteria in Table 6 were calculated to 
include an allowance for error in measurement of both the background and 
spike concentrations, assuming a spike to background ratio of 5:1. This 
error will be accounted for to the extent that the spike to background 
ratio approaches 5:1 (Reference 14) and is applied to spike 
concentrations of 100 [micro]g/L and higher. If spiking is performed at 
a concentration lower than 100 [micro]g/L, the laboratory must use the 
QC acceptance criteria in Table 6, the optional QC acceptance criteria 
calculated for the specific spike concentration in Table 7, or optional 
in-house criteria (section 8.3.4). To use the acceptance criteria in 
Table 7: (1) Calculate recovery (X[min]) using the equation in Table 7, 
substituting the spike concentration (T) for C; (2) Calculate overall 
precision (S[min]) using the equation in Table 7, substituting X[min] 
for X; (3) Calculate the range for recovery at the spike concentration 
as (100 X[min]/T)  2.44(100 S[min]/T)% (Reference 
14). For analytes in Table 3 not listed in Table 6, QC acceptance 
criteria must be developed by the laboratory. EPA has provided guidance 
for development of QC acceptance criteria (References 12 and 13). 
Alternatively, acceptance criteria may be based on laboratory control 
charts.
    8.3.4 After analysis of a minimum of 20 MS/MSD samples for each 
target analyte and surrogate, and if the laboratory chooses to develop 
and apply the optional in-house QC limits (Section 8.3.3), the 
laboratory should calculate and apply the optional in-house QC limits 
for recovery and RPD of future MS/MSD samples (Section 8.3). The QC 
limits for recovery are calculated as the mean observed recovery 3 standard deviations, and the upper QC limit for RPD is 
calculated as the mean RPD plus 3 standard deviations of the RPDs. The 
in-house QC limits must be updated at least every two years and re-
established after any major change in the analytical instrumentation or 
process. If in-house QC limits are developed, at least 80% of the 
analytes tested in the MS/MSD must have in-house QC acceptance criteria 
that are tighter than those in Table 6, and the remaining analytes 
(those other than the analytes included in the 80%) must meet the 
acceptance criteria in Table 6. If an in-house QC limit for the RPD is 
greater than the limit in Table 6, then the limit in Table 6 must be 
used. Similarly, if an in-house lower limit for recovery is below the 
lower limit in Table 6, then the lower limit in Table 6 must be used, 
and if an in-house upper limit for recovery is above the upper limit in 
Table 6, then the upper limit in Table 6 must be used.
    8.4 Laboratory control sample (LCS)--A QC check sample (laboratory 
control sample, LCS; on-going precision and recovery sample, OPR) 
containing each analyte of interest (Section 1.3) and surrogate must be 
prepared and analyzed with each extraction batch of up to 20 samples to 
demonstrate acceptable recovery of the analytes of interest from a clean 
sample matrix.
    8.4.1 Prepare the LCS by adding QC check sample concentrate (section 
8.2.1) to reagent water. Include all analytes of interest (section 1.3) 
in the LCS. The LCS may be the same sample prepared for the DOC (section 
8.2.1). The volume of reagent water must be the same as the volume used 
for the sample, blank (section 8.5), and MS/MSD (Section 8.3). Also add 
an aliquot of the surrogate spiking solution (section 6.8). The 
concentration of the analytes in reagent water should be the same as the 
concentration in the DOC (section 8.2.2).
    8.4.2 Analyze the LCS prior to analysis of field samples in the 
extraction batch. Determine the concentration (A) of each analyte. 
Calculate the percent recovery (PS) as 100 (A/T)%, where T is the true 
value of the concentration in the LCS.
    8.4.3 Compare the percent recovery (PS) for each analyte with its 
corresponding QC acceptance criterion in Table 6. For analytes of 
interest in Table 3 not listed in Table 6, use the QC acceptance 
criteria developed for the LCS (section 8.4.5), or limits based on 
laboratory control charts. If the recoveries for all analytes of 
interest fall within their respective QC acceptance criteria, analysis 
of blanks and field samples may proceed. If any individual PS falls 
outside the range, proceed according to section 8.4.4.
    Note: The large number of analytes in Tables 1-3 present a 
substantial probability that one or more will fail the acceptance 
criteria when all analytes are tested simultaneously. Because a re-test 
is allowed in event of failure (sections 8.1.7 and 8.4.3), it may be 
prudent to extract and analyze two LCSs together and evaluate results of 
the second

[[Page 280]]

analysis against the QC acceptance criteria only if an analyte fails the 
first test.
    8.4.4 Repeat the test only for those analytes that failed to meet 
the acceptance criteria (PS). If these analytes now pass, system 
performance is acceptable and analysis of blanks and samples may 
proceed. Repeated failure, however, will confirm a general problem with 
the measurement system. If this occurs, repeat the test using a fresh 
LCS (section 8.2.2) or an LCS prepared with a fresh QC check sample 
concentrate (section 8.2.1), or perform and document system repair. 
Subsequent to analysis of the LCS prepared with a fresh sample 
concentrate, or to system repair, repeat the LCS test (section 8.4). If 
failure of the LCS indicates a systemic problem with samples in the 
batch, re-extract and re-analyze the samples in the batch. See section 
8.1.7 for disposition of repeated failures.
    Note: To maintain the validity of the test and re-test, system 
maintenance and/or adjustment is not permitted between the pair of 
tests.
    8.4.5 After analysis of 20 LCS samples, and if the laboratory 
chooses to develop and apply in-house QC limits, the laboratory should 
calculate and apply in-house QC limits for recovery to future LCS 
samples (section 8.4). Limits for recovery in the LCS should be 
calculated as the mean recovery 3 standard 
deviations. A minimum of 80% of the analytes tested for in the LCS must 
have QC acceptance criteria tighter than those in Table 6, and the 
remaining analytes (those other than the analytes included in the 80%) 
must meet the acceptance criteria in Table 6. If an in-house lower limit 
for recovery is lower than the lower limit in Table 6, the lower limit 
in Table 6 must be used, and if an in-house upper limit for recovery is 
higher than the upper limit in Table 6, the upper limit in Table 6 must 
be used. Many of the analytes and surrogates do not contain acceptance 
criteria. The laboratory should use 60-140% as interim acceptance 
criteria for recoveries of spiked analytes and surrogates that do not 
have recovery limits specified in Table 8, and at least 80% of the 
surrogates must meet the 60-140% interim criteria until in-house LCS and 
surrogate limits are developed. Alternatively, acceptance criteria for 
analytes that do not have recovery limits in Table 6 may be based on 
laboratory control charts. In-house QC acceptance criteria must be 
updated at least every two years.
    8.5 Blank--A blank must be extracted and analyzed with each 
extraction batch to demonstrate that the reagents and equipment used for 
preparation and analysis are free from contamination.
    8.5.1 Spike the surrogates into the blank. Extract and concentrate 
the blank using the same procedures and reagents used for the samples, 
LCS, and MS/MSD in the batch. Analyze the blank immediately after 
analysis of the LCS (section 8.4) and prior to analysis of the MS/MSD 
and samples to demonstrate freedom from contamination.
    8.5.2 If an analyte of interest is found in the blank: At a 
concentration greater than the MDL for the analyte, at a concentration 
greater than one-third the regulatory compliance limit, or at a 
concentration greater than one-tenth the concentration in a sample in 
the extraction batch, whichever is greater, analysis of samples must be 
halted, and the problem corrected. If the contamination is traceable to 
the extraction batch, samples affected by the blank must be re-extracted 
and the extracts re-analyzed. If, however, continued re-testing results 
in repeated blank contamination, the laboratory must document and report 
the failures (e.g., as qualifiers on results), unless the failures are 
not required to be reported as determined by the regulatory/control 
authority. Results associated with blank contamination for an analyte 
regulated in a discharge cannot be used to demonstrate regulatory 
compliance. QC failures do not relieve a discharger or permittee of 
reporting timely results.
    8.6 Internal standards responses.
    8.6.1 Calibration verification--The responses (GC peak heights or 
areas) of the internal standards in the calibration verification must be 
within 50% to 200% (1/2 to 2x) of their respective responses in the mid-
point calibration standard. If they are not, repeat the calibration 
verification (Section 7.4) test or perform and document system repair. 
Subsequent to repair, repeat the calibration verification. If the 
responses are still not within 50% to 200%, re-calibrate the instrument 
(Section 7) and repeat the calibration verification test.
    8.6.2 Samples, blanks, LCSs, and MS/MSDs--The responses (GC peak 
heights or areas) of each internal standard in each sample, blank, and 
MS/MSD must be within 50% to 200% (1/2 to 2x) of its respective response 
in the LCS for the extraction batch. If, as a group, all internal 
standards are not within this range, perform and document system repair, 
repeat the calibration verification (section 8.4), and re-analyze the 
affected samples. If a single internal standard is not within the 50% to 
200% range, use an alternate internal standard for quantitation of the 
analyte referenced to the affected internal standard. It may be 
necessary to use the data system to calculate a new response factor from 
calibration data for the alternate internal standard/analyte pair. If an 
internal standard fails the 50-200% criteria and no analytes are 
detected in the sample, ignore the failure or report it if required by 
the regulatory/control authority.
    8.7 Surrogate recoveries--The laboratory must evaluate surrogate 
recovery data in each sample against its in-house surrogate recovery 
limits. The laboratory may use 60-

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140% as interim acceptance criteria for recoveries for surrogates not 
listed in Table 8. At least 80% of the surrogates must meet the 60-140% 
interim criteria until in-house limits are developed. Alternatively, 
surrogate recovery limits may be developed from laboratory control 
charts, but such limits must be at least as restrictive as those in 
Table 8. Spike the surrogates into all samples, blanks, LCSs, and MS/
MSDs. Compare surrogate recoveries against the QC acceptance criteria in 
Table 8 and/or those developed in section 7.3.3 or 8.4.5. If any 
recovery fails its criteria, attempt to find and correct the cause of 
the failure. See section 8.1.7 for disposition of failures.
    8.8 DDT and endrin decomposition (breakdown)--If DDT and/or endrin 
are to be analyzed using this method, the DDT/endrin decomposition test 
in section 13.8 must be performed to reliably quantify these two 
pesticides.
    8.9 As part of the QC program for the laboratory, control charts or 
statements of accuracy for wastewater samples must be assessed and 
records maintained (40 CFR 136.7(c)(1)(viii)). After analysis of five or 
more spiked wastewater samples as in section 8.3, calculate the average 
percent recovery (PX) and the standard deviation of the 
percent recovery (sp). Express the accuracy assessment as a percent 
interval from PX -2sp to PX +2sp. For example, if 
PX = 90% and sp = 10%, the accuracy interval is expressed as 
70-110%. Update the accuracy assessment for each analyte on a regular 
basis (e.g., after each 5-10 new accuracy measurements). If desired, 
statements of accuracy for laboratory performance, independent of 
performance on samples, may be developed using LCSs.
    8.10 It is recommended that the laboratory adopt additional quality 
assurance practices for use with this method. The specific practices 
that are most productive depend upon the needs of the laboratory and the 
nature of the samples. Field duplicates may be analyzed to assess the 
precision of environmental measurements. Whenever possible, the 
laboratory should analyze standard reference materials and participate 
in relevant performance evaluation studies.

            9. Sample Collection, Preservation, and Handling

    9.1 Collect samples as grab samples in amber or clear glass bottles, 
or in refrigerated bottles using automatic sampling equipment. If clear 
glass is used, protect samples from light. Collect 1-L of ambient 
waters, effluents, and other aqueous samples. If the sensitivity of the 
analytical system is sufficient, a smaller volume (e.g., 250 mL), but no 
less than 100 mL, may be used. Conventional sampling practices 
(Reference 15) should be followed, except that the bottle must not be 
pre-rinsed with sample before collection. Automatic sampling equipment 
must be as free as possible of polyvinyl chloride or other tubing or 
other potential sources of contamination. If needed, collect additional 
sample(s) for the MS/MSD (section 8.3).
    9.2 Ice or refrigerate samples at <=6 [deg]C from the time of 
collection until extraction, but do not freeze. If residual chlorine is 
present, add 80 mg of sodium thiosulfate per liter of sample and mix 
well. Any method suitable for field use may be employed to test for 
residual chlorine (Reference 16). Add more sodium sulfate if 80 mg/L is 
insufficient but do not add excess sodium thiosulfate. If sodium 
thiosulfate interferes in the determination of the analytes, an 
alternate preservative (e.g., ascorbic acid or sodium sulfite) may be 
used. If preservative has been added, shake the sample vigorously for 
one minute. Maintain the hermetic seal on the sample bottle until time 
of analysis.
    9.3 All samples must be extracted within 7 days of collection and 
sample extracts must be analyzed within 40 days of extraction.

                             10. Extraction

    10.1 This section contains procedures for separatory funnel liquid-
liquid extraction (SFLLE) and continuous liquid-liquid extraction 
(CLLE). SFLLE is faster, but may not be as effective as CLLE for 
recovery of polar analytes such as phenol. SFLLE is labor intensive and 
may result in formation of emulsions that are difficult to break. CLLE 
is less labor intensive, avoids emulsion formation, but requires more 
time (18-24 hours) and more hood space, and may require more solvent. 
The procedures assume base-neutral extraction followed by acid 
extraction. For some matrices and analytes of interest, improved results 
may be obtained by acid-neutral extraction followed by base extraction. 
A single acid or base extraction may also be performed. If an extraction 
scheme alternate to base-neutral followed by acid extraction is used, 
all QC tests must be performed and all QC acceptance criteria must be 
met with that extraction scheme as an integral part of this method. 
Solid-phase extraction (SPE) may be used provided requirements in 
section 8.1.2 are met.
    10.2 Separatory funnel liquid-liquid extraction (SFLLE) and extract 
concentration.
    10.2.1 The SFLLE procedure below assumes a sample volume of 1 L. 
When a different sample volume is extracted, adjust the volume of 
methylene chloride accordingly.
    10.2.2 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Pour the entire sample into the 
separatory funnel. Pipet the surrogate standard spiking solution 
(section 6.8) into the separatory funnel. If the sample will be used for 
the LCS or MS or MSD, pipet the

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appropriate check sample concentrate (section 8.2.1 or 8.3.2) into the 
separatory funnel. Mix well. Check the pH of the sample with wide-range 
pH paper and adjust to pH 11-13 with sodium hydroxide solution.
    10.2.3 Add 60 mL of methylene chloride to the sample bottle, seal, 
and shake for approximately 30 seconds to rinse the inner surface. 
Transfer the solvent to the separatory funnel and extract the sample by 
shaking the funnel for two minutes with periodic venting to release 
excess pressure. Allow the organic layer to separate from the water 
phase for a minimum of 10 minutes. If the emulsion interface between 
layers is more than one-third the volume of the solvent layer, the 
analyst must employ mechanical techniques to complete the phase 
separation. The optimum technique depends upon the sample, but may 
include stirring, filtration of the emulsion through glass wool or 
phase-separation paper, salting, centrifugation, or other physical 
methods. Collect the methylene chloride extract in a flask. If the 
emulsion cannot be broken (recovery of <80% of the methylene chloride), 
transfer the sample, solvent, and emulsion into a continuous extractor 
and proceed as described in section 10.3.
    10.2.4 Add a second 60-mL volume of methylene chloride to the sample 
bottle and repeat the extraction procedure a second time, combining the 
extracts in the Erlenmeyer flask. Perform a third extraction in the same 
manner.
    10.2.5 Adjust the pH of the aqueous phase to less than 2 using 
sulfuric acid. Serially extract the acidified aqueous phase three times 
with 60 mL aliquots of methylene chloride. Collect and combine the 
extracts in a flask in the same manner as the base/neutral extracts.
    Note: Base/neutral and acid extracts may be combined for 
concentration and analysis provided all QC tests are performed and all 
QC acceptance criteria met for the analytes of interest with the 
combined extract as an integral part of this method, and provided that 
the analytes of interest are as reliably identified and quantified as 
when the extracts are analyzed separately. If doubt exists as to whether 
identification and quantitation will be affected by use of a combined 
extract, the fractions must be analyzed separately.
    10.2.6 For each fraction or the combined fractions, assemble a 
Kuderna-Danish (K-D) concentrator by attaching a 10-mL concentrator tube 
to a 500-mL evaporative flask. Other concentration devices or techniques 
may be used in place of the K-D concentrator so long as the requirements 
in section 8.2 are met.
    10.2.7 For each fraction or the combined fractions, pour the extract 
through a solvent-rinsed drying column containing about 10 cm of 
anhydrous sodium sulfate, and collect the extract in the K-D 
concentrator. Rinse the Erlenmeyer flask and column with 20-30 mL of 
methylene chloride to complete the quantitative transfer.
    10.2.8 Add one or two clean boiling chips and attach a three-ball 
Snyder column to the evaporative flask for each fraction (section 
10.2.7). Pre-wet the Snyder column by adding about 1 mL of methylene 
chloride to the top. Place the K-D apparatus on a hot water bath (60-65 
[deg]C) so that the concentrator tube is partially immersed in the hot 
water, and the entire lower rounded surface of the flask is bathed with 
hot vapor. Adjust the vertical position of the apparatus and the water 
temperature as required to complete the concentration in 15-20 minutes. 
At the proper rate of distillation, the balls of the column will 
actively chatter but the chambers will not flood with condensed solvent. 
When the apparent volume of liquid reaches 1 mL or other determined 
amount, remove the K-D apparatus from the water bath and allow to drain 
and cool for at least 10 minutes. Remove the Snyder column and rinse the 
flask and its lower joint into the concentrator tube with 1-2 mL of 
methylene chloride. A 5-mL syringe is recommended for this operation. If 
the sample will be cleaned up, reserve the K-D apparatus for 
concentration of the cleaned up extract. Adjust the volume to 5 mL with 
methylene chloride and proceed to section 11 for cleanup; otherwise, 
further concentrate the extract for GC/MS analysis per section 10.2.9 or 
10.2.10.
    10.2.9 Micro Kuderna-Danish concentration--Add another one or two 
clean boiling chips to the concentrator tube for each fraction and 
attach a two-ball micro-Snyder column. Pre-wet the Snyder column by 
adding about 0.5 mL of methylene chloride to the top. Place the K-D 
apparatus on a hot water bath (60-65 [deg]C) so that the concentrator 
tube is partially immersed in hot water. Adjust the vertical position of 
the apparatus and the water temperature as required to complete the 
concentration in 5-10 minutes. At the proper rate of distillation the 
balls of the column will actively chatter but the chambers will not 
flood with condensed solvent. When the apparent volume of liquid reaches 
about 1 mL or other determined amount, remove the K-D apparatus from the 
water bath and allow it to drain and cool for at least 10 minutes. 
Remove the Snyder column and rinse the flask and its lower joint into 
the concentrator tube with approximately 0.2 mL of or methylene 
chloride. Adjust the final volume to 1.0 mL or a volume appropriate to 
the sensitivity desired (e.g., to meet lower MDLs or for selected ion 
monitoring). Record the volume, stopper the concentrator tube and store 
refrigerated if further processing will not be performed immediately. If 
the extracts will be stored longer than two days, they should be 
transferred to

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fluoropolymer-lined screw-cap vials and labeled base/neutral or acid 
fraction as appropriate. Mark the level of the extract on the vial so 
that solvent loss can be detected.
    10.2.10 Nitrogen evaporation and solvent exchange--Extracts may be 
concentrated for analysis using nitrogen evaporation in place of micro 
K-D concentration (section 10.2.9). Extracts that have been cleaned up 
using sulfur removal (section 11.2) and are ready for analysis are 
exchanged into methylene chloride.
    10.2.10.1 Transfer the vial containing the sample extract to the 
nitrogen evaporation (blowdown) device (section 5.8). Lower the vial 
into the water bath and begin concentrating. If the more volatile 
analytes (section 1.2) are to be concentrated, use room temperature for 
concentration; otherwise, a slightly elevated (e.g., 30-45 [deg]C) may 
be used. During the solvent evaporation process, keep the solvent level 
below the water level of the bath and do not allow the extract to become 
dry. Adjust the flow of nitrogen so that the surface of the solvent is 
just visibly disturbed. A large vortex in the solvent may cause analyte 
loss.
    10.2.10.2 Extracts to be solvent exchanged--When the volume of the 
liquid is approximately 200 [micro]L, add 2 to 3 mL of methylene 
chloride and continue concentrating to approximately 100 [micro]L. 
Repeat the addition of solvent and concentrate once more. Adjust the 
final extract volume to be consistent with the volume extracted and the 
sensitivity desired.
    10.2.10.3 For extracts that have been cleaned up by GPC and that are 
to be concentrated to a nominal volume of 1 mL, adjust the final volume 
to compensate the GPC loss. For a 50% GPC loss, concentrate the extract 
to 1/2000 of the volume extracted. For example, if the volume extracted 
is 950 mL, adjust the final volume to 0.48 mL. For extracts that have 
not been cleaned up by GPC and are to be concentrated to a nominal 
volume of 1.0 mL, adjust the final extract volume to 1/1000 of the 
volume extracted. For example, if the volume extracted is 950 mL, adjust 
the final extract volume to 0.95 mL. Alternative means of compensating 
the loss during GPC are acceptable so long as they produce results as 
accurate as results produced using the procedure detailed in this 
Section. An alternative final volume may be used, if desired, and the 
calculations adjusted accordingly.
    Note: The difference in the volume fraction for an extract cleaned 
up by GPC accounts for the loss in GPC cleanup. Also, by preserving the 
ratio between the volume extracted and the final extract volume, the 
concentrations and detection limits do not need to be adjusted for 
differences in the volume extracted and the extract volume.
    10.2.11 Transfer the concentrated extract to a vial with 
fluoropolymer-lined cap. Seal the vial and label with the sample number. 
Store in the dark at room temperature until ready for GC analysis. If GC 
analysis will not be performed on the same day, store the vial in the 
dark at <=6 [deg]C. Analyze the extract by GC/MS per the procedure in 
section 12.
    10.2.12 Determine the original sample volume by refilling the sample 
bottle to the mark and transferring the liquid to an appropriately sized 
graduated cylinder. For sample volumes on the order of 1000 mL, record 
the sample volume to the nearest 10 mL; for sample volumes on the order 
of 100 mL, record the volume to the nearest 1 mL. Sample volumes may 
also be determined by weighing the container before and after filling to 
the mark with water.
    10.3 Continuous liquid/liquid extraction (CLLE).
    Note: With CLLE, phenol, 2,4-dimethyl phenol, and some other 
analytes may be preferentially extracted into the base-neutral fraction. 
Determine an analyte in the fraction in which it is identified and 
quantified most reliably. Also, the short-chain phthalate esters (e.g., 
dimethyl phthalate, diethyl phthalate) and some other compounds may 
hydrolyze during prolonged exposure to basic conditions required for 
continuous extraction, resulting in low recovery of these analytes. When 
these analytes are of interest, their recovery may be improved by 
performing the acid extraction first.
    10.3.1 Use CLLE when experience with a sample from a given source 
indicates an emulsion problem, or when an emulsion is encountered during 
SFLLE. CLLE may be used for all samples, if desired.
    10.3.2 Mark the water meniscus on the side of the sample bottle for 
later determination of sample volume. Check the pH of the sample with 
wide-range pH paper and adjust to pH 11-13 with sodium hydroxide 
solution. Transfer the sample to the continuous extractor. Pipet 
surrogate standard spiking solution (section 6.8) into the sample. If 
the sample will be used for the LCS or MS or MSD, pipet the appropriate 
check sample concentrate (section 8.2.1 or 8.3.2) into the extractor. 
Mix well. Add 60 mL of methylene chloride to the sample bottle, seal, 
and shake for 30 seconds to rinse the inner surface. Transfer the 
solvent to the extractor.
    10.3.3 Repeat the sample bottle rinse with an additional 50-100 mL 
portion of methylene chloride and add the rinse to the extractor.
    10.3.4 Add a suitable volume of methylene chloride to the distilling 
flask (generally 200-500 mL), add sufficient reagent water to ensure 
proper operation, and extract for 18-24 hours. A shorter or longer 
extraction time may be used if all QC acceptance criteria are met. Test 
and, if necessary, adjust the pH of the water during the second or third 
hour of the extraction. After extraction, allow the apparatus to cool, 
then detach the distilling flask. Dry, concentrate, and seal the extract

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per sections 10.2.6 through 10.2.11. See the note at section 10.2.5 
regarding combining extracts of the base/neutral and acid fractions.
    10.3.5 Charge the distilling flask with methylene chloride and 
attach it to the continuous extractor. Carefully, while stirring, adjust 
the pH of the aqueous phase to less than 2 using sulfuric acid. Extract 
for 18-24 hours. A shorter or longer extraction time may be used if all 
QC acceptance criteria are met. Test and, if necessary, adjust the pH of 
the water during the second or third hour of the extraction. After 
extraction, allow the apparatus to cool, then detach the distilling 
flask. Dry, concentrate, and seal the extract per sections 10.2.6 
through 10.2.11. Determine the sample volume per section 10.2.12.

                           11. Extract Cleanup

    Note: Cleanup may not be necessary for relatively clean samples 
(e.g., treated effluents, groundwater, drinking water). If particular 
circumstances require the use of a cleanup procedure, the laboratory may 
use any or all of the procedures below or any other appropriate 
procedure. Before using a cleanup procedure, the laboratory must 
demonstrate that the requirements of section 8.1.2 can be met using the 
cleanup procedure as an integral part of this method.

    11.1 Gel permeation chromatography (GPC).
    11.1.1 Calibration.
    11.1.1.1 Load the calibration solution (section 6.12) into the 
sample loop.
    11.1.1.2 Inject the calibration solution and record the signal from 
the detector. The elution pattern will be corn oil, bis(2-ethylhexyl) 
phthalate, pentachlorophenol, perylene, and sulfur.
    11.1.1.3 Set the ``dump time'' to allow 85% removal of 
the corn oil and 85% collection of the phthalate.
    11.1.1.4 Set the ``collect time'' to the peak minimum between 
perylene and sulfur.
    11.1.1.5 Verify calibration with the calibration solution after 
every 20 or fewer extracts. Calibration is verified if the recovery of 
the pentachlorophenol is greater than 85%. If calibration is not 
verified, recalibrate using the calibration solution, and re-extract and 
clean up the preceding extracts using the calibrated GPC system.
    11.1.2 Extract cleanup--GPC requires that the column not be 
overloaded. The column specified in this method is designed to handle a 
maximum of 0.5 g of high molecular weight material in a 5-mL extract. If 
the extract is known or expected to contain more than 0.5 g, the extract 
is split into fractions for GPC and the fractions are combined after 
elution from the column. The solids content of the extract may be 
obtained gravimetrically by evaporating the solvent from a 50-[micro]L 
aliquot.
    11.1.2.1 Filter the extract or load through the filter holder to 
remove particulates. Load the extract into the sample loop. The maximum 
capacity of the column is 0.5-1.0 g. If necessary, split the extract 
into multiple aliquots to prevent column overload.
    11.1.2.2 Elute the extract using the calibration data determined in 
Section 11.1.1. Collect the eluate in the K-D apparatus reserved in 
section 10.2.8.
    11.1.3 Concentrate the cleaned up extract per sections 10.2.8 and 
10.2.9 or 10.2.10.
    11.1.4 Rinse the sample loading tube thoroughly with methylene 
chloride between extracts to prepare for the next sample.
    11.1.5 If a particularly dirty extract is encountered, run a 
methylene chloride blank through the system to check for carry-over.
    11.2 Sulfur removal.
    Note: Separate procedures using copper or TBA sulfite are provided 
in this section for sulfur removal. They may be used separately or in 
combination, if desired.
    11.2.1 Removal with copper (Reference 17).
    Note: If an additional compound (Table 3) is to be determined; 
sulfur is to be removed; copper will be used for sulfur removal; and a 
sulfur matrix is known or suspected to be present, the laboratory must 
demonstrate that the additional compound can be successfully extracted 
and treated with copper in the sulfur matrix. Some of the additional 
compounds (Table 3) are known not to be amenable to sulfur removal with 
copper (e.g., Atrazine and Diazinon).
    11.2.1.1 Quantitatively transfer the extract from section 10.2.8 to 
a 40- to 50-mL flask or bottle. If there is evidence of water in the 
concentrator tube after the transfer, rinse the tube with small portions 
of hexane:acetone (40:60) and add to the flask or bottle. Mark and set 
aside the concentrator tube for use in re-concentrating the extract.
    11.2.1.2 Add 10-20 g of granular anhydrous sodium sulfate to the 
flask. Swirl to dry the extract.
    11.2.1.3 Add activated copper (section 6.13.1.4) and allow to stand 
for 30--60 minutes, swirling occasionally. If the copper does not remain 
bright, add more and swirl occasionally for another 30-60 minutes.
    11.2.1.4 After drying and sulfur removal, quantitatively transfer 
the extract to a nitrogen-evaporation vial or tube and proceed to 
section 10.2.10 for nitrogen evaporation and solvent exchange, taking 
care to leave the sodium sulfate and copper in the flask.
    11.2.2 Removal with TBA sulfite.
    11.2.2.1 Using small volumes of hexane, quantitatively transfer the 
extract to a 40- to 50-mL centrifuge tube with fluoropolymer-lined screw 
cap.
    11.2.2.2 Add 1-2 mL of TBA sulfite reagent (section 6.13.2.4), 2-3 
mL of 2-propanol, and approximately 0.7 g of sodium sulfite (section 
6.13.2.2) crystals to the tube. Cap and

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shake for 1-2 minutes. If the sample is colorless or if the initial 
color is unchanged, and if clear crystals (precipitated sodium sulfite) 
are observed, sufficient sodium sulfite is present. If the precipitated 
sodium sulfite disappears, add more crystalline sodium sulfite in 
approximately 0.5 g portions until a solid residue remains after 
repeated shaking.
    11.2.2.3 Add 5-10 mL of reagent water and shake for 1-2 minutes. 
Centrifuge to settle the solids.
    11.2.2.4 Quantitatively transfer the hexane (top) layer through a 
small funnel containing a few grams of granular anhydrous sodium sulfate 
to a nitrogen-evaporation vial or tube and proceed to section 10.2.10 
for nitrogen evaporation and solvent exchange.

                12. Gas Chromatography/Mass Spectrometry

    12.1 Establish the operating conditions in Table 4 or 5 for analysis 
of a base/neutral or acid extract, respectively. For analysis of a 
combined extract (section 10.2.5, note), use the operating conditions in 
Table 4 MDLs and MLs for the analytes are given in Tables 1, 2, and 3. 
Retention times for many of the analytes are given in Tables 4 and 5. 
Examples of the separations achieved are shown in Figure 2 for the 
combined extract. Alternative columns or chromatographic conditions may 
be used if the requirements of section 8.2 are met. Verify system 
performance per section 13.
    12.2 Analysis of a standard or extract.
    12.2.1 Bring the standard or concentrated extract (section 10.2.9 or 
10.2.11) to room temperature and verify that any precipitate has 
redissolved. Verify the level on the extract and bring to the mark with 
solvent if required.
    12.2.2 Add the internal standard solution (section 6.9) to the 
extract. Mix thoroughly.
    12.2.3 Inject an appropriate volume of the sample extract or 
standard solution using split, splitless, solvent purge, large-volume, 
or on-column injection. If the sample is injected manually the solvent-
flush technique should be used. The injection volume depends upon the 
technique used and the ability to meet MDLs or reporting limits for 
regulatory compliance. Injected volumes must be the same for standards 
and sample extracts. Record the volume injected to two significant 
figures.
    12.2.3.1 Start the GC column oven program upon injection. Start MS 
data collection after the solvent peak elutes. Stop data collection 
after benzo(ghi)perylene elutes for the base/neutral or combined 
fractions, or after pentachlorophenol elutes for the acid fraction. 
Return the column to the initial temperature for analysis of the next 
standard solution or extract.
    12.2.3.2 If the concentration of any analyte of interest exceeds the 
calibration range, either extract and analyze a smaller sample volume, 
or dilute and analyze the diluted extract after bringing the 
concentrations of the internal standards to the levels in the undiluted 
extract.
    12.2.4 Perform all qualitative and quantitative measurements as 
described in Sections 14 and 15. When standards and extracts are not 
being used for analyses, store them refrigerated at <=6 [deg]C protected 
from light in screw-cap vials equipped with un-pierced fluoropolymer-
lined septa.

                          13. Performance Tests

    13.1 At the beginning of each 12-hour shift during which standards 
or extracts will be analyzed, perform the tests in sections 13.2-13.4 to 
verify system performance. If an extract is concentrated for greater 
sensitivity (e.g., by SIM), all tests must be performed at levels 
consistent with the reduced extract volume.
    13.2 DFTPP--Inject the DFTPP standard (section 6.10) and verify that 
the criteria for DFTPP in section 7.2.1.1 and Table 9A (Reference 18) 
for a quadrupole MS, or Table 9B (Reference 19) for a time-of-flight MS, 
are met.
    13.3 GC resolution--The resolution should be verified on the mid-
point concentration of the initial calibration as well as the laboratory 
designated continuing calibration verification level if closely eluting 
isomers are to be reported (e.g., benzo(b)fluoranthene and 
benzo(k)fluoranthene). Sufficient gas chromatographic resolution is 
achieved if the height of the valley between two isomer peaks is less 
than 50% of the average of the two peak heights.
    13.4 Calibration verification--Verify calibration per sections 7.3 
and Table 6.
    13.5 Peak tailing--Verify the tailing factor specifications are met 
per Section 7.2.1.1.
    13.6 Laboratory control sample and blank--Analyze the extracts of 
the LCS and blank at the beginning of analyses of samples in the 
extraction batch (section 3.1). The LCS must meet the requirements in 
section 8.4, and the blank must meet the requirements in section 8.5 
before sample extracts may be analyzed.
    13.7 Analysis of DFTPP, the DDT/Endrin decomposition test (if used), 
the LCS, and the blank are outside of the 12-hour analysis shift 
(section 3.1). The total time for DFTPP, DDT/Endrin, the LCS, the blank, 
and the 12-hour shift must not exceed 15 hours.
    13.8 Decomposition of DDT and endrin--If DDT and/or endrin are to be 
determined, this test must be performed prior to calibration 
verification (section 13.4). The QC acceptance criteria (section 13.8.3) 
must be met before analyzing samples for DDE and/or Endrin. DDT 
decomposes to DDE and DDD. Endrin decomposes to endrin aldehyde and 
endrin ketone.
    13.8.1 Inject 1 [micro]L of the DDT and endrin decomposition 
solution (section 6.14). As

[[Page 286]]

noted in section 6.14, other injection volumes may be used as long as 
the concentrations of DDT and endrin in the solution are adjusted to 
introduce the masses of the two analytes into the instrument that are 
listed in section 6.14.
    13.8.2 Measure the areas of the peaks for DDT, DDE, DDD, Endrin, 
Endrin aldehyde, and Endrin ketone. Calculate the percent breakdown as 
shown in the equations below:
[GRAPHIC] [TIFF OMITTED] TR28AU17.015

    13.8.3 Both the % breakdown of DDT and of Endrin must be less than 
20%, otherwise the system is not performing acceptably for DDT and 
endrin. In this case, repair the GC column system that failed and repeat 
the performance tests (sections 13.2 to 13.6) until the specification is 
met.

    Note: DDT and endrin decomposition are usually caused by 
accumulation of particulates in the injector and in the front end of the 
column. Cleaning and silanizing the injection port liner, and breaking 
off a short section of the front end of the column will usually 
eliminate the decomposition problem. Either of these corrective actions 
may affect retention times, GC resolution, and calibration linearity.

                     14. Qualitative Identification

    14.1 Identification is accomplished by comparison of data from 
analysis of a sample or blank with data stored in the GC/MS data system 
(sections 5.6.5 and 7.2.1.2). Identification of an analyte is confirmed 
per sections 14.1.1 through 14.1.4.
    14.1.1 The signals for the quantitation and secondary m/z's stored 
in the data system for each analyte of interest must be present and must 
maximize within the same two consecutive scans.
    14.1.2 The retention time for the analyte should be within  10 seconds of the analyte in the calibration 
verification run at the beginning of the shift (section 7.3 or 13.4).
    Note: Retention time windows other than  10 
seconds may be appropriate depending on the performance of the gas 
chromatograph or observed retention time drifts due to certain types of 
matrix effects. Relative retention time (RRT) may be used as an 
alternative to absolute retention times if retention time drift is a 
concern. RRT is a unitless quantity (see Sec. 22.2), although some 
procedures refer to ``RRT units'' in providing the specification for the 
agreement between the RRT values in the sample and the calibration 
verification or other standard. When significant retention time drifts 
are observed, dilutions or spiked samples may help the analyst determine 
the effects of the matrix on elution of the target analytes and to 
assist in qualitative identification.
    14.1.3 Either the background corrected EICP areas, or the corrected 
relative intensities of the mass spectral peaks at the GC peak maximum, 
must agree within 50% to 200% (1/2 to 2 times) for the quantitation and 
secondary m/z's in the reference mass spectrum stored in the data system 
(section 7.2.1.2), or from a reference library. For example, if a peak 
has an intensity of 20% relative to the base peak, the analyte is 
identified if the intensity of the peak in the sample is in the range of 
10% to 40% of the base peak. If identification is ambiguous, an 
experienced spectrometrist (section 1.7) must determine the presence or 
absence of the compound.
    14.2 Structural isomers that produce very similar mass spectra 
should be identified as individual isomers if they have sufficiently 
different gas chromatographic retention times. Sufficient gas 
chromatographic resolution is achieved if the height of the valley 
between two isomer peaks is less than 50% of the average of the two peak 
heights. Otherwise, structural isomers are identified as isomeric pairs.

                            15. Calculations

    15.1 When an analyte has been identified, quantitation of that 
analyte is based on the integrated abundance from the EICP of the 
primary characteristic m/z in Table 4 or 5. Calculate the concentration 
in the extract

[[Page 287]]

using the response factor (RF) determined in Section 7.2.2 and Equation 
2. If the concentration of an analyte exceeds the calibration range, 
dilute the extract by the minimum amount to bring the concentration into 
the calibration range, and re-analyze the extract. Determine a dilution 
factor (DF) from the amount of the dilution. For example, if the extract 
is diluted by a factor of 2, DF = 2.
[GRAPHIC] [TIFF OMITTED] TR28AU17.016

where:

Cex = Concentration of the analyte in the extract, in 
          [micro]g/mL, and the other terms are as defined in section 
          7.2.2.
    Calculate the concentration of the analyte in the sample using the 
concentration in the extract, the extract volume, the sample volume, and 
the dilution factor, per Equation 3:
[GRAPHIC] [TIFF OMITTED] TR28AU17.017

where:

Csamp = Concentration of the analyte in the sample
Cex = Concentration of the analyte in the extract, in 
          [micro]g/mL
Vex = Volume of extract (mL)
Vs = Volume of sample (L)
DF = Dilution factor

    15.2 Reporting of results. As noted in section 1.4.1, EPA has 
promulgated this method at 40 CFR part 136 for use in wastewater 
compliance monitoring under the National Pollutant Discharge Elimination 
System (NPDES). The data reporting practices described here are focused 
on such monitoring needs and may not be relevant to other uses of the 
method.
    15.2.1 Report results for wastewater samples in [micro]g/L without 
correction for recovery. (Other units may be used if required by in a 
permit.) Report all QC data with the sample results.
    15.2.2 Reporting level. Unless specified otherwise by a regulatory 
authority or in a discharge permit, results for analytes that meet the 
identification criteria are reported down to the concentration of the ML 
established by the laboratory through calibration of the instrument (see 
section 7.3.2 and the glossary for the derivation of the ML). EPA 
considers the terms ``reporting limit,'' ``quantitation limit,'' ``limit 
of quantitation,'' and ``minimum level'' to be synonymous.
    15.2.2.1 Report a result for each analyte in each field sample or QC 
standard at or above the ML to 3 significant figures. Report a result 
for each analyte found in each field sample or QC standard below the ML 
as ``ML'' where ML is the concentration of the analyte at the ML, or as 
required by the regulatory/control authority or permit. Report a result 
for each analyte in a blank at or above the MDL to 2 significant 
figures. Report a result for each analyte found in a blank below the MDL 
as ``MDL,'' where MDL is the concentration of the analyte at the MDL, or 
as required by the regulatory/control authority or permit.
    15.2.2.2 In addition to reporting results for samples and blanks 
separately, the concentration of each analyte in a blank associated with 
the sample may be subtracted from the result for that sample, but only 
if requested or required by a regulatory authority or in a permit. In 
this case, both the sample result and the blank results must be reported 
together.
    15.2.2.3 Report a result for an analyte found in a sample or extract 
that has been diluted at the least dilute level at which the area at the 
quantitation m/z is within the calibration range (i.e., above the ML for 
the analyte) and the MS/MSD recovery and RPD are within their respective 
QC acceptance criteria (Table 6). This may require reporting results for 
some analytes from different analyses.
    15.2.3 Results from tests performed with an analytical system that 
is not in control (i.e., that does not meet acceptance criteria for any 
QC test in this method) must be documented and reported (e.g., as a 
qualifier on results), unless the failure is not required to be reported 
as determined by the regulatory/control authority. Results associated 
with a QC failure cannot be used to demonstrate regulatory compliance. 
QC failures do not relieve a discharger or permittee of reporting

[[Page 288]]

timely results. If the holding time would be exceeded for a re-analysis 
of the sample, the regulatory/control authority should be consulted for 
disposition.

                         16. Method Performance

    16.1 The basic version of this method was tested by 15 laboratories 
using reagent water, drinking water, surface water, and industrial 
wastewaters spiked at six concentrations over the range 5-1300 [micro]g/
L (Reference 2). Single operator precision, overall precision, and 
method accuracy were found to be directly related to the concentration 
of the analyte and essentially independent of the sample matrix. Linear 
equations to describe these relationships are presented in Table 7.
    16.2 As noted in section 1.1, this method was validated through an 
interlaboratory study in the early 1980s. However, the fundamental 
chemistry principles used in this method remain sound and continue to 
apply.
    16.3 A chromatogram of the combined acid/base/neutral calibration 
standard is shown in Figure 2.

                        17. Pollution Prevention

    17.1 Pollution prevention encompasses any technique that reduces or 
eliminates the quantity or toxicity of waste at the point of generation. 
Many opportunities for pollution prevention exist in laboratory 
operations. EPA has established a preferred hierarchy of environmental 
management techniques that places pollution prevention as the management 
option of first choice. Whenever feasible, the laboratory should use 
pollution prevention techniques to address waste generation. When wastes 
cannot be reduced at the source, the Agency recommends recycling as the 
next best option.
    17.2 The analytes in this method are used in extremely small amounts 
and pose little threat to the environment when managed properly. 
Standards should be prepared in volumes consistent with laboratory use 
to minimize the disposal of excess volumes of expired standards. This 
method utilizes significant quantities of methylene chloride. 
Laboratories are encouraged to recover and recycle this and other 
solvents during extract concentration.
    17.3 For information about pollution prevention that may be applied 
to laboratories and research institutions, consult Less is Better: 
Laboratory Chemical Management for Waste Reduction, available from the 
American Chemical Society's Department of Governmental Relations and 
Science Policy, 1155 16th Street NW., Washington DC 20036, 202-872-4477.

                          18. Waste Management

    18.1 The laboratory is responsible for complying with all Federal, 
State, and local regulations governing waste management, particularly 
the hazardous waste identification rules and land disposal restrictions, 
and to protect the air, water, and land by minimizing and controlling 
all releases from fume hoods and bench operations. Compliance is also 
required with any sewage discharge permits and regulations. An overview 
of requirements can be found in Environmental Management Guide for Small 
Laboratories (EPA 233-B-98-001).
    18.2 Samples at pH <2, or pH 12, are hazardous and must 
be handled and disposed of as hazardous waste, or neutralized and 
disposed of in accordance with all federal, state, and local 
regulations. It is the laboratory's responsibility to comply with all 
federal, state, and local regulations governing waste management, 
particularly the hazardous waste identification rules and land disposal 
restrictions. The laboratory using this method has the responsibility to 
protect the air, water, and land by minimizing and controlling all 
releases from fume hoods and bench operations. Compliance is also 
required with any sewage discharge permits and regulations. For further 
information on waste management, see ``The Waste Management Manual for 
Laboratory Personnel,'' also available from the American Chemical 
Society at the address in section 17.3.
    18.3 Many analytes in this method decompose above 500 [ordm]C. Low-
level waste such as absorbent paper, tissues, and plastic gloves may be 
burned in an appropriate incinerator. Gross quantities of neat or highly 
concentrated solutions of toxic or hazardous chemicals should be 
packaged securely and disposed of through commercial or governmental 
channels that are capable of handling these types of wastes.
    18.4 For further information on waste management, consult The Waste 
Management Manual for Laboratory Personnel and Less is Better-Laboratory 
Chemical Management for Waste Reduction, available from the American 
Chemical Society's Department of Government Relations and Science 
Policy, 1155 16th Street NW., Washington, DC 20036, 202-872-4477.

                             19. References

1. ``Sampling and Analysis Procedures for Screening of Industrial 
          Effluents for Priority Pollutants,'' U.S. Environmental 
          Protection Agency, Environmental Monitoring and Support 
          Laboratory, Cincinnati, Ohio 45268, March 1977, Revised April 
          1977.
2. ``EPA Method Study 30, Method 625, Base/Neutrals, Acids, and 
          Pesticides,'' EPA 600/4-84-053, National Technical Information 
          Service, PB84-206572, Springfield, Virginia 22161, June 1984.
3. 40 CFR part 136, appendix B.

[[Page 289]]

4. Olynyk, P., Budde, W.L. and Eichelberger, J.W. ``Method Detection 
          Limit for Methods 624 and 625,'' Unpublished report, May 14, 
          1980.
5. Annual Book of ASTM Standards, Volume 11.02, D3694-96, ``Standard 
          Practices for Preparation of Sample Containers and for 
          Preservation of Organic Constituents,'' American Society for 
          Testing and Materials, Philadelphia.
6. Solutions to Analytical Chemistry Problems with Clean Water Act 
          Methods, EPA 821-R-07-002, March 2007.
7. ``Carcinogens-Working With Carcinogens,'' Department of Health, 
          Education, and Welfare, Public Health Service, Center for 
          Disease Control, National Institute for Occupational Safety 
          and Health, Publication No. 77-206, August 1977.
8. ``OSHA Safety and Health Standards, General Industry,'' (29 CFR part 
          1910), Occupational Safety and Health Administration, OSHA 
          2206 (Revised, January 1976).
9. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
          Society Publication, Committee on Chemical Safety, 7th 
          Edition, 2003.
10. Johnson, R.A., and Wichern, D.W., ``Applied Multivariate Statistical 
          Analysis,'' 3rd edition, Prentice Hall, Englewood Cliffs, NJ, 
          1992.
11. 40 CFR 136.6(b)(4)(x).
12. 40 CFR 136.6(b)(2)(i).
13. Protocol for EPA Approval of New Methods for Organic and Inorganic 
          Analytes in Wastewater and Drinking Water (EPA-821-B-98-003) 
          March 1999.
14. Provost, L.P. and Elder, R.S. ``Interpretation of Percent Recovery 
          Data,'' American Laboratory, 15, 58-63 (1983). (The value 2.44 
          used in the equation in section 8.3.3 is two times the value 
          1.22 derived in this report.)
15. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
          Practices for Sampling Water,'' American Society for Testing 
          and Materials, Philadelphia.
16. 40 CFR 136.3(a), Table IB, Chlorine--Total Residual.
17. ``Manual of Analytical Methods for the Analysis of Pesticides in 
          Human and Environmental Samples,'' EPA-600/8-80-038, U.S. 
          Environmental Protection Agency, Health Effects Research 
          Laboratory, Research Triangle Park, North Carolina.
18. Eichelberger, J.W., Harris, L.E., and Budde, W.L. ``Reference 
          Compound to Calibrate Ion Abundance Measurement in Gas 
          Chromatography-Mass Spectrometry,'' Analytical Chemistry, 47, 
          995 (1975).
19. Letter of approval of acceptance criteria for DFTPP for time-of-
          flight mass spectrometers from William A. Telliard and Herb 
          Brass of EPA to Jack Cochran of LECO Corporation, February 9, 
          2005.

                               20. Tables

                            Table 1--Non Pesticide/PCB Base/Neutral Extractables \1\
----------------------------------------------------------------------------------------------------------------
                             Analyte                               CAS registry   MDL \4\ (ug/L)   ML \5\ (ug/L)
----------------------------------------------------------------------------------------------------------------
Acenaphthene....................................................         83-32-9             1.9             5.7
Acenaphthylene..................................................        208-96-8             3.5            10.5
Anthracene......................................................        120-12-7             1.9             5.7
Benzidine \2\...................................................         92-87-5              44             132
Benzo(a)anthracene..............................................         56-55-3             7.8            23.4
Benzo(a)pyrene..................................................         50-32-8             2.5             7.5
Benzo(b)fluoranthene............................................        205-99-2             4.8            14.4
Benzo(k)fluoranthene............................................        207-08-9             2.5             7.5
Benzo(ghi)perylene..............................................        191-24-2             4.1            12.3
Benzyl butyl phthalate..........................................         85-68-7             2.5             7.5
bis(2-Chloroethoxy)methane......................................        111-91-1             5.3            15.9
bis(2-Ethylhexyl)phthalate......................................        117-81-7             2.5             7.5
bis(2-Chloroisopropyl) ether (2,2'-Oxybis[1-chloropropane]).....        108-60-1             5.7            17.1
4-Bromophenyl phenyl ether......................................        101-55-3             1.9             5.7
2-Chloronaphthalene.............................................         91-58-7             1.9             5.7
4-Chlorophenyl phenyl ether.....................................       7005-72-3             4.2            12.6
Chrysene........................................................        218-01-9             2.5             7.5
Dibenz(a,h)anthracene...........................................         53-70-3             2.5             7.5
Di-n-butylphthalate.............................................         84-74-2             2.5             7.5
3,3'-Dichlorobenzidine..........................................         91-94-1            16.5            49.5
Diethyl phthalate...............................................         84-66-2             1.9             5.7
Dimethyl phthalate..............................................        131-11-3             1.6             4.8
2,4-Dinitrotoluene..............................................        121-14-2             5.7            17.1
2,6-Dinitrotoluene..............................................        606-20-2             1.9             5.7
Di-n-octylphthalate.............................................        117-84-0             2.5             7.5
Fluoranthene....................................................        206-44-0             2.2             6.6
Fluorene........................................................         86-73-7             1.9             5.7
Hexachlorobenzene...............................................        118-74-1             1.9             5.7
Hexachlorobutadiene.............................................         87-68-3             0.9             2.7
Hexachloroethane................................................         67-72-1             1.6             4.8
Indeno(1,2,3-cd)pyrene..........................................        193-39-5             3.7            11.1

[[Page 290]]

 
Isophorone......................................................         78-59-1             2.2             6.6
Naphthalene.....................................................         91-20-3             1.6             4.8
Nitrobenzene....................................................         98-95-3             1.9             5.7
N-Nitrosodi-n-propylamine \3\...................................        621-64-7              --              --
Phenanthrene....................................................         85-01-8             5.4            16.2
Pyrene..........................................................        129-00-0             1.9             5.7
1,2,4-Trichlorobenzene..........................................        120-82-1             1.9             5.7
----------------------------------------------------------------------------------------------------------------
\1\ All analytes in this table are Priority Pollutants (40 CFR part 423, appendix A).
\2\ Included for tailing factor testing.
\3\ See section 1.2.
\4\ MDL values from the 1984 promulgated version of Method 625.
\5\ ML = Minimum Level--see Glossary for definition and derivation.


                                         Table 2--Acid Extractables \1\
----------------------------------------------------------------------------------------------------------------
                             Analyte                               CAS registry   MDL \3\ (ug/L)   ML \4\ (ug/L)
----------------------------------------------------------------------------------------------------------------
4-Chloro-3-methylphenol.........................................         59-50-7             3.0             9.0
2-Chlorophenol..................................................         95-57-8             3.3             9.9
2,4-Dichlorophenol..............................................        120-83-2             2.7             8.1
2,4-Dimethylphenol..............................................        105-67-9             2.7             8.1
2,4-Dinitrophenol...............................................         51-28-5              42             126
2-Methyl-4,6-dinitrophenol......................................        534-52-1              24              72
2-Nitrophenol...................................................         88-75-5             3.6            10.8
4-Nitrophenol...................................................        100-02-7             2.4             7.2
Pentachlorophenol \2\...........................................         87-86-5             3.6            10.8
Phenol..........................................................        108-95-2             1.5             4.5
2,4,6-Trichlorophenol...........................................         88-06-2             2.7             8.1
----------------------------------------------------------------------------------------------------------------
\1\ All analytes in this table are Priority Pollutants (40 CFR part 423, appendix A).
\2\ See section 1.2; included for tailing factor testing.
\3\ MDL values from the 1984 promulgated version of Method 625.
\4\ ML = Minimum Level--see Glossary for definition and derivation.


                                Table 3--Additional Extractable Analytes \1\, \2\
----------------------------------------------------------------------------------------------------------------
                             Analyte                               CAS registry   MDL \7\ (ug/L)   ML \8\ (ug/L)
----------------------------------------------------------------------------------------------------------------
Acetophenone....................................................         98-86-2
2-Acetylaminofluorene...........................................         53-96-3
1-Acetyl-2-thiourea.............................................        591-08-2
Alachlor........................................................      15972-60-8
Aldrin \3\......................................................        309-00-2             1.9             5.7
Ametryn.........................................................        834-12-8
2-Aminoanthraquinone............................................        117-79-3
Aminoazobenzene.................................................         60-09-3
4-Aminobiphenyl.................................................         92-67-1
3-Amino-9-ethylcarbazole........................................        132-32-1
Anilazine.......................................................        101-05-3
Aniline.........................................................         62-53-3
o-Anisidine.....................................................         90-04-0
Aramite.........................................................        140-57-8
Atraton.........................................................       1610-17-9
Atrazine........................................................       1912-24-9
Azinphos-methyl.................................................         86-50-0
Barban..........................................................        101-27-9
Benzanthrone....................................................         82-05-3
Benzenethiol....................................................        108-98-5
Benzoic acid....................................................         65-85-0
2,3-Benzofluorene...............................................        243-17-4
p-Benzoquinone..................................................        106-51-4
Benzyl alcohol..................................................        100-51-6
alpha-BHC \3\,\4\...............................................        319-84-6
beta-BHC \3\....................................................        319-85-7             3.1             9.3
gamma-BHC (Lindane) \3\,\4\.....................................         58-89-8             4.2            12.6
delta-BHC \3\...................................................        319-86-8
Biphenyl........................................................         92-52-4
Bromacil........................................................        314-40-9
2-Bromochlorobenzene............................................        694-80-4
3-Bromochlorobenzene............................................        108-39-2

[[Page 291]]

 
Bromoxynil......................................................       1689-84-5
Butachlor.......................................................       2318-4669
Butylate........................................................       2008-41-5
n-C10 (n-decane)................................................        124-18-5
n-C12 (n-undecane)..............................................        112-40-2
n-C14 (n-tetradecane)...........................................        629-59-4
n-C16 (n-hexadecane)............................................        544-76-3
n-C18 (n-octadecane)............................................        593-45-3
n-C20 (n-eicosane)..............................................        112-95-8
n-C22 (n-docosane)..............................................        629-97-0
n-C24 (n-tetracosane)...........................................        646-31-1
n-C26 (n-hexacosane)............................................        630-01-3
n-C28 (n-octacosane)............................................        630-02-4
n-C30 (n-triacontane)...........................................        638-68-6
Captafol........................................................       2425-06-1
Captan..........................................................        133-06-2
Carbaryl........................................................         63-25-2
Carbazole.......................................................         86-74-8
Carbofuran......................................................       1563-66-2
Carboxin........................................................       5234-68-4
Carbophenothion.................................................        786-19-6
Chlordane \3\,\5\...............................................         57-74-9
bis(2-Chloroethyl) ether \3\,\4\................................        111-44-4             5.7            17.1
Chloroneb.......................................................       2675-77-6
4-Chloroaniline.................................................        106-47-8
Chlorobenzilate.................................................        510-15-6
Chlorfenvinphos.................................................        470-90-6
4-Chloro-2-methylaniline........................................         95-69-2
3-(Chloromethyl)pyridine hydrochloride..........................       6959-48-4
4-Chloro-2-nitroaniline.........................................         89-63-4
Chlorpropham....................................................        101-21-3
Chlorothalonil..................................................       1897-45-6
1-Chloronaphthalene.............................................         90-13-1
3-Chloronitrobenzene............................................        121-73-3
4-Chloro-1,2-phenylenediamine...................................         95-83-0
4-Chloro-1,3-phenylenediamine...................................       5131-60-2
2-Chlorobiphenyl................................................       2051-60-7
Chlorpyrifos....................................................       2921-88-2
Coumaphos.......................................................         56-72-4
m + p-Cresol....................................................      65794-96-9
o-Cresol........................................................         95-48-7
p-Cresidine.....................................................        120-71-8
Crotoxyphos.....................................................       7700-17-6
2-Cyclohexyl-4,6-dinitro-phenol.................................        131-89-5
Cyanazine.......................................................      21725-46-2
Cycloate........................................................       1134-23-2
p-Cymene........................................................         99-87-6
Dacthal (DCPA)..................................................       1861-32-1
4,4'-DDD \3\....................................................         72-54-8             2.8             8.4
4,4'-DDE \3\....................................................         72-55-9             5.6            16.8
4,4'-DDT \3\....................................................         50-29-3             4.7            14.1
Demeton-O.......................................................        298-03-3
Demeton-S.......................................................        126-75-0
Diallate (cis or trans).........................................       2303-16-4
2,4-Diaminotoluene..............................................         95-80-7
Diazinon........................................................        333-41-5
Dibenz(a,j)acridine.............................................        224-42-0
Dibenzofuran....................................................        132-64-9
Dibenzo(a,e)pyrene..............................................        192-65-4
Dibenzothiophene................................................        132-65-0
1,2-Dibromo-3-chloropropane.....................................         96-12-8
3,5-Dibromo-4-hydroxybenzonitrile...............................       1689-84-5
2,6-Di-tert-butyl-p-benzoquinone................................        719-22-2
Dichlone........................................................        117-80-6
2,3-Dichloroaniline.............................................        608-27-5
2,3-Dichlorobiphenyl............................................      16605-91-7
2,6-Dichloro-4-nitroaniline.....................................         99-30-9
2,3-Dichloronitrobenzene........................................       3209-22-1
1,3-Dichloro-2-propanol.........................................         96-23-1
2,6-Dichlorophenol..............................................        120-83-2
Dichlorvos......................................................         62-73-7

[[Page 292]]

 
Dicrotophos.....................................................        141-66-2
Dieldrin \3\....................................................         60-57-1             2.5             7.5
1,2:3,4-Diepoxybutane...........................................       1464-53-5
Di(2-ethylhexyl) adipate........................................        103-23-1
Diethylstilbestrol..............................................         56-53-1
Diethyl sulfate.................................................         64-67-5
Dilantin (5,5-Diphenylhydantoin)................................         57-41-0
Dimethoate......................................................         60-51-5
3,3[min]-Dimethoxybenzidine.....................................        119-90-4
Dimethylaminoazobenzene.........................................         60-11-7
7,12-Dimethylbenz(a)anthracene..................................         57-97-6
3,3[min]-Dimethylbenzidine......................................        119-93-7
N,N-Dimethylformamide...........................................         68-12-2
3,6-Dimethylphenathrene.........................................       1576-67-6
alpha, alpha-Dimethylphenethylamine.............................        122-09-8
Dimethyl sulfone................................................         67-71-0
1,2-Dinitrobenzene..............................................        528-29-0
1,3-Dinitrobenzene..............................................         99-65-0
1,4-Dinitrobenzene..............................................        100-25-4
Dinocap.........................................................      39300-45-3
Dinoseb.........................................................         88-85-7
Diphenylamine...................................................        122-39-4
Diphenyl ether..................................................        101-84-8
1,2-Diphenylhydrazine...........................................        122-66-7
Diphenamid......................................................        957-51-7
Diphenyldisulfide...............................................        882-33-7
Disulfoton......................................................        298-04-4
Disulfoton sulfoxide............................................       2497-07-6
Disulfoton sulfone..............................................       2497-06-5
Endosulfan I \3\,\4\............................................        959-98-8
Endosulfan II \3\,\4\...........................................      33213-65-9
Endosulfan sulfate \3\..........................................       1031-07-8             5.6            16.8
Endrin \3\,\4\..................................................         72-20-8
Endrin aldehyde \3\,\4\.........................................       7421-93-4
Endrin ketone \3\,\4\...........................................      53494-70-5
EPN.............................................................       2104-64-5
EPTC............................................................        759-94-4
Ethion..........................................................        563-12-2
Ethoprop........................................................      13194-48-4
Ethyl carbamate.................................................         51-79-6
Ethyl methanesulfonate..........................................         65-50-0
Ethylenethiourea................................................         96-45-7
Etridiazole.....................................................       2593-15-9
Ethynylestradiol-3-methyl ether.................................         72-33-3
Famphur.........................................................         52-85-7
Fenamiphos......................................................      22224-92-6
Fenarimol.......................................................      60168-88-9
Fensulfothion...................................................        115-90-2
Fenthion........................................................         55-38-9
Fluchloralin....................................................      33245-39-5
Fluridone.......................................................      59756-60-4
Heptachlor \3\..................................................         76-44-8             1.9             5.7
Heptachlor epoxide \3\..........................................       1024-57-3             2.2             6.6
2,2[min],3,3[min],4,4[min],6-Heptachlorobiphenyl................      52663-71-5
2,2[min],4,4[min],5[min],6-Hexachlorobiphenyl...................      60145-22-4
Hexachlorocyclopentadiene \3\,\4\...............................         77-47-4
Hexachlorophene.................................................         70-30-4
Hexachloropropene...............................................       1888-71-7
Hexamethylphosphoramide.........................................        680-31-9
Hexanoic acid...................................................        142-62-1
Hexazinone......................................................      51235-04-2
Hydroquinone....................................................        123-31-9
Isodrin.........................................................        465-73-6
2-Isopropylnaphthalene..........................................       2027-17-0
Isosafrole......................................................        120-58-1
Kepone..........................................................        143-50-0
Leptophos.......................................................      21609-90-5
Longifolene.....................................................        475-20-7
Malachite green.................................................        569-64-2
Malathion.......................................................        121-75-5
Maleic anhydride................................................        108-31-6

[[Page 293]]

 
Merphos.........................................................        150-50-5
Mestranol.......................................................         72-33-3
Methapyrilene...................................................         91-80-5
Methoxychlor....................................................         72-43-5
2-Methylbenzothioazole..........................................        120-75-2
3-Methylcholanthrene............................................         56-49-5
4,4[min]-Methylenebis(2-chloroaniline)..........................        101-14-4
4,4[min]-Methylenebis(N,N-dimethylaniline)......................        101-61-1
4,5-Methylenephenanthrene.......................................        203-64-5
1-Methylfluorene................................................       1730-37-6
Methyl methanesulfonate.........................................         66-27-3
2-Methylnaphthalene.............................................         91-57-6
Methylparaoxon..................................................        950-35-6
Methyl parathion................................................        298-00-0
1-Methylphenanthrene............................................        832-69-9
2-(Methylthio)benzothiazole.....................................        615-22-5
Metolachlor.....................................................       5218-45-2
Metribuzin......................................................      21087-64-9
Mevinphos.......................................................       7786-34-7
Mexacarbate.....................................................        315-18-4
MGK 264.........................................................        113-48-4
Mirex...........................................................       2385-85-5
Molinate........................................................       2212-67-1
Monocrotophos...................................................       6923-22-4
Naled...........................................................        300-76-5
Napropamide.....................................................      15299-99-7
1,4-Naphthoquinone..............................................        130-15-4
1-Naphthylamine.................................................        134-32-7
2-Naphthylamine.................................................         91-59-8
1,5-Naphthalenediamine..........................................       2243-62-1
Nicotine........................................................         54-11-5
5-Nitroacenaphthene.............................................        602-87-9
2-Nitroaniline..................................................         88-74-4
3-Nitroaniline..................................................         99-09-2
4-Nitroaniline..................................................        100-01-6
5-Nitro-o-anisidine.............................................         99-59-2
4-Nitrobiphenyl.................................................         92-93-3
Nitrofen........................................................       1836-75-5
5-Nitro-o-toluidine.............................................         99-55-8
Nitroquinoline-1-oxide..........................................         56-57-5
N-Nitrosodi-n-butylamine \ 4\...................................        924-16-3
N-Nitrosodiethylamine \4\.......................................         55-18-5
N-Nitrosodimethylamine \3\,\4\..................................         62-75-9
N-Nitrosodiphenylamine \3\,\4\..................................         86-30-6
N-Nitrosomethylethylamine \4\...................................      10595-95-6
N-Nitrosomethylphenylamine \4\..................................        614-00-6
N-Nitrosomorpholine \4\.........................................         59-89-2
N-Nitrosopiperidine \4\.........................................        100-75-5
N-Nitrosopyrrolidine \4\........................................        930-55-2
trans-Nonachlor.................................................      39765-80-5
Norflurazon.....................................................      27314-13-2
2,2[min],3,3[min],4,5[min],6,6[min]-Octachlorobiphenyl..........      40186-71-8
Octamethyl pyrophosphoramide....................................        152-16-9
4,4'-Oxydianiline...............................................        101-80-4
Parathion.......................................................         56-38-2
PCB-1016 \3\,\5\................................................      12674-11-2
PCB-1221 \3\,\5\................................................      11104-28-2              30              90
PCB-1232 \3\,\5\................................................      11141-16-5
PCB-1242 \3\,\5\................................................      53469-21-9
PCB-1248 \3\,\5\................................................      12672-29-6
PCB-1254 \3\,\5\................................................      11097-69-1              36             108
PCB-1260 \3\,\5\................................................      11098-82-5
PCB-1268 \3\,\5\................................................      11100-14-4
Pebulate........................................................       1114-71-2
Pentachlorobenzene..............................................        608-93-5
Pentachloronitrobenzene.........................................         82-68-8
2,2[min],3,4[min],6-Pentachlorobiphenyl.........................      68194-05-8
Pentachloroethane...............................................         76-01-7
Pentamethylbenzene..............................................        700-12-9
Perylene........................................................        198-55-0
Phenacetin......................................................         62-44-2

[[Page 294]]

 
cis-Permethrin..................................................      61949-76-6
trans-Permethrin................................................      61949-77-7
Phenobarbital...................................................         50-06-6
Phenothiazene...................................................         92-84-2
1,4-Phenylenediamine............................................        624-18-0
1-Phenylnaphthalene.............................................        605-02-7
2-Phenylnaphthalene.............................................        612-94-2
Phorate.........................................................        298-02-2
Phosalone.......................................................       2310-18-0
Phosmet.........................................................        732-11-6
Phosphamidon....................................................      13171-21-6
Phthalic anhydride..............................................         85-44-9
alpha-Picoline (2-Methylpyridine)...............................        109-06-8
Piperonyl sulfoxide.............................................        120-62-7
Prometon........................................................       1610-18-0
Prometryn.......................................................       7287-19-6
Pronamide.......................................................      23950-58-5
Propachlor......................................................       1918-16-7
Propazine.......................................................        139-40-2
Propylthiouracil................................................         51-52-5
Pyridine........................................................        110-86-1
Resorcinol (1,3-Benzenediol)....................................        108-46-3
Safrole.........................................................         94-59-7
Simazine........................................................        122-34-9
Simetryn........................................................       1014-70-6
Squalene........................................................       7683-64-9
Stirofos........................................................      22248-79-9
Strychnine......................................................         57-24-9
Styrene \9\.....................................................        100-42-5
Sulfallate......................................................         95-06-7
Tebuthiuron.....................................................      34014-18-1
Terbacil........................................................       5902-51-2
Terbufos........................................................      13071-79-9
Terbutryn.......................................................        886-50-0
alpha-Terpineol.................................................         98-55-5
1,2,4,5-Tetrachlorobenzene......................................         95-94-3
2,2[min],4,4[min]-Tetrachlorobiphenyl...........................       2437-79-8
2,3,7,8-Tetrachlorodibenzo-p-dioxin.............................       1746-01-6
2,3,4,6-Tetrachlorophenol.......................................         58-90-2
Tetrachlorvinphos...............................................      22248-79-9
Tetraethyl dithiopyrophosphate..................................       3689-24-5
Tetraethyl pyrophosphate........................................        107-49-3
Thianaphthene (2,3-Benzothiophene)..............................         95-15-8
Thioacetamide...................................................         62-55-5
Thionazin.......................................................        297-97-2
Thiophenol (Benzenethiol).......................................        108-98-5
Thioxanthone....................................................        492-22-8
Toluene-1,3-diisocyanate........................................      26471-62-5
Toluene-2,4-diisocyanate........................................        584-84-9
o-Toluidine.....................................................         95-53-4
Toxaphene \3\,\5\...............................................       8001-35-2
Triadimefon.....................................................      43121-43-3
1,2,3-Trichlorobenzene..........................................         87-61-6
2,4,5-Trichlorobiphenyl.........................................      15862-07-4
2,3,6-Trichlorophenol...........................................        933-75-5
2,4,5-Trichlorophenol...........................................         95-95-4
Tricyclazole....................................................      41814-78-2
Trifluralin.....................................................       1582-09-8
1,2,3-Trimethoxybenzene.........................................        634-36-6
2,4,5-Trimethylaniline..........................................        137-17-7
Trimethyl phosphate.............................................        512-56-1
Triphenylene....................................................        217-59-4
Tripropyleneglycolmethyl ether..................................      20324-33-8
1,3,5-Trinitrobenzene...........................................         99-35-4
Tris(2,3-dibromopropyl) phosphate...............................        126-72-7
Tri-p-tolyl phosphate...........................................         78-32-0
O,O,O-Triethyl phosphorothioate.................................        126-68-1
Trithiane.......................................................        291-29-4
Vernolate.......................................................       1929-77-7  ..............
----------------------------------------------------------------------------------------------------------------
\1\ Compounds that have been demonstrated amenable to extraction and gas chromatography.
\2\ Determine each analyte in the fraction that gives the most accurate result.

[[Page 295]]

 
\3\ Priority Pollutant (40 CFR part 423, appendix A).
\4\ See section 1.2.
\5\ These compounds are mixtures of various isomers.
\6\ Detected as azobenzene.
\7\ MDL values from the 1984 promulgated version of Method 625.
\8\ ML = Minimum Level--see Glossary for definition and derivation.
\9\ Styrene may be susceptible to losses during sampling, preservation, and/or extraction of full-volume (1 L)
  water samples. However, styrene is not regulated at 40 CFR part 136, and it is also listed as an analyte in
  EPA Method 624.1 and EPA Method 1625C, where such losses may be less than using Method 625.1.


                               Table 4--Chromatographic Conditions and Characteristic m/z's for Base/Neutral Extractables
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                        Characteristic m/z's
                                                                Retention  -----------------------------------------------------------------------------
                           Analyte                              time (sec)        Electron impact ionization                Chemical ionization
                                                                   \1\     -----------------------------------------------------------------------------
                                                                              Primary       Second       Second      Methane      Methane      Methane
--------------------------------------------------------------------------------------------------------------------------------------------------------
N-Nitrosodimethylamine.......................................          385           42           74           44  ...........
bis(2-Chloroethyl) ether.....................................          704           93           63           95           63          107          109
bis(2-Chloroisopropyl) ether.................................          799           45           77           79           77          135          137
Hexachloroethane.............................................          823          117          201          199          199          201          203
N-Nitrosodi-n-propylamine....................................          830          130           42          101  ...........
Nitrobenzene.................................................          849           77          123           65          124          152          164
Isophorone...................................................          889           82           95          138          139          167          178
bis(2-Chloroethoxy) methane..................................          939           93           95          123           65          107          137
1,2,4-Trichlorobenzene.......................................          958          180          182          145          181          183          209
Naphthalene..................................................          967          128          129          127          129          157          169
Hexachlorobutadiene..........................................         1006          225          223          227          223          225          227
Hexachlorocyclopentadiene....................................         1142          237          235          272          235          237          239
2-Chloronaphthalene..........................................         1200          162          164          127          163          191          203
Acenaphthylene...............................................         1247          152          151          153          152          153          181
Dimethyl phthalate...........................................         1273          163          194          164          151          163          164
2,6-Dinitrotoluene...........................................         1300          165           89          121          183          211          223
Acenaphthene.................................................         1304          154          153          152          154          155          183
2,4-Dinitrotoluene...........................................         1364          165           63          182          183          211          223
Fluorene.....................................................         1401          166          165          167          166          167          195
4-Chlorophenyl phenyl ether..................................         1409          204          206          141  ...........
Diethyl phthalate............................................         1414          149          177          150          177          223          251
N-Nitrosodiphenylamine.......................................         1464          169          168          167          169          170          198
4-Bromophenyl phenyl ether...................................         1498          248          250          141          249          251          277
alpha-BHC....................................................         1514          183          181          109  ...........
Hexachlorobenzene............................................         1522          284          142          249          284          286          288
beta-BHC.....................................................         1544          183          181          109  ...........
gamma-BHC....................................................         1557          181          183          109  ...........
Phenanthrene.................................................         1583          178          179          176          178          179          207
Anthracene...................................................         1592          178          179          176          178          179          207
delta-BHC....................................................         1599          183          109          181  ...........
Heptachlor...................................................         1683          100          272          274  ...........
Di-n-butyl phthalate.........................................         1723          149          150          104          149          205          279
Aldrin.......................................................         1753           66          263          220  ...........
Fluoranthene.................................................         1817          202          101          100          203          231          243
Heptachlor epoxide...........................................         1820          353          355          351  ...........
gamma-Chlordane..............................................         1834          373          375          377  ...........
Pyrene.......................................................         1852          202          101          100          203          231          243
Benzidine\ 2\................................................         1853          184           92          185          185          213          225
alpha-Chlordane..............................................         1854          373          375          377  ...........
Endosulfan I.................................................         1855          237          339          341  ...........
4,4[min]-DDE.................................................         1892          246          248          176  ...........
Dieldrin.....................................................         1907           79          263          279  ...........
Endrin.......................................................         1935           81          263           82  ...........
Endosulfan II................................................         2014          237          339          341  ...........
4,4[min]-DDD.................................................         2019          235          237          165  ...........
Endrin aldehyde..............................................         2031           67          345          250  ...........
Butyl benzyl phthalate.......................................         2060          149           91          206          149          299          327
Endosulfan sulfate...........................................         2068          272          387          422  ...........
4,4[min]-DDT.................................................         2073          235          237          165  ...........
Chrysene.....................................................         2083          228          226          229          228          229          257
3,3[min]-Dichlorobenzidine...................................         2086          252          254          126  ...........
Benzo(a)anthracene...........................................         2090          228          229          226          228          229          257

[[Page 296]]

 
bis(2-Ethylhexyl) phthalate..................................         2124          149          167          279          149
Di-n-octyl phthalate.........................................         2240          149           43           57  ...........
Benzo(b)fluoranthene.........................................         2286          252          253          125          252          253          281
Benzo(k)fluoranthene.........................................         2293          252          253          125          252          253          281
Benzo(a)pyrene...............................................         2350          252          253          125          252          253          281
Indeno(1,2,3-cd) pyrene......................................         2650          276          138          277          276          277          305
Dibenz(a,h)anthracene........................................         2660          278          139          279          278          279          307
Benzo(ghi)perylene...........................................         2750          276          138          277          276          277          305
Toxaphene....................................................  ...........          159          231          233  ...........
PCB 1016.....................................................  ...........          224          260          294  ...........
PCB 1221.....................................................  ...........          190          224          260  ...........
PCB 1232.....................................................  ...........          190          224          260  ...........
PCB 1242.....................................................  ...........          224          260          294  ...........
PCB 1248.....................................................  ...........          294          330          262  ...........
PCB 1254.....................................................  ...........          294          330          362  ...........
PCB 1260.....................................................  ...........          330          362          394  ...........  ...........
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Column: 30 m x 0.25 mm ID; 94% methyl, 5% phenyl, 1% vinyl bonded phase fused silica capillary.
Conditions: 5 min at 30 [deg]C; 30-280 at 8 [deg]C per min; isothermal at 280 [deg]C until benzo(ghi)perylene elutes.
Gas velocity: 30 cm/sec at 30 [deg]C (at constant pressure).
\2\ See section 1.2; included for tailing factor testing.


                                   Table 5--Chromatographic Conditions and Characteristic m/z's for Acid Extractables
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                        Characteristic m/z's
                                                                Retention  -----------------------------------------------------------------------------
                           Analyte                              Time (sec)        Electron impact ionization                Chemical ionization
                                                                   \1\     -----------------------------------------------------------------------------
                                                                               Prime        Second       Second      Methane      Methane      Methane
--------------------------------------------------------------------------------------------------------------------------------------------------------
2-Chlorophenol...............................................          705          128           64          130          129          131          157
Phenol.......................................................          700           94           65           66           95          123          135
2-Nitrophenol................................................          900          139           65          109          140          168          122
2,4-Dimethylphenol...........................................          924          122          107          121          123          151          163
2,4-Dichlorophenol...........................................          947          162          164           98          163          165          167
4-Chloro-3-methylphenol......................................         1091          142          107          144          143          171          183
2,4,6-Trichlorophenol........................................         1165          196          198          200          197          199          201
2,4-Dinitrophenol............................................         1325          184           63          154          185          213          225
4-Nitrophenol................................................         1354           65          139          109          140          168          122
2-Methyl-4,6-dinitrophenol...................................         1435          198          182           77          199          227          239
Pentachlorophenol............................................         1561          266          264          268          267          265          269
--------------------------------------------------------------------------------------------------------------------------------------------------------
Column: 30 m x 0.25 mm ID; 94% methyl, 5% phenyl, 1% vinyl bonded phase fused silica capillary.
Conditions: 5 min at 30 [deg]C; 30-250 at 8 [deg]C per min; isothermal at 280 [deg]C until pentachlorophenol elutes.
Gas velocity: 30 cm/sec at 30 [deg]C (at constant pressure).


                                 Table 6--QC Acceptance Criteria--Method 625 \1\
----------------------------------------------------------------------------------------------------------------
                                    Range for Q     Limit for s     Range for X    Range for P1,   Limit for RPD
             Analyte                  (%) \2\         (%) \3\         (%) \3\        P2(%) \3\          (%)
----------------------------------------------------------------------------------------------------------------
Acenaphthene....................          70-130              29          60-132          47-145              48
Acenaphthylene..................          60-130              45          54-126          33-145              74
Aldrin..........................           7-152              39           7-152           D-166              81
Anthracene......................          58-130              40          43-120          27-133              66
Benzo(a)anthracene..............          42-133              32          42-133          33-143              53
Benzo(b)fluoranthene............          42-140              43          42-140          24-159              71
Benzo(k)fluoranthene............          25-146              38          25-146          11-162              63
Benzo(a)pyrene..................          32-148              43          32-148          17-163              72
Benzo(ghi)perylene..............          13-195              61           D-195           D-219              97
Benzyl butyl phthalate..........          43-140              36           D-140           D-152              60
beta-BHC........................          42-131              37          42-131          24-149              61
delta-BHC.......................           D-130              77           D-120           D-120             129
bis(2-Chloroethyl)ether.........          52-130              65          43-126          12-158             108
bis(2-Chloroethoxy)methane......          52-164              32          49-165          33-184              54
bis(2-Chloroisopropyl) ether....          63-139              46          63-139          36-166              76
bis(2-Ethylhexyl) phthalate.....          43-137              50          29-137           8-158              82

[[Page 297]]

 
4-Bromophenyl phenyl ether......          70-130              26          65-120          53-127              43
2-Chloronaphthalene.............          70-130              15          65-120          60-120              24
4-Chlorophenyl phenyl ether.....          57-145              36          38-145          25-158              61
Chrysene........................          44-140              53          44-140          17-168              87
4,4[min]-DDD....................           D-135              56           D-135           D-145              93
4,4[min]-DDE....................          19-130              46          19-120           4-136              77
4,4[min]-DDT....................           D-171              81           D-171           D-203             135
Dibenz(a,h)anthracene...........          13-200              75           D-200           D-227             126
Di-n-butyl phthalate............          52-130              28           8-120           1-120              47
3,3[min]-Dichlorobenzidine......          18-213              65           8-213           D-262             108
Dieldrin........................          70-130              38          44-119          29-136              62
Diethyl phthalate...............          47-130              60           D-120           D-120             100
Dimethyl phthalate..............          50-130             110           D-120           D-120             183
2,4-Dinitrotoluene..............          53-130              25          48-127          39-139              42
2,6-Dinitrotoluene..............          68-137              29          68-137          50-158              48
Di-n-octyl phthalate............          21-132              42          19-132           4-146              69
Endosulfan sulfate..............           D-130              42           D-120           D-120              70
Endrin aldehyde.................           D-189              45           D-189           D-209              75
Fluoranthene....................          47-130              40          43-121          26-137              66
Fluorene........................          70-130              23          70-120          59-121              38
Heptachlor......................           D-172              44           D-172           D-192              74
Heptachlor epoxide..............          70-130              61          71-120          26-155             101
Hexachlorobenzene...............          38-142              33           8-142           D-152              55
Hexachlorobutadiene.............          68-130              38          38-120          24-120              62
Hexachloroethane................          55-130              32          55-120          40-120              52
Indeno(1,2,3-cd)pyrene..........          13-151              60           D-151           D-171              99
Isophorone......................          52-180              56          47-180          21-196              93
Naphthalene.....................          70-130              39          36-120          21-133              65
Nitrobenzene....................          54-158              37          54-158          35-180              62
N-Nitrosodi-n-propylamine.......          59-170              52          14-198           D-230              87
PCB-1260........................          19-130              77          19-130           D-164             128
Phenanthrene....................          67-130              24          65-120          54-120              39
Pyrene..........................          70-130              30          70-120          52-120              49
1,2,4-Trichlorobenzene..........          61-130              30          57-130          44-142              50
4-Chloro-3-methylphenol.........          68-130              44          41-128          22-147              73
2-Chlorophenol..................          55-130              37          36-120          23-134              61
2,4-Dichlorophenol..............          64-130              30          53-122          39-135              50
2,4-Dimethylphenol..............          58-130              35          42-120          32-120              58
2,4-Dinitrophenol...............          39-173              79           D-173           D-191             132
2-Methyl-4,6-dinitrophenol......          56-130             122          53-130           D-181             203
2-Nitrophenol...................          61-163              33          45-167          29-182              55
4-Nitrophenol...................          35-130              79          13-129           D-132             131
Pentachlorophenol...............          42-152              52          38-152          14-176              86
Phenol..........................          48-130              39          17-120           5-120              64
2,4,6-Trichlorophenol...........          69-130              35          52-129          37-144              58
----------------------------------------------------------------------------------------------------------------
\1\ Acceptance criteria are based upon method performance data in Table 7 and from EPA Method 1625. Where
  necessary, limits for recovery have been broadened to assure applicability to concentrations below those used
  to develop Table 7.
\2\ Test concentration = 100 [micro]g/mL.
\3\ Test concentration = 100 [micro]g/L.
Q = Calibration verification (sections 7.3.1 and 13.4).
s = Standard deviation for four recovery measurements in the DOC test (section 8.2.4).
X = Average recovery for four recovery measurements in the DOC test (section 8.2.4).
P1, P2 = MS/MSD recovery (section 8.3.2, section 8.4.2).
RPD = MS/MSD relative percent difference (RPD; section 8.3.3).
D = Detected; result must be greater than zero.


                  Table 7--Precision and Recovery as Functions of Concentration--Method 625 \1\
----------------------------------------------------------------------------------------------------------------
                                                                                 Single analyst      Overall
                                                                  Recovery,        precision,       precision,
                           Analyte                                  X[min]          sr[min]           S[min]
                                                                 ([micro]g/L)     ([micro]g/L)     ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Acenaphthene.................................................     0.96C + 0.19      0.15 X-0.12      0.21 X-0.67
Acenaphthylene...............................................     0.89C + 0.74      0.24 X-1.06      0.26 X-0.54
Aldrin.......................................................     0.78C + 1.66      0.27 X-1.28    0.43 X + 1.13
Anthracene...................................................     0.80C + 0.68      0.21 X-0.32      0.27 X-0.64
Benzo(a)anthracene...........................................       0.88C-0.60    0.15 X + 0.93      0.26 X-0.28
Benzo(b)fluoranthene.........................................       0.93C-1.80    0.22 X + 0.43    0.29 X + 0.96
Benzo(k)fluoranthene.........................................       0.87C-1.56    0.19 X + 1.03    0.35 X + 0.40
Benzo(a)pyrene...............................................       0.90C-0.13    0.22 X + 0.48    0.32 X + 1.35
Benzo(ghi)perylene...........................................       0.98C-0.86    0.29 X + 2.40      0.51 X-0.44
Benzyl butyl phthalate.......................................       0.66C-1.68    0.18 X + 0.94    0.53 X + 0.92

[[Page 298]]

 
beta-BHC.....................................................       0.87C-0.94      0.20 X-0.58      0.30 X-1.94
delta-BHC....................................................       0.29C-1.09    0.34 X + 0.86      0.93 X-0.17
bis(2-Chloroethyl) ether.....................................       0.86C-1.54      0.35 X-0.99    0.35 X + 0.10
bis(2-Chloroethoxy) methane..................................       1.12C-5.04    0.16 X + 1.34    0.26 X + 2.01
bis(2-Chloroisopropyl) ether.................................       1.03C-2.31    0.24 X + 0.28    0.25 X + 1.04
bis(2-Ethylhexyl) phthalate..................................       0.84C-1.18    0.26 X + 0.73    0.36 X + 0.67
4-Bromophenyl phenyl ether...................................       0.91C-1.34    0.13 X + 0.66    0.16 X + 0.66
2-Chloronaphthalene..........................................     0.89C + 0.01    0.07 X + 0.52    0.13 X + 0.34
4-Chlorophenyl phenyl ether..................................     0.91C + 0.53      0.20 X-0.94      0.30 X-0.46
Chrysene.....................................................       0.93C-1.00    0.28 X + 0.13      0.33 X-0.09
4,4[min]-DDD.................................................       0.56C-0.40      0.29 X-0.32      0.66 X-0.96
4,4[min]-DDE.................................................       0.70C-0.54      0.26 X-1.17      0.39 X-1.04
4,4[min]-DDT.................................................       0.79C-3.28    0.42 X + 0.19      0.65 X-0.58
Dibenz(a,h)anthracene........................................     0.88C + 4.72    0.30 X + 8.51    0.59 X + 0.25
Di-n-butyl phthalate.........................................     0.59C + 0.71    0.13 X + 1.16    0.39 X + 0.60
3,3'-Dichlorobenzidine.......................................      1.23C-12.65    0.28 X + 7.33    0.47 X + 3.45
Dieldrin.....................................................       0.82C-0.16      0.20 X-0.16      0.26 X-0.07
Diethyl phthalate............................................     0.43C + 1.00    0.28 X + 1.44    0.52 X + 0.22
Dimethyl phthalate...........................................     0.20C + 1.03    0.54 X + 0.19      1.05 X-0.92
2,4-Dinitrotoluene...........................................       0.92C-4.81    0.12 X + 1.06    0.21 X + 1.50
2,6-Dinitrotoluene...........................................       1.06C-3.60    0.14 X + 1.26    0.19 X + 0.35
Di-n-octyl phthalate.........................................       0.76C-0.79    0.21 X + 1.19    0.37 X + 1.19
Endosulfan sulfate...........................................     0.39C + 0.41    0.12 X + 2.47      0.63 X-1.03
Endrin aldehyde..............................................       0.76C-3.86    0.18 X + 3.91      0.73 X-0.62
Fluoranthene.................................................     0.81C + 1.10    0.22 X + 0.73      0.28 X-0.60
Fluorene.....................................................       0.90C-0.00    0.12 X + 0.26    0.13 X + 0.61
Heptachlor...................................................       0.87C-2.97      0.24 X-0.56      0.50 X-0.23
Heptachlor epoxide...........................................       0.92C-1.87      0.33 X-0.46    0.28 X + 0.64
Hexachlorobenzene............................................     0.74C + 0.66      0.18 X-0.10      0.43 X-0.52
Hexachlorobutadiene..........................................       0.71C-1.01    0.19 X + 0.92    0.26 X + 0.49
Hexachloroethane.............................................       0.73C-0.83    0.17 X + 0.67    0.17 X + 0.80
Indeno(1,2,3-cd)pyrene.......................................       0.78C-3.10    0.29 X + 1.46    0.50 X + 0.44
Isophorone...................................................     1.12C + 1.41    0.27 X + 0.77    0.33 X + 0.26
Naphthalene..................................................     0.76C + 1.58      0.21 X-0.41      0.30 X-0.68
Nitrobenzene.................................................       1.09C-3.05    0.19 X + 0.92    0.27 X + 0.21
N-Nitrosodi-n-propylamine....................................       1.12C-6.22    0.27 X + 0.68    0.44 X + 0.47
PCB-1260.....................................................      0.81C-10.86    0.35 X + 3.61    0.43 X + 1.82
Phenanthrene.................................................       0.87C-0.06    0.12 X + 0.57    0.15 X + 0.25
Pyrene.......................................................       0.84C-0.16    0.16 X + 0.06    0.15 X + 0.31
1,2,4-Trichlorobenzene.......................................       0.94C-0.79    0.15 X + 0.85    0.21 X + 0.39
4-Chloro-3-methylphenol......................................     0.84C + 0.35    0.23 X + 0.75    0.29 X + 1.31
2-Chlorophenol...............................................     0.78C + 0.29    0.18 X + 1.46    0.28 X + 0.97
2,4-Dichlorophenol...........................................     0.87C + 0.13    0.15 X + 1.25    0.21 X + 1.28
2,4-Dimethylphenol...........................................     0.71C + 4.41    0.16 X + 1.21    0.22 X + 1.31
2,4-Dinitrophenol............................................      0.81C-18.04    0.38 X + 2.36   0.42 X + 26.29
2-Methyl-4,6-Dinitrophenol...................................      1.04C-28.04   0.05 X + 42.29   0.26 X + 23.10
2-Nitrophenol................................................       1.07C-1.15    0.16 X + 1.94    0.27 X + 2.60
4-Nitrophenol................................................       0.61C-1.22    0.38 X + 2.57    0.44 X + 3.24
Pentachlorophenol............................................     0.93C + 1.99    0.24 X + 3.03    0.30 X + 4.33
Phenol.......................................................     0.43C + 1.26    0.26 X + 0.73    0.35 X + 0.58
2,4,6-Trichlorophenol........................................       0.91C-0.18    0.16 X + 2.22    0.22 X + 1.81
----------------------------------------------------------------------------------------------------------------
\1\ Regressions based on data from Reference 2.
X[min] = Expected recovery for one or more measurements of a sample containing a concentration of C, in [micro]g/
  L.
sr[min] = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
S[min] = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  [micro]g/L.
C = True value for the concentration, in [micro]g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in [micro]g/L.


           Table 8--Suggested Internal and Surrogate Standards
------------------------------------------------------------------------
                                           Range for surrogate recovery
                                                      (%) \1\
          Base/neutral fraction          -------------------------------
                                            Calibration    Recovery from
                                           verification       samples
------------------------------------------------------------------------
Acenaphthalene-d8.......................          66-152          33-168
Acenaphthene-d10........................          71-141          30-180
Aniline-d5..............................
Anthracene-d10..........................          58-171          23-142

[[Page 299]]

 
Benzo(a)anthracene-d12..................          28-357          22-329
Benzo(a)pyrene-d12......................          32-194          32-194
4-Chloroaniline-d4......................           1-145           1-145
bis(2-Chloroethyl) ether-d8.............          52-194          25-222
Chrysene-d12............................          23-290          23-290
Decafluorobiphenyl......................
4,4[min]-Dibromobiphenyl................
4,4[min]-Dibromooctafluorobiphenyl......
1,4-Dichlorobenzene-d4..................          65-153          11-245
2,2[min]-Difluorobiphenyl...............
Dimethyl phthalate-d6...................          47-211           1-500
Fluoranthene-d10........................          47-215          30-187
Fluorene-d10............................          61-164          38-172
4-Fluoroaniline.........................
1-Fluoronaphthalene.....................
2-Fluoronaphthalene.....................
2-Methylnaphthalene-d10.................          50-150          50-150
Naphthalene-d8..........................          71-141          22-192
Nitrobenzene-d5.........................          46-219          15-314
2,3,4,5,6-Pentafluorobiphenyl...........
Perylene-d12............................
Phenanthrene-d10........................          67-149          34-168
Pyrene-d10..............................          48-210          28-196
Pyridine-d5.............................
Acid fraction...........................
2-Chlorophenol-d4.......................          55-180          33-180
2,4-Dichlorophenol-d3...................          64-157          34-182
4,6-Dinitro-2-methylphenol-d2...........          56-177          22-307
2-Fluorophenol..........................
4-Methylphenol-d8.......................          25-111          25-111
2-Nitrophenol-d4........................          61-163          37-163
4-Nitrophenol-d4........................          35-287           6-500
Pentafluorophenol.......................
2-Perfluoromethylphenol.................
Phenol-d5...............................          48-208           8-424
------------------------------------------------------------------------
\1\ Recovery from samples is the wider of the criteria in the CLP SOW
  for organics or in Method 1625.


     Table 9A--DFTPP Key m/z's and Abundance Criteria for Quadrupole
                             Instruments \1\
------------------------------------------------------------------------
             m/z                          Abundance criteria
------------------------------------------------------------------------
51..........................  30-60 percent of m/z 198.
68..........................  Less than 2 percent of m/z 69.
70..........................  Less than 2 percent of m/z 69.
127.........................  40-60 percent of base peak m/z 198.
197.........................  Less than 1 percent of m/z 198.
198.........................  Base peak, 100 percent relative abundance.
199.........................  5-9 percent of m/z 198.
275.........................  10-30 percent of m/z 198.
365.........................  Greater than 1 percent of m/z 198.
441.........................  Present but less than m/z 443.
442.........................  40-100 percent of m/z 198.
443.........................  17-23 percent of m/z 442.
------------------------------------------------------------------------
\1\ Criteria in these tables are for quadrupole and time-of-flight
  instruments. Alternative tuning criteria from other published EPA
  reference methods may be used provided method performance is not
  adversely affected. Alternative tuning criteria specified by an
  instrument manufacturer may also be used for another type of mass
  spectrometer, provided method performance is not adversely affected.


   Table 9B--DFTPP Key m/z's and Abundance Criteria for Time-of-flight
                             Instruments \1\
------------------------------------------------------------------------
             m/z                          Abundance criteria
------------------------------------------------------------------------
51..........................  10-85 percent of the base peak.
68..........................  Less than 2 percent of m/z 69.
70..........................  Less than 2 percent of m/z 69.
127.........................  10-80 percent of the base peak.
197.........................  Less than 2 percent of Mass 198.

[[Page 300]]

 
198.........................  Base peak, or greater than 50% of m/z 442.
199.........................  5-9 percent of m/z 198.
275.........................  10-60 percent of the base peak.
365.........................  Greater than 0.5 percent of m/z 198.
441.........................  Less than 150 percent of m/z 443.
442.........................  Base peak or greater than 30 percent of m/
                               z 198.
443.........................  15-24 percent of m/z 442.
------------------------------------------------------------------------
\1\ Criteria in these tables are for quadrupole and time-of-flight
  instruments. Alternative tuning criteria from other published EPA
  reference methods may be used provided method performance is not
  adversely affected. Alternative tuning criteria specified by an
  instrument manufacturer may also be used for another type of mass
  spectrometer, or for an alternative carrier gas, provided method
  performance is not adversely affected.

                               21. Figures

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[GRAPHIC] [TIFF OMITTED] TR28AU17.018


[[Page 302]]


[GRAPHIC] [TIFF OMITTED] TR28AU17.019

                              22. Glossary

    These definitions and purposes are specific to this method but have 
been conformed to common usage to the extent possible.
    22.1 Units of weight and measure and their abbreviations.
    22.1.1 Symbols.
 [deg]C degrees Celsius
[micro]g microgram
[micro]L microliter
< less than
 greater than
<= less than or equal to
% percent
    22.1.2 Abbreviations (in alphabetical order).
cm centimeter
g gram
h hour
ID inside diameter
in. inch
L liter
m mass or meter
mg milligram
min minute
mL milliliter
mm millimeter
ms millisecond
m/z mass-to-charge ratio
N normal; gram molecular weight of solute divided by hydrogen equivalent 
of solute, per liter of solution
ng nanogram
pg picogram
ppb part-per-billion
ppm part-per-million
ppt part-per-trillion
psig pounds-per-square inch gauge
    22.2 Definitions and acronyms (in alphabetical order).
    Analyte--A compound or mixture of compounds (e.g., PCBs) tested for 
by this method. The analytes are listed in Tables 1-3.
    Batch--See Extraction.
    Blank--An aliquot of reagent water that is treated exactly as a 
sample including exposure to all glassware, equipment, solvents, 
reagents, internal standards, and surrogates that are used with samples. 
The blank is used to determine if analytes or interferences are present 
in the laboratory environment, the reagents, or the apparatus.
    Calibration--The process of determining the relationship between the 
output or response of a measuring instrument and the value of an input 
standard. Historically, EPA has referred to a multi-point calibration as 
the ``initial calibration,'' to differentiate it from a single-point 
calibration verification.
    Calibration standard--A solution prepared from stock solutions and/
or a secondary standards and containing the analytes of interest, 
surrogates, and internal standards. The calibration standard is used to 
calibrate the response of the GC/MS instrument against analyte 
concentration.

[[Page 303]]

    Calibration verification standard--The mid-point calibration 
standard used to verify calibration. See sections 7.3 and 13.4.
    Descriptor--In SIM, the beginning and ending retention times for the 
RT window, the m/z's sampled in the RT window, and the dwell time at 
each m/z.
    Extracted ion current profile (EICP)--The line described by the 
signal at a given m/z.
    Extraction Batch--A set of up to 20 field samples (not including QC 
samples) started through the extraction process on a given 24-hour shift 
(section 3.1). Each extraction batch must be accompanied by a blank 
(section 8.5), a laboratory control sample (LCS, section 8.4), and a 
matrix spike and duplicate (MS/MSD; Section 8.3), resulting in a minimum 
of five analyses (1 sample, 1 blank, 1 LCS, 1 MS, and 1 MSD) and a 
maximum of 24 analyses (20 field samples, 1 blank, 1 LCS, 1 MS, and 1 
MSD) for the batch. If greater than 20 samples are to be extracted in a 
24-hour shift, the samples must be separated into extraction batches of 
20 or fewer samples.
    Field Duplicates--Two samples collected at the same time and placed 
under identical conditions, and treated identically throughout field and 
laboratory procedures. Results of analyses of the field duplicates 
provide an estimate of the precision associated with sample collection, 
preservation, and storage, as well as with laboratory procedures.
    Field blank--An aliquot of reagent water or other reference matrix 
that is placed in a sample container in the field, and treated as a 
sample in all respects, including exposure to sampling site conditions, 
storage, preservation, and all analytical procedures. The purpose of the 
field blank is to determine if the field or sample transporting 
procedures and environments have contaminated the sample.
    GC--Gas chromatograph or gas chromatography.
    Internal standard--A compound added to an extract or standard 
solution in a known amount and used as a reference for quantitation of 
the analytes of interest and surrogates. In this method the internal 
standards are stable isotopically labeled analogs of selected method 
analytes (Table 8). Also see Internal standard quantitation.
    Internal standard quantitation--A means of determining the 
concentration of an analyte of interest (Tables 1-3) by reference to a 
compound not expected to be found in a sample.
    DOC--Initial demonstration of capability (section 8.2); four 
aliquots of reagent water spiked with the analytes of interest and 
analyzed to establish the ability of the laboratory to generate 
acceptable precision and recovery. A DOC is performed prior to the first 
time this method is used and any time the method or instrumentation is 
modified.
    Laboratory Control Sample (LCS; laboratory fortified blank; section 
8.4)--An aliquot of reagent water spiked with known quantities of the 
analytes of interest and surrogates. The LCS is analyzed exactly like a 
sample. Its purpose is to assure that the results produced by the 
laboratory remain within the limits specified in this method for 
precision and recovery.
    Laboratory fortified sample matrix--See Matrix spike.
    Laboratory reagent blank--A blank run on laboratory reagents; e.g., 
methylene chloride (section 11.1.5).
    Matrix spike (MS) and matrix spike duplicate (MSD) (laboratory 
fortified sample matrix and duplicate)--Two aliquots of an environmental 
sample to which known quantities of the analytes of interest and 
surrogates are added in the laboratory. The MS/MSD are prepared and 
analyzed exactly like a field sample. Their purpose is to quantify any 
additional bias and imprecision caused by the sample matrix. The 
background concentrations of the analytes in the sample matrix must be 
determined in a separate aliquot and the measured values in the MS/MSD 
corrected for background concentrations.
    May--This action, activity, or procedural step is neither required 
nor prohibited.
    May not--This action, activity, or procedural step is prohibited.
    Method blank--See blank.
    Method detection limit (MDL)--A detection limit determined by the 
procedure at 40 CFR part 136, appendix B. The MDLs determined by EPA in 
the original version of the method are listed in Tables 1, 2 and 3. As 
noted in section 1.5, use the MDLs in Tables 1, 2, and 3 in conjunction 
with current MDL data from the laboratory actually analyzing samples to 
assess the sensitivity of this procedure relative to project objectives 
and regulatory requirements (where applicable).
    Minimum level (ML)--The term ``minimum level'' refers to either the 
sample concentration equivalent to the lowest calibration point in a 
method or a multiple of the method detection limit (MDL), whichever is 
higher. Minimum levels may be obtained in several ways: They may be 
published in a method; they may be based on the lowest acceptable 
calibration point used by a laboratory; or they may be calculated by 
multiplying the MDL in a method, or the MDL determined by a laboratory, 
by a factor of 3. For the purposes of NPDES compliance monitoring, EPA 
considers the following terms to be synonymous: ``quantitation limit,'' 
``reporting limit,'' and ``minimum level.''
    MS--Mass spectrometer or mass spectrometry, or matrix spike (a QC 
sample type).
    MSD--Matrix spike duplicate (a QC sample type).
    Must--This action, activity, or procedural step is required.

[[Page 304]]

    m/z--The ratio of the mass of an ion (m) detected in the mass 
spectrometer to the charge (z) of that ion.
    Preparation blank--See blank.
    Quality control check sample (QCS)--See Laboratory Control Sample.
    Reagent water--Water demonstrated to be free from the analytes of 
interest and potentially interfering substances at the MDLs for the 
analytes in this method.
    Regulatory compliance limit (or regulatory concentration limit)--A 
limit on the concentration or amount of a pollutant or contaminant 
specified in a nationwide standard, in a permit, or otherwise 
established by a regulatory/control authority.
    Relative retention time (RRT)--The ratio of the retention time of an 
analyte to the retention time of its associated internal standard. RRT 
compensates for small changes in the GC temperature program that can 
affect the absolute retention times of the analyte and internal 
standard. RRT is a unitless quantity.
    Relative standard deviation (RSD)--The standard deviation times 100 
divided by the mean. Also termed ``coefficient of variation.''
    RF--Response factor. See section 7.2.2.
    RSD--See relative standard deviation.
    Safety Data Sheet (SDS)--Written information on a chemical's 
toxicity, health hazards, physical properties, fire, and reactivity, 
including storage, spill, and handling precautions that meet the 
requirements of OSHA, 29 CFR 1910.1200(g) and appendix D to Sec.  
1910.1200. United Nations Globally Harmonized System of Classification 
and Labelling of Chemicals (GHS), third revised edition, United Nations, 
2009.
    Selected Ion Monitoring (SIM)--An MS technique in which a few m/z's 
are monitored. When used with gas chromatography, the m/z's monitored 
are usually changed periodically throughout the chromatographic run, to 
correlate with the characteristic m/z's of the analytes, surrogates, and 
internal standards as they elute from the chromatographic column. The 
technique is often used to increase sensitivity and minimize 
interferences.
    Signal-to-noise ratio (S/N)--The height of the signal as measured 
from the mean (average) of the noise to the peak maximum divided by the 
width of the noise.
    Should--This action, activity, or procedural step is suggested but 
not required.
    SPE--Solid-phase extraction; an extraction technique in which an 
analyte is extracted from an aqueous solution by passage over or through 
a material capable of reversibly adsorbing the analyte. Also termed 
liquid-solid extraction.
    Stock solution--A solution containing an analyte that is prepared 
using a reference material traceable to EPA, the National Institute of 
Science and Technology (NIST), or a source that will attest to the 
purity, authenticity, and concentration of the standard.
    Surrogate--A compound unlikely to be found in a sample, and which is 
spiked into sample in a known amount before extraction or other 
processing, and is quantitated with the same procedures used to quantify 
other sample components. The purpose of the surrogate is to monitor 
method performance with each sample.

                         Method 1613, Revision B

 Tetra- Through Octa-Chlorinated Dioxins and Furans by Isotope Dilution 
                                HRGC/HRMS

                        1.0 Scope and Application

    1.1 This method is for determination of tetra- through octa-
chlorinated dibenzo-p-dioxins (CDDs) and dibenzofurans (CDFs) in water, 
soil, sediment, sludge, tissue, and other sample matrices by high 
resolution gas chromatography/high resolution mass spectrometry (HRGC/
HRMS). The method is for use in EPA's data gathering and monitoring 
programs associated with the Clean Water Act, the Resource Conservation 
and Recovery Act, the Comprehensive Environmental Response, Compensation 
and Liability Act, and the Safe Drinking Water Act. The method is based 
on a compilation of EPA, industry, commercial laboratory, and academic 
methods (References 1-6).
    1.2 The seventeen 2,3,7,8-substituted CDDs/CDFs listed in Table 1 
may be determined by this method. Specifications are also provided for 
separate determination of 2,3,7,8-tetrachloro-dibenzo-p-dioxin (2,3,7,8-
TCDD) and 2,3,7,8-tetrachloro-dibenzofuran (2,3,7,8-TCDF).
    1.3 The detection limits and quantitation levels in this method are 
usually dependent on the level of interferences rather than instrumental 
limitations. The minimum levels (MLs) in Table 2 are the levels at which 
the CDDs/CDFs can be determined with no interferences present. The 
Method Detection Limit (MDL) for 2,3,7,8-TCDD has been determined as 4.4 
pg/L (parts-per-quadrillion) using this method.
    1.4 The GC/MS portions of this method are for use only by analysts 
experienced with HRGC/HRMS or under the close supervision of such 
qualified persons. Each laboratory that uses this method must 
demonstrate the ability to generate acceptable results using the 
procedure in Section 9.2.
    1.5 This method is ``performance-based''. The analyst is permitted 
to modify the method to overcome interferences or lower the cost of 
measurements, provided that all performance criteria in this method are 
met. The requirements for establishing method equivalency are given in 
Section 9.1.2.

[[Page 305]]

    1.6 Any modification of this method, beyond those expressly 
permitted, shall be considered a major modification subject to 
application and approval of alternate test procedures under 40 CFR 136.4 
and 136.5.

                          2.0 Summary of Method

    Flow charts that summarize procedures for sample preparation, 
extraction, and analysis are given in Figure 1 for aqueous and solid 
samples, Figure 2 for multi-phase samples, and Figure 3 for tissue 
samples.
    2.1 Extraction.
    2.1.1 Aqueous samples (samples containing less than 1% solids)--
Stable isotopically labeled analogs of 15 of the 2,3,7,8-substituted 
CDDs/CDFs are spiked into a 1 L sample, and the sample is extracted by 
one of three procedures:
    2.1.1.1 Samples containing no visible particles are extracted with 
methylene chloride in a separatory funnel or by the solid-phase 
extraction technique summarized in Section 2.1.1.3. The extract is 
concentrated for cleanup.
    2.1.1.2 Samples containing visible particles are vacuum filtered 
through a glass-fiber filter. The filter is extracted in a Soxhlet/Dean-
Stark (SDS) extractor (Reference 7), and the filtrate is extracted with 
methylene chloride in a separatory funnel. The methylene chloride 
extract is concentrated and combined with the SDS extract prior to 
cleanup.
    2.1.1.3 The sample is vacuum filtered through a glass-fiber filter 
on top of a solid-phase extraction (SPE) disk. The filter and disk are 
extracted in an SDS extractor, and the extract is concentrated for 
cleanup.
    2.1.2 Solid, semi-solid, and multi-phase samples (but not tissue)--
The labeled compounds are spiked into a sample containing 10 g (dry 
weight) of solids. Samples containing multiple phases are pressure 
filtered and any aqueous liquid is discarded. Coarse solids are ground 
or homogenized. Any non-aqueous liquid from multi-phase samples is 
combined with the solids and extracted in an SDS extractor. The extract 
is concentrated for cleanup.
    2.1.3 Fish and other tissue--The sample is extracted by one of two 
procedures:
    2.1.3.1 Soxhlet or SDS extraction--A 20 g aliquot of sample is 
homogenized, and a 10 g aliquot is spiked with the labeled compounds. 
The sample is mixed with sodium sulfate, allowed to dry for 12-24 hours, 
and extracted for 18-24 hours using methylene chloride:hexane (1:1) in a 
Soxhlet extractor. The extract is evaporated to dryness, and the lipid 
content is determined.
    2.1.3.2 HCl digestion--A 20 g aliquot is homogenized, and a 10 g 
aliquot is placed in a bottle and spiked with the labeled compounds. 
After equilibration, 200 mL of hydrochloric acid and 200 mL of methylene 
chloride:hexane (1:1) are added, and the bottle is agitated for 12-24 
hours. The extract is evaporated to dryness, and the lipid content is 
determined.
    2.2 After extraction, \37\Cl4-labeled 2,3,7,8-TCDD is 
added to each extract to measure the efficiency of the cleanup process. 
Sample cleanups may include back-extraction with acid and/or base, and 
gel permeation, alumina, silica gel, Florisil and activated carbon 
chromatography. High-performance liquid chromatography (HPLC) can be 
used for further isolation of the 2,3,7,8-isomers or other specific 
isomers or congeners. Prior to the cleanup procedures cited above, 
tissue extracts are cleaned up using an anthropogenic isolation column, 
a batch silica gel adsorption, or sulfuric acid and base back-
extraction, depending on the tissue extraction procedure used.
    2.3 After cleanup, the extract is concentrated to near dryness. 
Immediately prior to injection, internal standards are added to each 
extract, and an aliquot of the extract is injected into the gas 
chromatograph. The analytes are separated by the GC and detected by a 
high-resolution (=10,000) mass spectrometer. Two exact m/z's 
are monitored for each analyte.
    2.4 An individual CDD/CDF is identified by comparing the GC 
retention time and ion-abundance ratio of two exact m/z's with the 
corresponding retention time of an authentic standard and the 
theoretical or acquired ion-abundance ratio of the two exact m/z's. The 
non-2,3,7,8 substituted isomers and congeners are identified when 
retention times and ion-abundance ratios agree within predefined limits. 
Isomer specificity for 2,3,7,8-TCDD and 2,3,7,8-TCDF is achieved using 
GC columns that resolve these isomers from the other tetra-isomers.
    2.5 Quantitative analysis is performed using selected ion current 
profile (SICP) areas, in one of three ways:
    2.5.1 For the 15 2,3,7,8-substituted CDDs/CDFs with labeled analogs 
(see Table 1), the GC/MS system is calibrated, and the concentration of 
each compound is determined using the isotope dilution technique.
    2.5.2 For 1,2,3,7,8,9-HxCDD, OCDF, and the labeled compounds, the 
GC/MS system is calibrated and the concentration of each compound is 
determined using the internal standard technique.
    2.5.3 For non-2,3,7,8-substituted isomers and for all isomers at a 
given level of chlorination (i.e., total TCDD), concentrations are 
determined using response factors from calibration of the CDDs/CDFs at 
the same level of chlorination.
    2.6 The quality of the analysis is assured through reproducible 
calibration and testing of the extraction, cleanup, and GC/MS systems.

[[Page 306]]

                             3.0 Definitions

    Definitions are given in the glossary at the end of this method.

                   4.0 Contamination and Interferences

    4.1 Solvents, reagents, glassware, and other sample processing 
hardware may yield artifacts and/or elevated baselines causing 
misinterpretation of chromatograms (References 8-9). Specific selection 
of reagents and purification of solvents by distillation in all-glass 
systems may be required. Where possible, reagents are cleaned by 
extraction or solvent rinse.
    4.2 Proper cleaning of glassware is extremely important, because 
glassware may not only contaminate the samples but may also remove the 
analytes of interest by adsorption on the glass surface.
    4.2.1 Glassware should be rinsed with solvent and washed with a 
detergent solution as soon after use as is practical. Sonication of 
glassware containing a detergent solution for approximately 30 seconds 
may aid in cleaning. Glassware with removable parts, particularly 
separatory funnels with fluoropolymer stopcocks, must be disassembled 
prior to detergent washing.
    4.2.2 After detergent washing, glassware should be rinsed 
immediately, first with methanol, then with hot tap water. The tap water 
rinse is followed by another methanol rinse, then acetone, and then 
methylene chloride.
    4.2.3 Do not bake reusable glassware in an oven as a routine part of 
cleaning. Baking may be warranted after particularly dirty samples are 
encountered but should be minimized, as repeated baking of glassware may 
cause active sites on the glass surface that will irreversibly adsorb 
CDDs/CDFs.
    4.2.4 Immediately prior to use, the Soxhlet apparatus should be pre-
extracted with toluene for approximately three hours (see Sections 
12.3.1 through 12.3.3). Separatory funnels should be shaken with 
methylene chloride/toluene (80/20 mixture) for two minutes, drained, and 
then shaken with pure methylene chloride for two minutes.
    4.3 All materials used in the analysis shall be demonstrated to be 
free from interferences by running reference matrix method blanks 
initially and with each sample batch (samples started through the 
extraction process on a given 12-hour shift, to a maximum of 20 
samples).
    4.3.1 The reference matrix must simulate, as closely as possible, 
the sample matrix under test. Ideally, the reference matrix should not 
contain the CDDs/CDFs in detectable amounts, but should contain 
potential interferents in the concentrations expected to be found in the 
samples to be analyzed. For example, a reference sample of human adipose 
tissue containing pentachloronaphthalene can be used to exercise the 
cleanup systems when samples containing pentachloronaphthalene are 
expected.
    4.3.2 When a reference matrix that simulates the sample matrix under 
test is not available, reagent water (Section 7.6.1) can be used to 
simulate water samples; playground sand (Section 7.6.2) or white quartz 
sand (Section 7.3.2) can be used to simulate soils; filter paper 
(Section 7.6.3) can be used to simulate papers and similar materials; 
and corn oil (Section 7.6.4) can be used to simulate tissues.
    4.4 Interferences coextracted from samples will vary considerably 
from source to source, depending on the diversity of the site being 
sampled. Interfering compounds may be present at concentrations several 
orders of magnitude higher than the CDDs/CDFs. The most frequently 
encountered interferences are chlorinated biphenyls, methoxy biphenyls, 
hydroxydiphenyl ethers, benzylphenyl ethers, polynuclear aromatics, and 
pesticides. Because very low levels of CDDs/CDFs are measured by this 
method, the elimination of interferences is essential. The cleanup steps 
given in Section 13 can be used to reduce or eliminate these 
interferences and thereby permit reliable determination of the CDDs/CDFs 
at the levels shown in Table 2.
    4.5 Each piece of reusable glassware should be numbered to associate 
that glassware with the processing of a particular sample. This will 
assist the laboratory in tracking possible sources of contamination for 
individual samples, identifying glassware associated with highly 
contaminated samples that may require extra cleaning, and determining 
when glassware should be discarded.
    4.6 Cleanup of tissue--The natural lipid content of tissue can 
interfere in the analysis of tissue samples for the CDDs/CDFs. The lipid 
contents of different species and portions of tissue can vary widely. 
Lipids are soluble to varying degrees in various organic solvents and 
may be present in sufficient quantity to overwhelm the column 
chromatographic cleanup procedures used for cleanup of sample extracts. 
Lipids must be removed by the lipid removal procedures in Section 13.7, 
followed by alumina (Section 13.4) or Florisil (Section 13.8), and 
carbon (Section 13.5) as minimum additional cleanup steps. If 
chlorodiphenyl ethers are detected, as indicated by the presence of 
peaks at the exact m/z's monitored for these interferents, alumina and/
or Florisil cleanup must be employed to eliminate these interferences.

                               5.0 Safety

    5.1 The toxicity or carcinogenicity of each compound or reagent used 
in this method has not been precisely determined; however, each chemical 
compound should be

[[Page 307]]

treated as a potential health hazard. Exposure to these compounds should 
be reduced to the lowest possible level.
    5.1.1 The 2,3,7,8-TCDD isomer has been found to be acnegenic, 
carcinogenic, and teratogenic in laboratory animal studies. It is 
soluble in water to approximately 200 ppt and in organic solvents to 
0.14%. On the basis of the available toxicological and physical 
properties of 2,3,7,8-TCDD, all of the CDDs/CDFs should be handled only 
by highly trained personnel thoroughly familiar with handling and 
cautionary procedures and the associated risks.
    5.1.2 It is recommended that the laboratory purchase dilute standard 
solutions of the analytes in this method. However, if primary solutions 
are prepared, they shall be prepared in a hood, and a NIOSH/MESA 
approved toxic gas respirator shall be worn when high concentrations are 
handled.
    5.2 The laboratory is responsible for maintaining a current 
awareness file of OSHA regulations regarding the safe handling of the 
chemicals specified in this method. A reference file of material safety 
data sheets (MSDSs) should also be made available to all personnel 
involved in these analyses. It is also suggested that the laboratory 
perform personal hygiene monitoring of each analyst who uses this method 
and that the results of this monitoring be made available to the 
analyst. Additional information on laboratory safety can be found in 
References 10-13. The references and bibliography at the end of 
Reference 13 are particularly comprehensive in dealing with the general 
subject of laboratory safety.
    5.3 The CDDs/CDFs and samples suspected to contain these compounds 
are handled using essentially the same techniques employed in handling 
radioactive or infectious materials. Well-ventilated, controlled access 
laboratories are required. Assistance in evaluating the health hazards 
of particular laboratory conditions may be obtained from certain 
consulting laboratories and from State Departments of Health or Labor, 
many of which have an industrial health service. The CDDs/CDFs are 
extremely toxic to laboratory animals. Each laboratory must develop a 
strict safety program for handling these compounds. The practices in 
References 2 and 14 are highly recommended.
    5.3.1 Facility--When finely divided samples (dusts, soils, dry 
chemicals) are handled, all operations (including removal of samples 
from sample containers, weighing, transferring, and mixing) should be 
performed in a glove box demonstrated to be leak tight or in a fume hood 
demonstrated to have adequate air flow. Gross losses to the laboratory 
ventilation system must not be allowed. Handling of the dilute solutions 
normally used in analytical and animal work presents no inhalation 
hazards except in the case of an accident.
    5.3.2 Protective equipment--Disposable plastic gloves, apron or lab 
coat, safety glasses or mask, and a glove box or fume hood adequate for 
radioactive work should be used. During analytical operations that may 
give rise to aerosols or dusts, personnel should wear respirators 
equipped with activated carbon filters. Eye protection equipment 
(preferably full face shields) must be worn while working with exposed 
samples or pure analytical standards. Latex gloves are commonly used to 
reduce exposure of the hands. When handling samples suspected or known 
to contain high concentrations of the CDDs/CDFs, an additional set of 
gloves can also be worn beneath the latex gloves.
    5.3.3 Training--Workers must be trained in the proper method of 
removing contaminated gloves and clothing without contacting the 
exterior surfaces.
    5.3.4 Personal hygiene--Hands and forearms should be washed 
thoroughly after each manipulation and before breaks (coffee, lunch, and 
shift).
    5.3.5 Confinement--Isolated work areas posted with signs, segregated 
glassware and tools, and plastic absorbent paper on bench tops will aid 
in confining contamination.
    5.3.6 Effluent vapors--The effluents of sample splitters from the 
gas chromatograph (GC) and from roughing pumps on the mass spectrometer 
(MS) should pass through either a column of activated charcoal or be 
bubbled through a trap containing oil or high-boiling alcohols to 
condense CDD/CDF vapors.
    5.3.7 Waste Handling--Good technique includes minimizing 
contaminated waste. Plastic bag liners should be used in waste cans. 
Janitors and other personnel must be trained in the safe handling of 
waste.
    5.3.8 Decontamination
    5.3.8.1 Decontamination of personnel--Use any mild soap with plenty 
of scrubbing action.
    5.3.8.2 Glassware, tools, and surfaces--Chlorothene NU Solvent is 
the least toxic solvent shown to be effective. Satisfactory cleaning may 
be accomplished by rinsing with Chlorothene, then washing with any 
detergent and water. If glassware is first rinsed with solvent, then the 
dish water may be disposed of in the sewer. Given the cost of disposal, 
it is prudent to minimize solvent wastes.
    5.3.9 Laundry--Clothing known to be contaminated should be collected 
in plastic bags. Persons who convey the bags and launder the clothing 
should be advised of the hazard and trained in proper handling. The 
clothing may be put into a washer without contact if the launderer knows 
of the potential problem. The washer should be run through a cycle 
before being used again for other clothing.
    5.3.10 Wipe tests--A useful method of determining cleanliness of 
work surfaces and

[[Page 308]]

tools is to wipe the surface with a piece of filter paper. Extraction 
and analysis by GC with an electron capture detector (ECD) can achieve a 
limit of detection of 0.1 [micro]g per wipe; analysis using this method 
can achieve an even lower detection limit. Less than 0.1 [micro]g per 
wipe indicates acceptable cleanliness; anything higher warrants further 
cleaning. More than 10 [micro]g on a wipe constitutes an acute hazard 
and requires prompt cleaning before further use of the equipment or work 
space, and indicates that unacceptable work practices have been 
employed.
    5.3.11 Table or wrist-action shaker--The use of a table or wrist-
action shaker for extraction of tissues presents the possibility of 
breakage of the extraction bottle and spillage of acid and flammable 
organic solvent. A secondary containment system around the shaker is 
suggested to prevent the spread of acid and solvents in the event of 
such a breakage. The speed and intensity of shaking action should also 
be adjusted to minimize the possibility of breakage.

                       6.0 Apparatus and Materials

    Note: Brand names, suppliers, and part numbers are for illustration 
purposes only and no endorsement is implied. Equivalent performance may 
be achieved using apparatus and materials other than those specified 
here. Meeting the performance requirements of this method is the 
responsibility of the laboratory.

    6.1 Sampling Equipment for Discrete or Composite Sampling
    6.1.1 Sample bottles and caps
    6.1.1.1 Liquid samples (waters, sludges and similar materials 
containing 5% solids or less)--Sample bottle, amber glass, 1.1 L 
minimum, with screw cap.
    6.1.1.2 Solid samples (soils, sediments, sludges, paper pulps, 
filter cake, compost, and similar materials that contain more than 5% 
solids)--Sample bottle, wide mouth, amber glass, 500 mL minimum.
    6.1.1.3 If amber bottles are not available, samples shall be 
protected from light.
    6.1.1.4 Bottle caps--Threaded to fit sample bottles. Caps shall be 
lined with fluoropolymer.
    6.1.1.5 Cleaning
    6.1.1.5.1 Bottles are detergent water washed, then solvent rinsed 
before use.
    6.1.1.5.2 Liners are detergent water washed, rinsed with reagent 
water (Section 7.6.1) followed by solvent, and baked at approximately 
200 [deg]C for a minimum of 1 hour prior to use.
    6.1.2 Compositing equipment--Automatic or manual compositing system 
incorporating glass containers cleaned per bottle cleaning procedure 
above. Only glass or fluoropolymer tubing shall be used. If the sampler 
uses a peristaltic pump, a minimum length of compressible silicone 
rubber tubing may be used in the pump only. Before use, the tubing shall 
be thoroughly rinsed with methanol, followed by repeated rinsing with 
reagent water to minimize sample contamination. An integrating flow 
meter is used to collect proportional composite samples.
    6.2 Equipment for Glassware Cleaning--Laboratory sink with overhead 
fume hood.
    6.3 Equipment for Sample Preparation
    6.3.1 Laboratory fume hood of sufficient size to contain the sample 
preparation equipment listed below.
    6.3.2 Glove box (optional).
    6.3.3 Tissue homogenizer--VirTis Model 45 Macro homogenizer 
(American Scientific Products H-3515, or equivalent) with stainless 
steel Macro-shaft and Turbo-shear blade.
    6.3.4 Meat grinder--Hobart, or equivalent, with 3-5 mm holes in 
inner plate.
    6.3.5 Equipment for determining percent moisture
    6.3.5.1 Oven--Capable of maintaining a temperature of 110 5 [deg]C.
    6.3.5.2 Dessicator.
    6.3.6 Balances
    6.3.6.1 Analytical--Capable of weighing 0.1 mg.
    6.3.6.2 Top loading--Capable of weighing 10 mg.
    6.4 Extraction Apparatus
    6.4.1 Water samples
    6.4.1.1 pH meter, with combination glass electrode.
    6.4.1.2 pH paper, wide range (Hydrion Papers, or equivalent).
    6.4.1.3 Graduated cylinder, 1 L capacity.
    6.4.1.4 Liquid/liquid extraction--Separatory funnels, 250 mL, 500 
mL, and 2000 mL, with fluoropolymer stopcocks.
    6.4.1.5 Solid-phase extraction
    6.4.1.5.1 One liter filtration apparatus, including glass funnel, 
glass frit support, clamp, adapter, stopper, filtration flask, and 
vacuum tubing (Figure 4). For wastewater samples, the apparatus should 
accept 90 or 144 mm disks. For drinking water or other samples 
containing low solids, smaller disks may be used.
    6.4.1.5.2 Vacuum source capable of maintaining 25 in. Hg, equipped 
with shutoff valve and vacuum gauge.
    6.4.1.5.3 Glass-fiber filter--Whatman GMF 150 (or equivalent), 1 
micron pore size, to fit filtration apparatus in Section 6.4.1.5.1.
    6.4.1.5.4 Solid-phase extraction disk containing octadecyl 
(C18) bonded silica uniformly enmeshed in an inert matrix--
Fisher Scientific 14-378F (or equivalent), to fit filtration apparatus 
in Section 6.4.1.5.1.
    6.4.2 Soxhlet/Dean-Stark (SDS) extractor (Figure 5)--For filters and 
solid/sludge samples.
    6.4.2.1 Soxhlet--50 mm ID, 200 mL capacity with 500 mL flask (Cal-
Glass LG-6900, or equivalent, except substitute 500 mL round-bottom 
flask for 300 mL flat-bottom flask).

[[Page 309]]

    6.4.2.2 Thimble--43 x 123 to fit Soxhlet (Cal-Glass LG-6901-122, or 
equivalent).
    6.4.2.3 Moisture trap--Dean Stark or Barret with fluoropolymer 
stopcock, to fit Soxhlet.
    6.4.2.4 Heating mantle--Hemispherical, to fit 500 mL round-bottom 
flask (Cal-Glass LG-8801-112, or equivalent).
    6.4.2.5 Variable transformer--Powerstat (or equivalent), 110 volt, 
10 amp.
    6.4.3 Apparatus for extraction of tissue.
    6.4.3.1 Bottle for extraction (if digestion/extraction using HCl is 
used)'' 500-600 mL wide-mouth clear glass, with fluoropolymer-lined cap.
    6.4.3.2 Bottle for back-extraction--100-200 mL narrow-mouth clear 
glass with fluoropolymer-lined cap.
    6.4.3.3 Mechanical shaker--Wrist-action or platform-type rotary 
shaker that produces vigorous agitation (Sybron Thermolyne Model LE 
``Big Bill'' rotator/shaker, or equivalent).
    6.4.3.4 Rack attached to shaker table to permit agitation of four to 
nine samples simultaneously.
    6.4.4 Beakers--400-500 mL.
    6.4.5 Spatulas--Stainless steel.
    6.5 Filtration Apparatus.
    6.5.1 Pyrex glass wool--Solvent-extracted by SDS for three hours 
minimum.

    Note: Baking glass wool may cause active sites that will 
irreversibly adsorb CDDs/CDFs.

    6.5.2 Glass funnel--125-250 mL.
    6.5.3 Glass-fiber filter paper--Whatman GF/D (or equivalent), to fit 
glass funnel in Section 6.5.2.
    6.5.4 Drying column--15-20 mm ID Pyrex chromatographic column 
equipped with coarse-glass frit or glass-wool plug.
    6.5.5 Buchner funnel--15 cm.
    6.5.6 Glass-fiber filter paper--to fit Buchner funnel in Section 
6.5.5.
    6.5.7 Filtration flasks--1.5-2.0 L, with side arm.
    6.5.8 Pressure filtration apparatus--Millipore YT30 142 HW, or 
equivalent.
    6.6 Centrifuge Apparatus.
    6.6.1 Centrifuge--Capable of rotating 500 mL centrifuge bottles or 
15 mL centrifuge tubes at 5,000 rpm minimum.
    6.6.2 Centrifuge bottles--500 mL, with screw-caps, to fit 
centrifuge.
    6.6.3 Centrifuge tubes--12-15 mL, with screw-caps, to fit 
centrifuge.
    6.7 Cleanup Apparatus.
    6.7.1 Automated gel permeation chromatograph (Analytical Biochemical 
Labs, Inc, Columbia, MO, Model GPC Autoprep 1002, or equivalent).
    6.7.1.1 Column--600-700 mm long x 25 mm ID, packed with 70 g of
SX-3 Bio-beads (Bio-Rad Laboratories, Richmond, CA, or equivalent).
    6.7.1.2 Syringe--10 mL, with Luer fitting.
    6.7.1.3 Syringe filter holder--stainless steel, and glass-fiber or 
fluoropolymer filters (Gelman 4310, or equivalent).
    6.7.1.4 UV detectors--254 nm, preparative or semi-preparative flow 
cell (Isco, Inc., Type 6; Schmadzu, 5 mm path length; Beckman-Altex 
152W, 8 [micro]L micro-prep flow cell, 2 mm path; Pharmacia UV-1, 3 mm 
flow cell; LDC Milton-Roy UV-3, monitor 1203; or equivalent).
    6.7.2 Reverse-phase high-performance liquid chromatograph.
    6.7.2.1 Column oven and detector--Perkin-Elmer Model LC-65T (or 
equivalent) operated at 0.02 AUFS at 235 nm.
    6.7.2.2 Injector--Rheodyne 7120 (or equivalent) with 50 [micro]L 
sample loop.
    6.7.2.3 Column--Two 6.2 mm x 250 mm Zorbax-ODS columns in series 
(DuPont Instruments Division, Wilmington, DE, or equivalent), operated 
at 50 [deg]C with 2.0 mL/min methanol isocratic effluent.
    6.7.2.4 Pump--Altex 110A (or equivalent).
    6.7.3 Pipets.
    6.7.3.1 Disposable, pasteur--150 mm long x 5-mm ID (Fisher 
Scientific 13-678-6A, or equivalent).
    6.7.3.2 Disposable, serological--10 mL (6 mm ID).
    6.7.4 Glass chromatographic columns.
    6.7.4.1 150 mm long x 8-mm ID, (Kontes K-420155, or equivalent) with 
coarse-glass frit or glass-wool plug and 250 mL reservoir.
    6.7.4.2 200 mm long x 15 mm ID, with coarse-glass frit or glass-wool 
plug and 250 mL reservoir.
    6.7.4.3 300 mm long x 25 mm ID, with 300 mL reservoir and glass or 
fluoropolymer stopcock.
    6.7.5 Stirring apparatus for batch silica cleanup of tissue 
extracts.
    6.7.5.1 Mechanical stirrer--Corning Model 320, or equivalent.
    6.7.5.2 Bottle--500-600 mL wide-mouth clear glass.
    6.7.6 Oven--For baking and storage of adsorbents, capable of 
maintaining a constant temperature (5 [deg]C) in 
the range of 105-250 [deg]C.
    6.8 Concentration Apparatus.
    6.8.1 Rotary evaporator--Buchi/Brinkman-American Scientific No. 
E5045-10 or equivalent, equipped with a variable temperature water bath.
    6.8.1.1 Vacuum source for rotary evaporator equipped with shutoff 
valve at the evaporator and vacuum gauge.
    6.8.1.2 A recirculating water pump and chiller are recommended, as 
use of tap water for cooling the evaporator wastes large volumes of 
water and can lead to inconsistent performance as water temperatures and 
pressures vary.
    6.8.1.3 Round-bottom flask--100 mL and 500 mL or larger, with 
ground-glass fitting compatible with the rotary evaporator.
    6.8.2 Kuderna-Danish (K-D) Concentrator.

[[Page 310]]

    6.8.2.1 Concentrator tube--10 mL, graduated (Kontes K-570050-1025, 
or equivalent) with calibration verified. Ground-glass stopper (size 19/
22 joint) is used to prevent evaporation of extracts.
    6.8.2.2 Evaporation flask--500 mL (Kontes K-570001-0500, or 
equivalent), attached to concentrator tube with springs (Kontes K-
662750-0012 or equivalent).
    6.8.2.3 Snyder column--Three-ball macro (Kontes K-503000-0232, or 
equivalent).
    6.8.2.4 Boiling chips.
    6.8.2.4.1 Glass or silicon carbide--Approximately 10/40 mesh, 
extracted with methylene chloride and baked at 450 [deg]C for one hour 
minimum.
    6.8.2.4.2 Fluoropolymer (optional)--Extracted with methylene 
chloride.
    6.8.2.5 Water bath--Heated, with concentric ring cover, capable of 
maintaining a temperature within 2 [deg]C, 
installed in a fume hood.
    6.8.3 Nitrogen blowdown apparatus--Equipped with water bath 
controlled in the range of 30-60 [deg]C (N-Evap, Organomation 
Associates, Inc., South Berlin, MA, or equivalent), installed in a fume 
hood.
    6.8.4 Sample vials.
    6.8.4.1 Amber glass--2-5 mL with fluoropolymer-lined screw-cap.
    6.8.4.2 Glass--0.3 mL, conical, with fluoropolymer-lined screw or 
crimp cap.
    6.9 Gas Chromatograph--Shall have splitless or on-column injection 
port for capillary column, temperature program with isothermal hold, and 
shall meet all of the performance specifications in Section 10.
    6.9.1 GC column for CDDs/CDFs and for isomer specificity for 
2,3,7,8-TCDD--60 5 m long x 0.32 0.02 mm ID; 0.25 [micro]m 5% phenyl, 94% methyl, 1% 
vinyl silicone bonded-phase fused-silica capillary column (J&W DB-5, or 
equivalent).
    6.9.2 GC column for isomer specificity for 2,3,7,8-TCDF--30 5 m long x 0.32 0.02 mm ID; 0.25 
[micro]m bonded-phase fused-silica capillary column (J&W DB-225, or 
equivalent).
    6.10 Mass Spectrometer--28-40 eV electron impact ionization, shall 
be capable of repetitively selectively monitoring 12 exact m/z's minimum 
at high resolution (=10,000) during a period of approximately 
one second, and shall meet all of the performance specifications in 
Section 10.
    6.11 GC/MS Interface--The mass spectrometer (MS) shall be interfaced 
to the GC such that the end of the capillary column terminates within 1 
cm of the ion source but does not intercept the electron or ion beams.
    6.12 Data System--Capable of collecting, recording, and storing MS 
data.

                       7.0 Reagents and Standards

    7.1 pH Adjustment and Back-Extraction.
    7.1.1 Potassium hydroxide--Dissolve 20 g reagent grade KOH in 100 mL 
reagent water.
    7.1.2 Sulfuric acid--Reagent grade (specific gravity 1.84).
    7.1.3 Hydrochloric acid--Reagent grade, 6N.
    7.1.4 Sodium chloride--Reagent grade, prepare at 5% (w/v) solution 
in reagent water.
    7.2 Solution Drying and Evaporation.
    7.2.1 Solution drying--Sodium sulfate, reagent grade, granular, 
anhydrous (Baker 3375, or equivalent), rinsed with methylene chloride 
(20 mL/g), baked at 400 [deg]C for one hour minimum, cooled in a 
dessicator, and stored in a pre-cleaned glass bottle with screw-cap that 
prevents moisture from entering. If, after heating, the sodium sulfate 
develops a noticeable grayish cast (due to the presence of carbon in the 
crystal matrix), that batch of reagent is not suitable for use and 
should be discarded. Extraction with methylene chloride (as opposed to 
simple rinsing) and baking at a lower temperature may produce sodium 
sulfate that is suitable for use.
    7.2.2 Tissue drying--Sodium sulfate, reagent grade, powdered, 
treated and stored as above.
    7.2.3 Prepurified nitrogen.
    7.3 Extraction.
    7.3.1 Solvents--Acetone, toluene, cyclohexane, hexane, methanol, 
methylene chloride, and nonane; distilled in glass, pesticide quality, 
lot-certified to be free of interferences.
    7.3.2 White quartz sand, 60/70 mesh--For Soxhlet/Dean-Stark 
extraction (Aldrich Chemical, Cat. No. 27-437-9, or equivalent). Bake at 
450 [deg]C for four hours minimum.
    7.4 GPC Calibration Solution--Prepare a solution containing 300 mg/
mL corn oil, 15 mg/mL bis(2-ethylhexyl) phthalate, 1.4 mg/mL 
pentachlorophenol, 0.1 mg/mL perylene, and 0.5 mg/mL sulfur.
    7.5 Adsorbents for Sample Cleanup.
    7.5.1 Silica gel.
    7.5.1.1 Activated silica gel--100-200 mesh, Supelco 1-3651 (or 
equivalent), rinsed with methylene chloride, baked at 180 [deg]C for a 
minimum of one hour, cooled in a dessicator, and stored in a precleaned 
glass bottle with screw-cap that prevents moisture from entering.
    7.5.1.2 Acid silica gel (30% w/w)--Thoroughly mix 44.0 g of 
concentrated sulfuric acid with 100.0 g of activated silica gel in a 
clean container. Break up aggregates with a stirring rod until a uniform 
mixture is obtained. Store in a bottle with a fluoropolymer-lined screw-
cap.
    7.5.1.3 Basic silica gel--Thoroughly mix 30 g of 1N sodium hydroxide 
with 100 g of activated silica gel in a clean container. Break up 
aggregates with a stirring rod until a uniform mixture is obtained. 
Store in a bottle with a fluoropolymer-lined screw-cap.
    7.5.1.4 Potassium silicate.

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    7.5.1.4.1 Dissolve 56 g of high purity potassium hydroxide (Aldrich, 
or equivalent) in 300 mL of methanol in a 750-1000 mL flat-bottom flask.
    7.5.1.4.2 Add 100 g of silica gel and a stirring bar, and stir on a 
hot plate at 60-70 [deg]C for one to two hours.
    7.5.1.4.3 Decant the liquid and rinse the potassium silicate twice 
with 100 mL portions of methanol, followed by a single rinse with 100 mL 
of methylene chloride.
    7.5.1.4.4 Spread the potassium silicate on solvent-rinsed aluminum 
foil and dry for two to four hours in a hood.
    7.5.1.4.5 Activate overnight at 200-250 [deg]C.
    7.5.2 Alumina--Either one of two types of alumina, acid or basic, 
may be used in the cleanup of sample extracts, provided that the 
laboratory can meet the performance specifications for the recovery of 
labeled compounds described in Section 9.3. The same type of alumina 
must be used for all samples, including those used to demonstrate 
initial precision and recovery (Section 9.2) and ongoing precision and 
recovery (Section 15.5).
    7.5.2.1 Acid alumina--Supelco 19996-6C (or equivalent). Activate by 
heating to 130 [deg]C for a minimum of 12 hours.
    7.5.2.2 Basic alumina--Supelco 19944-6C (or equivalent). Activate by 
heating to 600 [deg]C for a minimum of 24 hours. Alternatively, activate 
by heating in a tube furnace at 650-700 [deg]C under an air flow rate of 
approximately 400 cc/minute. Do not heat over 700 [deg]C, as this can 
lead to reduced capacity for retaining the analytes. Store at 130 [deg]C 
in a covered flask. Use within five days of baking.
    7.5.3 Carbon.
    7.5.3.1 Carbopak C--(Supelco 1-0258, or equivalent).
    7.5.3.2 Celite 545--(Supelco 2-0199, or equivalent).
    7.5.3.3 Thoroughly mix 9.0 g Carbopak C and 41.0 g Celite 545 to 
produce an 18% w/w mixture. Activate the mixture at 130 [deg]C for a 
minimum of six hours. Store in a dessicator.
    7.5.4 Anthropogenic isolation column--Pack the column in Section 
6.7.4.3 from bottom to top with the following:
    7.5.4.1 2 g silica gel (Section 7.5.1.1).
    7.5.4.2 2 g potassium silicate (Section 7.5.1.4).
    7.5.4.3 2 g granular anhydrous sodium sulfate (Section 7.2.1).
    7.5.4.4 10 g acid silica gel (Section 7.5.1.2).
    7.5.4.5 2 g granular anhydrous sodium sulfate.
    7.5.5 Florisil column.
    7.5.5.1 Florisil--60-100 mesh, Floridin Corp (or equivalent). 
Soxhlet extract in 500 g portions for 24 hours.
    7.5.5.2 Insert a glass wool plug into the tapered end of a graduated 
serological pipet (Section 6.7.3.2). Pack with 1.5 g (approx 2 mL) of 
Florisil topped with approx 1 mL of sodium sulfate (Section 7.2.1) and a 
glass wool plug.
    7.5.5.3 Activate in an oven at 130-150 [deg]C for a minimum of 24 
hours and cool for 30 minutes. Use within 90 minutes of cooling.
    7.6 Reference Matrices--Matrices in which the CDDs/CDFs and 
interfering compounds are not detected by this method.
    7.6.1 Reagent water--Bottled water purchased locally, or prepared by 
passage through activated carbon.
    7.6.2 High-solids reference matrix--Playground sand or similar 
material. Prepared by extraction with methylene chloride and/or baking 
at 450 [deg]C for a minimum of four hours.
    7.6.3 Paper reference matrix--Glass-fiber filter, Gelman Type A, or 
equivalent. Cut paper to simulate the surface area of the paper sample 
being tested.
    7.6.4 Tissue reference matrix--Corn or other vegetable oil. May be 
prepared by extraction with methylene chloride.
    7.6.5 Other matrices--This method may be verified on any reference 
matrix by performing the tests given in Section 9.2. Ideally, the matrix 
should be free of the CDDs/CDFs, but in no case shall the background 
level of the CDDs/CDFs in the reference matrix exceed three times the 
minimum levels in Table 2. If low background levels of the CDDs/CDFs are 
present in the reference matrix, the spike level of the analytes used in 
Section 9.2 should be increased to provide a spike-to-background ratio 
in the range of 1:1 to 5:1 (Reference 15).
    7.7 Standard Solutions--Purchased as solutions or mixtures with 
certification to their purity, concentration, and authenticity, or 
prepared from materials of known purity and composition. If the chemical 
purity is 98% or greater, the weight may be used without correction to 
compute the concentration of the standard. When not being used, 
standards are stored in the dark at room temperature in screw-capped 
vials with fluoropolymer-lined caps. A mark is placed on the vial at the 
level of the solution so that solvent loss by evaporation can be 
detected. If solvent loss has occurred, the solution should be replaced.
    7.8 Stock Solutions.
    7.8.1 Preparation--Prepare in nonane per the steps below or purchase 
as dilute solutions (Cambridge Isotope Laboratories (CIL), Woburn, MA, 
or equivalent). Observe the safety precautions in Section 5, and the 
recommendation in Section 5.1.2.
    7.8.2 Dissolve an appropriate amount of assayed reference material 
in solvent. For example, weigh 1-2 mg of 2,3,7,8-TCDD to three 
significant figures in a 10 mL ground-glass-stoppered volumetric flask 
and fill to the mark with nonane. After the TCDD is completely 
dissolved, transfer the solution to a clean 15 mL vial with 
fluoropolymer-lined cap.
    7.8.3 Stock standard solutions should be checked for signs of 
degradation prior to the

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preparation of calibration or performance test standards. Reference 
standards that can be used to determine the accuracy of calibration 
standards are available from CIL and may be available from other 
vendors.
    7.9 PAR Stock Solution
    7.9.1 All CDDs/CDFs--Using the solutions in Section 7.8, prepare the 
PAR stock solution to contain the CDDs/CDFs at the concentrations shown 
in Table 3. When diluted, the solution will become the PAR (Section 
7.14).
    7.9.2 If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, 
prepare the PAR stock solution to contain these compounds only.
    7.10 Labeled-Compound Spiking Solution.
    7.10.1 All CDDs/CDFs--From stock solutions, or from purchased 
mixtures, prepare this solution to contain the labeled compounds in 
nonane at the concentrations shown in Table 3. This solution is diluted 
with acetone prior to use (Section 7.10.3).
    7.10.2 If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, 
prepare the labeled-compound solution to contain these compounds only. 
This solution is diluted with acetone prior to use (Section 7.10.3).
    7.10.3 Dilute a sufficient volume of the labeled compound solution 
(Section 7.10.1 or 7.10.2) by a factor of 50 with acetone to prepare a 
diluted spiking solution. Each sample requires 1.0 mL of the diluted 
solution, but no more solution should be prepared than can be used in 
one day.
    7.11 Cleanup Standard--Prepare \37\Cl\4\-2,3,7,8-TCDD in nonane at 
the concentration shown in Table 3. The cleanup standard is added to all 
extracts prior to cleanup to measure the efficiency of the cleanup 
process.
    7.12 Internal Standard(s).
    7.12.1 All CDDs/CDFs--Prepare the internal standard solution to 
contain \13\C\12\-1,2,3,4-TCDD and \13\C\2\-1,2,3,7,8,9-HxCDD in nonane 
at the concentration shown in Table 3.
    7.12.2 If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, 
prepare the internal standard solution to contain \13\C\12\-1,2,3,4-TCDD 
only.
    7.13 Calibration Standards (CS1 through CS5)--Combine the solutions 
in Sections 7.9 through 7.12 to produce the five calibration solutions 
shown in Table 4 in nonane. These solutions permit the relative response 
(labeled to native) and response factor to be measured as a function of 
concentration. The CS3 standard is used for calibration verification 
(VER). If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, 
combine the solutions appropriate to these compounds.
    7.14 Precision and Recovery (PAR) Standard--Used for determination 
of initial (Section 9.2) and ongoing (Section 15.5) precision and 
recovery. Dilute 10 [micro]L of the precision and recovery standard 
(Section 7.9.1 or 7.9.2) to 2.0 mL with acetone for each sample matrix 
for each sample batch. One mL each are required for the blank and OPR 
with each matrix in each batch.
    7.15 GC Retention Time Window Defining Solution and Isomer 
Specificity Test Standard--Used to define the beginning and ending 
retention times for the dioxin and furan isomers and to demonstrate 
isomer specificity of the GC columns employed for determination of 
2,3,7,8-TCDD and 2,3,7,8-TCDF. The standard must contain the compounds 
listed in Table 5 (CIL EDF--4006, or equivalent), at a minimum. It is 
not necessary to monitor the window-defining compounds if only 2,3,7,8-
TCDD and 2,3,7,8-TCDF are to be determined. In this case, an isomer-
specificity test standard containing the most closely eluted isomers 
listed in Table 5 (CIL EDF-4033, or equivalent) may be used.
    7.16 QC Check Sample--A QC Check Sample should be obtained from a 
source independent of the calibration standards. Ideally, this check 
sample would be a certified reference material containing the CDDs/CDFs 
in known concentrations in a sample matrix similar to the matrix under 
test.
    7.17 Stability of Solutions--Standard solutions used for 
quantitative purposes (Sections 7.9 through 7.15) should be analyzed 
periodically, and should be assayed against reference standards (Section 
7.8.3) before further use.

     8.0 Sample Collection, Preservation, Storage, and Holding Times

    8.1 Collect samples in amber glass containers following conventional 
sampling practices (Reference 16). Aqueous samples that flow freely are 
collected in refrigerated bottles using automatic sampling equipment. 
Solid samples are collected as grab samples using wide-mouth jars.
    8.2 Maintain aqueous samples in the dark at 0-4 [deg]C from the time 
of collection until receipt at the laboratory. If residual chlorine is 
present in aqueous samples, add 80 mg sodium thiosulfate per liter of 
water. EPA Methods 330.4 and 330.5 may be used to measure residual 
chlorine (Reference 17). If sample pH is greater than 9, adjust to pH 7-
9 with sulfuric acid.
    Maintain solid, semi-solid, oily, and mixed-phase samples in the 
dark at <4 [deg]C from the time of collection until receipt at the 
laboratory.
    Store aqueous samples in the dark at 0-4 [deg]C. Store solid, semi-
solid, oily, mixed-phase, and tissue samples in the dark at <-10 [deg]C.
    8.3 Fish and Tissue Samples.
    8.3.1 Fish may be cleaned, filleted, or processed in other ways in 
the field, such that the laboratory may expect to receive whole fish, 
fish fillets, or other tissues for analysis.
    8.3.2 Fish collected in the field should be wrapped in aluminum 
foil, and must be maintained at a temperature less than 4 [deg]C

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from the time of collection until receipt at the laboratory.
    8.3.3 Samples must be frozen upon receipt at the laboratory and 
maintained in the dark at <-10 [deg]C until prepared. Maintain unused 
sample in the dark at <-10 [deg]C.
    8.4 Holding Times.
    8.4.1 There are no demonstrated maximum holding times associated 
with CDDs/CDFs in aqueous, solid, semi-solid, tissues, or other sample 
matrices. If stored in the dark at 0-4 [deg]C and preserved as given 
above (if required), aqueous samples may be stored for up to one year. 
Similarly, if stored in the dark at <-10 [deg]C, solid, semi-solid, 
multi-phase, and tissue samples may be stored for up to one year.
    8.4.2 Store sample extracts in the dark at <-10 [deg]C until 
analyzed. If stored in the dark at <-10 [deg]C, sample extracts may be 
stored for up to one year.

                  9.0 Quality Assurance/Quality Control

    9.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program (Reference 18). The minimum 
requirements of this program consist of an initial demonstration of 
laboratory capability, analysis of samples spiked with labeled compounds 
to evaluate and document data quality, and analysis of standards and 
blanks as tests of continued performance. Laboratory performance is 
compared to established performance criteria to determine if the results 
of analyses meet the performance characteristics of the method.
    If the method is to be applied to sample matrix other than water 
(e.g., soils, filter cake, compost, tissue) the most appropriate 
alternate matrix (Sections 7.6.2 through 7.6.5) is substituted for the 
reagent water matrix (Section 7.6.1) in all performance tests.
    9.1.1 The analyst shall make an initial demonstration of the ability 
to generate acceptable accuracy and precision with this method. This 
ability is established as described in Section 9.2.
    9.1.2 In recognition of advances that are occurring in analytical 
technology, and to allow the analyst to overcome sample matrix 
interferences, the analyst is permitted certain options to improve 
separations or lower the costs of measurements. These options include 
alternate extraction, concentration, cleanup procedures, and changes in 
columns and detectors. Alternate determinative techniques, such as the 
substitution of spectroscopic or immuno-assay techniques, and changes 
that degrade method performance, are not allowed. If an analytical 
technique other than the techniques specified in this method is used, 
that technique must have a specificity equal to or better than the 
specificity of the techniques in this method for the analytes of 
interest.
    9.1.2.1 Each time a modification is made to this method, the analyst 
is required to repeat the procedure in Section 9.2. If the detection 
limit of the method will be affected by the change, the laboratory is 
required to demonstrate that the MDL (40 CFR part 136, appendix B) is 
lower than one-third the regulatory compliance level or one-third the ML 
in this method, whichever is higher. If calibration will be affected by 
the change, the analyst must recalibrate the instrument per Section 10.
    9.1.2.2 The laboratory is required to maintain records of 
modifications made to this method. These records include the following, 
at a minimum:
    9.1.2.2.1 The names, titles, addresses, and telephone numbers of the 
analyst(s) who performed the analyses and modification, and of the 
quality control officer who witnessed and will verify the analyses and 
modifications.
    9.1.2.2.2 A listing of pollutant(s) measured, by name and CAS 
Registry number.
    9.1.2.2.3 A narrative stating reason(s) for the modifications.
    9.1.2.2.4 Results from all quality control (QC) tests comparing the 
modified method to this method, including:
    (a) Calibration (Section 10.5 through 10.7).
    (b) Calibration verification (Section 15.3).
    (c) Initial precision and recovery (Section 9.2).
    (d) Labeled compound recovery (Section 9.3).
    (e) Analysis of blanks (Section 9.5).
    (f) Accuracy assessment (Section 9.4).
    9.1.2.2.5 Data that will allow an independent reviewer to validate 
each determination by tracing the instrument output (peak height, area, 
or other signal) to the final result. These data are to include:
    (a) Sample numbers and other identifiers.
    (b) Extraction dates.
    (c) Analysis dates and times.
    (d) Analysis sequence/run chronology.
    (e) Sample weight or volume (Section 11).
    (f) Extract volume prior to each cleanup step (Section 13).
    (g) Extract volume after each cleanup step (Section 13).
    (h) Final extract volume prior to injection (Section 14).
    (i) Injection volume (Section 14.3).
    (j) Dilution data, differentiating between dilution of a sample or 
extract (Section 17.5).
    (k) Instrument and operating conditions.
    (l) Column (dimensions, liquid phase, solid support, film thickness, 
etc).
    (m) Operating conditions (temperatures, temperature program, flow 
rates).
    (n) Detector (type, operating conditions, etc).
    (o) Chromatograms, printer tapes, and other recordings of raw data.
    (p) Quantitation reports, data system outputs, and other data to 
link the raw data to the results reported.

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    9.1.3 Analyses of method blanks are required to demonstrate freedom 
from contamination (Section 4.3). The procedures and criteria for 
analysis of a method blank are described in Sections 9.5 and 15.6.
    9.1.4 The laboratory shall spike all samples with labeled compounds 
to monitor method performance. This test is described in Section 9.3. 
When results of these spikes indicate atypical method performance for 
samples, the samples are diluted to bring method performance within 
acceptable limits. Procedures for dilution are given in Section 17.5.
    9.1.5 The laboratory shall, on an ongoing basis, demonstrate through 
calibration verification and the analysis of the ongoing precision and 
recovery aliquot that the analytical system is in control. These 
procedures are described in Sections 15.1 through 15.5.
    9.1.6 The laboratory shall maintain records to define the quality of 
data that is generated. Development of accuracy statements is described 
in Section 9.4.
    9.2 Initial Precision and Recovery (IPR)--To establish the ability 
to generate acceptable precision and recovery, the analyst shall perform 
the following operations.
    9.2.1 For low solids (aqueous) samples, extract, concentrate, and 
analyze four 1 L aliquots of reagent water spiked with the diluted 
labeled compound spiking solution (Section 7.10.3) and the precision and 
recovery standard (Section 7.14) according to the procedures in Sections 
11 through 18. For an alternative sample matrix, four aliquots of the 
alternative reference matrix (Section 7.6) are used. All sample 
processing steps that are to be used for processing samples, including 
preparation (Section 11), extraction (Section 12), and cleanup (Section 
13), shall be included in this test.
    9.2.2 Using results of the set of four analyses, compute the average 
concentration (X) of the extracts in ng/mL and the standard deviation of 
the concentration (s) in ng/mL for each compound, by isotope dilution 
for CDDs/CDFs with a labeled analog, and by internal standard for 
1,2,3,7,8,9-HxCDD, OCDF, and the labeled compounds.
    9.2.3 For each CDD/CDF and labeled compound, compare s and X with 
the corresponding limits for initial precision and recovery in Table 6. 
If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, compare s 
and X with the corresponding limits for initial precision and recovery 
in Table 6a. If s and X for all compounds meet the acceptance criteria, 
system performance is acceptable and analysis of blanks and samples may 
begin. If, however, any individual s exceeds the precision limit or any 
individual X falls outside the range for accuracy, system performance is 
unacceptable for that compound. Correct the problem and repeat the test 
(Section 9.2).
    9.3 The laboratory shall spike all samples with the diluted labeled 
compound spiking solution (Section 7.10.3) to assess method performance 
on the sample matrix.
    9.3.1 Analyze each sample according to the procedures in Sections 11 
through 18.
    9.3.2 Compute the percent recovery of the labeled compounds and the 
cleanup standard using the internal standard method (Section 17.2).
    9.3.3 The recovery of each labeled compound must be within the 
limits in Table 7 when all 2,3,7,8-substituted CDDs/CDFs are determined, 
and within the limits in Table 7a when only 2,3,7,8-TCDD and 2,3,7,8-
TCDF are determined. If the recovery of any compound falls outside of 
these limits, method performance is unacceptable for that compound in 
that sample. To overcome such difficulties, water samples are diluted 
and smaller amounts of soils, sludges, sediments, and other matrices are 
reanalyzed per Section 18.4.
    9.4 Recovery of labeled compounds from samples should be assessed 
and records should be maintained.
    9.4.1 After the analysis of five samples of a given matrix type 
(water, soil, sludge, pulp, etc.) for which the labeled compounds pass 
the tests in Section 9.3, compute the average percent recovery (R) and 
the standard deviation of the percent recovery (SR) for the labeled 
compounds only. Express the assessment as a percent recovery interval 
from R-2SR to R = 2SR for each matrix. For 
example, if R = 90% and SR = 10% for five analyses of pulp, 
the recovery interval is expressed as 70-110%.
    9.4.2 Update the accuracy assessment for each labeled compound in 
each matrix on a regular basis (e.g., after each 5-10 new measurements).
    9.5 Method Blanks--Reference matrix method blanks are analyzed to 
demonstrate freedom from contamination (Section 4.3).
    9.5.1 Prepare, extract, clean up, and concentrate a method blank 
with each sample batch (samples of the same matrix started through the 
extraction process on the same 12-hour shift, to a maximum of 20 
samples). The matrix for the method blank shall be similar to sample 
matrix for the batch, e.g., a 1 L reagent water blank (Section 7.6.1), 
high-solids reference matrix blank (Section 7.6.2), paper matrix blank 
(Section 7.6.3); tissue blank (Section 7.6.4) or alternative reference 
matrix blank (Section 7.6.5). Analyze the blank immediately after 
analysis of the OPR (Section 15.5) to demonstrate freedom from 
contamination.
    9.5.2 If any 2,3,7,8-substituted CDD/CDF (Table 1) is found in the 
blank at greater than the minimum level (Table 2) or one-third the 
regulatory compliance level, whichever is greater; or if any potentially 
interfering compound is found in the blank at the minimum level for each 
level of

[[Page 315]]

chlorination given in Table 2 (assuming a response factor of 1 relative 
to the \13\C12-1,2,3,4-TCDD internal standard for compounds 
not listed in Table 1), analysis of samples is halted until the blank 
associated with the sample batch shows no evidence of contamination at 
this level. All samples must be associated with an uncontaminated method 
blank before the results for those samples may be reported for 
regulatory compliance purposes.
    9.6 QC Check Sample--Analyze the QC Check Sample (Section 7.16) 
periodically to assure the accuracy of calibration standards and the 
overall reliability of the analytical process. It is suggested that the 
QC Check Sample be analyzed at least quarterly.
    9.7 The specifications contained in this method can be met if the 
apparatus used is calibrated properly and then maintained in a 
calibrated state. The standards used for calibration (Section 10), 
calibration verification (Section 15.3), and for initial (Section 9.2) 
and ongoing (Section 15.5) precision and recovery should be identical, 
so that the most precise results will be obtained. A GC/MS instrument 
will provide the most reproducible results if dedicated to the settings 
and conditions required for the analyses of CDDs/CDFs by this method.
    9.8 Depending on specific program requirements, field replicates may 
be collected to determine the precision of the sampling technique, and 
spiked samples may be required to determine the accuracy of the analysis 
when the internal standard method is used.

                            10.0 Calibration

    10.1 Establish the operating conditions necessary to meet the 
minimum retention times for the internal standards in Section 10.2.4 and 
the relative retention times for the CDDs/CDFs in Table 2.
    10.1.1 Suggested GC operating conditions:

Injector temperature: 270 [deg]C
Interface temperature: 290 [deg]C
Initial temperature: 200 [deg]C
Initial time: Two minutes
Temperature program:
200-220 [deg]C, at 5 [deg]C/minute
220 [deg]C for 16 minutes
220-235 [deg]C, at 5 [deg]C/minute
235 [deg]C for seven minutes
235-330 [deg]C, at 5 [deg]C/minute

    Note: All portions of the column that connect the GC to the ion 
source shall remain at or above the interface temperature specified 
above during analysis to preclude condensation of less volatile 
compounds.

    Optimize GC conditions for compound separation and sensitivity. Once 
optimized, the same GC conditions must be used for the analysis of all 
standards, blanks, IPR and OPR aliquots, and samples.
    10.1.2 Mass spectrometer (MS) resolution--Obtain a selected ion 
current profile (SICP) of each analyte in Table 3 at the two exact m/z's 
specified in Table 8 and at =10,000 resolving power by 
injecting an authentic standard of the CDDs/CDFs either singly or as 
part of a mixture in which there is no interference between closely 
eluted components.
    10.1.2.1 The analysis time for CDDs/CDFs may exceed the long-term 
mass stability of the mass spectrometer. Because the instrument is 
operated in the high-resolution mode, mass drifts of a few ppm (e.g., 5 
ppm in mass) can have serious adverse effects on instrument performance. 
Therefore, a mass-drift correction is mandatory and a lock-mass m/z from 
PFK is used for drift correction. The lock-mass m/z is dependent on the 
exact m/z's monitored within each descriptor, as shown in Table 8. The 
level of PFK metered into the HRMS during analyses should be adjusted so 
that the amplitude of the most intense selected lock-mass m/z signal 
(regardless of the descriptor number) does not exceed 10% of the full-
scale deflection for a given set of detector parameters. Under those 
conditions, sensitivity changes that might occur during the analysis can 
be more effectively monitored.

    Note: Excessive PFK (or any other reference substance) may cause 
noise problems and contamination of the ion source necessitating 
increased frequency of source cleaning.

    10.1.2.2 If the HRMS has the capability to monitor resolution during 
the analysis, it is acceptable to terminate the analysis when the 
resolution falls below 10,000 to save reanalysis time.
    10.1.2.3 Using a PFK molecular leak, tune the instrument to meet the 
minimum required resolving power of 10,000 (10% valley) at m/z 304.9824 
(PFK) or any other reference signal close to m/z 304 (from TCDF). For 
each descriptor (Table 8), monitor and record the resolution and exact 
m/z's of three to five reference peaks covering the mass range of the 
descriptor. The resolution must be greater than or equal to 10,000, and 
the deviation between the exact m/z and the theoretical m/z (Table 8) 
for each exact m/z monitored must be less than 5 ppm.
    10.2 Ion Abundance Ratios, Minimum Levels, Signal-to-Noise Ratios, 
and Absolute Retention Times--Choose an injection volume of either 1 
[micro]L or 2 [micro]L, consistent with the capability of the HRGC/HRMS 
instrument. Inject a 1 [micro]L or 2 [micro]L aliquot of the CS1 
calibration solution (Table 4) using the GC conditions from Section 
10.1.1. If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, the 
operating conditions and specifications below apply to analysis of those 
compounds only.

[[Page 316]]

    10.2.1 Measure the SICP areas for each analyte, and compute the ion 
abundance ratios at the exact m/z's specified in Table 8. Compare the 
computed ratio to the theoretical ratio given in Table 9.
    10.2.1.1 The exact m/z's to be monitored in each descriptor are 
shown in Table 8. Each group or descriptor shall be monitored in 
succession as a function of GC retention time to ensure that all CDDs/
CDFs are detected. Additional m/z's may be monitored in each descriptor, 
and the m/z's may be divided among more than the five descriptors listed 
in Table 8, provided that the laboratory is able to monitor the m/z's of 
all the CDDs/CDFs that may elute from the GC in a given retention-time 
window. If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, the 
descriptors may be modified to include only the exact m/z's for the 
tetra-and penta-isomers, the diphenyl ethers, and the lock m/z's.
    10.2.1.2 The mass spectrometer shall be operated in a mass-drift 
correction mode, using perfluorokerosene (PFK) to provide lock m/z's. 
The lock-mass for each group of m/z's is shown in Table 8. Each lock 
mass shall be monitored and shall not vary by more than 20% throughout its respective retention time window. 
Variations of the lock mass by more than 20% indicate the presence of 
coeluting interferences that may significantly reduce the sensitivity of 
the mass spectrometer. Reinjection of another aliquot of the sample 
extract will not resolve the problem. Additional cleanup of the extract 
may be required to remove the interferences.
    10.2.2 All CDDs/CDFs and labeled compounds in the CS1 standard shall 
be within the QC limits in Table 9 for their respective ion abundance 
ratios; otherwise, the mass spectrometer shall be adjusted and this test 
repeated until the m/z ratios fall within the limits specified. If the 
adjustment alters the resolution of the mass spectrometer, resolution 
shall be verified (Section 10.1.2) prior to repeat of the test.
    10.2.3 Verify that the HRGC/HRMS instrument meets the minimum levels 
in Table 2. The peaks representing the CDDs/CDFs and labeled compounds 
in the CS1 calibration standard must have signal-to-noise ratios (S/N) 
greater than or equal to 10.0. Otherwise, the mass spectrometer shall be 
adjusted and this test repeated until the minimum levels in Table 2 are 
met.
    10.2.4 The absolute retention time of \13\C12-1,2,3,4-
TCDD (Section 7.12) shall exceed 25.0 minutes on the DB-5 column, and 
the retention time of \13\C12-1,2,3,4-TCDD shall exceed 15.0 
minutes on the DB-225 column; otherwise, the GC temperature program 
shall be adjusted and this test repeated until the above-stated minimum 
retention time criteria are met.
2010.3 Retention-Time Windows--Analyze the window defining mixtures 
(Section 7.15) using the optimized temperature program in Section 10.1. 
Table 5 gives the elution order (first/last) of the window-defining 
compounds. If 2,3,7,8-TCDD and 2,3,7,8-TCDF only are to be analyzed, 
this test is not required.
    10.4 Isomer Specificity.
    10.4.1 Analyze the isomer specificity test standards (Section 7.15) 
using the procedure in Section 14 and the optimized conditions for 
sample analysis (Section 10.1.1).
    10.4.2 Compute the percent valley between the GC peaks that elute 
most closely to the 2,3,7,8-TCDD and TCDF isomers, on their respective 
columns, per Figures 6 and 7.
    10.4.3 Verify that the height of the valley between the most closely 
eluted isomers and the 2,3,7,8-substituted isomers is less than 25% 
(computed as 100 x/y in Figures 6 and 7). If the valley exceeds 25%, 
adjust the analytical conditions and repeat the test or replace the GC 
column and recalibrate (Sections 10.1.2 through 10.7).
    10.5 Calibration by Isotope Dilution--Isotope dilution calibration 
is used for the 15 2,3,7,8-substituted CDDs/CDFs for which labeled 
compounds are added to samples prior to extraction. The reference 
compound for each CDD/CDF compound is shown in Table 2.
    10.5.1 A calibration curve encompassing the concentration range is 
prepared for each compound to be determined. The relative response (RR) 
(labeled to native) vs. concentration in standard solutions is plotted 
or computed using a linear regression. Relative response is determined 
according to the procedures described below. Five calibration points are 
employed.
    10.5.2 The response of each CDD/CDF relative to its labeled analog 
is determined using the area responses of both the primary and secondary 
exact m/z's specified in Table 8, for each calibration standard, as 
follows:
[GRAPHIC] [TIFF OMITTED] TR15SE97.002

where:

A1n and A2n = The areas of the primary and 
          secondary m/z's for the CDD/CDF.
A1l and A2l = The areas of the primary and 
          secondary m/z's for the labeled compound.
Cl = The concentration of the labeled compound in the 
          calibration standard (Table 4).
Cn = The concentration of the native compound in the 
          calibration standard (Table 4).

    10.5.3 To calibrate the analytical system by isotope dilution, 
inject a volume of calibration standards CS1 through CS5 (Section 7.13 
and Table 4) identical to the volume chosen in Section 10.2, using the 
procedure in Section 14 and the conditions in Section

[[Page 317]]

10.1.1 and Table 2. Compute the relative response (RR) at each 
concentration.
    10.5.4 Linearity--If the relative response for any compound is 
constant (less than 20% coefficient of variation) over the five-point 
calibration range, an averaged relative response may be used for that 
compound; otherwise, the complete calibration curve for that compound 
shall be used over the five-point calibration range.
    10.6 Calibration by Internal Standard--The internal standard method 
is applied to determination of 1,2,3,7,8,9-HxCDD (Section 17.1.2), OCDF 
(Section 17.1.1), the non 2,3,7,8-substituted compounds, and to the 
determination of labeled compounds for intralaboratory statistics 
(Sections 9.4 and 15.5.4).
    10.6.1 Response factors--Calibration requires the determination of 
response factors (RF) defined by the following equation:
[GRAPHIC] [TIFF OMITTED] TR15SE97.003

where:

A1s and A2s = The areas of the primary and 
          secondary m/z's for the CDD/CDF.
A1is and A2is = The areas of the primary and 
          secondary m/z's for the internal standard.
Cis = The concentration of the internal standard (Table 4).
Cs = The concentration of the compound in the calibration 
          standard (Table 4).

    Note: There is only one m/z for \37\Cl4-2,3,7,8-TCDD. See 
Table 8.

    10.6.2 To calibrate the analytical system by internal standard, 
inject 1.0 [micro]L or 2.0 [micro]L of calibration standards CS1 through 
CS5 (Section 7.13 and Table 4) using the procedure in Section 14 and the 
conditions in Section 10.1.1 and Table 2. Compute the response factor 
(RF) at each concentration.
    10.6.3 Linearity--If the response factor (RF) for any compound is 
constant (less than 35% coefficient of variation) over the five-point 
calibration range, an averaged response factor may be used for that 
compound; otherwise, the complete calibration curve for that compound 
shall be used over the five-point range.
    10.7 Combined Calibration--By using calibration solutions (Section 
7.13 and Table 4) containing the CDDs/CDFs and labeled compounds and the 
internal standards, a single set of analyses can be used to produce 
calibration curves for the isotope dilution and internal standard 
methods. These curves are verified each shift (Section 15.3) by 
analyzing the calibration verification standard (VER, Table 4). 
Recalibration is required if any of the calibration verification 
criteria (Section 15.3) cannot be met.
    10.8 Data Storage--MS data shall be collected, recorded, and stored.
    10.8.1 Data acquisition--The signal at each exact m/z shall be 
collected repetitively throughout the monitoring period and stored on a 
mass storage device.
    10.8.2 Response factors and multipoint calibrations--The data system 
shall be used to record and maintain lists of response factors (response 
ratios for isotope dilution) and multipoint calibration curves. 
Computations of relative standard deviation (coefficient of variation) 
shall be used to test calibration linearity. Statistics on initial 
performance (Section 9.2) and ongoing performance (Section 15.5) should 
be computed and maintained, either on the instrument data system, or on 
a separate computer system.

                         11.0 Sample Preparation

    11.1 Sample preparation involves modifying the physical form of the 
sample so that the CDDs/CDFs can be extracted efficiently. In general, 
the samples must be in a liquid form or in the form of finely divided 
solids in order for efficient extraction to take place. Table 10 lists 
the phases and suggested quantities for extraction of various sample 
matrices.
    For samples known or expected to contain high levels of the CDDs/
CDFs, the smallest sample size representative of the entire sample 
should be used (see Section 17.5).
    For all samples, the blank and IPR/OPR aliquots must be processed 
through the same steps as the sample to check for contamination and 
losses in the preparation processes.
    11.1.1 For samples that contain particles, percent solids and 
particle size are determined using the procedures in Sections 11.2 and 
11.3, respectively.
    11.1.2 Aqueous samples--Because CDDs/CDFs may be bound to suspended 
particles, the preparation of aqueous samples is dependent on the solids 
content of the sample.
    11.1.2.1 Aqueous samples visibly absent particles are prepared per 
Section 11.4 and extracted directly using the separatory funnel or SPE 
techniques in Sections 12.1 or 12.2, respectively.
    11.1.2.2 Aqueous samples containing visible particles and containing 
one percent suspended solids or less are prepared using the procedure in 
Section 11.4. After preparation, the sample is extracted directly using 
the SPE technique in 12.2 or filtered per Section 11.4.3. After 
filtration, the particles and filter are extracted using the SDS 
procedure in Section 12.3 and the filtrate is extracted using the 
separatory funnel procedure in Section 12.1.
    11.1.2.3 For aqueous samples containing greater than one percent 
solids, a sample aliquot sufficient to provide 10 g of dry solids is 
used, as described in Section 11.5.

[[Page 318]]

    11.1.3 Solid samples are prepared using the procedure described in 
Section 11.5 followed by extraction via the SDS procedure in Section 
12.3.
    11.1.4 Multiphase samples--The phase(s) containing the CDDs/CDFs is 
separated from the non-CDD/CDF phase using pressure filtration and 
centrifugation, as described in Section 11.6. The CDDs/CDFs will be in 
the organic phase in a multiphase sample in which an organic phase 
exists.
    11.1.5 Procedures for grinding, homogenization, and blending of 
various sample phases are given in Section 11.7.
    11.1.6 Tissue samples--Preparation procedures for fish and other 
tissues are given in Section 11.8.
    11.2 Determination of Percent Suspended Solids.

    Note: This aliquot is used for determining the solids content of the 
sample, not for determination of CDDs/CDFs.

    11.2.1 Aqueous liquids and multi-phase samples consisting of mainly 
an aqueous phase.
    11.2.1.1 Dessicate and weigh a GF/D filter (Section 6.5.3) to three 
significant figures.
    11.2.1.2 Filter 10.0 0.02 mL of well-mixed 
sample through the filter.
    11.2.1.3 Dry the filter a minimum of 12 hours at 110 5 [deg]C and cool in a dessicator.
    11.2.1.4 Calculate percent solids as follows:
    [GRAPHIC] [TIFF OMITTED] TR15SE97.004
    
    11.2.2 Non-aqueous liquids, solids, semi-solid samples, and multi-
phase samples in which the main phase is not aqueous; but not tissues.
    11.2.2.1 Weigh 5-10 g of sample to three significant figures in a 
tared beaker.
    11.2.2.2 Dry a minimum of 12 hours at 110 5 
[deg]C, and cool in a dessicator.
    11.2.2.3 Calculate percent solids as follows:
    [GRAPHIC] [TIFF OMITTED] TR15SE97.005
    
    11.3 Determination of Particle Size.
    11.3.1 Spread the dried sample from Section 11.2.2.2 on a piece of 
filter paper or aluminum foil in a fume hood or glove box.
    11.3.2 Estimate the size of the particles in the sample. If the size 
of the largest particles is greater than 1 mm, the particle size must be 
reduced to 1 mm or less prior to extraction using the procedures in 
Section 11.7.
    11.4 Preparation of Aqueous Samples Containing 1% Suspended Solids 
or Less.
    11.4.1 Aqueous samples visibly absent particles are prepared per the 
procedure below and extracted directly using the separatory funnel or 
SPE techniques in Sections 12.1 or 12.2, respectively. Aqueous samples 
containing visible particles and one percent suspended solids or less 
are prepared using the procedure below and extracted using either the 
SPE technique in Section 12.2 or further prepared using the filtration 
procedure in Section 11.4.3. The filtration procedure is followed by SDS 
extraction of the filter and particles (Section 12.3) and separatory 
funnel extraction of the filtrate (Section 12.1). The SPE procedure is 
followed by SDS extraction of the filter and disk.
    11.4.2 Preparation of sample and QC aliquots.
    11.4.2.1 Mark the original level of the sample on the sample bottle 
for reference. Weigh the sample plus bottle to 1.
    11.4.2.2 Spike 1.0 mL of the diluted labeled-compound spiking 
solution (Section 7.10.3) into the sample bottle. Cap the bottle and mix 
the sample by careful shaking. Allow the sample to equilibrate for one 
to two hours, with occasional shaking.
    11.4.2.3 For each sample or sample batch (to a maximum of 20 
samples) to be extracted during the same 12-hour shift, place two 1.0 L 
aliquots of reagent water in clean sample bottles or flasks.
    11.4.2.4 Spike 1.0 mL of the diluted labeled-compound spiking 
solution (Section 7.10.3) into both reagent water aliquots. One of these 
aliquots will serve as the method blank.
    11.4.2.5 Spike 1.0 mL of the PAR standard (Section 7.14) into the 
remaining reagent water aliquot. This aliquot will serve as the OPR 
(Section 15.5).
    11.4.2.6 If SPE is to be used, add 5 mL of methanol to the sample, 
cap and shake the

[[Page 319]]

sample to mix thoroughly, and proceed to Section 12.2 for extraction. If 
SPE is not to be used, and the sample is visibly absent particles, 
proceed to Section 12.1 for extraction. If SPE is not to be used and the 
sample contains visible particles, proceed to the following section for 
filtration of particles.
    11.4.3 Filtration of particles.
    11.4.3.1 Assemble a Buchner funnel (Section 6.5.5) on top of a clean 
filtration flask. Apply vacuum to the flask, and pour the entire 
contents of the sample bottle through a glass-fiber filter (Section 
6.5.6) in the Buchner funnel, swirling the sample remaining in the 
bottle to suspend any particles.
    11.4.3.2 Rinse the sample bottle twice with approximately 5 mL 
portions of reagent water to transfer any remaining particles onto the 
filter.
    11.4.3.3 Rinse any particles off the sides of the Buchner funnel 
with small quantities of reagent water.
    11.4.3.4 Weigh the empty sample bottle to 1 g. 
Determine the weight of the sample by difference. Save the bottle for 
further use.
    11.4.3.5 Extract the filtrate using the separatory funnel procedure 
in Section 12.1.
    11.4.3.6 Extract the filter containing the particles using the SDS 
procedure in Section 12.3.
    11.5 Preparation of Samples Containing Greater Than 1% Solids.
    11.5.1 Weigh a well-mixed aliquot of each sample (of the same matrix 
type) sufficient to provide 10 g of dry solids (based on the solids 
determination in Section 11.2) into a clean beaker or glass jar.
    11.5.2 Spike 1.0 mL of the diluted labeled compound spiking solution 
(Section 7.10.3) into the sample.
    11.5.3 For each sample or sample batch (to a maximum of 20 samples) 
to be extracted during the same 12-hour shift, weigh two 10 g aliquots 
of the appropriate reference matrix (Section 7.6) into clean beakers or 
glass jars.
    11.5.4 Spike 1.0 mL of the diluted labeled compound spiking solution 
(Section 7.10.3) into each reference matrix aliquot. One aliquot will 
serve as the method blank. Spike 1.0 mL of the PAR standard (Section 
7.14) into the other reference matrix aliquot. This aliquot will serve 
as the OPR (Section 15.5).
    11.5.5 Stir or tumble and equilibrate the aliquots for one to two 
hours.
    11.5.6 Decant excess water. If necessary to remove water, filter the 
sample through a glass-fiber filter and discard the aqueous liquid.
    11.5.7 If particles 1mm are present in the sample (as 
determined in Section 11.3.2), spread the sample on clean aluminum foil 
in a hood. After the sample is dry, grind to reduce the particle size 
(Section 11.7).
    11.5.8 Extract the sample and QC aliquots using the SDS procedure in 
Section 12.3.
    11.6 Multiphase Samples.
    11.6.1 Using the percent solids determined in Section 11.2.1 or 
11.2.2, determine the volume of sample that will provide 10 g of solids, 
up to 1 L of sample.
    11.6.2 Pressure filter the amount of sample determined in Section 
11.6.1 through Whatman GF/D glass-fiber filter paper (Section 6.5.3). 
Pressure filter the blank and OPR aliquots through GF/D papers also. If 
necessary to separate the phases and/or settle the solids, centrifuge 
these aliquots prior to filtration.
    11.6.3 Discard any aqueous phase (if present). Remove any non-
aqueous liquid present and reserve the maximum amount filtered from the 
sample (Section 11.6.1) or 10 g, whichever is less, for combination with 
the solid phase (Section 12.3.5).
    11.6.4 If particles 1mm are present in the sample (as 
determined in Section 11.3.2) and the sample is capable of being dried, 
spread the sample and QC aliquots on clean aluminum foil in a hood. 
After the aliquots are dry or if the sample cannot be dried, reduce the 
particle size using the procedures in Section 11.7 and extract the 
reduced particles using the SDS procedure in Section 12.3. If particles 
1mm are not present, extract the particles and filter in the 
sample and QC aliquots directly using the SDS procedure in Section 12.3.
    11.7 Sample grinding, homogenization, or blending--Samples with 
particle sizes greater than 1 mm (as determined in Section 11.3.2) are 
subjected to grinding, homogenization, or blending. The method of 
reducing particle size to less than 1 mm is matrix-dependent. In 
general, hard particles can be reduced by grinding with a mortar and 
pestle. Softer particles can be reduced by grinding in a Wiley mill or 
meat grinder, by homogenization, or in a blender.
    11.7.1 Each size-reducing preparation procedure on each matrix shall 
be verified by running the tests in Section 9.2 before the procedure is 
employed routinely.
    11.7.2 The grinding, homogenization, or blending procedures shall be 
carried out in a glove box or fume hood to prevent particles from 
contaminating the work environment.
    11.7.3 Grinding--Certain papers and pulps, slurries, and amorphous 
solids can be ground in a Wiley mill or heavy duty meat grinder. In some 
cases, reducing the temperature of the sample to freezing or to dry ice 
or liquid nitrogen temperatures can aid in the grinding process. Grind 
the sample aliquots from Section 11.5.7 or 11.6.4 in a clean grinder. Do 
not allow the sample temperature to exceed 50 [deg]C. Grind the blank 
and reference matrix aliquots using a clean grinder.
    11.7.4 Homogenization or blending--Particles that are not ground 
effectively, or particles greater than 1 mm in size after grinding, can 
often be reduced in size by high speed homogenization or blending. 
Homogenize and/or blend the particles or filter from

[[Page 320]]

Section 11.5.7 or 11.6.4 for the sample, blank, and OPR aliquots.
    11.7.5 Extract the aliquots using the SDS procedure in Section 12.3.
    11.8 Fish and Other Tissues--Prior to processing tissue samples, the 
laboratory must determine the exact tissue to be analyzed. Common 
requests for analysis of fish tissue include whole fish--skin on, whole 
fish--skin removed, edible fish fillets (filleted in the field or by the 
laboratory), specific organs, and other portions. Once the appropriate 
tissue has been determined, the sample must be homogenized.
    11.8.1 Homogenization.
    11.8.1.1 Samples are homogenized while still frozen, where 
practical. If the laboratory must dissect the whole fish to obtain the 
appropriate tissue for analysis, the unused tissues may be rapidly 
refrozen and stored in a clean glass jar for subsequent use.
    11.8.1.2 Each analysis requires 10 g of tissue (wet weight). 
Therefore, the laboratory should homogenize at least 20 g of tissue to 
allow for re-extraction of a second aliquot of the same homogenized 
sample, if re-analysis is required. When whole fish analysis is 
necessary, the entire fish is homogenized.
    11.8.1.3 Homogenize the sample in a tissue homogenizer (Section 
6.3.3) or grind in a meat grinder (Section 6.3.4). Cut tissue too large 
to feed into the grinder into smaller pieces. To assure homogeneity, 
grind three times.
    11.8.1.4 Transfer approximately 10 g (wet weight) of homogenized 
tissue to a clean, tared, 400-500 mL beaker. For the alternate HCl 
digestion/extraction, transfer the tissue to a clean, tared 500-600 mL 
wide-mouth bottle. Record the weight to the nearest 10 mg.
    11.8.1.5 Transfer the remaining homogenized tissue to a clean jar 
with a fluoropolymer-lined lid. Seal the jar and store the tissue at <-
10 [deg]C. Return any tissue that was not homogenized to its original 
container and store at <-10 [deg]C.
    11.8.2 QC aliquots.
    11.8.2.1 Prepare a method blank by adding approximately 10 g of the 
oily liquid reference matrix (Section 7.6.4) to a 400-500 mL beaker. For 
the alternate HCl digestion/extraction, add the reference matrix to a 
500-600 mL wide-mouth bottle. Record the weight to the nearest 10 mg.
    11.8.2.2 Prepare a precision and recovery aliquot by adding 
approximately 10 g of the oily liquid reference matrix (Section 7.6.4) 
to a separate 400-500 mL beaker or wide-mouth bottle, depending on the 
extraction procedure to be used. Record the weight to the nearest 10 mg. 
If the initial precision and recovery test is to be performed, use four 
aliquots; if the ongoing precision and recovery test is to be performed, 
use a single aliquot.
    11.8.3 Spiking
    11.8.3.1 Spike 1.0 mL of the labeled compound spiking solution 
(Section 7.10.3) into the sample, blank, and OPR aliquot.
    11.8.3.2 Spike 1.0 mL of the PAR standard (Section 7.14) into the 
OPR aliquot.
    11.8.4 Extract the aliquots using the procedures in Section 12.4.

                    12.0 Extraction and Concentration

    Extraction procedures include separatory funnel (Section 12.1) and 
solid phase (Section 12.2) for aqueous liquids; Soxhlet/Dean-Stark 
(Section 12.3) for solids, filters, and SPE disks; and Soxhlet 
extraction (Section 12.4.1) and HCl digestion (Section 12.4.2) for 
tissues. Acid/base back-extraction (Section 12.5) is used for initial 
cleanup of extracts.
    Macro-concentration procedures include rotary evaporation (Section 
12.6.1), heating mantle (Section 12.6.2), and Kuderna-Danish (K-D) 
evaporation (Section 12.6.3). Micro-concentration uses nitrogen blowdown 
(Section 12.7).
    12.1 Separatory funnel extraction of filtrates and of aqueous 
samples visibly absent particles.
    12.1.1 Pour the spiked sample (Section 11.4.2.2) or filtrate 
(Section 11.4.3.5) into a 2 L separatory funnel. Rinse the bottle or 
flask twice with 5 mL of reagent water and add these rinses to the 
separatory funnel.
    12.1.2 Add 60 mL methylene chloride to the empty sample bottle 
(Section 12.1.1), seal, and shake 60 seconds to rinse the inner surface. 
Transfer the solvent to the separatory funnel, and extract the sample by 
shaking the funnel for two minutes with periodic venting. Allow the 
organic layer to separate from the aqueous phase for a minimum of 10 
minutes. If an emulsion forms and is more than one-third the volume of 
the solvent layer, employ mechanical techniques to complete the phase 
separation (see note below). Drain the methylene chloride extract 
through a solvent-rinsed glass funnel approximately one-half full of 
granular anhydrous sodium sulfate (Section 7.2.1) supported on clean 
glass-fiber paper into a solvent-rinsed concentration device (Section 
12.6).

    Note: If an emulsion forms, the analyst must employ mechanical 
techniques to complete the phase separation. The optimum technique 
depends upon the sample, but may include stirring, filtration through 
glass wool, use of phase separation paper, centrifugation, use of an 
ultrasonic bath with ice, addition of NaCl, or other physical methods. 
Alternatively, solid-phase or other extraction techniques may be used to 
prevent emulsion formation. Any alternative technique is acceptable so 
long as the requirements in Section 9 are met.

    Experience with aqueous samples high in dissolved organic materials 
(e.g., paper mill effluents) has shown that acidification of the

[[Page 321]]

sample prior to extraction may reduce the formation of emulsions. Paper 
industry methods suggest that the addition of up to 400 mL of ethanol to 
a 1 L effluent sample may also reduce emulsion formation. However, 
studies by EPA suggest that the effect may be a result of sample 
dilution, and that the addition of reagent water may serve the same 
function. Mechanical techniques may still be necessary to complete the 
phase separation. If either acidification or addition of ethanol is 
utilized, the laboratory must perform the startup tests described in 
Section 9.2 using the same techniques.
    12.1.3 Extract the water sample two more times with 60 mL portions 
of methylene chloride. Drain each portion through the sodium sulfate 
into the concentrator. After the third extraction, rinse the separatory 
funnel with at least 20 mL of methylene chloride, and drain this rinse 
through the sodium sulfate into the concentrator. Repeat this rinse at 
least twice. Set aside the funnel with sodium sulfate if the extract is 
to be combined with the extract from the particles.
    12.1.4 Concentrate the extract using one of the macro-concentration 
procedures in Section 12.6.
    12.1.4.1 If the extract is from a sample visibly absent particles 
(Section 11.1.2.1), adjust the final volume of the concentrated extract 
to approximately 10 mL with hexane, transfer to a 250 mL separatory 
funnel, and back-extract using the procedure in Section 12.5.
    12.1.4.2 If the extract is from the aqueous filtrate (Section 
11.4.3.5), set aside the concentration apparatus for addition of the SDS 
extract from the particles (Section 12.3.9.1.2).
    12.2 SPE of Samples Containing Less Than 1% Solids (References 19-
20).
    12.2.1 Disk preparation.
    12.2.1.1 Place an SPE disk on the base of the filter holder (Figure 
4) and wet with toluene. While holding a GMF 150 filter above the SPE 
disk with tweezers, wet the filter with toluene and lay the filter on 
the SPE disk, making sure that air is not trapped between the filter and 
disk. Clamp the filter and SPE disk between the 1 L glass reservoir and 
the vacuum filtration flask.
    12.2.1.2 Rinse the sides of the filtration flask with approx 15 mL 
of toluene using a squeeze bottle or syringe. Apply vacuum momentarily 
until a few drops appear at the drip tip. Release the vacuum and allow 
the filter/disk to soak for approx one minute. Apply vacuum and draw all 
of the toluene through the filter/disk. Repeat the wash step with approx 
15 mL of acetone and allow the filter/disk to air dry.
    12.2.1.3 Re-wet the filter/disk with approximately 15 mL of 
methanol, allowing the filter/disk to soak for approximately one minute. 
Pull the methanol through the filter/disk using the vacuum, but retain a 
layer of methanol approximately 1 mm thick on the filter. Do not allow 
the disk to go dry from this point until the end of the extraction.
    12.2.1.4 Rinse the filter/disk with two 50-mL portions of reagent 
water by adding the water to the reservoir and pulling most through, 
leaving a layer of water on the surface of the filter.
    12.2.2 Extraction.
    12.2.2.1 Pour the spiked sample (Section 11.4.2.2), blank (Section 
11.4.2.4), or IPR/OPR aliquot (Section 11.4.2.5) into the reservoir and 
turn on the vacuum to begin the extraction. Adjust the vacuum to 
complete the extraction in no less than 10 minutes. For samples 
containing a high concentration of particles (suspended solids), 
filtration times may be eight hours or longer.
    12.2.2.2 Before all of the sample has been pulled through the 
filter/disk, rinse the sample bottle with approximately 50 mL of reagent 
water to remove any solids, and pour into the reservoir. Pull through 
the filter/disk. Use additional reagent water rinses until all visible 
solids are removed.
    12.2.2.3 Before all of the sample and rinses have been pulled 
through the filter/disk, rinse the sides of the reservoir with small 
portions of reagent water.
    12.2.2.4 Allow the filter/disk to dry, then remove the filter and 
disk and place in a glass Petri dish. Extract the filter and disk per 
Section 12.3.
    12.3 SDS Extraction of Samples Containing Particles, and of Filters 
and/or Disks.
    12.3.1 Charge a clean extraction thimble (Section 6.4.2.2) with 5.0 
g of 100/200 mesh silica (Section 7.5.1.1) topped with 100 g of quartz 
sand (Section 7.3.2).

    Note: Do not disturb the silica layer throughout the extraction 
process.

    12.3.2 Place the thimble in a clean extractor. Place 30-40 mL of 
toluene in the receiver and 200-250 mL of toluene in the flask.
    12.3.3 Pre-extract the glassware by heating the flask until the 
toluene is boiling. When properly adjusted, one to two drops of toluene 
will fall per second from the condenser tip into the receiver. Extract 
the apparatus for a minimum of three hours.
    12.3.4 After pre-extraction, cool and disassemble the apparatus. 
Rinse the thimble with toluene and allow to air dry.
    12.3.5 Load the wet sample, filter, and/or disk from Section 
11.4.3.6, 11.5.8, 11.6.4, 11.7.3, 11.7.4, or 12.2.2.4 and any nonaqueous 
liquid from Section 11.6.3 into the thimble and manually mix into the 
sand layer with a clean metal spatula, carefully breaking up any large 
lumps of sample.
    12.3.6 Reassemble the pre-extracted SDS apparatus, and add a fresh 
charge of toluene to the receiver and reflux flask. Apply power

[[Page 322]]

to the heating mantle to begin refluxing. Adjust the reflux rate to 
match the rate of percolation through the sand and silica beds until 
water removal lessens the restriction to toluene flow. Frequently check 
the apparatus for foaming during the first two hours of extraction. If 
foaming occurs, reduce the reflux rate until foaming subsides.
    12.3.7 Drain the water from the receiver at one to two hours and 
eight to nine hours, or sooner if the receiver fills with water. Reflux 
the sample for a total of 16-24 hours. Cool and disassemble the 
apparatus. Record the total volume of water collected.
    12.3.8 Remove the distilling flask. Drain the water from the Dean-
Stark receiver and add any toluene in the receiver to the extract in the 
flask.
    12.3.9 Concentrate the extract using one of the macro-concentration 
procedures in Section 12.6 per the following:
    12.3.9.1 Extracts from the particles in an aqueous sample containing 
less than 1% solids (Section 11.4.3.6).
    12.3.9.1.1 Concentrate the extract to approximately 5 mL using the 
rotary evaporator or heating mantle procedures in Section 12.6.1 or 
12.6.2.
    12.3.9.1.2 Quantitatively transfer the extract through the sodium 
sulfate (Section 12.1.3) into the apparatus that was set aside (Section 
12.1.4.2) and reconcentrate to the level of the toluene.
    12.3.9.1.3 Adjust to approximately 10 mL with hexane, transfer to a 
250 mL separatory funnel, and proceed with back-extraction (Section 
12.5).
    12.3.9.2 Extracts from particles (Sections 11.5 through 11.6) or 
from the SPE filter and disk (Section 12.2.2.4)--Concentrate to 
approximately 10 mL using the rotary evaporator or heating mantle 
(Section 12.6.1 or 12.6.2), transfer to a 250 mL separatory funnel, and 
proceed with back-extraction (Section 12.5).
    12.4 Extraction of Tissue--Two procedures are provided for tissue 
extraction.
    12.4.1 Soxhlet extraction (Reference 21).
    12.4.1.1 Add 30-40 g of powdered anhydrous sodium sulfate to each of 
the beakers (Section 11.8.4) and mix thoroughly. Cover the beakers with 
aluminum foil and allow to equilibrate for 12-24 hours. Remix prior to 
extraction to prevent clumping.
    12.4.1.2 Assemble and pre-extract the Soxhlet apparatus per Sections 
12.3.1 through 12.3.4, except use the methylene chloride:hexane (1:1) 
mixture for the pre-extraction and rinsing and omit the quartz sand. The 
Dean-Stark moisture trap may also be omitted, if desired.
    12.4.1.3 Reassemble the pre-extracted Soxhlet apparatus and add a 
fresh charge of methylene chloride:hexane to the reflux flask.
    12.4.1.4 Transfer the sample/sodium sulfate mixture (Section 
12.4.1.1) to the Soxhlet thimble, and install the thimble in the Soxhlet 
apparatus.
    12.4.1.5 Rinse the beaker with several portions of solvent mixture 
and add to the thimble. Fill the thimble/receiver with solvent. Extract 
for 18-24 hours.
    12.4.1.6 After extraction, cool and disassemble the apparatus.
    12.4.1.7 Quantitatively transfer the extract to a macro-
concentration device (Section 12.6), and concentrate to near dryness. 
Set aside the concentration apparatus for re-use.
    12.4.1.8 Complete the removal of the solvent using the nitrogen 
blowdown procedure (Section 12.7) and a water bath temperature of 60 
[deg]C. Weigh the receiver, record the weight, and return the receiver 
to the blowdown apparatus, concentrating the residue until a constant 
weight is obtained.
    12.4.1.9 Percent lipid determination--The lipid content is 
determined by extraction of tissue with the same solvent system 
(methylene chloride:hexane) that was used in EPA's National Dioxin Study 
(Reference 22) so that lipid contents are consistent with that study.
    12.4.1.9.1 Redissolve the residue in the receiver in hexane and 
spike 1.0 mL of the cleanup standard (Section 7.11) into the solution.
    12.4.1.9.2 Transfer the residue/hexane to the anthropogenic 
isolation column (Section 13.7.1) or bottle for the acidified silica gel 
batch cleanup (Section 13.7.2), retaining the boiling chips in the 
concentration apparatus. Use several rinses to assure that all material 
is transferred. If necessary, sonicate or heat the receiver slightly to 
assure that all material is re-dissolved. Allow the receiver to dry. 
Weigh the receiver and boiling chips.
    12.4.1.9.3 Calculate the lipid content to the nearest three 
significant figures as follows:
[GRAPHIC] [TIFF OMITTED] TR15SE97.006

    12.4.1.9.4 It is not necessary to determine the lipid content of the 
blank, IPR, or OPR aliquots.
    12.4.2 HCl digestion/extraction and concentration (References 23-
26).
    12.4.2.1 Add 200 mL of 6 N HCl and 200 mL of methylene 
chloride:hexane (1:1) to the sample and QC aliquots (Section 11.8.4).
    12.4.2.2 Cap and shake each bottle one to three times. Loosen the 
cap in a hood to vent excess pressure. Shake each bottle for 10-30 
seconds and vent.
    12.4.2.3 Tightly cap and place on shaker. Adjust the shaker action 
and speed so that the acid, solvent, and tissue are in constant motion. 
However, take care to avoid such violent action that the bottle may be 
dislodged from the shaker. Shake for 12-24 hours.

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    12.4.2.4 After digestion, remove the bottles from the shaker. Allow 
the bottles to stand so that the solvent and acid layers separate.
    12.4.2.5 Decant the solvent through a glass funnel with glass-fiber 
filter (Sections 6.5.2 through 6.5.3) containing approximately 10 g of 
granular anhydrous sodium sulfate (Section 7.2.1) into a macro-
concentration apparatus (Section 12.6). Rinse the contents of the bottle 
with two 25 mL portions of hexane and pour through the sodium sulfate 
into the apparatus.
    12.4.2.6 Concentrate the solvent to near dryness using a macro-
concentration procedure (Section 12.6).
    12.4.2.7 Complete the removal of the solvent using the nitrogen 
blowdown apparatus (Section 12.7) and a water bath temperature of 60 
[deg]C. Weigh the receiver, record the weight, and return the receiver 
to the blowdown apparatus, concentrating the residue until a constant 
weight is obtained.
    12.4.2.8 Percent lipid determination--The lipid content is 
determined in the same solvent system [methylene chloride:hexane (1:1)] 
that was used in EPA's National Dioxin Study (Reference 22) so that 
lipid contents are consistent with that study.
    12.4.2.8.1 Redissolve the residue in the receiver in hexane and 
spike 1.0 mL of the cleanup standard (Section 7.11) into the solution.
    12.4.2.8.2 Transfer the residue/hexane to the narrow-mouth 100-200 
mL bottle retaining the boiling chips in the receiver. Use several 
rinses to assure that all material is transferred, to a maximum hexane 
volume of approximately 70 mL. Allow the receiver to dry. Weigh the 
receiver and boiling chips.
    12.4.2.8.3 Calculate the percent lipid per Section 12.4.1.9.3. It is 
not necessary to determine the lipid content of the blank, IPR, or OPR 
aliquots.
    12.4.2.9 Clean up the extract per Section 13.7.3.
    12.5 Back-Extraction with Base and Acid.
    12.5.1 Spike 1.0 mL of the cleanup standard (Section 7.11) into the 
separatory funnels containing the sample and QC extracts from Section 
12.1.4.1, 12.3.9.1.3, or 12.3.9.2.
    12.5.2 Partition the extract against 50 mL of potassium hydroxide 
solution (Section 7.1.1). Shake for two minutes with periodic venting 
into a hood. Remove and discard the aqueous layer. Repeat the base 
washing until no color is visible in the aqueous layer, to a maximum of 
four washings. Minimize contact time between the extract and the base to 
prevent degradation of the CDDs/CDFs. Stronger potassium hydroxide 
solutions may be employed for back-extraction, provided that the 
laboratory meets the specifications for labeled compound recovery and 
demonstrates acceptable performance using the procedure in Section 9.2.
    12.5.3 Partition the extract against 50 mL of sodium chloride 
solution (Section 7.1.4) in the same way as with base. Discard the 
aqueous layer.
    12.5.4 Partition the extract against 50 mL of sulfuric acid (Section 
7.1.2) in the same way as with base. Repeat the acid washing until no 
color is visible in the aqueous layer, to a maximum of four washings.
    12.5.5 Repeat the partitioning against sodium chloride solution and 
discard the aqueous layer.
    12.5.6 Pour each extract through a drying column containing 7-10 cm 
of granular anhydrous sodium sulfate (Section 7.2.1). Rinse the 
separatory funnel with 30-50 mL of solvent, and pour through the drying 
column. Collect each extract in a round-bottom flask. Re-concentrate the 
sample and QC aliquots per Sections 12.6 through 12.7, and clean up the 
samples and QC aliquots per Section 13.
    12.6 Macro-Concentration--Extracts in toluene are concentrated using 
a rotary evaporator or a heating mantle; extracts in methylene chloride 
or hexane are concentrated using a rotary evaporator, heating mantle, or 
Kuderna-Danish apparatus.
    12.6.1 Rotary evaporation--Concentrate the extracts in separate 
round-bottom flasks.
    12.6.1.1 Assemble the rotary evaporator according to manufacturer's 
instructions, and warm the water bath to 45 [deg]C. On a daily basis, 
preclean the rotary evaporator by concentrating 100 mL of clean 
extraction solvent through the system. Archive both the concentrated 
solvent and the solvent in the catch flask for a contamination check if 
necessary. Between samples, three 2-3 mL aliquots of solvent should be 
rinsed down the feed tube into a waste beaker.
    12.6.1.2 Attach the round-bottom flask containing the sample extract 
to the rotary evaporator. Slowly apply vacuum to the system, and begin 
rotating the sample flask.
    12.6.1.3 Lower the flask into the water bath, and adjust the speed 
of rotation and the temperature as required to complete concentration in 
15-20 minutes. At the proper rate of concentration, the flow of solvent 
into the receiving flask will be steady, but no bumping or visible 
boiling of the extract will occur.

    Note: If the rate of concentration is too fast, analyte loss may 
occur.

    12.6.1.4 When the liquid in the concentration flask has reached an 
apparent volume of approximately 2 mL, remove the flask from the water 
bath and stop the rotation. Slowly and carefully admit air into the 
system. Be sure not to open the valve so quickly that the sample is 
blown out of the flask. Rinse the feed tube with approximately 2 mL of 
solvent.

[[Page 324]]

    12.6.1.5 Proceed to Section 12.6.4 for preparation for back-
extraction or micro-concentration and solvent exchange.
    12.6.2 Heating mantle--Concentrate the extracts in separate round-
bottom flasks.
    12.6.2.1 Add one or two clean boiling chips to the round-bottom 
flask, and attach a three-ball macro Snyder column. Prewet the column by 
adding approximately 1 mL of solvent through the top. Place the round-
bottom flask in a heating mantle, and apply heat as required to complete 
the concentration in 15-20 minutes. At the proper rate of distillation, 
the balls of the column will actively chatter, but the chambers will not 
flood.
    12.6.2.2 When the liquid has reached an apparent volume of 
approximately 10 mL, remove the round-bottom flask from the heating 
mantle and allow the solvent to drain and cool for at least 10 minutes. 
Remove the Snyder column and rinse the glass joint into the receiver 
with small portions of solvent.
    12.6.2.3 Proceed to Section 12.6.4 for preparation for back-
extraction or micro-concentration and solvent exchange.
    12.6.3 Kuderna-Danish (K-D)--Concentrate the extracts in separate 
500 mL K-D flasks equipped with 10 mL concentrator tubes. The K-D 
technique is used for solvents such as methylene chloride and hexane. 
Toluene is difficult to concentrate using the K-D technique unless a 
water bath fed by a steam generator is used.
    12.6.3.1 Add one to two clean boiling chips to the receiver. Attach 
a three-ball macro Snyder column. Prewet the column by adding 
approximately 1 mL of solvent through the top. Place the K-D apparatus 
in a hot water bath so that the entire lower rounded surface of the 
flask is bathed with steam.
    12.6.3.2 Adjust the vertical position of the apparatus and the water 
temperature as required to complete the concentration in 15-20 minutes. 
At the proper rate of distillation, the balls of the column will 
actively chatter but the chambers will not flood.
    12.6.3.3 When the liquid has reached an apparent volume of 1 mL, 
remove the K-D apparatus from the bath and allow the solvent to drain 
and cool for at least 10 minutes. Remove the Snyder column and rinse the 
flask and its lower joint into the concentrator tube with 1-2 mL of 
solvent. A 5 mL syringe is recommended for this operation.
    12.6.3.4 Remove the three-ball Snyder column, add a fresh boiling 
chip, and attach a two-ball micro Snyder column to the concentrator 
tube. Prewet the column by adding approximately 0.5 mL of solvent 
through the top. Place the apparatus in the hot water bath.
    12.6.3.5 Adjust the vertical position and the water temperature as 
required to complete the concentration in 5-10 minutes. At the proper 
rate of distillation, the balls of the column will actively chatter but 
the chambers will not flood.
    12.6.3.6 When the liquid reaches an apparent volume of 0.5 mL, 
remove the apparatus from the water bath and allow to drain and cool for 
at least 10 minutes.
    12.6.3.7 Proceed to 12.6.4 for preparation for back-extraction or 
micro-concentration and solvent exchange.
    12.6.4 Preparation for back-extraction or micro-concentration and 
solvent exchange.
    12.6.4.1 For back-extraction (Section 12.5), transfer the extract to 
a 250 mL separatory funnel. Rinse the concentration vessel with small 
portions of hexane, adjust the hexane volume in the separatory funnel to 
10-20 mL, and proceed to back-extraction (Section 12.5).
    12.6.4.2 For determination of the weight of residue in the extract, 
or for clean-up procedures other than back-extraction, transfer the 
extract to a blowdown vial using two to three rinses of solvent. Proceed 
with micro-concentration and solvent exchange (Section 12.7).
    12.7 Micro-Concentration and Solvent Exchange.
    12.7.1 Extracts to be subjected to GPC or HPLC cleanup are exchanged 
into methylene chloride. Extracts to be cleaned up using silica gel, 
alumina, carbon, and/or Florisil are exchanged into hexane.
    12.7.2 Transfer the vial containing the sample extract to a nitrogen 
blowdown device. Adjust the flow of nitrogen so that the surface of the 
solvent is just visibly disturbed.

    Note: A large vortex in the solvent may cause analyte loss.

    12.7.3 Lower the vial into a 45 [deg]C water bath and continue 
concentrating.
    12.7.3.1 If the extract is to be concentrated to dryness for weight 
determination (Sections 12.4.1.8, 12.4.2.7, and 13.7.1.4), blow dry 
until a constant weight is obtained.
    12.7.3.2 If the extract is to be concentrated for injection into the 
GC/MS or the solvent is to be exchanged for extract cleanup, proceed as 
follows:
    12.7.4 When the volume of the liquid is approximately 100 L, add 2-3 
mL of the desired solvent (methylene chloride for GPC and HPLC, or 
hexane for the other cleanups) and continue concentration to 
approximately 100 [micro]L. Repeat the addition of solvent and 
concentrate once more.
    12.7.5 If the extract is to be cleaned up by GPC, adjust the volume 
of the extract to 5.0 mL with methylene chloride. If the extract is to 
be cleaned up by HPLC, further concentrate the extract to 30 [micro]L. 
Proceed with GPC or HPLC cleanup (Section 13.2 or 13.6, respectively).
    12.7.6 If the extract is to be cleaned up by column chromatography 
(alumina, silica gel, Carbopak/Celite, or Florisil), bring the final

[[Page 325]]

volume to 1.0 mL with hexane. Proceed with column cleanups (Sections 
13.3 through 13.5 and 13.8).
    12.7.7 If the extract is to be concentrated for injection into the 
GC/MS (Section 14), quantitatively transfer the extract to a 0.3 mL 
conical vial for final concentration, rinsing the larger vial with 
hexane and adding the rinse to the conical vial. Reduce the volume to 
approximately 100 [micro]L. Add 10 [micro]L of nonane to the vial, and 
evaporate the solvent to the level of the nonane. Seal the vial and 
label with the sample number. Store in the dark at room temperature 
until ready for GC/MS analysis. If GC/MS analysis will not be performed 
on the same day, store the vial at <-10 [deg]C.

                          13.0 Extract Cleanup

    13.1 Cleanup may not be necessary for relatively clean samples 
(e.g., treated effluents, groundwater, drinking water). If particular 
circumstances require the use of a cleanup procedure, the analyst may 
use any or all of the procedures below or any other appropriate 
procedure. Before using a cleanup procedure, the analyst must 
demonstrate that the requirements of Section 9.2 can be met using the 
cleanup procedure. If only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be 
determined, the cleanup procedures may be optimized for isolation of 
these two compounds.
    13.1.1 Gel permeation chromatography (Section 13.2) removes high 
molecular weight interferences that cause GC column performance to 
degrade. It should be used for all soil and sediment extracts and may be 
used for water extracts that are expected to contain high molecular 
weight organic compounds (e.g., polymeric materials, humic acids).
    13.1.2 Acid, neutral, and basic silica gel (Section 13.3), alumina 
(Section 13.4), and Florisil (Section 13.8) are used to remove nonpolar 
and polar interferences. Alumina and Florisil are used to remove 
chlorodiphenyl ethers.
    13.1.3 Carbopak/Celite (Section 13.5) is used to remove nonpolar 
interferences.
    13.1.4 HPLC (Section 13.6) is used to provide specificity for the 
2,3,7,8-substituted and other CDD and CDF isomers.
    13.1.5 The anthropogenic isolation column (Section 13.7.1), 
acidified silica gel batch adsorption procedure (Section 13.7.2), and 
sulfuric acid and base back-extraction (Section 13.7.3) are used for 
removal of lipids from tissue samples.
    13.2 Gel Permeation Chromatography (GPC).
    13.2.1 Column packing.
    13.2.1.1 Place 70-75 g of SX-3 Bio-beads (Section 6.7.1.1) in a 400-
500 mL beaker.
    13.2.1.2 Cover the beads with methylene chloride and allow to swell 
overnight (a minimum of 12 hours).
    13.2.1.3 Transfer the swelled beads to the column (Section 6.7.1.1) 
and pump solvent through the column, from bottom to top, at 4.5-5.5 mL/
minute prior to connecting the column to the detector.
    13.2.1.4 After purging the column with solvent for one to two hours, 
adjust the column head pressure to 7-10 psig and purge for four to five 
hours to remove air. Maintain a head pressure of 7-10 psig. Connect the 
column to the detector (Section 6.7.1.4).
    13.2.2 Column calibration.
    13.2.2.1 Load 5 mL of the calibration solution (Section 7.4) into 
the sample loop.
    13.2.2.2 Inject the calibration solution and record the signal from 
the detector. The elution pattern will be corn oil, bis(2-ethyl 
hexyl)phthalate, pentachlorophenol, perylene, and sulfur.
    13.2.2.3 Set the ``dump time'' to allow 85% removal of 
the corn oil and 85% collection of the phthalate.
    13.2.2.4 Set the ``collect time'' to the peak minimum between 
perylene and sulfur.
    13.2.2.5 Verify the calibration with the calibration solution after 
every 20 extracts. Calibration is verified if the recovery of the 
pentachlorophenol is greater than 85%. If calibration is not verified, 
the system shall be recalibrated using the calibration solution, and the 
previous 20 samples shall be re-extracted and cleaned up using the 
calibrated GPC system.
    13.2.3 Extract cleanup--GPC requires that the column not be 
overloaded. The column specified in this method is designed to handle a 
maximum of 0.5 g of high molecular weight material in a 5 mL extract. If 
the extract is known or expected to contain more than 0.5 g, the extract 
is split into aliquots for GPC, and the aliquots are combined after 
elution from the column. The residue content of the extract may be 
obtained gravimetrically by evaporating the solvent from a 50 [micro]L 
aliquot.
    13.2.3.1 Filter the extract or load through the filter holder 
(Section 6.7.1.3) to remove the particles. Load the 5.0 mL extract onto 
the column.
    13.2.3.2 Elute the extract using the calibration data determined in 
Section 13.2.2. Collect the eluate in a clean 400-500 mL beaker.
    13.2.3.3 Rinse the sample loading tube thoroughly with methylene 
chloride between extracts to prepare for the next sample.
    13.2.3.4 If a particularly dirty extract is encountered, a 5.0 mL 
methylene chloride blank shall be run through the system to check for 
carry-over.
    13.2.3.5 Concentrate the eluate per Sections 12.6 and 12.7 for 
further cleanup or injection into the GC/MS.
    13.3 Silica Gel Cleanup.
    13.3.1 Place a glass-wool plug in a 15 mm ID chromatography column 
(Section 6.7.4.2). Pack the column bottom to top with: 1 g silica gel 
(Section 7.5.1.1), 4 g basic silica gel (Section 7.5.1.3), 1 g silica 
gel, 8 g acid silica

[[Page 326]]

gel (Section 7.5.1.2), 2 g silica gel, and 4 g granular anhydrous sodium 
sulfate (Section 7.2.1). Tap the column to settle the adsorbents.
    13.3.2 Pre-elute the column with 50-100 mL of hexane. Close the 
stopcock when the hexane is within 1 mm of the sodium sulfate. Discard 
the eluate. Check the column for channeling. If channeling is present, 
discard the column and prepare another.
    13.3.3 Apply the concentrated extract to the column. Open the 
stopcock until the extract is within 1 mm of the sodium sulfate.
    13.3.4 Rinse the receiver twice with 1 mL portions of hexane, and 
apply separately to the column. Elute the CDDs/CDFs with 100 mL hexane, 
and collect the eluate.
    13.3.5 Concentrate the eluate per Sections 12.6 and 12.7 for further 
cleanup or injection into the HPLC or GC/MS.
    13.3.6 For extracts of samples known to contain large quantities of 
other organic compounds (such as paper mill effluents), it may be 
advisable to increase the capacity of the silica gel column. This may be 
accomplished by increasing the strengths of the acid and basic silica 
gels. The acid silica gel (Section 7.5.1.2) may be increased in strength 
to as much as 44% w/w (7.9 g sulfuric acid added to 10 g silica gel). 
The basic silica gel (Section 7.5.1.3) may be increased in strength to 
as much as 33% w/w (50 mL 1N NaOH added to 100 g silica gel), or the 
potassium silicate (Section 7.5.1.4) may be used.

    Note: The use of stronger acid silica gel (44% w/w) may lead to 
charring of organic compounds in some extracts. The charred material may 
retain some of the analytes and lead to lower recoveries of CDDs/CDFs. 
Increasing the strengths of the acid and basic silica gel may also 
require different volumes of hexane than those specified above to elute 
the analytes off the column. Therefore, the performance of the method 
after such modifications must be verified by the procedure in Section 
9.2.

    13.4 Alumina Cleanup.
    13.4.1 Place a glass-wool plug in a 15 mm ID chromatography column 
(Section 6.7.4.2).
    13.4.2 If using acid alumina, pack the column by adding 6 g acid 
alumina (Section 7.5.2.1). If using basic alumina, substitute 6 g basic 
alumina (Section 7.5.2.2). Tap the column to settle the adsorbents.
    13.4.3 Pre-elute the column with 50-100 mL of hexane. Close the 
stopcock when the hexane is within 1 mm of the alumina.
    13.4.4 Discard the eluate. Check the column for channeling. If 
channeling is present, discard the column and prepare another.
    13.4.5 Apply the concentrated extract to the column. Open the 
stopcock until the extract is within 1 mm of the alumina.
    13.4.6 Rinse the receiver twice with 1 mL portions of hexane and 
apply separately to the column. Elute the interfering compounds with 100 
mL hexane and discard the eluate.
    13.4.7 The choice of eluting solvents will depend on the choice of 
alumina (acid or basic) made in Section 13.4.2.
    13.4.7.1 If using acid alumina, elute the CDDs/CDFs from the column 
with 20 mL methylene chloride:hexane (20:80 v/v). Collect the eluate.
    13.4.7.2 If using basic alumina, elute the CDDs/CDFs from the column 
with 20 mL methylene chloride:hexane (50:50 v/v). Collect the eluate.
    13.4.8 Concentrate the eluate per Sections 12.6 and 12.7 for further 
cleanup or injection into the HPLC or GC/MS.
    13.5 Carbon Column.
    13.5.1 Cut both ends from a 10 mL disposable serological pipet 
(Section 6.7.3.2) to produce a 10 cm column. Fire-polish both ends and 
flare both ends if desired. Insert a glass-wool plug at one end, and 
pack the column with 0.55 g of Carbopak/Celite (Section 7.5.3.3) to form 
an adsorbent bed approximately 2 cm long. Insert a glass-wool plug on 
top of the bed to hold the adsorbent in place.
    13.5.2 Pre-elute the column with 5 mL of toluene followed by 2 mL of 
methylene chloride: methanol:toluene (15:4:1 v/v), 1 mL of methylene 
chloride:cyclohexane (1:1 v/v), and 5 mL of hexane. If the flow rate of 
eluate exceeds 0.5 mL/minute, discard the column.
    13.5.3 When the solvent is within 1 mm of the column packing, apply 
the sample extract to the column. Rinse the sample container twice with 
1 mL portions of hexane and apply separately to the column. Apply 2 mL 
of hexane to complete the transfer.
    13.5.4 Elute the interfering compounds with two 3 mL portions of 
hexane, 2 mL of methylene chloride:cyclohexane (1:1 v/v), and 2 mL of 
methylene chloride:methanol:toluene (15:4:1 v/v). Discard the eluate.
    13.5.5 Invert the column, and elute the CDDs/CDFs with 20 mL of 
toluene. If carbon particles are present in the eluate, filter through 
glass-fiber filter paper.
    13.5.6 Concentrate the eluate per Sections 12.6 and 12.7 for further 
cleanup or injection into the HPLC or GC/MS.
    13.6 HPLC (Reference 6).
    13.6.1 Column calibration.
    13.6.1.1 Prepare a calibration standard containing the 2,3,7,8-
substituted isomers and/or other isomers of interest at a concentration 
of approximately 500 pg/[micro]L in methylene chloride.
    13.6.1.2 Inject 30 [micro]L of the calibration solution into the 
HPLC and record the signal from the detector. Collect the eluant for 
reuse. The elution order will be the tetra- through octa-isomers.
    13.6.1.3 Establish the collection time for the tetra-isomers and for 
the other isomers of interest. Following calibration, flush the 
injection system with copious quantities of

[[Page 327]]

methylene chloride, including a minimum of five 50 [micro]L injections 
while the detector is monitored, to ensure that residual CDDs/CDFs are 
removed from the system.
    13.6.1.4 Verify the calibration with the calibration solution after 
every 20 extracts. Calibration is verified if the recovery of the CDDs/
CDFs from the calibration standard (Section 13.6.1.1) is 75-125% 
compared to the calibration (Section 13.6.1.2). If calibration is not 
verified, the system shall be recalibrated using the calibration 
solution, and the previous 20 samples shall be re-extracted and cleaned 
up using the calibrated system.
    13.6.2 Extract cleanup--HPLC requires that the column not be 
overloaded. The column specified in this method is designed to handle a 
maximum of 30 [micro]L of extract. If the extract cannot be concentrated 
to less than 30 [micro]L, it is split into fractions and the fractions 
are combined after elution from the column.
    13.6.2.1 Rinse the sides of the vial twice with 30 [micro]L of 
methylene chloride and reduce to 30 [micro]L with the evaporation 
apparatus (Section 12.7).
    13.6.2.2 Inject the 30 [micro]L extract into the HPLC.
    13.6.2.3 Elute the extract using the calibration data determined in 
Section 13.6.1. Collect the fraction(s) in a clean 20 mL concentrator 
tube containing 5 mL of hexane:acetone (1:1 v/v).
    13.6.2.4 If an extract containing greater than 100 ng/mL of total 
CDD or CDF is encountered, a 30 [micro]L methylene chloride blank shall 
be run through the system to check for carry-over.
    13.6.2.5 Concentrate the eluate per Section 12.7 for injection into 
the GC/MS.
    13.7 Cleanup of Tissue Lipids--Lipids are removed from the Soxhlet 
extract using either the anthropogenic isolation column (Section 13.7.1) 
or acidified silica gel (Section 13.7.2), or are removed from the HCl 
digested extract using sulfuric acid and base back-extraction (Section 
13.7.3).
    13.7.1 Anthropogenic isolation column (References 22 and 27)--Used 
for removal of lipids from the Soxhlet/SDS extraction (Section 12.4.1).
    13.7.1.1 Prepare the column as given in Section 7.5.4.
    13.7.1.2 Pre-elute the column with 100 mL of hexane. Drain the 
hexane layer to the top of the column, but do not expose the sodium 
sulfate.
    13.7.1.3 Load the sample and rinses (Section 12.4.1.9.2) onto the 
column by draining each portion to the top of the bed. Elute the CDDs/
CDFs from the column into the apparatus used for concentration (Section 
12.4.1.7) using 200 mL of hexane.
    13.7.1.4 Concentrate the cleaned up extract (Sections 12.6 through 
12.7) to constant weight per Section 12.7.3.1. If more than 500 mg of 
material remains, repeat the cleanup using a fresh anthropogenic 
isolation column.
    13.7.1.5 Redissolve the extract in a solvent suitable for the 
additional cleanups to be used (Sections 13.2 through 13.6 and 13.8).
    13.7.1.6 Spike 1.0 mL of the cleanup standard (Section 7.11) into 
the residue/solvent.
    13.7.1.7 Clean up the extract using the procedures in Sections 13.2 
through 13.6 and 13.8. Alumina (Section 13.4) or Florisil (Section 13.8) 
and carbon (Section 13.5) are recommended as minimum additional cleanup 
steps.
    13.7.1.8 Following cleanup, concentrate the extract to 10 [micro]L 
as described in Section 12.7 and proceed with the analysis in Section 
14.
    13.7.2 Acidified silica gel (Reference 28)--Procedure alternate to 
the anthropogenic isolation column (Section 13.7.1) that is used for 
removal of lipids from the Soxhlet/SDS extraction (Section 12.4.1).
    13.7.2.1 Adjust the volume of hexane in the bottle (Section 
12.4.1.9.2) to approximately 200 mL.
    13.7.2.2 Spike 1.0 mL of the cleanup standard (Section 7.11) into 
the residue/solvent.
    13.7.2.3 Drop the stirring bar into the bottle, place the bottle on 
the stirring plate, and begin stirring.
    13.7.2.4 Add 30-100 g of acid silica gel (Section 7.5.1.2) to the 
bottle while stirring, keeping the silica gel in motion. Stir for two to 
three hours.

    Note: 30 grams of silica gel should be adequate for most samples and 
will minimize contamination from this source.

    13.7.2.5 After stirring, pour the extract through approximately 10 g 
of granular anhydrous sodium sulfate (Section 7.2.1) contained in a 
funnel with glass-fiber filter into a macro contration device (Section 
12.6). Rinse the bottle and sodium sulfate with hexane to complete the 
transfer.
    13.7.2.6 Concentrate the extract per Sections 12.6 through 12.7 and 
clean up the extract using the procedures in Sections 13.2 through 13.6 
and 13.8. Alumina (Section 13.4) or Florisil (Section 13.8) and carbon 
(Section 13.5) are recommended as minimum additional cleanup steps.
    13.7.3 Sulfuric acid and base back-extraction. Used with HCl 
digested extracts (Section 12.4.2).
    13.7.3.1 Spike 1.0 mL of the cleanup standard (Section 7.11) into 
the residue/solvent (Section 12.4.2.8.2).
    13.7.3.2 Add 10 mL of concentrated sulfuric acid to the bottle. 
Immediately cap and shake one to three times. Loosen cap in a hood to 
vent excess pressure. Cap and shake the bottle so that the residue/
solvent is exposed to the acid for a total time of approximately 45 
seconds.
    13.7.3.3 Decant the hexane into a 250 mL separatory funnel making 
sure that no acid

[[Page 328]]

is transferred. Complete the quantitative transfer with several hexane 
rinses.
    13.7.3.4 Back extract the solvent/residue with 50 mL of potassium 
hydroxide solution per Section 12.5.2, followed by two reagent water 
rinses.
    13.7.3.5 Drain the extract through a filter funnel containing 
approximately 10 g of granular anhydrous sodium sulfate in a glass-fiber 
filter into a macro concentration device (Section 12.6).
    13.7.3.6 Concentrate the cleaned up extract to a volume suitable for 
the additional cleanups given in Sections 13.2 through 13.6 and 13.8. 
Gel permeation chromatography (Section 13.2), alumina (Section 13.4) or 
Florisil (Section 13.8), and Carbopak/Celite (Section 13.5) are 
recommended as minimum additional cleanup steps.
    13.7.3.7 Following cleanup, concentrate the extract to 10 L as 
described in Section 12.7 and proceed with analysis per Section 14.
    13.8 Florisil Cleanup (Reference 29).
    13.8.1 Pre-elute the activated Florisil column (Section 7.5.3) with 
10 mL of methylene chloride followed by 10 mL of hexane:methylene 
chloride (98:2 v/v) and discard the solvents.
    13.8.2 When the solvent is within 1 mm of the packing, apply the 
sample extract (in hexane) to the column. Rinse the sample container 
twice with 1 mL portions of hexane and apply to the column.
    13.8.3 Elute the interfering compounds with 20 mL of 
hexane:methylene chloride (98:2) and discard the eluate.
    13.8.4 Elute the CDDs/CDFs with 35 mL of methylene chloride and 
collect the eluate. Concentrate the eluate per Sections 12.6 through 
12.7 for further cleanup or for injection into the HPLC or GC/MS.

                         14.0 HRGC/HRMS Analysis

    14.1 Establish the operating conditions given in Section 10.1.
    14.2 Add 10 uL of the appropriate internal standard solution 
(Section 7.12) to the sample extract immediately prior to injection to 
minimize the possibility of loss by evaporation, adsorption, or 
reaction. If an extract is to be reanalyzed and evaporation has 
occurred, do not add more instrument internal standard solution. Rather, 
bring the extract back to its previous volume (e.g., 19 L) with pure 
nonane only (18 L if 2 L injections are used).
    14.3 Inject 1.0 [micro]L or 2.0 [micro]L of the concentrated extract 
containing the internal standard solution, using on-column or splitless 
injection. The volume injected must be identical to the volume used for 
calibration (Section 10). Start the GC column initial isothermal hold 
upon injection. Start MS data collection after the solvent peak elutes. 
Stop data collection after the OCDD and OCDF have eluted. If only 
2,3,7,8-TCDD and 2,3,7,8-TCDF are to be determined, stop data collection 
after elution of these compounds. Return the column to the initial 
temperature for analysis of the next extract or standard.

                 15.0 System and Laboratory Performance

    15.1 At the beginning of each 12-hour shift during which analyses 
are performed, GC/MS system performance and calibration are verified for 
all CDDs/CDFs and labeled compounds. For these tests, analysis of the 
CS3 calibration verification (VER) standard (Section 7.13 and Table 4) 
and the isomer specificity test standards (Section 7.15 and Table 5) 
shall be used to verify all performance criteria. Adjustment and/or 
recalibration (Section 10) shall be performed until all performance 
criteria are met. Only after all performance criteria are met may 
samples, blanks, IPRs, and OPRs be analyzed.
    15.2 MS Resolution--A static resolving power of at least 10,000 (10% 
valley definition) must be demonstrated at the appropriate m/z before 
any analysis is performed. Static resolving power checks must be 
performed at the beginning and at the end of each 12-hour shift 
according to procedures in Section 10.1.2. Corrective actions must be 
implemented whenever the resolving power does not meet the requirement.
    15.3 Calibration Verification.
    15.3.1 Inject the VER standard using the procedure in Section 14.
    15.3.2 The m/z abundance ratios for all CDDs/CDFs shall be within 
the limits in Table 9; otherwise, the mass spectrometer shall be 
adjusted until the m/z abundance ratios fall within the limits 
specified, and the verification test shall be repeated. If the 
adjustment alters the resolution of the mass spectrometer, resolution 
shall be verified (Section 10.1.2) prior to repeat of the verification 
test.
    15.3.3 The peaks representing each CDD/CDF and labeled compound in 
the VER standard must be present with S/N of at least 10; otherwise, the 
mass spectrometer shall be adjusted and the verification test repeated.
    15.3.4 Compute the concentration of each CDD/CDF compound by isotope 
dilution (Section 10.5) for those compounds that have labeled analogs 
(Table 1). Compute the concentration of the labeled compounds by the 
internal standard method (Section 10.6). These concentrations are 
computed based on the calibration data in Section 10.
    15.3.5 For each compound, compare the concentration with the 
calibration verification limit in Table 6. If only 2,3,7,8-TCDD and 
2,3,7,8-TCDF are to be determined, compare the concentration to the 
limit in Table 6a. If all compounds meet the acceptance criteria, 
calibration has been verified and analysis of standards and sample 
extracts may proceed. If, however, any compound fails its respective 
limit, the measurement system is not performing properly for

[[Page 329]]

that compound. In this event, prepare a fresh calibration standard or 
correct the problem causing the failure and repeat the resolution 
(Section 15.2) and verification (Section 15.3) tests, or recalibrate 
(Section 10).
    15.4 Retention Times and GC Resolution.
    15.4.1 Retention times.
    15.4.1.1 Absolute--The absolute retention times of the 
\13\C12-1,2,3,4-TCDD and \13\C12-1,2,3,7,8,9-HxCDD 
GCMS internal standards in the verification test (Section 15.3) shall be 
within 15 seconds of the retention times obtained 
during calibration (Sections 10.2.1 and 10.2.4).
    15.4.1.2 Relative--The relative retention times of CDDs/CDFs and 
labeled compounds in the verification test (Section 15.3) shall be 
within the limits given in Table 2.
    15.4.2 GC resolution.
    15.4.2.1 Inject the isomer specificity standards (Section 7.15) on 
their respective columns.
    15.4.2.2 The valley height between 2,3,7,8-TCDD and the other tetra-
dioxin isomers at m/z 319.8965, and between 2,3,7,8-TCDF and the other 
tetra-furan isomers at m/z 303.9016 shall not exceed 25% on their 
respective columns (Figures 6 and 7).
    15.4.3 If the absolute retention time of any compound is not within 
the limits specified or if the 2,3,7,8-isomers are not resolved, the GC 
is not performing properly. In this event, adjust the GC and repeat the 
verification test (Section 15.3) or recalibrate (Section 10), or replace 
the GC column and either verify calibration or recalibrate.
    15.5 Ongoing Precision and Recovery.
    15.5.1 Analyze the extract of the ongoing precision and recovery 
(OPR) aliquot (Section 11.4.2.5, 11.5.4, 11.6.2, 11.7.4, or 11.8.3.2) 
prior to analysis of samples from the same batch.
    15.5.2 Compute the concentration of each CDD/CDF by isotope dilution 
for those compounds that have labeled analogs (Section 10.5). Compute 
the concentration of 1,2,3,7,8,9-HxCDD, OCDF, and each labeled compound 
by the internal standard method (Section 10.6).
    15.5.3 For each CDD/CDF and labeled compound, compare the 
concentration to the OPR limits given in Table 6. If only 2,3,7,8-TCDD 
and 2,3,7,8-TCDF are to be determined, compare the concentration to the 
limits in Table 6a. If all compounds meet the acceptance criteria, 
system performance is acceptable and analysis of blanks and samples may 
proceed. If, however, any individual concentration falls outside of the 
range given, the extraction/concentration processes are not being 
performed properly for that compound. In this event, correct the 
problem, re-prepare, extract, and clean up the sample batch and repeat 
the ongoing precision and recovery test (Section 15.5).
    15.5.4 Add results that pass the specifications in Section 15.5.3 to 
initial and previous ongoing data for each compound in each matrix. 
Update QC charts to form a graphic representation of continued 
laboratory performance. Develop a statement of laboratory accuracy for 
each CDD/CDF in each matrix type by calculating the average percent 
recovery (R) and the standard deviation of percent recovery 
(SR). Express the accuracy as a recovery interval from R-
2SR to R = 2SR. For example, if R = 95% and 
SR = 5%, the accuracy is 85-105%.
    15.6 Blank--Analyze the method blank extracted with each sample 
batch immediately following analysis of the OPR aliquot to demonstrate 
freedom from contamination and freedom from carryover from the OPR 
analysis. The results of the analysis of the blank must meet the 
specifications in Section 9.5.2 before sample analyses may proceed.

                     16.0 Qualitative Determination

    A CDD, CDF, or labeled compound is identified in a standard, blank, 
or sample when all of the criteria in Sections 16.1 through 16.4 are 
met.
    16.1 The signals for the two exact m/z's in Table 8 must be present 
and must maximize within the same two seconds.
    16.2 The signal-to-noise ratio (S/N) for the GC peak at each exact 
m/z must be greater than or equal to 2.5 for each CDD or CDF detected in 
a sample extract, and greater than or equal to 10 for all CDDs/CDFs in 
the calibration standard (Sections 10.2.3 and 15.3.3).
    16.3 The ratio of the integrated areas of the two exact m/z's 
specified in Table 8 must be within the limit in Table 9, or within 
10% of the ratio in the midpoint (CS3) calibration 
or calibration verification (VER), whichever is most recent.
    16.4 The relative retention time of the peak for a 2,3,7,8-
substituted CDD or CDF must be within the limit in Table 2. The 
retention time of peaks representing non-2,3,7,8-substituted CDDs/CDFs 
must be within the retention time windows established in Section 10.3.
    16.5 Confirmatory Analysis--Isomer specificity for 2,3,7,8-TCDF 
cannot be achieved on the DB-5 column. Therefore, any sample in which 
2,3,7,8-TCDF is identified by analysis on a DB-5 column must have a 
confirmatory analysis performed on a DB-225, SP-2330, or equivalent GC 
column. The operating conditions in Section 10.1.1 may be adjusted to 
optimize the analysis on the second GC column, but the GC/MS must meet 
the mass resolution and calibration specifications in Section 10.
    16.6 If the criteria for identification in Sections 16.1 through 
16.5 are not met, the CDD or CDF has not been identified and the results 
may not be reported for regulatory compliance purposes. If interferences 
preclude identification, a new aliquot of sample

[[Page 330]]

must be extracted, further cleaned up, and analyzed.
    17.0 Quantitative Determination
    17.1 Isotope Dilution Quantitation--By adding a known amount of a 
labeled compound to every sample prior to extraction, correction for 
recovery of the CDD/CDF can be made because the CDD/CDF and its labeled 
analog exhibit similar effects upon extraction, concentration, and gas 
chromatography. Relative response (RR) values are used in conjunction 
with the initial calibration data described in Section 10.5 to determine 
concentrations directly, so long as labeled compound spiking levels are 
constant, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR15SE97.007

where:

Cex = The concentration of the CDD/CDF in the extract, and 
          the other terms are as defined in Section 10.5.2.

    17.1.1 Because of a potential interference, the labeled analog of 
OCDF is not added to the sample. Therefore, OCDF is quantitated against 
labeled OCDD. As a result, the concentration of OCDF is corrected for 
the recovery of the labeled OCDD. In instances where OCDD and OCDF 
behave differently during sample extraction, concentration, and cleanup 
procedures, this may decrease the accuracy of the OCDF results. However, 
given the low toxicity of this compound relative to the other dioxins 
and furans, the potential decrease in accuracy is not considered 
significant.
    17.1.2 Because \13\C12-1,2,3,7,8,9-HxCDD is used as an 
instrument internal standard (i.e., not added before extraction of the 
sample), it cannot be used to quantitate the 1,2,3,7,8,9-HxCDD by strict 
isotope dilution procedures. Therefore, 1,2,3,7,8,9-HxCDD is quantitated 
using the averaged response of the labeled analogs of the other two 
2,3,7,8-substituted HxCDD's: 1,2,3,4,7,8-HxCDD and 1,2,3,6,7,8-HxCDD. As 
a result, the concentration of 1,2,3,7,8,9-HxCDD is corrected for the 
average recovery of the other two HxCDD's.
    17.1.3 Any peaks representing non-2,3,7,8-substituted CDDs/CDFs are 
quantitated using an average of the response factors from all of the 
labeled 2,3,7,8-isomers at the same level of chlorination.
    17.2 Internal Standard Quantitation and Labeled Compound Recovery.
    17.2.1 Compute the concentrations of 1,2,3,7,8,9-HxCDD, OCDF, the 
\13\C-labeled analogs and the \37\C-labeled cleanup standard in the 
extract using the response factors determined from the initial 
calibration data (Section 10.6) and the following equation:
[GRAPHIC] [TIFF OMITTED] TR15SE97.008

where:

Cex = The concentration of the CDD/CDF in the extract, and 
          the other terms are as defined in Section 10.6.1.

    Note: There is only one m/z for the \37\Cl-labeled standard.

    17.2.2 Using the concentration in the extract determined above, 
compute the percent recovery of the \13\C-labeled compounds and the 
\37\C-labeled cleanup standard using the following equation:
[GRAPHIC] [TIFF OMITTED] TR15SE97.009

    17.3 The concentration of a CDD/CDF in the solid phase of the sample 
is computed using the concentration of the compound in the extract and 
the weight of the solids (Section 11.5.1), as follows:
[GRAPHIC] [TIFF OMITTED] TR15SE97.010

where:

Cex = The concentration of the compound in the extract.
Vex = The extract volume in mL.
Ws = The sample weight (dry weight) in kg.

    17.4 The concentration of a CDD/CDF in the aqueous phase of the 
sample is computed using the concentration of the compound in

[[Page 331]]

the extract and the volume of water extracted (Section 11.4 or 11.5), as 
follows:
[GRAPHIC] [TIFF OMITTED] TR15SE97.011

where:

Cex = The concentration of the compound in the extract.
Vex = The extract volume in mL.
Vs = The sample volume in liters.

    17.5 If the SICP area at either quantitation m/z for any compound 
exceeds the calibration range of the system, a smaller sample aliquot is 
extracted.
    17.5.1 For aqueous samples containing 1% solids or less, dilute 100 
mL, 10 mL, etc., of sample to 1 L with reagent water and re-prepare, 
extract, clean up, and analyze per Sections 11 through 14.
    17.5.2 For samples containing greater than 1% solids, extract an 
amount of sample equal to \1/10\, \1/100\, etc., of the amount used in 
Section 11.5.1. Re-prepare, extract, clean up, and analyze per Sections 
11 through 14.
    17.5.3 If a smaller sample size will not be representative of the 
entire sample, dilute the sample extract by a factor of 10, adjust the 
concentration of the instrument internal standard to 100 pg/[micro]L in 
the extract, and analyze an aliquot of this diluted extract by the 
internal standard method.
    17.6 Results are reported to three significant figures for the CDDs/
CDFs and labeled compounds found in all standards, blanks, and samples.
    17.6.1 Reporting units and levels.
    17.6.1.1 Aqueous samples--Report results in pg/L (parts-per-
quadrillion).
    17.6.1.2 Samples containing greater than 1% solids (soils, 
sediments, filter cake, compost)--Report results in ng/kg based on the 
dry weight of the sample. Report the percent solids so that the result 
may be corrected.
    17.6.1.3 Tissues--Report results in ng/kg of wet tissue, not on the 
basis of the lipid content of the sample. Report the percent lipid 
content, so that the data user can calculate the concentration on a 
lipid basis if desired.
    17.6.1.4 Reporting level.
    17.6.1.4.1 Standards (VER, IPR, OPR) and samples--Report results at 
or above the minimum level (Table 2). Report results below the minimum 
level as not detected or as required by the regulatory authority.
    17.6.1.4.2 Blanks--Report results above one-third the ML.
    17.6.2 Results for CDDs/CDFs in samples that have been diluted are 
reported at the least dilute level at which the areas at the 
quantitation m/z's are within the calibration range (Section 17.5).
    17.6.3 For CDDs/CDFs having a labeled analog, results are reported 
at the least dilute level at which the area at the quantitation m/z is 
within the calibration range (Section 17.5) and the labeled compound 
recovery is within the normal range for the method (Section 9.3 and 
Tables 6, 6a, 7, and 7a).
    17.6.4 Additionally, if requested, the total concentration of all 
isomers in an individual level of chlorination (i.e., total TCDD, total 
TCDF, total Paced, etc.) may be reported by summing the concentrations 
of all isomers identified in that level of chlorination, including both 
2,3,7,8-substituted and non-2,3,7,8-substituted isomers.

                    18.0 Analysis of Complex Samples

    18.1 Some samples may contain high levels (10 ng/L; 
1000 ng/kg) of the compounds of interest, interfering 
compounds, and/or polymeric materials. Some extracts will not 
concentrate to 10 [micro]L (Section 12.7); others may overload the GC 
column and/or mass spectrometer.
    18.2 Analyze a smaller aliquot of the sample (Section 17.5) when the 
extract will not concentrate to 10 [micro]L after all cleanup procedures 
have been exhausted.
    18.3 Chlorodiphenyl Ethers--If chromatographic peaks are detected at 
the retention time of any CDDs/CDFs in any of the m/z channels being 
monitored for the chlorodiphenyl ethers (Table 8), cleanup procedures 
must be employed until these interferences are removed. Alumina (Section 
13.4) and Florisil (Section 13.8) are recommended for removal of 
chlorodiphenyl ethers.
    18.4 Recovery of Labeled Compounds--In most samples, recoveries of 
the labeled compounds will be similar to those from reagent water or 
from the alternate matrix (Section 7.6).
    18.4.1 If the recovery of any of the labeled compounds is outside of 
the normal range (Table 7), a diluted sample shall be analyzed (Section 
17.5).
    18.4.2 If the recovery of any of the labeled compounds in the 
diluted sample is outside of normal range, the calibration verification 
standard (Section 7.13) shall be analyzed and calibration verified 
(Section 15.3).

[[Page 332]]

    18.4.3 If the calibration cannot be verified, a new calibration must 
be performed and the original sample extract reanalyzed.
    18.4.4 If the calibration is verified and the diluted sample does 
not meet the limits for labeled compound recovery, the method does not 
apply to the sample being analyzed and the result may not be reported 
for regulatory compliance purposes. In this case, alternate extraction 
and cleanup procedures in this method must be employed to resolve the 
interference. If all cleanup procedures in this method have been 
employed and labeled compound recovery remains outside of the normal 
range, extraction and/or cleanup procedures that are beyond this scope 
of this method will be required to analyze these samples.

                        19.0 Pollution Prevention

    19.1 The solvents used in this method pose little threat to the 
environment when managed properly. The solvent evaporation techniques 
used in this method are amenable to solvent recovery, and it is 
recommended that the laboratory recover solvents wherever feasible.
    19.2 Standards should be prepared in volumes consistent with 
laboratory use to minimize disposal of standards.

                          20.0 Waste Management

    20.1 It is the laboratory's responsibility to comply with all 
federal, state, and local regulations governing waste management, 
particularly the hazardous waste identification rules and land disposal 
restrictions, and to protect the air, water, and land by minimizing and 
controlling all releases from fume hoods and bench operations. 
Compliance is also required with any sewage discharge permits and 
regulations.
    20.2 Samples containing HCl to pH <2 are hazardous and must be 
neutralized before being poured down a drain or must be handled as 
hazardous waste.
    20.3 The CDDs/CDFs decompose above 800 [deg]C. Low-level waste such 
as absorbent paper, tissues, animal remains, and plastic gloves may be 
burned in an appropriate incinerator. Gross quantities (milligrams) 
should be packaged securely and disposed of through commercial or 
governmental channels that are capable of handling extremely toxic 
wastes.
    20.4 Liquid or soluble waste should be dissolved in methanol or 
ethanol and irradiated with ultraviolet light with a wavelength shorter 
than 290 nm for several days. Use F40 BL or equivalent lamps. Analyze 
liquid wastes, and dispose of the solutions when the CDDs/CDFs can no 
longer be detected.
    20.5 For further information on waste management, consult ``The 
Waste Management Manual for Laboratory Personnel'' and ``Less is 
Better--Laboratory Chemical Management for Waste Reduction,'' available 
from the American Chemical Society's Department of Government Relations 
and Science Policy, 1155 16th Street N.W., Washington, D.C. 20036.

                         21.0 Method Performance

    Method performance was validated and performance specifications were 
developed using data from EPA's international interlaboratory validation 
study (References 30-31) and the EPA/paper industry Long-Term 
Variability Study of discharges from the pulp and paper industry (58 FR 
66078).

                             22.0 References

    1. Tondeur, Yves. ``Method 8290: Analytical Procedures and Quality 
Assurance for Multimedia Analysis of Polychlorinated Dibenzo-p-dioxins 
and Dibenzofurans by High Resolution Gas Chromatography/High Resolution 
Mass Spectrometry,'' USEPA EMSL, Las Vegas, Nevada, June 1987.
    2. ``Measurement of 2,3,7,8-Tetrachlorinated Dibenzo-p-dioxin (TCDD) 
and 2,3,7,8-Tetrachlorinated Dibenzofuran (TCDF) in Pulp, Sludges, 
Process Samples and Wastewaters from Pulp and Paper Mills,'' Wright 
State University, Dayton, OH 45435, June 1988.
    3. ``NCASI Procedures for the Preparation and Isomer Specific 
Analysis of Pulp and Paper Industry Samples for 2,3,7,8-TCDD and 
2,3,7,8-TCDF,'' National Council of the Paper Industry for Air and 
Stream Improvement Inc., 260 Madison Avenue, New York, NY 10016, 
Technical Bulletin No. 551, Pre-Release Copy, July 1988.
    4. ``Analytical Procedures and Quality Assurance Plan for the 
Determination of PCDD/PCDF in Fish,'' USEPA, Environmental Research 
Laboratory, 6201 Congdon Boulevard, Duluth, MN 55804, April 1988.
    5. Tondeur, Yves. ``Proposed GC/MS Methodology for the Analysis of 
PCDDs and PCDFs in Special Analytical Services Samples,'' Triangle 
Laboratories, Inc., 801-10 Capitola Dr, Research Triangle Park, NC 
27713, January 1988; updated by personal communication September 1988.
    6. Lamparski, L.L. and Nestrick, T.J. ``Determination of Tetra-, 
Hexa-, Hepta-, and Octachlorodibenzo-p-dioxin Isomers in Particulate 
Samples at Parts per Trillion Levels,'' Analytical Chemistry, 52: 2045-
2054, 1980.
    7. Lamparski, L.L. and Nestrick, T.J. ``Novel Extraction Device for 
the Determination of Chlorinated Dibenzo-p-dioxins (PCDDs) and 
Dibenzofurans (PCDFs) in Matrices Containing Water,'' Chemosphere, 
19:27-31, 1989.
    8. Patterson, D.G., et. al. ``Control of Interferences in the 
Analysis of Human Adipose Tissue for 2,3,7,8-Tetrachlorodibenzo-p-

[[Page 333]]

dioxin,'' Environmental Toxicological Chemistry, 5:355-360, 1986.
    9. Stanley, John S. and Sack, Thomas M. ``Protocol for the Analysis 
of 2,3,7,8-Tetrachlorodibenzo-p-dioxin by High Resolution Gas 
Chromatography/High Resolution Mass Spectrometry,'' USEPA EMSL, Las 
Vegas, Nevada 89114, EPA 600/4-86-004, January 1986.
    10. ``Working with Carcinogens,'' Department of Health, Education, & 
Welfare, Public Health Service, Centers for Disease Control, NIOSH, 
Publication 77-206, August 1977, NTIS PB-277256.
    11. ``OSHA Safety and Health Standards, General Industry,'' OSHA 
2206, 29 CFR 1910.
    12. ``Safety in Academic Chemistry Laboratories,'' ACS Committee on 
Chemical Safety, 1979.
    13. ``Standard Methods for the Examination of Water and 
Wastewater,'' 18th edition and later revisions, American Public Health 
Association, 1015 15th St, N.W., Washington, DC 20005, 1-35: Section 
1090 (Safety), 1992.
    14. ``Method 613--2,3,7,8-Tetrachlorodibenzo-p-dioxin,'' 40 CFR 136 
(49 FR 43234), October 26, 1984, Section 4.1.
    15. Provost, L.P. and Elder, R.S. ``Interpretation of Percent 
Recovery Data,'' American Laboratory, 15: 56-83, 1983.
    16. ``Standard Practice for Sampling Water,'' ASTM Annual Book of 
Standards, ASTM, 1916 Race Street, Philadelphia, PA 19103-1187, 1980.
    17. ``Methods 330.4 and 330.5 for Total Residual Chlorine,'' USEPA, 
EMSL, Cincinnati, OH 45268, EPA 600/4-79-020, March 1979.
    18. ``Handbook of Analytical Quality Control in Water and Wastewater 
Laboratories,'' USEPA EMSL, Cincinnati, OH 45268, EPA-600/4-79-019, 
March 1979.
    19. Williams, Rick. Letter to Bill Telliard, June 4, 1993, available 
from the EPA Sample Control Center operated by DynCorp Viar, Inc., 300 N 
Lee St, Alexandria, VA 22314, 703-519-1140.
    20. Barkowski, Sarah. Fax to Sue Price, August 6, 1992, available 
from the EPA Sample Control Center operated by DynCorp Viar, Inc., 300 N 
Lee St, Alexandria VA 22314, 703-519-1140.
    21. ``Analysis of Multi-media, Multi-concentration Samples for 
Dioxins and Furans, PCDD/PCDF Analyses Data Package'', Narrative for 
Episode 4419, MRI Project No. 3091-A, op.cit. February 12, 1993, 
Available from the EPA Sample Control Center operated by DynCorp Viar 
Inc, 300 N Lee St, Alexandria, VA 22314 (703-519-1140).
    22. ``Analytical Procedures and Quality Assurance Plan for the 
Determination of PCDD/PCDF in Fish'', U.S. Environmental Protection 
Agency, Environmental Research Laboratory, Duluth, MN 55804, EPA/600/3-
90/022, March 1990.
    23. Afghan, B.K., Carron, J., Goulden, P.D., Lawrence, J., Leger, 
D., Onuska, F., Sherry, J., and Wilkenson, R.J., ``Recent Advances in 
Ultratrace Analysis of Dioxins and Related Halogenated Hydrocarbons'', 
Can J. Chem., 65: 1086-1097, 1987.
    24. Sherry, J.P. and Tse, H. ``A Procedure for the Determination of 
Polychlorinated Dibenzo-p-dioxins in Fish'', Chemosphere, 20: 865-872, 
1990.
    25. ``Preliminary Fish Tissue Study'', Results of Episode 4419, 
available from the EPA Sample Control Center operated by DynCorp Viar, 
Inc., 300 N Lee St, Alexandria, VA 22314, 703-519-1140.
    26. Nestrick, Terry L. DOW Chemical Co., personal communication with 
D.R. Rushneck, April 8, 1993. Details available from the U.S. 
Environmental Protection Agency Sample Control Center operated by 
DynCorp Viar Inc, 300 N Lee St, Alexandria, VA 22314, 703-519-1140.
    27. Barnstadt, Michael. ``Big Fish Column'', Triangle Laboratories 
of RTP, Inc., SOP 129-90, 27 March 27, 1992.
    28. ``Determination of Polychlorinated Dibenzo-p-Dioxins (PCDD) and 
Dibenzofurans (PCDF) in Environmental Samples Using EPA Method 1613'', 
Chemical Sciences Department, Midwest Research Institute, 425 Volker 
Boulevard, Kansas City, MO 44110-2299, Standard Operating Procedure No. 
CS-153, January 15, 1992.
    29. Ryan, John J. Raymonde Lizotte and William H. Newsome, J. 
Chromatog. 303 (1984) 351-360.
    30. Telliard, William A., McCarty, Harry B., and Riddick, Lynn S. 
``Results of the Interlaboratory Validation Study of USEPA Method 1613 
for the Analysis of Tetra-through Octachlorinated Dioxins and Furans by 
Isotope Dilution GC/MS,'' Chemosphere, 27, 41-46 (1993).
    31. ``Results of the International Interlaboratory Validation Study 
of USEPA Method 1613'', October 1994, available from the EPA Sample 
Control Center operated by DynCorp Viar, Inc., 300 N Lee St, Alexandria, 
VA 22314, 703-519-1140.

                         23.0 Tables and Figures

[[Page 334]]



   Table 1--Chlorinated Dibenzo-p-Dioxins and Furans Determined by Isotope Dilution and Internal Standard High
                  Resolution Gas Chromatography (HRGC)/High Resolution Mass Spectrometry (HRMS)
----------------------------------------------------------------------------------------------------------------
                 CDDs/CDFs \1\                   CAS registry            Labeled analog            CAS registry
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD..................................       1746-01-6  \13\C12-2,3,7,8-TCDD............      76523-40-5
                                                                \37\Cl4-2,3,7,8-TCDD............      85508-50-5
Total TCDD....................................      41903-57-5
2,3,7,8-TCDF..................................      51207-31-9  \13\C12-2,3,7,8-TCDF............      89059-46-1
Total-TCDF....................................      55722-27-5
1,2,3,7,8-PeCDD...............................      40321-76-4  \13\C12-1,2,3,7,8-PeCDD.........     109719-79-1
Total-PeCDD...................................      36088-22-9
1,2,3,7,8-PeCDF...............................      57117-41-6  \13\C12-1,2,3,7,8-PeCDF.........     109719-77-9
2,3,4,7,8-PeCDF...............................      57117-31-4  \13\C12-2,3,4,7,8-PeCDF.........     116843-02-8
Total-PeCDF...................................      30402-15-4
1,2,3,4,7,8-HxCDD.............................      39227-28-6  \13\C12-1,2,3,4,7,8-HxCDD.......     109719-80-4
1,2,3,6,7,8-HxCDD.............................      57653-85-7  \13\C12-1,2,3,6,7,8-HxCDD.......     109719-81-5
1,2,3,7,8,9-HxCDD.............................      19408-74-3  \13\C12-1,2,3,7,8,9-HxCDD.......     109719-82-6
Total-HxCDD...................................      34465-46-8
1,2,3,4,7,8-HxCDF.............................      70648-26-9  \13\C12-1,2,3,4,7,8-HxCDF.......     114423-98-2
1,2,3,6,7,8-HxCDF.............................      57117-44-9  \13\C12-1,2,3,6,7,8-HxCDF.......     116843-03-9
1,2,3,7,8,9-HxCDF.............................      72918-21-9  \13\C12-1,2,3,7,8,9-HxCDF.......     116843-04-0
2,3,4,6,7,8-HxCDF.............................      60851-34-5  \13\C12-2,3,4,6,7,8-HxCDF.......     116843-05-1
Total-HxCDF...................................      55684-94-1
1,2,3,4,6,7,8-HpCDD...........................      35822-46-9  \13\C12-1,2,3,4,6,7,8-HpCDD.....     109719-83-7
Total-HpCDD...................................      37871-00-4
1,2,3,4,6,7,8-HpCDF...........................      67562-39-4  \13\C12-1,2,3,4,6,7,8-HpCDF.....     109719-84-8
1,2,3,4,7,8,9-HpCDF...........................      55673-89-7  \13\C12-1,2,3,4,7,8,9-HpCDF.....     109719-94-0
Total-HpCDF...................................      38998-75-3
OCDD..........................................       3268-87-9  \13\C12-OCDD....................     114423-97-1
OCDF..........................................      39001-02-0  Not used........................
----------------------------------------------------------------------------------------------------------------
\1\ Chlorinated dibenzo-p-dioxins and chlorinated dibenzofurans.
 TCDD = Tetrachlorodibenzo-p-dioxin.
 TCDF = Tetrachlorodibenzofuran.
 PeCDD = Pentachlorodibenzo-p-dioxin.
 PeCDF = Pentachlorodibenzofuran.
 HxCDD = Hexachlorodibenzo-p-dioxin.
 HxCDF = Hexachlorodibenzofuran.
 HpCDD = Heptachlorodibenzo-p-dioxin.
 HpCDF = Heptachlorodibenzofuran.
 OCDD = Octachlorodibenzo-p-dioxin.
 OCDF = Octachlorodibenzofuran.


  Table 2--Retention Time References, Quantitation References, Relative Retention Times, and Minimum Levels for
                                                  CDDS and DCFS
----------------------------------------------------------------------------------------------------------------
                                                                                        Minimum level \1\
                                                                                --------------------------------
                                          Retention time and        Relative                            Extract
               CDD/CDF                  quantitation reference   retention time  Water (pg/ Solid (ng/    (pg/
                                                                                  L; ppq)    kg; ppt)  [micro]L;
                                                                                                          ppb)
----------------------------------------------------------------------------------------------------------------
                    Compounds using \13\ C12-1,2,3,4-TCDD as the Injection Internal Standard
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDF.........................  \13\ C12-2,3,7,8-TCDF...     0.999-1.003         10          1        0.5
2,3,7,8-TCDD.........................  \13\ C12-2,3,7,8-TCDD...     0.999-1.002         10          1        0.5
1,2,3,7,8-Pe.........................  \13\ C12-1,2,3,7,8-PeCDF     0.999-1.002         50          5        2.5
2,3,4,7,8-PeCDF......................  \13\ C12-2,3,4,7,8-PeCDF     0.999-1.002         50          5        2.5
1,2,3,7,8-PeCDD......................  \13\ C12-1,2,3,7,8-PeCDD     0.999-1.002         50          5        2.5
\13\ C12-2,3,7,8-TCDF................  \13\ C12-1,2,3,4-TCDD...     0.923-1.103
\13\ C12-2,3,7,8-TCDD................  \13\ C12-1,2,3,4-TCDD...     0.976-1.043
\13\ C12-2,3,7,8-TCDD................  \13\ C12-1,2,3,4-TCDD...     0.989-1.052
\13\ C12-1,2,3,7,8-PeCDF.............  \13\ C12-1,2,3,4-TCDD...     1.000-1.425
\13\ C12-2,3,4,7,8-PeCDF.............  \13\ C12-1,2,3,4-TCDD...     1.001-1.526
\13\ C12-1,2,3,7,8-PeCDF.............  \13\ C12-1,2,3,4-TCDD...     1.000-1.567
----------------------------------------------------------------------------------------------------------------
                  Compounds using \13\ C12-1,2,3,7,8,9-HxCDD as the Injection Internal Standard
----------------------------------------------------------------------------------------------------------------
1,2,3,4,7,8-HxCDF....................  \13\ C12-1,2,3,4,7,8-        0.999-1.001         50          5        2.5
                                        HxCDF.
1,2,3,6,7,8-HxCDF....................  \13\ C12-1,2,3,6,7,8-        0.997-1.005         50          5        2.5
                                        HxCDF.
1,2,3,7,8,9-HxCDF....................  \13\ C12-1,2,3,7,8,9-        0.999-1.001         50          5        2.5
                                        HxCDF.
2,3,4,6,7,8-HxCDF....................  \13\ C12-2,3,4,6,7,8-        0.999-1.001         50          5        2.5
                                        HxCDF.
1,2,3,4,7,8-HxCDD....................  \13\ C12-1,2,3,4,7,8-        0.999-1.001         50          5        2.5
                                        HxCDD.
1,2,3,6,7,8-HxCDD....................  \13\ C12-1,2,3,6,7,8-        0.998-1.004         50          5        2.5
                                        HxCDD.
1,2,3,7,8,9-HxCDD....................  (\2\)...................     1.000-1.019         50          5        2.5
1,2,3,4,6,7,8-HpCDF..................  \13\ C12-1,2,3,4,6,7,8-      0.999-1.001         50          5        2.5
                                        HpCDF.

[[Page 335]]

 
1,2,3,4,7,8,9-HpCDF..................  \13\ C12-1,2,3,4,7,8,9-      0.999-1.001         50          5        2.5
                                        HpCDF.
1,2,3,4,6,7,8-HpCDD..................  \13\ C12-1,2,3,4,6,7,8-      0.999-1.001         50          5        2.5
                                        HpCDD.
OCDF.................................  \13\ C12-OCDD...........     0.999-1.001        100         10        5.0
OCDD.................................  \13\ C12-OCDD...........     0.999-1.001        100         10        5.0
1,2,3,4,6,7,8,-HxCDF.................  \13\ C12-1,2,3,7,8,9-        0.949-0.975
                                        HpCDD.
\13\ C121,2,3,7,8,9-HxCDF............  \13\ C12-1,2,3,7,8,9-        0.977-1.047
                                        HpCDD.
\13\ C122,3,4,6,7,8,-HxCDF...........  \13\ C12-1,2,3,7,8,9-        0.959-1.021
                                        HpCDD.
\13\ C121,2,3,4,7,8,-HxCDF...........  \13\ C12-1,2,3,7,8,9-        0.977-1.000
                                        HpCDD.
\13\ C121,2,3,6,7,8,-HxCDF...........  \13\ C12-1,2,3,7,8,9-        0.981-1.003
                                        HpCDD.
\13\ C121,2,3,4,6,7,8-HxCDF..........  \13\ C12-1,2,3,7,8,9-        1.043-1.085
                                        HpCDD.
\13\ C121,2,3,4,7,8,9-HxCDF..........  \13\ C12-1,2,3,7,8,9-        1.057-1.151
                                        HpCDD.
\13\ C121,2,3,4,6,7,8-HxCDF..........  \13\ C12-1,2,3,7,8,9-        1.086-1.110
                                        HpCDD.
\13\ C12OCDD.........................  \13\ C12-1,2,3,7,8,9-        1.032-1.311
                                        HpCDD.
----------------------------------------------------------------------------------------------------------------
\1\ The Minimum Level (ML) for each analyte is defined as the level at which the entire analytical system must
  give a recognizable signal and acceptable calibration point. It is equivalent to the concentration of the
  lowest calibration standard, assuming that all method-specified sample weights, volumes, and cleanup
  procedures have been employed.
\2\ The retention time reference for 1,2,3,7,8,9-HxCDD is \13\C12-1,2,3,6,7,8-HxCDD, and 1,2,3,7,8,9-HxCDD is
  quantified using the averaged responses for \13\C12-1,2,3,4,7,8-HxCDD and \13\C12-1,2,3,6,7,8-HxCDD.


        Table 3--Concentration of Stock and Spiking Solutions Containing CDDS/CDFS and Labeled Compounds
----------------------------------------------------------------------------------------------------------------
                                                               Labeled      Labeled
                                                              compound      compound    PAR stock    PAR spiking
                          CDD/CDF                               stock       spiking      solution   solution \4\
                                                            solution \1\    solution   \3\ (ng/mL)     (ng/mL)
                                                               (ng/mL)    \2\ (ng/mL)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD..............................................  ............  ...........           40           0.8
2,3,7,8-TCDF..............................................  ............  ...........           40           0.8
1,2,3,7,8-PeCDD...........................................  ............  ...........          200           4
1,2,3,7,8-PeCDF...........................................  ............  ...........          200           4
2,3,4,7,8-PeCDF...........................................  ............  ...........          200           4
1,2,3,4,7,8-HxCDD.........................................  ............  ...........          200           4
1,2,3,6,7,8-HxCDD.........................................  ............  ...........          200           4
1,2,3,7,8,9-HxCDD.........................................  ............  ...........          200           4
1,2,3,4,7,8-HxCDF.........................................  ............  ...........          200           4
1,2,3,6,7,8-HxCDF.........................................  ............  ...........          200           4
1,2,3,7,8,9-HxCDF.........................................  ............  ...........          200           4
2,3,4,6,7,8-HxCDF.........................................  ............  ...........          200           4
1,2,3,4,6,7,8-HpCDD.......................................  ............  ...........          200           4
1,2,3,4,6,7,8-HpCDF.......................................  ............  ...........          200           4
1,2,3,4,7,8,9-HpCDF.......................................  ............  ...........          200           4
OCDD......................................................  ............  ...........          400           8
OCDF......................................................  ............  ...........          400           8
\13\C12-2,3,7,8-TCDD......................................         100              2
\13\C12-2,3,7,8-TCDF......................................         100              2
\13\C12-1,2,3,7,8-PeCDD...................................         100              2
\13\C12-1,2,3,7,8-PeCDF...................................         100              2
\13\C12-2,3,4,7,8-PeCDF...................................         100              2
\13\C12-1,2,3,4,7,8-HxCDD.................................         100              2
\13\C12-1,2,3,6,7,8-HxCDD.................................         100              2
\13\C12-1,2,3,4,7,8-HxCDF.................................         100              2
\13\C12-1,2,3,6,7,8-HxCDF.................................         100              2
\13\C12-1,2,3,7,8,9-HxCDF.................................         100              2
\13\C12-2,3,4,6,7,8-HxCDF.................................         100              2
\13\C12-1,2,3,4,6,7,8-HpCDD...............................         100              2
\13\C12-1,2,3,4,6,7,8-HpCDF...............................         100              2
\13\C12-1,2,3,4,7,8,9-HpCDF...............................         100              2
\13\C12-OCDD..............................................         200              4
Cleanup Standard \5\
    \37\Cl4-2,3,7,8-TCDD..................................           0.8
Internal Standards \6\
    \13\C12-1,2,3,4-TCDD..................................         200
    \13\C12-1,2,3,7,8,9-HxCDD.............................         200
----------------------------------------------------------------------------------------------------------------
\1\ Section 7.10--prepared in nonane and diluted to prepare spiking solution.
\2\ Section 7.10.3--prepared in acetone from stock solution daily.

[[Page 336]]

 
\3\ Section 7.9--prepared in nonane and diluted to prepare spiking solution.
\4\ Section 7.14--prepared in acetone from stock solution daily.
\5\ Section 7.11--prepared in nonane and added to extract prior to cleanup.
\6\ Section 7.12--prepared in nonane and added to the concentrated extract immediately prior to injection into
  the GC (Section 14.2).


  Table 4--Concentration of CDDS/CDFS in Calibration and Calibration Verification Solutions \1\ (Section 15.3)
----------------------------------------------------------------------------------------------------------------
                                                   CDD/CDF    CS2 (ng/mL)  CS3 (ng/mL)  CS4 (ng/mL)  CS5 (ng/mL)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD..................................           0.5            2           10           40          200
2,3,7,8-TCDF..................................           0.5            2           10           40          200
1,2,3,7,8-PeCDD...............................           2.5           10           50          200         1000
1,2,3,7,8-PeCDF...............................           2.5           10           50          200         1000
2,3,4,7,8-PeCDF...............................           2.5           10           50          200         1000
1,2,3,4,7,8-HxCDD.............................           2.5           10           50          200         1000
1,2,3,6,7,8-HxCDD.............................           2.5           10           50          200         1000
1,2,3,7,8,9-HxCDD.............................           2.5           10           50          200         1000
1,2,3,4,7,8-HxCDF.............................           2.5           10           50          200         1000
1,2,3,6,7,8-HxCDF.............................           2.5           10           50          200         1000
1,2,3,7,8,9-HxCDF.............................           2.5           10           50          200         1000
2,3,4,6,7,8-HxCDF.............................           2.5           10           50          200         1000
1,2,3,4,6,7,8-HpCDD...........................           2.5           10           50          200         1000
1,2,3,4,6,7,8-HpCDF...........................           2.5           10           50          200         1000
1,2,3,4,7,8,9-HpCDF...........................           2.5           10           50          200         1000
OCDD..........................................           5.0           20          100          400         2000
OCDF..........................................           5.0           20          100          400         2000
\13\ C12-2,3,7,8-TCDD.........................         100            100          100          100          100
\13\ C12-2,3,7,8-TCDF.........................         100            100          100          100          100
\13\ C12-1,2,3,7,8-PeCDD......................         100            100          100          100          100
\13\ C12-PeCDF................................         100            100          100          100          100
\13\ C12-2,3,4,7,8-PeCDF......................         100            100          100          100          100
\13\ C12-1,2,3,4,7,8-HxCDD....................         100            100          100          100          100
\13\ C12-1,2,3,6,7,8-HxCDD....................         100            100          100          100          100
\13\ C12-1,2,3,4,7,8-HxCDF....................         100            100          100          100          100
\13\ C12-1,2,3,6,7,8-HxCDF....................         100            100          100          100          100
\13\ C12-1,2,3,7,8,9-HxCDF....................         100            100          100          100          100
\13\ C12-1,2,3,4,6,7,8-HpCDD..................         100            100          100          100          100
\13\ C12-1,2,3,4,6,7,8-HpCDF..................         100            100          100          100          100
\13\ C12-1,2,3,4,7,8,9-Hp CDF.................         100            100          100          100          100
\13\ C12-OCDD.................................         200            200          200          200          200
Cleanup Standard:
    \37\ C14-2,3,7,8-TCDD.....................           0.5            2           10           40          200
Internal Standards:
\13\ C12-1,2,3,4-TCDD.........................         100            100          100          100          100
\13\ C12-1,2,3,7,8,9-HxCDD....................         100            100          100          100          100
----------------------------------------------------------------------------------------------------------------


     Table 5--GC Retention Time Window Defining Solution and Isomer Specificity Test Standard (Section 7.15)
----------------------------------------------------------------------------------------------------------------
                             DB-5 column GC retention-time window defining solution
-----------------------------------------------------------------------------------------------------------------
               CDD/CDF                                First eluted                          Last eluted
----------------------------------------------------------------------------------------------------------------
TCDF.................................  1,3,6,8-..................................  1,2,8,9-
TCDD.................................  1,3,6,8-..................................  1,2,8,9-
PeCDF................................  1,3,4,6,8-................................  1,2,3,8,9-
PeCDD................................  1,2,4,7,9-................................  1,2,3,8,9-
HxCDF................................  1,2,3,4,6,8-..............................  1,2,3,4,8,9-
HxCDD................................  1,2,4,6,7,9-..............................  1,2,3,4,6,7-
HpCDF................................  1,2,3,4,6,7,8-............................  1,2,3,4,7,8,9-
HpCDD................................  1,2,3,4,6,7,9-............................  1,2,3,4,6,7,8-
----------------------------------------------------------------------------------------------------------------


               DB-5 Column TCDD Specificity Test Standard
 
                         1,2,3,7 = 1,2,3,8-TCDD
                              2,3,7,8-TCDD
                              1,2,3,9-TCDD
 
           DB-225 Column TCDF Isomer Specificity Test Standard
 
                              2,3,4,7-TCDF
                              2,3,7,8-TCDF
                              1,2,3,9-TCDF
 


[[Page 337]]


              Table 6--Acceptance Criteria for Performance Tests When All CDDS/CDFS Are Tested \1\
----------------------------------------------------------------------------------------------------------------
                                                                   IPR \2 3\
                  CDD/CDF                     Test conc. ----------------------------  OPR (ng/mL)   VER (ng/mL)
                                               (ng/mL)      s (ng/mL)     X (ng/mL)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD...............................           10           2.8  8.3-12.9      6.7-15.8      7.8-12.9
2,3,7,8-TCDF...............................           10           2.0  8.7-13.7      7.5-15.8      8.4-12.0
1,2,3,7,8-PeCDD............................           50           7.5    38-66         35-71         39-65
1,2,3,7,8-PeCDF............................           50           7.5    43-62         40-67         41-60
2,3,4,7,8-PeCDF............................           50           8.6    36-75         34-80         41-61
1,2,3,4,7,8-HxCDD..........................           50           9.4    39-76         35-82         39-64
1,2,3,6,7,8-HxCDD..........................           50           7.7    42-62         38-67         39-64
1,2,3,7,8,9-HxCDD..........................           50          11.1    37-71         32-81         41-61
1,2,3,4,7,8-HxCDF..........................           50           8.7    41-59         36-67         45-56
1,2,3,6,7,8-HxCDF..........................           50           6.7    46-60         42-65         44-57
1,2,3,7,8,9-HxCDF..........................           50           6.4    42-61         39-65         45-56
2,3,4,6,7,8-HxCDF..........................           50           7.4    37-74         35-78         44-57
1,2,3,4,6,7,8-HpCDD........................           50           7.7    38-65         35-70         43-58
1,2,3,4,6,7,8-HpCDF........................           50           6.3    45-56         41-61         45-55
1,2,3,4,7,8,9-HpCDF........................           50           8.1    43-63         39-69         43-58
OCDD.......................................          100          19     89-127        78-144        79-126
OCDF.......................................          100          27     74-146        63-170        63-159
\13\C12-2,3,7,8-TCDD.......................          100          37     28-134        20-175        82-121
\13\C12-2,3,7,8-TCDF.......................          100          35     31-113        22-152        71-140
\13\C12-1,2,3,7,8-PeCDD....................          100          39     27-184        21-227        62-160
\13\C12-1,2,3,7,8-PeCDF....................          100          34     27-156        21-192        76-130
\13\C12-2,3,4,7,8-PeCDF....................          100          38     16-279        13-328        77-130
\13\C12-1,2,3,4,7,8-HxCDD..................          100          41     29-147        21-193        85-117
\13\C12-1,2,3,6,7,8-HxCDD..................          100          38     34-122        25-163        85-118
\13\C12-1,2,3,4,7,8-HxCDF..................          100          43     27-152        19-202        76-131
\13\C12-1,2,3,6,7,8-HxCDF..................          100          35     30-122        21-159        70-143
\13\C12-1,2,3,7,8,9-HxCDF..................          100          40     24-157        17-205        74-135
\13\C12-2,3,4,6,7,8,-HxCDF.................          100          37     29-136        22-176        73-137
\13\C12-1,2,3,4,6,7,8-HpCDD................          100          35     34-129        26-166        72-138
\13\C12-1,2,3,4,6,7,8-HpCDF................          100          41     32-110        21-158        78-129
\13\C12-1,2,3,4,7,8,9-HpCDF................          100          40     28-141        20-186        77-129
\13\C12-OCDD...............................          200          95     41-276        26-397        96-415
\37\Cl4-2,3,7,8-TCDD.......................           10           3.6  3.9-15.4      3.1-19.1      7.9-12.7
----------------------------------------------------------------------------------------------------------------
\1\ All specifications are given as concentration in the final extract, assuming a 20 [micro]L volume.
\2\ s = standard deviation of the concentration.
\3\ X = average concentration.


          Table 6a--Acceptance Criteria for Performance Tests When Only Tetra Compounds are Tested \1\
----------------------------------------------------------------------------------------------------------------
                                                                   IPR \2 3\
                   CDD/CDF                     Test Conc. ---------------------------  OPR (ng/mL)   VER (ng/mL)
                                                (ng/mL)     s (ng/mL)     X (ng/mL)
----------------------------------------------------------------------------------------------------------------
2,3,7,8-TCDD................................           10          2.7  8.7-12.4      7.314.6       8.2-12.3
2,3,7,8-TCDF................................           10          2.0  9.1-13.1      8.0-14.7      8.6-11.6
\13\C12-2,3,7,8-TCDD........................          100           35   32-115        25-141        85-117
\13\C12-2,3,7,8-TCDF........................          100           34    35-99        26-126        76-131
\37\Cl4-2,3,7,8-TCDD........................           10          3.4  4.5-13.4      3.7-15.8      8.3-12.1
----------------------------------------------------------------------------------------------------------------
\1\ All specifications are given as concentration in the final extract, assuming a 20 [micro]L volume.
\2\ s = standard deviation of the concentration.
\3\ X = average concentration.


  Table 7--Labeled Compounds Recovery in Samples When all CDDS/CDFS are
                                 Tested
------------------------------------------------------------------------
                                               Labeled compound recovery
            Compound               Test conc. --------------------------
                                    (ng/mL)     (ng/mL) \1\      (%)
------------------------------------------------------------------------
\13\C12-2,3,7,8-TCDD............          100   25-164            25-164
\13\C12-2,3,7,8-TCDF............          100   24-169            24-169
\13\C12-1,2,3,7,8-PeCDD.........          100   25-181            25-181
\13\C12-1,2,3,7,8-PeCDF.........          100   24-185            24-185
\13\C12-2,3,4,7,8-PeCDF.........          100   21-178            21-178
\13\C12-1,2,3,4,7,8-HxCDD.......          100   32-141            32-141
\13\C12-1,2,3,6,7,8-HxCDD.......          100   28-130            28-130
\13\C12-1,2,3,4,7,8-HxCDF.......          100   26-152            26-152
\13\C12-1,2,3,6,7,8-HxCDF.......          100   26-123            26-123

[[Page 338]]

 
\13\C12-1,2,3,7,8,9-HxCDF.......          100   29-147            29-147
\13\C12-2,3,4,6,7,8-HxCDF.......          100   28-136            28-136
\13\C12-1,2,3,4,6,7,8-HpCDD.....          100   23-140            23-140
\13\C12-1,2,3,4,6,7,8-HpCDF.....          100   28-143            28-143
\13\C12-1,2,3,4,7,8,9-HpCDF.....          100   26-138            26-138
\13\C12-OCDD....................          200   34-313            17-157
\37\Cl4-2,3,7,8-TCDD............           10  3.5-19.7           35-197
------------------------------------------------------------------------
\1\ Specification given as concentration in the final extract, assuming
  a 20-[micro]L volume.


Table 7a--Labeled Compound Recovery in Samples When Only Tetra Compounds
                               are Tested
------------------------------------------------------------------------
                                               Labeled compound recovery
            Compound               Test conc. --------------------------
                                    (ng/mL)     (ng/mL) \1\      (%)
------------------------------------------------------------------------
\13\C12-2,3,7,8-TCDD............          100   31-137            31-137
\13\C12-2,3,7,8-TCDF............          100   29-140            29-140
\37\Cl4-2,3,7,8-TCDD............           10  4.2-16.4           42-164
------------------------------------------------------------------------
\1\ Specification given as concentration in the final extract, assuming
  a 20 [micro]L volume.


          Table 8--Descriptors, Exact M/Z's, M/Z Types, and Elemental Compositions of the CDDs and CDFs
----------------------------------------------------------------------------------------------------------------
                            Exact M/Z
        Descriptor             \1\               M/Z type            Elemental composition       Substance \2\
----------------------------------------------------------------------------------------------------------------
1........................     292.9825  Lock                       C7F11....................  PFK
                              303.9016  M                          C12H4\35\Cl4O............  TCDF
                              305.8987  M = 2                      C12H4\35\Cl3\37\ClO......  TCDF
                              315.9419  M                          \13\C12H4\35\Cl4O........  TCDF \3\
                              317.9389  M = 2                      \13\C12H4\35\Cl3\37\ClO..  TCDF \3\
                              319.8965  M                          C12H4\35\Cl4O2...........  TCDD
                              321.8936  M = 2                      C12H4\35\Cl3\37\ClO2.....  TCDD
                              327.8847  M                          C12H4\37\Cl4O2...........  TCDD \4\
                              330.9792  QC                         C7F13....................  PFK
                              331.9368  M                          \13\C12H4\35\Cl4O2.......  TCDD \3\
                              333.9339  M = 2                      \13\C12H4\35\Cl3\37\ClO2.  TCDD \3\
                              375.8364  M = 2                      C12H4\35\Cl5\37\ClO......  HxCDPE
2........................     339.8597  M = 2                      C12H3\35\Cl4\37\ClO......  PeCDF
                              341.8567  M = 4                      C12H3\35\Cl3\37\Cl2O.....  PeCDF
                              351.9000  M = 2                      \13\C12H3\35\Cl4\37\ClO..  PeCDF
                              353.8970  M = 4                      \13\C12H3\35\Cl3\37\Cl2O.  PeCDF \3\
                              354.9792  Lock                       C9F13....................  PFK
                              355.8546  M = 2                      C12H3\35\Cl4\37\ClO2.....  PeCDD
                              357.8516  M = 4                      C12H3\35\Cl3\37\Cl2O2....  PeCDD
                              367.8949  M = 2                      \13\C12H3\35\Cl4\37\ClO2.  PeCDD \3\
                              369.8919  M = 4                      \13\C12H3\35\Cl3\37\Cl2O2  PeCDD \3\
                              409.7974  M = 2                      C12H3\35\Cl6\37\ClO......  HpCDPE
3........................     373.8208  M = 2                      C12H2\35\Cl5\37\ClO......  HxCDF
                              375.8178  M = 4                      C12H2\35\Cl4\37\Cl2O.....  HxCDF
                              383.8639  M                          \13\C12H2\35\Cl6O........  HxCDF \3\
                              385.8610  M = 2                      \13\C12H2\35\Cl5\37\ClO..  HxCDF \3\
                              389.8157  M = 2                      C12H2\35\Cl5\37\ClO2.....  HxCDD
                              391.8127  M = 4                      C12H2\35\Cl4\37\Cl2O2....  HxCDD
                              392.9760  Lock                       C9F15....................  PFK
                              401.8559  M = 2                      \13\C12H2\35\Cl5\37\ClO2.  HxCDD \3\
                              403.8529  M = 4                      \13\C12H2\35\Cl4\37\Cl2O2  HxCDD \3\
                              430.9729  QC                         C9F17....................  PFK
                              445.7555  M = 4                      C12H2\35\Cl6\37\Cl2O.....  OCDPE
4........................     407.7818  M = 2                      C12H\35\Cl6\37\ClO.......  HpCDF
                              409.7789  M = 4                      C12H\35\Cl5\37\Cl2O......  HpCDF
                              417.8253  M                          \13\C12H\35\Cl7O.........  HpCDF \3\
                              419.8220  M = 2                      \13\C12H\35\Cl6\37\ClO...  HpCDF \3\
                              423.7766  M = 2                      C12H\35\Cl6\37\ClO2......  HpCDD
                              425.7737  M = 4                      C12H\35\Cl5\37\Cl2O2.....  HpCDD

[[Page 339]]

 
                              430.9729  Lock                       C9F17....................  PFK
                              435.8169  M = 2                      \13\C12H\35\Cl6\37\ClO2..  HpCDD \3\
                              437.8140  M = 4                      \13\C12H\35\Cl5\37\Cl2O2.  HpCDD \3\
                              479.7165  M = 4                      C12H\35\Cl7\37\Cl2O......  NCDPE
5........................     441.7428  M = 2                      C12\35\Cl7\37\ClO........  OCDF
                              442.9728  Lock                       C10F17...................  PFK
                              443.7399  M = 4                      C12\35\Cl6\37\Cl2O.......  OCDF
                              457.7377  M = 2                      C12\35\Cl7\37\ClO2.......  OCDD
                              459.7348  M = 4                      C12\35\Cl6\37\Cl2O2......  OCDD
                              469.7779  M = 2                      \13\C12\35\Cl7\37\ClO2...  OCDD \3\
                              471.7750  M = 4                      \13\C12\35\Cl6\37\Cl2O2..  OCDD \3\
                              513.6775  M = 4                      C12\35\Cl8\37\Cl2O.......  DCDPE
----------------------------------------------------------------------------------------------------------------
\1\ Nuclidic masses used:
 H = 1.007825.
 O = 15.994915.
 C = 12.00000.
 \35\Cl = 34.968853.
 \13\C = 13.003355.
 \37\Cl = 36.965903.
 F = 18.9984.
\2\ TCDD = Tetrachlorodibenzo-p-dioxin.
 PeCDD = Pentachlorodibenzo-p-dioxin.
 HxCDD = Hexachlorodibenzo-p-dioxin.
 HpCDD = Heptachlorodibenzo-p-dioxin.
 OCDD = Octachlorodibenzo-p-dioxin.
 HxCDPE = Hexachlorodiphenyl ether.
 OCDPE = Octachlorodiphenyl ether.
 DCDPE = Decachlorodiphenyl ether.
 TCDF = Tetrachlorodibenzofuran.
 PeCDF = Pentachlorodibenzofuran.
 HxCDF = Hexachlorodibenzofuran.
 HpCDF = Heptachlorodibenzofuran.
 OCDF = Octachlorodibenzofuran.
 HpCDPE = Heptachlorodiphenyl ether.
 NCDPE = Nonachlorodiphenyl ether.
 PFK = Perfluorokerosene.
\3\ Labeled compound.
\4\ There is only one m/z for \37\Cl4-2,3,7,8,-TCDD (cleanup standard).


                             Table 9--Theoretical Ion Abundance Ratios and QC Limits
----------------------------------------------------------------------------------------------------------------
                                                                                              QC limit \1\
        Number of chlorine atoms                M/Z's forming ratio        Theoretical -------------------------
                                                                              ratio        Lower        Upper
----------------------------------------------------------------------------------------------------------------
4 \2\...................................  M/(M = 2)......................         0.77         0.65         0.89
5.......................................  (M = 2)/(M = 4)................         1.55         1.32         1.78
6.......................................  (M = 2)/(M = 4)................         1.24         1.05         1.43
6 \3\...................................  M/(M = 2)......................         0.51         0.43         0.59
7.......................................  (M = 2)/(M = 4)................         1.05         0.88         1.20
7 \4\...................................  M/(M = 2)......................         0.44         0.37         0.51
8.......................................  (M = 2)/(M = 4)................         0.89         0.76         1.02
----------------------------------------------------------------------------------------------------------------
\1\ QC limits represent 15% windows around the theoretical ion abundance ratios.
\2\ Does not apply to \37\Cl4-2,3,7,8-TCDD (cleanup standard).
\3\ Used for \13\C12-HxCDF only.
\4\ Used for \13\C12-HpCDF only.


                 Table 10--Suggested Sample Quantities To Be Extracted for Various Matrices \1\
----------------------------------------------------------------------------------------------------------------
                                                                                                    Quantity
        Sample Matrix \2\                 Example        Percent solids          Phase             extracted
----------------------------------------------------------------------------------------------------------------
Single-phase:
    Aqueous......................  Drinking water......              <1  (\3\)...............  1000 mL.
                                   Groundwater
                                   Treated wastewater
    Solid........................  Dry soil............   20  Solid...............  10 g.
                                   Compost
                                   Ash
    Organic......................  Waste solvent.......              <1  Organic.............  10 g.
                                   Waste oil
                                   Organic polymer
    Tissue.......................  Fish................  ..............  Organic.............  10 g.
                                   Human adipose

[[Page 340]]

 
Multi-phase:
    Liquid/Solid:
        Aqueous/Solid............  Wet soil............            1-30  Solid...............  10 g.
                                   Untreated effluent..
                                   Digested municipal
                                    sludge.
                                   Filter cake.........
                                   Paper pulp..........
        Organic/solid............  Industrial sludge...           1-100  Both................  10 g.
                                   Oily waste
    Liquid/Liquid:
        Aqueous/organic..........  In-process effluent.              <1  Organic.............  10 g.
                                   Untreated effluent
                                   Drum waste
        Aqueous/organic/solid....  Untreated effluent..    1  Organic and solid...  10 g.
                                   Drum waste
----------------------------------------------------------------------------------------------------------------
\1\ The quantity of sample to be extracted is adjusted to provide 10 g of solids (dry weight). One liter of
  aqueous samples containing 1% solids will contain 10 g of solids. For aqueous samples containing greater than
  1% solids, a lesser volume is used so that 10 g of solids (dry weight) will be extracted.
\2\ The sample matrix may be amorphous for some samples. In general, when the CDDs/CDFs are in contact with a
  multiphase system in which one of the phases is water, they will be preferentially dispersed in or adsorbed on
  the alternate phase because of their low solubility in water.
\3\ Aqueous samples are filtered after spiking with the labeled compounds. The filtrate and the materials
  trapped on the filter are extracted separately, and the extracts are combined for cleanup and analysis.


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                24.0 Glossary of Definitions and Purposes

    These definitions and purposes are specific to this method but have 
been conformed to common usage as much as possible.
    24.1 Units of weight and Measure and Their Abbreviations.
    24.1.1 Symbols:

[deg]C--degrees Celsius
[micro]L--microliter
[micro]m--micrometer
<--less than
--greater than
%--percent

24.1.2 Alphabetical abbreviations:

amp--ampere
cm--centimeter
g--gram
h--hour
D--inside diameter
in.--inch
L--liter
M--Molecular ion
m--meter
mg--milligram
min--minute
mL--milliliter
mm--millimeter
m/z--mass-to-charge ratio

[[Page 348]]

N--normal; gram molecular weight of solute divided by hydrogen 
          equivalent of solute, per liter of solution
OD--outside diameter
pg--picogram
ppb--part-per-billion
ppm--part-per-million
ppq--part-per-quadrillion
ppt--part-per-trillion
psig--pounds-per-square inch gauge
v/v--volume per unit volume
w/v--weight per unit volume

    24.2 Definitions and Acronyms (in Alphabetical Order).
    Analyte--A CDD or CDF tested for by this method. The analytes are 
listed in Table 1.
    Calibration Standard (CAL)--A solution prepared from a secondary 
standard and/or stock solutions and used to calibrate the response of 
the instrument with respect to analyte concentration.
    Calibration Verification Standard (VER)--The mid-point calibration 
standard (CS3) that is used in to verify calibration. See Table 4.
    CDD--Chlorinated Dibenzo-p-ioxin--The isomers and congeners of 
tetra-through octa-chlorodibenzo-p-dioxin.
    CDF--Chlorinated Dibenzofuran--The isomers and congeners of tetra-
through octa-chlorodibenzofuran.
    CS1, CS2, CS3, CS4, CS5--See Calibration standards and Table 4.
    Field Blank--An aliquot of reagent water or other reference matrix 
that is placed in a sample container in the laboratory or the field, and 
treated as a sample in all respects, including exposure to sampling site 
conditions, storage, preservation, and all analytical procedures. The 
purpose of the field blank is to determine if the field or sample 
transporting procedures and environments have contaminated the sample.
    GC--Gas chromatograph or gas chromatography.
    GPC--Gel permeation chromatograph or gel permeation chromatography.
    HPLC--High performance liquid chromatograph or high performance 
liquid chromatography.
    HRGC--High resolution GC.
    HRMS--High resolution MS.
    IPR--Initial precision and recovery; four aliquots of the diluted 
PAR standard analyzed to establish the ability to generate acceptable 
precision and accuracy. An IPR is performed prior to the first time this 
method is used and any time the method or instrumentation is modified.
    K-D--Kuderna-Danish concentrator; a device used to concentrate the 
analytes in a solvent.
    Laboratory Blank--See method blank.
    Laboratory Control sample (LCS)--See ongoing precision and recovery 
standard (OPR).
    Laboratory Reagent Blank--See method blank.
    May--This action, activity, or procedural step is neither required 
nor prohibited.
    May Not--This action, activity, or procedural step is prohibited.
    Method Blank--An aliquot of reagent water that is treated exactly as 
a sample including exposure to all glassware, equipment, solvents, 
reagents, internal standards, and surrogates that are used with samples. 
The method blank is used to determine if analytes or interferences are 
present in the laboratory environment, the reagents, or the apparatus.
    Minimum Level (ML)--The level at which the entire analytical system 
must give a recognizable signal and acceptable calibration point for the 
analyte. It is equivalent to the concentration of the lowest calibration 
standard, assuming that all method-specified sample weights, volumes, 
and cleanup procedures have been employed.
    MS--Mass spectrometer or mass spectrometry.
    Must--This action, activity, or procedural step is required.
    OPR--Ongoing precision and recovery standard (OPR); a laboratory 
blank spiked with known quantities of analytes. The OPR is analyzed 
exactly like a sample. Its purpose is to assure that the results 
produced by the laboratory remain within the limits specified in this 
method for precision and recovery.
    PAR--Precision and recovery standard; secondary standard that is 
diluted and spiked to form the IPR and OPR.
    PFK--Perfluorokerosene; the mixture of compounds used to calibrate 
the exact m/z scale in the HRMS.
    Preparation Blank--See method blank.
    Primary Dilution Standard--A solution containing the specified 
analytes that is purchased or prepared from stock solutions and diluted 
as needed to prepare calibration solutions and other solutions.
    Quality Control Check Sample (QCS)--A sample containing all or a 
subset of the analytes at known concentrations. The QCS is obtained from 
a source external to the laboratory or is prepared from a source of 
standards different from the source of calibration standards. It is used 
to check laboratory performance with test materials prepared external to 
the normal preparation process.
    Reagent Water--Water demonstrated to be free from the analytes of 
interest and potentially interfering substances at the method detection 
limit for the analyte.
    Relative Standard Deviation (RSD)--The standard deviation times 100 
divided by the mean. Also termed ``coefficient of variation.''
    RF--Response factor. See Section 10.6.1.
    RR--Relative response. See Section 10.5.2.
    RSD--See relative standard deviation.

[[Page 349]]

    SDS--Soxhlet/Dean-Stark extractor; an extraction device applied to 
the extraction of solid and semi-solid materials (Reference 7).
    Should--This action, activity, or procedural step is suggested but 
not required.
    SICP--Selected ion current profile; the line described by the signal 
at an exact m/z.
    SPE--Solid-phase extraction; an extraction technique in which an 
analyte is extracted from an aqueous sample by passage over or through a 
material capable of reversibly adsorbing the analyte. Also termed 
liquid-solid extraction.
    Stock Solution--A solution containing an analyte that is prepared 
using a reference material traceable to EPA, the National Institute of 
Science and Technology (NIST), or a source that will attest to the 
purity and authenticity of the reference material.
    TCDD--Tetrachlorodibenzo-p-dioxin.
    TCDF--Tetrachlorodibenzofuran.
    VER--See calibration verification standard.

 Method 1624 Revision B--Volatile Organic Compounds by Isotope Dilution 
                                  GC/MS

                        1. Scope and Application

    1.1 This method is designed to determine the volatile toxic organic 
pollutants associated with the 1976 Consent Decree and additional 
compounds amenable to purge and trap gas chromatography-mass 
spectrometry (GC/MS).
    1.2 The chemical compounds listed in table 1 may be determined in 
municipal and industrial discharges by this method. The methmd is 
designed to meet the survey requirements of Effluent Guidelines Division 
(EGD) and the National Pollutants Discharge Elimination System (NPDES) 
under 40 CFR 136.1 and 136.5. Any modifications of this method, beyond 
those expressly permitted, shall be considered as major modifications 
subject to application and approval of alternate test procedures under 
40 CFR 136.4 and 136.5.
    1.3 The detection limit of this method is usually dependent on the 
level of interferences rather than instrumental limitations. The limits 
in table 2 represent the minimum quantity that can be detected with no 
interferences present.
    1.4 The GC/MS portions of this method are for use only by analysts 
experienced with GC/MS or under the close supervision of such qualified 
persons. Laboratories unfamiliar with the analyses of environmental 
samples by GC/MS should run the performance tests in reference 1 before 
beginning.

                          2. Summary of Method

    2.1 Stable isotopically labeled analogs of the compounds of interest 
are added to a 5 mL water sample. The sample is purged at 20-25 [deg]C 
with an inert gas in a specially designed chamber. The volatile organic 
compounds are transferred from the aqueous phase into the gaseous phase 
where they are passed into a sorbent column and trapped. After purging 
is completed, the trap is backflushed and heated rapidly to desorb the 
compounds into a gas chromatograph (GC). The compounds are separated by 
the GC and detected by a mass spectrometer (MS) (references 2 and 3). 
The labeled compounds serve to correct the variability of the analytical 
technique.
    2.2 Identification of a compound (qualitative analysis) is performed 
by comparing the GC retention time and the background corrected 
characteristic spectral masses with those of authentic standards.
    2.3 Quantitative analysis is performed by GC/MS using extracted ion 
current profile (EICP) areas. Isotope dilution is used when labeled 
compounds are available; otherwise, an internal standard method is used.
    2.4 Quality is assured through reproducible calibration and testing 
of the purge and trap and GC/MS systems.

                   3. Contamination and Interferences

    3.1 Impurities in the purge gas, organic compounds out-gassing from 
the plumbing upstream of the trap, and solvent vapors in the laboratory 
account for the majority of contamination problems. The analytical 
system is demonstrated to be free from interferences under conditions of 
the analysis by analyzing blanks initially and with each sample lot 
(samples analyzed on the same 8 hr shift), as described in Section 8.5.
    3.2 Samples can be contaminated by diffusion of volatile organic 
compounds (particularly methylene chloride) through the bottle seal 
during shipment and storage. A field blank prepared from reagent water 
and carried through the sampling and handling protocol serves as a check 
on such contamination.
    3.3 Contamination by carry-over can occur when high level and low 
level samples are analyzed sequentially. To reduce carry-over, the 
purging device and sample syringe are rinsed between samples with 
reagent water. When an unusually concentrated sample is encountered, it 
is followed by analysis of a reagent water blank to check for carry-
over. For samples containing large amounts of water soluble materials, 
suspended solids, high boiling compounds, or high levels or purgeable 
compounds, the purge device is washed with soap solution, rinsed with 
tap and distilled water, and dried in an oven at 100-125 [deg]C. The 
trap and other parts of the system are also subject to contamination; 
therefore, frequent bakeout and purging of the entire system may be 
required.
    3.4 Interferences resulting from samples will vary considerably from 
source to source, depending on the diversity of the industrial complex 
or municipality being sampled.

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                                4. Safety

    4.1 The toxicity or carcinogenicity of each compound or reagent used 
in this method has not been precisely determined; however, each chemical 
compound should be treated as a potential health hazard. Exposure to 
these compounds should be reduced to the lowest possible level. The 
laboratory is responsible for maintaining a current awareness file of 
OSHA regulations regarding the safe handling of the chemicals specified 
in this method. A reference file of data handling sheets should also be 
made available to all personnel involved in these analyses. Additional 
information on laboratory safety can be found in references 4-6.
    4.2 The following compounds covered by this method have been 
tentatively classified as known or suspected human or mammalian 
carcinogens: benzene, carbon tetrachloride, chloroform, and vinyl 
chloride. Primary standards of these toxic compounds should be prepared 
in a hood, and a NIOSH/MESA approved toxic gas respirator should be worn 
when high concentrations are handled.

                       5. Apparatus and Materials

    5.1 Sample bottles for discrete sampling.
    5.1.1 Bottle--25 to 40 mL with screw cap (Pierce 13075, or 
equivalent). Detergent wash, rinse with tap and distilled water, and dry 
at 105 [deg]C for one hr minimum before use.
    5.1.2 Septum--Teflon-faced silicone (Pierce 12722, or equivalent), 
cleaned as above and baked at 100-200 [deg]C, for one hour minimum.
    5.2 Purge and trap device--consists of purging device, trap, and 
desorber. Complete devices are commercially available.
    5.2.1 Purging device--designed to accept 5 mL samples with water 
column at least 3 cm deep. The volume of the gaseous head space between 
the water and trap shall be less than 15 mL. The purge gas shall be 
introduced less than 5 mm from the base of the water column and shall 
pass through the water as bubbles with a diameter less than 3 mm. The 
purging device shown in Figure 1 meets these criteria.
    5.2.2 Trap--25 to 30 cm x 2.5 mm i.d. minimum, containing the 
following:
    5.2.2.1 Methyl silicone packing--one 0.2 cm, 3 
percent OV-1 on 60/80 mesh Chromosorb W, or equivalent.
    5.2.2.2 Porous polymer--15 1.0 cm, Tenax GC 
(2,6-diphenylene oxide polymer), 60/80 mesh, chromatographic grade, or 
equivalent.
    5.2.2.3 Silica gel--8 1.0 cm, Davison 
Chemical, 35/60 mesh, grade 15, or equivalent. The trap shown in Figure 
2 meets these specifications.
    5.2.3 Desorber--shall heat the trap to 175 5 
[deg]C in 45 seconds or less. The polymer section of the trap shall not 
exceed 180 [deg]C, and the remaining sections shall not exceed 220 
[deg]C. The desorber shown in Figure 2 meets these specifications.
    5.2.4 The purge and trap device may be a separate unit or coupled to 
a GC as shown in Figures 3 and 4.
    5.3 Gas chromatograph--shall be linearly temperature programmable 
with initial and final holds, shall contain a glass jet separator as the 
MS interface, and shall produce results which meet the calibration 
(Section 7), quality assurance (Section 8), and performance tests 
(Section 11) of this method.
    5.3.1 Column--2.8 0.4 m x 2 0.5 mm i. d. glass, packekd with one percent SP-1000 on 
Carbopak B, 60/80 mesh, or equivalent.
    5.4 Mass spectrometer--70 eV electron impact ionization; shall 
repetitively scan from 20 to 250 amu every 2-3 seconds, and produce a 
unit resolution (valleys between m/z 174-176 less than 10 percent of the 
height of the m/z 175 peak), background corrected mass spectrum from 50 
ng 4-bromo-fluorobenzene (BFB) injected into the GC. The BFB spectrum 
shall meet the mass-intensity criteria in Table 3. All portions of the 
GC column, transfer lines, and separator which connect the GC column to 
the ion source shall remain at or above the column temperature during 
analysis to preclude condensation of less volatile compounds.
    5.5 Data system--shall collect and record MS data, store mass 
intensity data in spectral libraries, process GC/MS data and generate 
reports, and shall calculate and record response factors.
    5.5.1 Data acquisition--mass spectra shall be collected continuously 
throughout the analysis and stored on a mass storage device.
    5.5.2 Mass spectral libraries--user created libraries containing 
mass spectra obtained from analysis of authentic standards shall be 
employed to reverse search GC/MS runs for the compounds of interest 
(Section 7.2).
    5.5.3 Data processing--the data system shall be used to search, 
locate, identify, and quantify the compounds of interest in each GC/MS 
analysis. Software routines shall be employed to compute retention times 
and EICP areas. Displays of spectra, mass chromatograms, and library 
comparisons are required to verify results.
    5.5.4 Response factors and multipoint calibrations--the data system 
shall be used to record and maintain lists of response factors (response 
ratios for isotope dilution) and generate multi-point calibration curves 
(Section 7). Computations of relative standard deviation (coefficient of 
variation) are useful for testing calibration linearity. Statistics on 
initial and on-going performance shall be maintained (Sections 8 and 
11).
    5.6 Syringes--5 mL glass hypodermic, with Luer-lok tips.
    5.7 Micro syringes--10, 25, and 100 uL.
    5.8 Syringe valves--2-way, with Luer ends (Telfon or Kel-F).

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    5.9 Syringe--5 mL, gas-tight, with shut-off valve.
    5.10 Bottles--15 mL., screw-cap with Telfon liner.
    5.11 Balance--analytical, capable of weighing 0.1 mg.

                        6. Reagents and Standards

    6.1 Reagent water--water in which the compounds of interest and 
interfering compounds are not detected by this method (Section 11.7). It 
may be generated by any of the following methods:
    6.1.1 Activated carbon--pass tap water through a carbon bed (Calgon 
Filtrasorb-300, or equivalent).
    6.1.2 Water purifier--pass tap water through a purifier (Millipore 
Super Q, or equivalent).
    6.1.3 Boil and purge--heat tap water to 90-100 [deg]C and bubble 
contaminant free inert gas through it for approx one hour. While still 
hot, transfer the water to screw-cap bottles and seal with a Teflon-
lined cap.
    6.2 Sodium thiosulfate--ACS granular.
    6.3 Methanol--pesticide quality or equivalent.
    6.4 Standard solutions--purchased as solution or mixtures with 
certification to their purity, concentration, and authenticity, or 
prepared from materials of known purity and composition. If compound 
purity is 96 percent or greater, the weight may be used without 
correction to calculate the concentration of the standard.
    6.5 Preparation of stock solutions--prepare in methanol using liquid 
or gaseous standards per the steps below. Observe the safety precautions 
given in Section 4.
    6.5.1 Place approx 9.8 mL of methanol in a 10 mL ground glass 
stoppered volumetric flask. Allow the flask to stand unstoppered for 
approximately 10 minutes or until all methanol wetted surfaces have 
dried. In each case, weigh the flask, immediately add the compound, then 
immediately reweigh to prevent evaporation losses from affecting the 
measurement.
    6.5.1.1 Liquids--using a 100 [micro]L syringe, permit 2 drops of 
liquid to fall into the methanol without contacting the leck of the 
flask. Alternatively, inject a known volume of the compound into the 
methanol in the flask using a micro-syringe.
    6.5.1.2 Gases (chloromethane, bromomethane, chloroethane, vinyl 
chloride)--fill a valved 5 mL gas-tight syringe with the compound. Lower 
the needle to approximately 5 mm above the methanol meniscus. Slowly 
introduce the compound above the surface of the meniscus. The gas will 
dissolve rapidly in the methanol.
    6.5.2 Fill the flask to volume, stopper, then mix by inverting 
several times. Calculate the concentration in mg/mL ([micro]g/[micro]L) 
from the weight gain (or density if a known volume was injected).
    6.5.3 Transfer the stock solution to a Teflon sealed screw-cap-
bottle. Store, with minimal headspace, in the dark at -10 to -20 [deg]C.
    6.5.4 Prepare fresh standards weekly for the gases and 2-
chloroethylvinyl ether. All other standards are replaced after one 
month, or sooner if comparison with check standards indicate a change in 
concentration. Quality control check standards that can be used to 
determine the accuracy of calibration standards are available from the 
US Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio.
    6.6 Labeled compound spiking solution--from stock standard solutions 
prepared as above, or from mixtures, prepare the spiking solution to 
contain a concentration such that a 5-10 [micro]L spike into each 5 mL 
sample, blank, or aqueous standard analyzed will result in a 
concentration of 20 [micro]g/L of each labeled compound. For the gases 
and for the water soluble compounds (acrolein, acrylonitrile, acetone, 
diethyl ether, and MEK), a concentration of 100 [micro]g/L may be used. 
Include the internal standards (Section 7.5) in this solution so that a 
concentration of 20 [micro]g/L in each sample, blank, or aqueous 
standard will be produced.
    6.7 Secondary standards--using stock solutions, prepare a secondary 
standard in methanol to contain each pollutant at a concentration of 500 
[micro]g/mL For the gases and water soluble compounds (Section 6.6), a 
concentration of 2.5 mg/mL may be used.
    6.7.1 Aqueous calibration standards--using a 25 [micro]L syringe, 
add 20 [micro]L of the secondary standard (Section 6.7) to 50, 100, 200, 
500, and 1000 mL of reagent water to produce concentrations of 200, 100, 
50, 20, and 10 [micro]g/L, respectively. If the higher concentration 
standard for the gases and water soluble compounds was chosen (Section 
6.6), these compounds will be at concentrations of 1000, 500, 250, 100, 
and 50 [micro]g/L in the aqueous calibration standards.
    6.7.2 Aqueous performance standard--an aqueous standard containing 
all pollutants, internal standards, labeled compounds, and BFB is 
prepared daily, and analyzed each shift to demonstrate performance 
(Section 11). This standard shall contain either 20 or 100 [micro]g/L of 
the labeled and pollutant gases and water soluble compounds, 10 
[micro]g/L BFB, and 20 [micro]g/L of all other pollutants, labeled 
compounds, and internal standards. It may be the nominal 20 [micro]g/L 
aqueous calibration standard (Section 6.7.1).
    6.7.3 A methanolic standard containing all pollutants and internal 
standards is prepared to demonstrate recovery of these compounds when 
syringe injection and purge and trap analyses are compared. This 
standard shall contain either 100 [micro]g/mL or 500 [micro]g/mL of the 
gases and water soluble compounds, and 100 [micro]g/mL of the remaining 
pollutants

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and internal standards (consistent with the amounts in the aqueous 
performance standard in 6.7.2).
    6.7.4 Other standards which may be needed are those for test of BFB 
performance (Section 7.1) and for collection of mass spectra for storage 
in spectral libraries (Section 7.2).

                             7. Calibration

    7.1 Assemble the gas chromatographic apparatus and establish 
operating conditions given in table 2. By injecting standards into the 
GC, demonstrate that the analytical system meets the detection limits in 
table 2 and the mass-intensity criteria in table 3 for 50 ng BFB.
    7.2 Mass spectral libraries--detection and identification of the 
compound of interest are dependent upon the spectra stored in user 
created libraries.
    7.2.1 Obtain a mass spectrum of each pollutant and labeled compound 
and each internal standard by analyzing an authentic standard either 
singly or as part of a mixture in which there is no interference between 
closely eluted components. That only a single compound is present is 
determined by examination of the spectrum. Fragments not attributable to 
the compound under study indicate the presence of an interfering 
compound. Adjust the analytical conditions and scan rate (for this test 
only) to produce an undistorted spectrum at the GC peak maximum. An 
undistorted spectrum will usually be obtained if five complete spectra 
are collected across the upper half of the GC peak. Software algorithms 
designed to ``enhance'' the spectrum may eliminate distortion, but may 
also eliminate authentic m/z's or introduce other distortion.
    7.2.3 The authentic reference spectrum is obtained under BFB tuning 
conditions (Section 7.1 and table 3) to normalize it to spectra from 
other instruments.
    7.2.4 The spectrum is edited by saving the 5 most intense mass 
spectral peaks and all other mass spectral peaks greater than 10 percent 
of the base peak. This spectrum is stored for reverse search and for 
compound confirmation.
    7.3 Assemble the purge and trap device. Pack the trap as shown in 
Figure 2 and condition overnight at 170-180 [deg]C by backflushing with 
an inert gas at a flow rate of 20-30 mL/min. Condition traps daily for a 
minimum of 10 minutes prior to use.
    7.3.1 Analyze the aqueous performance standard (Section 6.7.2) 
according to the purge and trap procedure in Section 10. Compute the 
area at the primary m/z (table 4) for each compound. Compare these areas 
to those obtained by injecting one [micro]L of the methanolic standard 
(Section 6.7.3) to determine compound recovery. The recovery shall be 
greater than 20 percent for the water soluble compounds, and 60-110 
percent for all other compounds. This recovery is demonstrated initially 
for each purge and trap GC/MS system. The test is repeated only if the 
purge and trap or GC/MS systems are modified in any way that might 
result in a change in recovery.
    7.3.2 Demonstrate that 100 ng toluene (or toluene-d8) produces an 
area at m/z 91 (or 99) approx one-tenth that required to exceed the 
linear range of the system. The exact value must be determined by 
experience for each instrument. It is used to match the calibration 
range of the instrument to the analytical range and detection limits 
required.
    7.4 Calibration by isotope dilution--the isotope dilution approach 
is used for the purgeable organic compounds when appropriate labeled 
compounds are available and when interferences do not preclude the 
analysis. If labeled compounds are not available, or interferences are 
present, internal standard methods (Section 7.5 or 7.6) are used. A 
calibration curve encompassing the concentration range of interest is 
prepared for each compound determined. The relative response (RR) vs 
concentration ([micro]g/L) is plotted or computed using a linear 
regression. An example of a calibration curve for toluene using toluene-
d8 is given in figure 5. Also shown are the 10 
percent error limits (dotted lines). Relative response is determined 
according to the procedures described below. A minimum of five data 
points are required for calibration (Section 7.4.4).
    7.4.1 The relative response (RR) of pollutant to labeled compound is 
determined from isotope ratio values calculated from acquired data. 
Three isotope ratios are used in this process:

    RX = the isotope ratio measured in the pure pollutant 
(figure 6A).
    Ry = the isotope ratio of pure labeled compound (figure 
6B).
    Rm = the isotope ratio measured in the analytical mixture 
of the pollutant and labeled compounds (figure 6C).

    The correct way to calculate RR is: RR = (Ry-
Rm) (RX + 1)/(Rm-
RX)(Ry + 1) If Rm is not between 
2Ry and 0.5RX, the method does not apply and the 
sample is analyzed by internal or external standard methods (Section 7.5 
or 7.6).
    7.4.2 In most cases, the retention times of the pollutant and 
labeled compound are the same and isotope ratios (R's) can be calculated 
from the EICP areas, where: R = (area at m1/z)/(area at 
m2/z) If either of the areas is zero, it is assigned a value 
of one in the calculations; that is, if: area of m1/z = 
50721, and area of m2/z = 0, then R = 50721/1 = 50720. The m/
z's are always selected such that RXRy. 
When there is a difference in retention times (RT) between the pollutant 
and labeled compounds, special precautions are required to determine the 
isotope ratios.
    RX, Ry, and Rm are defined as 
follows:


[[Page 353]]


    RX=[area m1/z (at RT1)]/1
    Ry = 1/[area m2/z (at RT2)]
    Rm=[area m1/z (at RT1)]/[area 
m2/z (at RT2)]

    7.4.3 An example of the above calculations can be taken from the 
data plotted in figure 6 for toluene and toluene-d8. For these data, 
RX = 168920/1 = 168900, Ry = 1/60960 = 0.00001640, 
and Rm = 96868/82508 = 1.174. The RR for the above data is 
then calculated using the equation given in Section 7.4.1. For the 
example, RR = 1.174.
    Note: Not all labeled compounds elute before their pollutant 
analogs.
    7.4.4 To calibrate the analytical system by isotope dilution, 
analyze a 5 mL aliquot of each of the aqueous calibration standards 
(Section 6.7.1) spiked with an appropriate constant amount of the 
labeled compound spiking solution (Section 6.6), using the purge and 
trap procedure in section 10. Compute the RR at each concentration.
    7.4.5 Linearity--if the ratio of relative response to concentration 
for any compound is constant (less than 20 percent coefficient of 
variation) over the 5 point calibration range, an averaged relative 
response/concentration ratio may be used for that compound; otherwise, 
the complete calibration curve for that compound shall be used over the 
5 point calibration range.
    7.5 Calibration by internal standard--used when criteria for isotope 
dilution (Section 7.4) cannot be met. The method is applied to 
pollutants having no labeled analog and to the labeled compounds. The 
internal standards used for volatiles analyses are bromochloromethane, 
2-bromo-1-chloropropane, and 1,4-dichlorobutane. Concentrations of the 
labeled compounds and pollutants without labeled analogs are computed 
relative to the nearest eluted internal standard, as shown in table 2.
    7.5.1 Response factors--calibration requires the determination of 
response factors (RF) which are defined by the following equation:
    RF = (AsxCis)/(AisxCs), 
where As is the EICP area at the characteristic m/z for the 
compound in the daily standard. Ais is the EICP area at the 
characteristic m/z for the internal standard.
    Cis is the concentration (ug/L) of the internal standard
    Cs is the concentration of the pollutant in the daily 
standard.
    7.5.2 The response factor is determined at 10, 20, 50, 100, and 200 
ug/L for the pollutants (optionally at five times these concentrations 
for gases and water soluble pollutants--see Section 6.7), in a way 
analogous to that for calibration by isotope dilution (Section 7.4.4). 
The RF is plotted against concentration for each compound in the 
standard (Cs) to produce a calibration curve.
    7.5.3 Linearity--if the response factor (RF) for any compound is 
constant (less than 35 percent coefficient of variation) over the 5 
point calibration range, an averaged response factor may be used for 
that compound; otherwise, the complete calibration curve for that 
compound shall be used over the 5 point range.
    7.6 Combined calibration--by adding the isotopically labeled 
compounds and internal standards (Section 6.6) to the aqueous 
calibration standards (Section 6.7.1), a single set of analyses can be 
used to produce calibration curves for the isotope dilution and internal 
standard methods. These curves are verified each shift (Section 11.5) by 
purging the aqueous performance standard (Section 6.7.2). Recalibration 
is required only if calibration and on-going performance (Section 11.5) 
criteria cannot be met.

                  8. Quality Assurance/Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability, 
analysis of samples spiked with labeled compounds to evaluate and 
document data quality, and analysis of standards and blanks as tests of 
continued performance. Laboratory performance is compared to established 
performance criteria to determine if the results of analyses meet the 
performance characteristics of the method.
    8.1.1 The analyst shall make an initial demonstration of the ability 
to generate acceptable accuracy and precision with this method. This 
ability is established as described in Section 8.2.
    8.1.2 The analyst is permitted to modify this method to improve 
separations or lower the costs of measurements, provided all performance 
specifications are met. Each time a modification is made to the method, 
the analyst is required to repeat the procedure in Section 8.2 to 
demonstrate method performance.
    8.1.3 Analyses of blanks are required to demonstrate freedom from 
contamination and that the compounds of interest and interfering 
compounds have not been carried over from a previous analysis (Section 
3). The procedures and criteria for analysis of a blank are described in 
Sections 8.5 and 11.7.
    8.1.4 The laboratory shall spike all samples with labeled compounds 
to monitor method performance. This test is described in Section 8.3. 
When results of these spikes indicate atypical method performance for 
samples, the samples are diluted to bring method performance within 
acceptable limits (Section 14.2).
    8.1.5 The laboratory shall, on an on-going basis, demonstrate 
through the analysis of the aqueous performance standard (Section 6.7.2) 
that the analysis system is in control. This procedure is described in 
Sections 11.1 and 11.5.

[[Page 354]]

    8.1.6 The laboratory shall maintain records to define the quality of 
data that is generated. Development of accuracy statements is described 
in Sections 8.4 and 11.5.2.
    8.2 Initial precision and accuracy--to establish the ability to 
generate acceptable precision and accuracy, the analyst shall perform 
the following operations:
    8.2.1 Analyze two sets of four 5-mL aliquots (8 aliquots total) of 
the aqueous performance standard (Section 6.7.2) according to the method 
beginning in Section 10.
    8.2.2 Using results of the first set of four analyses in Section 
8.2.1, compute the average recovery (X) in [micro]g/L and the standard 
deviation of the recovery (s) in [micro]g/L for each compound, by 
isotope dilution for polluitants with a labeled analog, and by internal 
standard for labeled compounds and pollutants with no labeled analog.
    8.2.3 For each compound, compare s and X with the corresponding 
limits for initial precision and accuracy found in table 5. If s and X 
for all compounds meet the acceptance criteria, system performance is 
acceptable and analysis of blanks and samples may begin. If individual X 
falls outside the range for accuracy, system performance is unacceptable 
for that compound.
    Note: The large number of compounds in table 5 present a substantial 
probability that one or more will fail one of the acceptance criteria 
when all compoulds are analyzed. To determine if the analytical system 
is out of control, or if the failure can be attributed to probability, 
proceed as follows:
    8.2.4 Using the results of the second set of four analyses, compute 
s and X for only those compounds which failed the test of the first set 
of four analyses (Section 8.2.3). If these compounds now pass, system 
performance is acceptable for all compounds and analysis of blanks and 
samples may begin. If, however, any of the same compounds fail again, 
the analysis system is not performing properly for the compound(s) in 
question. In this event, correct the problem and repeat the entire test 
(Section 8.2.1).
    8.3 The laboratory shall spike all samples with labeled compounds to 
assess method performance on the sample matrix.
    8.3.1 Spike and analyze each sample according to the method 
beginning in Section 10.
    8.3.2 Compute the percent recovery (P) of the labeled compounds 
using the internal standard method (Section 7.5).
    8.3.3 Compare the percent recovery for each compound with the 
corresponding labeled compound recovery limit in table 5. If the 
recovery of any compound falls outside its warning limit, method 
performance is unacceptable for that compound in that sample. Therefore, 
the sample matrix is complex and the sample is to be diluted and 
reanalyzed, per Section 14.2.
    8.4 As part of the QA program for the laboratory, method accuracy 
for wastewater samples shall be assessed and records shall be 
maintained. After the analysis of five wastewater samples for which the 
labeled compounds pass the tests in Section 8.3.3, compute the average 
percent recovery (P) and the standard deviation of the percent recovery 
(sp) for the labeled compounds only. Express the accuracy 
assessment as a percent recovery interval from P-2sp to P + 
2sp. For example, if P = 90% and sp = 10%, the 
accuracy interval is expressed as 70-110%. Update the accuracy 
assessment for each compound on a regular basis (e.g. after each 5-10 
new accuracy measurements).
    8.5 Blanks--reagent water blanks are analyzed to demonstrate freedom 
from carry-over (Section 3) and contamination.
    8.5.1 The level at which the purge and trap system will carry 
greater than 5 [micro]g/L of a pollutant of interest (table 1) into a 
succeeding blank shall be determined by analyzing successively larger 
concentrations of these compounds. When a sample contains this 
concentration or more, a blank shall be analyzed immediately following 
this sample to demonstrate no carry-over at the 5 [micro]g/L level.
    8.5.2 With each sample lot (samples analyzed on the same 8 hr 
shift), a blank shall be analyzed immediately after analysis of the 
aqueous performance standard (Section 11.1) to demonstrate freedom from 
contamination. If any of the compounds of interest (table 1) or any 
potentially interfering compound is found in a blank at greater than 10 
[micro]g/L (assuming a response factor of 1 relative to the nearest 
eluted internal standard for compounds not listed in table 1), analysis 
of samples is halted until the source of contamination is eliminated and 
a blank shows no evidence of contamination at this level.
    8.6 The specifications contained in this method can be met if the 
apparatus used is calibrated properly, then maintained in a calibrated 
state.
    The standards used for calibration (Section 7), calibration 
verification (Section 11.5) and for initial (Section 8.2) and on-going 
(Section 11.5) precision and accuracy should be identical, so that the 
most precise results will be obtained. The GC/MS instrument in 
particular will provide the most reproducible results if dedicated to 
the settings and conditions required for the analyses of volatiles by 
this method.
    8.7 Depending on specific program requirements, field replicates may 
be collected to determine the precision of the sampling technique, and 
spiked samples may be required to determine the accuracy of the analysis 
when internal or external standard methods are used.

[[Page 355]]

            9. Sample Collection, Preservation, and Handling

    9.1 Grab samples are collected in glass containers having a total 
volume greater than 20 mL. Fill sample bottles so that no air bubbles 
pass through the sample as the bottle is filled. Seal each bottle so 
that no air bubbles are entrapped. Maintain the hermetic seal on the 
sample bottle until time of analysis.
    9.2 Samples are maintained at 0-4 [deg]C from the time of collection 
until analysis. If the sample contains residual chlorine, add sodium 
thiosulfate preservative (10 mg/40 mL) to the empty sample bottles just 
prior to shipment to the sample site. EPA Methods 330.4 and 330.5 may be 
used for measurement of residual chlorine (Reference 8). If preservative 
has been added, shake bottle vigorously for one minute immediately after 
filling.
    9.3 Experimental evidence indicates that some aromatic compounds, 
notably benzene, toluene, and ethyl benzene are susceptible to rapid 
biological degradation under certain environmental conditions. 
Refrigeration alone may not be adequate to preserve these compounds in 
wastewaters for more than seven days. For this reason, a separate sample 
should be collected, acidified, and analyzed when these aromatics are to 
be determined. Collect about 500 mL of sample in a clean container.
    Adjust the pH of the sample to about 2 by adding HCl (1 + 1) while 
stirring. Check pH with narrow range (1.4 to 2.8) pH paper. Fill a 
sample container as described in Section 9.1. If residual chlorine is 
present, add sodium thiosulfate to a separate sample container and fill 
as in Section 9.1.
    9.4 All samples shall be analyzed within 14 days of collection.

                   10. Purge, Trap, and GC/MS Analysis

    10.1 Remove standards and samples from cold storage and bring to 20-
25 [deg].
    10.2 Adjust the purge gas flow rate to 40 4 
mL/min. Attach the trap inlet to the purging device and set the valve to 
the purge mode (figure 3). Open the syringe valve located on the purging 
device sample introduction needle (figure 1).
    10.3 Remove the plunger from a 5-mL syringe and attach a closed 
syringe valve. Open the sample bottle and carefully pour the sample into 
the syringe barrel until it overflows. Replace the plunger and compress 
the sample. Open the syringe valve and vent any residual air while 
adjusting the sample volume to 5.0 mL. Because this process of taking an 
aliquot destroys the validity of the sample for future analysis, fill a 
second syringe at this time to protect against possible loss of data. 
Add an appropriate amount of the labeled compound spiking solution 
(Section 6.6) through the valve bore, then close the valve.
    10.4 Attach the syringe valve assembly to the syringe valve on the 
purging device. Open both syringe valves and inject the sample into the 
purging chamber.
    10.5 Close both valves and purge the sample for 11.0 0.1 minutes at 20-25 [deg]C.
    10.6 After the 11 minute purge time, attach the trap to the 
chromatograph and set the purge and trap apparatus to the desorb mode 
(figure 4). Desorb the trapped compounds into the GC column by heating 
the trap to 170-180 [deg]C while backflushing with carrier gas at 20-60 
mL/min for four minutes. Start MS data acquisition upon start of the 
desorb cycle, and start the GC column temperature program 3 minutes 
later. Table 1 summarizes the recommended operating conditions for the 
gas chromatograph. Included in this table are retention times and 
detection limits that were achieved under these conditions. Other 
columns may be used provided the requirements in Section 8 can be met. 
If the priority pollutant gases produce GC peaks so broad that the 
precision and recovery specifications (Section 8.2) cannot be met, the 
column may be cooled to ambient or sub-ambient temperatures to sharpen 
these peaks.
    10.7 While analysis of the desorbed compounds proceeds, empty the 
purging chamber using the sample introduction syringe. Wash the chamber 
with two 5-mL portions of reagent water. After the purging device has 
been emptied, allow the purge gas to vent through the chamber until the 
frit is dry, so that it is ready for the next sample.
    10.8 After desorbing the sample for four minutes, recondition the 
trap by returning to the purge mode. Wait 15 seconds, then close the 
syringe valve on the purging device to begin gas flow through the trap. 
Maintain the trap temperature at 170-180 [deg]C. After approximately 
seven minutes, turn off the trap heater and open the syringe valve to 
stop the gas flow through the trap. When cool, the trap is ready for the 
next sample.

                         11. System Performance

    11.1 At the beginning of each 8 hr shift during which analyses are 
performed, system calibration and performance shall be verified for all 
pollutants and labeled compounds. For these tests, analysis of the 
aqueous performance standard (Section 6.7.2) shall be used to verify all 
performance criteria. Adjustment and/or recalibration (per Section 7) 
shall be performed until all performance criteria are met. Only after 
all performance criteria are met may blanks and samples be analyzed.
    11.2 BFB spectrum validity--the criteria in table 3 shall be met.
    11.3 Retention times--the absolute retention times of all compounds 
shall approximate those given in Table 2.

[[Page 356]]

    11.4 GC resolution--the valley height between toluene and toluene-d8 
(at m/z 91 and 99 plotted on the same graph) shall be less than 10 
percent of the taller of the two peaks.
    11.5 Calibration verification and on-going precision and accuracy--
compute the concentration of each polutant (Table 1) by isotope dilution 
(Section 7.4) for those compmunds which have labeled analogs. Compute 
the concentration of each pollutant (Table 1) which has no labeled 
analog by the internal standard method (Section 7.5). Compute the 
concentration of the labeled compounds by the internal standard method. 
These concentrations are computed based on the calibration data 
determined in Section 7.
    11.5.1 For each pollutant and labeled compound, compare the 
concentration with the corresponding limit for on-going accuracy in 
Table 5. If all compmunds meet the acceptance criteria, system 
performance is acceptable and analysis of blanks and samples may 
continue. If any individual value falls outside the range given, system 
performance is unacceptable for that compound.
    Note: The large number of compounds in Table 5 present a substantial 
probability that one or more will fail the acceptance criteria when all 
compounds are analyzed. To determine if the analytical system is out of 
control, or if the failure may be attributed to probability, proceed as 
follows:
    11.5.1.1 Analyze a second aliquot of the aqueous performance 
standard (Section 6.7.2).
    11.5.1.2 Compute the concentration for only those compounds which 
failed the first test (Section 11.5.1). If these compounds now pass, 
system performance is acceptable for all compounds and analyses of 
blanks and samples may proceed. If, however, any of the compounds fail 
again, the measurement system is not performing properly for these 
compounds. In this event, locate and correct the problem or recalibrate 
the system (Section 7), and repeat the entire test (Section 11.1) for 
all compounds.
    11.5.2 Add results which pass the specification in 11.5.1.2 to 
initial (Section 8.2) and previous on-going data. Update QC charts to 
form a graphic representation of laboratory performance (Figure 7). 
Develop a statement of accuracy for each pollutant and labeled compound 
by calculating the average percentage recovery (R) and the standard 
deviation of percent recovery (sr). Express the accuracy as a 
recovery interval from R-2sr to R + 2sr. For 
example, if R = 95% and sr = 5%, the accuracy is 85-105 
percent.

 12. Qualitative Determination--Accomplished by Comparison of Data from 
   Analysis of a Sample or Blank with Data from Analysis of the Shift 
 Standard (Section 11.1). Identification is Confirmed When Spectra and 
              Retention Times Agree Per the Criteria Below

    12.1 Labeled compounds and pollutants having no labeled analog:
    12.1.1 The signals for all characteristic masses stored in the 
spectral library (Section 7.2.4) shall be present and shall maximize 
within the same two consecutive scans.
    12.1.2 Either (1) the background corrected EICP areas, or (2) the 
corrected relative intensities of the mass spectral peaks at the GC peak 
maximum shall agree within a factor of two (0.5 to 2 times) for all 
masses stored in the library.
    12.1.3 The retention time relative to the nearest eluted internal 
standard shall be within 7 scans or 20 seconds, whichever is greater.
    12.2 Pollutants having a labeled analog:
    12.2.1 The signals for all characteristic masses stored in the 
spectral library (Section 7.2.4) shall be present and shall maximize 
within the same two consecutive scans.
    12.2.2 Either (1) the background corrected EICP areas, or (2) the 
corrected relative intensities of the mass spectral peaks at the GC peak 
maximum shall agree within a factor of two for all masses stored in the 
spectral library.
    12.2.3 The retention time difference between the pollutant and its 
labeled analog shall agree within 2 scans or 
6 seconds (whichever is greater) of this 
difference in the shift standard (Section 11.1).
    12.3 Masses present in the experimental mass spectrum that are not 
present in the reference mass spectrum shall be accounted for by 
contaminant or background ions. If the experimental mass spectrum is 
contaminated, an experienced spectrometrist (Section 1.4) is to 
determine the presence or absence of the compound.

                     13. Quantitative Determination

    13.1 Isotope dilution--by adding a known amount of a labeled 
compound to every sample prior to purging, correction for recovery of 
the pollutant can be made because the pollutant and its labeled analog 
exhibit the same effects upon purging, desorption, and gas 
chromatography. Relative response (RR) values for sample mixtures are 
used in conjunction with calibration curves described in Section 7.4 to 
determine concentrations directly, so long as labeled compound spiking 
levels are constant. For the toluene example given in Figure 6 (Section 
7.4.3), RR would be equal to 1.174. For this RR value, the toluene 
calibration curve given in Figure 5 indicates a concentration of 31.8 
[micro]g/L.

[[Page 357]]

    13.2 Internal standard--calculate the concentration using the 
response factor determined from calibration data (Section 7.5) and the 
following equation:
    Concentration = (As x Cis)/(Ais x 
RF) where the terms are as defined in Section 7.5.1.
    13.3 If the EICP area at the quantitation mass for any compound 
exceeds the calibration range of the system, the sample is diluted by 
successive factors of 10 and these dilutions are analyzed until the area 
is within the calibration range.
    13.4 Report results for all pollutants and labeled compounds (Table 
1) found in all standards, blanks, and samples, in [micro]g/L to three 
significant figures. Results for samples which have been diluted are 
reported at the least dilute level at which the area at the quantitation 
mass is within the calibration range (Section 13.3) and the labeled 
compound recovery is within the normal range for the Method (Section 
14.2).

                     14. Analysis of Complex Samples

    14.1 Untreated effluents and other samples frequently contain high 
levels (1000 [micro]g/L) of the compounds of interest and of 
interfering compounds. Some samples will foam excessively when purged; 
others will overload the trap/or GC column.
    14.2 Dilute 0.5 mL of sample with 4.5 mL of reagent water and 
analyze this diluted sample when labeled compound recovery is outside 
the range given in Table 5. If the recovery remains outside of the range 
for this diluted sample, the aqueous performance standard shall be 
analyzed (Section 11) and calibration verified (Section 11.5). If the 
recovery for the labeled compmund in the aqueous performance standard is 
outside the range given in Table 5, the analytical system is out of 
control. In this case, the instrumelt shall be repaired, the performance 
specifications in Section 11 shall be met, and the analysis of the 
undiluted sample shall be repeated. If the recovery for the aqueous 
performance standard is within the range given in Table 5, the method 
does not work on the sample being analyzed and the result may not be 
reported for regulatory compliance purposes.
    14.3 Reverse search computer programs can misinterpret the spectrum 
of chromatographically unresolved pollutant and labeled compound pairs 
with overlapping spectra when a high level of the pollutant is present. 
Examine each chromatogram for peaks greater than the height of the 
internal standard peaks. These peaks can obscure the compounds of 
interest.

                         15. Method Performance

    15.1 The specifications for this method were taken from the inter-
laboratory validation of EPA Method 624 (reference 9). Method 1624 has 
been shown to yield slightly better performance on treated effluents 
than Method 624. Additional method performance data can be found in 
Reference 10.

                               References

    1. ``Performance Tests for the Evaluation of Computerized Gas 
Chromatography/Mass Spectrometry Equipment and Laboratories,'' USEPA, 
EMSL/Cincinnati, OH 45268, EPA-600/4-80-025 (April 1980).
    2. Bellar, T.A. and Lichtenberg, J.J., ``Journal American Water 
Works Association,'' 66, 739 (1974).
    3. Bellar, T.A. and Lichtenberg, J.J., ``Semi-automated Headspace 
Analysis of Drinking Waters and Industrial Waters for Purgeable Volatile 
Organic Compounds,'' in Measurement of Organic Pollutants Water and 
Wastewater, C.E. VanHall, ed., American Society for Testing Materials, 
Philadelphia, PA, Special Technical Publication 686, (1978).
    4. ``Working with Carcinogens,'' DHEW, PHS, NIOSH, Publication 77-
206 (1977).
    5. ``OSHA Safety and Health Standards, General Industry,'' 29 CFR 
part 1910, OSHA 2206, (1976).
    6. ``Safety in Academic Chemistry Laboratories,'' American Chemical 
Society Publication, Committee on Chemical Safety (1979).
    7. ``Handbook of Analytical Quality Control in Water and Wastewater 
Laboratories,'' USEPA, EMSL/Cincinnati, OH 45268, EPA-4-79-019 (March 
1979).
    8. ``Methods 330.4 and 330.5 for Total Residual Chlorine,'' USEPA, 
EMSL/Cincinnati, OH 45268, EPA-4-79-020 (March 1979).
    9. ``EPA Method Study 29 EPA Method 624--Purgeables,'' EPA 600/4-84-
054, National Technical Information Service, PB84-209915, Springfield, 
Virginia 22161, June 1984.
    10. ``Colby, B.N., Beimer, R.G., Rushneck, D.R., and Telliard, W.A., 
``Isotope Dilution Gas Chromatography-Mass Spectrometry for the 
Determination of Priority Pollutants in Industrial Effluents,'' USEPA, 
Effluent Guidelines Division, Washington, DC 20460 (1980).

 Table 1--Volatile Organic Compounds Analyzed by Isotope Dilution Gc/MS
------------------------------------------------------------------------
                                             CAS
           Compound             Storet     registry    EPA-EGD    NPDES
------------------------------------------------------------------------
Acetone......................     81552      67-64-1     516 V
Acrolein.....................     34210     107-02-8     002 V     001 V
Acrylonitrile................     34215     107-13-1     003 V     002 V
Benzene......................     34030      71-43-2     004 V     003 V
Bromodichloromethane.........     32101      75-27-4     048 V     012 V

[[Page 358]]

 
Bromoform....................     32104      75-25-2     047 V     005 V
Bromomethane.................     34413      74-83-9     046 V     020 V
Carbon tetrachloride.........     32102      56-23-5     006 V     006 V
Chlorobenzene................     34301     108-90-7     007 V     007 V
Chloroethane.................     34311      75-00-3     016 V     009 V
2-chloroethylvinyl ether.....     34576     110-75-8     019 V     010 V
Chloroform...................     32106      67-66-1     023 V     011 V
Chloromethane................     34418      74-87-3     045 V     021 V
Dibromochloromethane.........     32105     124-48-1     051 V     008 V
1,1-dichloroethane...........     34496      75-34-3     013 V     014 V
1,2-dichloroethane...........     34536     107-06-2     010 V     015 V
1,1-dichloroethene...........     34501      75-35-4     029 V     016 V
Trans-1,2-dichloroethane.....     34546     156-60-5     030 V     026 V
1,2-dichloropropane..........     34541      78-87-5     032 V     017 V
Cis-1,3-dichloropropene......     34704   10061-01-5
Trans-1,3-dichloropropene....     34699   10061-02-6     033 V
Diethyl ether................     81576      60-29-7     515 V
P-dioxane....................     81582     123-91-1     527 V
Ethylbenzene.................     34371     100-41-4     038 V     019 V
Methylene chloride...........     34423      75-09-2     044 V     022 V
Methyl ethyl ketone..........     81595      78-93-3     514 V
1,1,2,2-tetrachloroethane....     34516      79-34-5     015 V     023 V
Tetrachlorethene.............     34475     127-18-4     085 V     024 V
Toluene......................     34010     108-88-3     086 V     025 V
1,1,1-trichloroethane........     34506      71-55-6     011 V     027 V
1,1,2-trichloroethane........     34511      79-00-5     014 V     028 V
Trichloroethene..............     39180      79-01-6     087 V     029 V
Vinyl chloride...............     39175      75-01-4     088 V     031 V
------------------------------------------------------------------------


  Table 2--Gas Chromatography of Purgeable Organic Compounds by Isotope
                             Dilution GC/MS
------------------------------------------------------------------------
                                                      Mean      Minimum
EGD                                           Ref  retention   level (2)
No.                  Compound                 EGD     time    ([micro]g/
(1)                                           No.    (sec)        L)
------------------------------------------------------------------------
181  Bromochloromethane (I.S.)..............  181      730          10
245  Chloromethane-d3.......................  181      147          50
345  Chloromethane..........................  245      148          50
246  Bromomethane-d3........................  181      243          50
346  Bromomethane...........................  246      246          50
288  Vinyl chloride-d3......................  181      301          50
388  Vinyl chloride.........................  288      304          10
216  Chloroethane-d5........................  181      378          50
316  Chloroethane...........................  216      386          50
244  Methylene chloride-d2..................  181      512          10
344  Methylene chloride.....................  244      517          10
616  Acetone-d6.............................  181      554          50
716  Acetone................................  616      565          50
002  Acrolein...............................  181      566          50
203  Acrylonitrile-d3.......................  181      606          50
303  Acrylonitrile..........................  203      612          50
229  1,1-dichloroethene-d2..................  181      696          10
329  1,1-dichloroethene.....................  229      696          10
213  1,1-dichloroethane-d3..................  181      778          10
313  1,1-dichloroethane.....................  213      786          10
615  Diethyl ether-d10......................  181      804          50
715  Diethyl ether..........................  615      820          50
230  Trans-1,2-dichloroethene-d2............  181      821          10
330  Trans-1,2-dichloroethene...............  230      821          10
614  Methyl ethyl ketone-d3.................  181      840          50
714  Methyl ethyl ketone....................  614      848          50
223  Chloroform-13C1........................  181      861          10
323  Chloroform.............................  223      861          10
210  1,2-dichloroethane-d4..................  181      901          10
310  1,2-dichloroethane.....................  210      910          10
211  1,1,1-trichloroethane-13C2.............  181      989          10
311  1,1,1-trichloroethane..................  211      999          10
527  p-dioxane..............................  181     1001          10
206  Carbon tetrachloride-13C1..............  182     1018          10
306  Carbon tetrachloride...................  206     1018          10
248  Bromodichloromethane-13C1..............  182     1045          10
348  Bromodichloromethane...................  248     1045          10
232  1,2-dichloropropane-d6.................  182     1123          10
332  1.2-dichloropropane....................  232     1134          10
233  Trans-1,3-dichloropropene-d4...........  182     1138          10
333  Trans-1,3-dichloropropene..............  233     1138          10
287  Trichloroethene-13C1...................  182     1172          10
387  Trichloroethene........................  287     1187          10
204  Benzene-d6.............................  182     1200          10
304  Benzene................................  204     1212          10
251  Chlorodibromemethane-13C1..............  182     1222          10
351  Chlorodibromomethane...................  251     1222          10
214  1,1,2-trichloroethane-13C2.............  182     1224          10
314  1,1,2-trichloroethane..................  214     1224          10
019  2-chloroethylvinyl ether...............  182     1278          10
182  2-bromo-1-chloropropane (I.S.).........  182     1306          10
247  Bromoform-13C1.........................  182     1386          10
347  Bromoform..............................  247     1386          10
215  1,1,2,2-tetrachloroethane-d2...........  183     1525          10
315  1,1,2,2-tetrachloroethane..............  215     1525          10
285  Tetrachloroethene-13C2.................  183     1528          10
385  Tetrachloroethene......................  285     1528          10
183  1,4-dichlorobutale (int std)...........  183     1555          10
286  Toluene-d8.............................  183     1603          10
386  Toluene................................  286     1619          10

[[Page 359]]

 
207  Chlorobenzene-d5.......................  183     1679          10
307  Chlorobenzene..........................  207     1679          10
238  Ethylbenzene-d10.......................  183     1802          10
338  Ethylbenzene...........................  238     1820          10
185  Bromofluorobenzene.....................  183     1985          10
------------------------------------------------------------------------
(1) Reference numbers beginning with 0, 1 or 5 indicate a pollutant
  quantified by the internal standard method; reference numbers
  beginning with 2 or 6 indicate a labeled compound quantified by the
  internal standard method; reference numbers beginning with 3 or 7
  indicate a pollutant quantified by isotope dilution.
(2) This is a minimum level at which the analytical system shall give
  recognizable mass spectra (background corrected) and acceptable
  calibration points. Column: 2.4m (8 ft) x 2 mm i.d. glass, packed with
  one percent SP-1000 coated on 60/80 Carbopak B. Carrier gas: helium at
  40 mL/min. Temperature program: 3 min at 45 [deg]C, 8 [deg]C per min
  to 240 [deg]C, hold at 240 [deg]C for 15 minutes.
 
Note: The specifications in this table were developed from data
  collected from three wastewater laboratories.


               Table 3--BFB Mass-Intensity Specifications
------------------------------------------------------------------------
 Mass                          Intensity required
------------------------------------------------------------------------
   50  15 to 40 percent of mass 95.
   75  30 to 60 percent of mass 95.
   95  base peak, 100 percent.
   96  5 to 9 percent of mass 95.
  173  <2 percent of mass 174.
  174  50 percent of mass 95.
  175  5 to 9 percent of mass 174
  176  95 to 101 percent of mass 174
  177  5 to 9 percent of mass 176.
------------------------------------------------------------------------


        Table 4--Volatile Organic Compound Characteristic Masses
------------------------------------------------------------------------
                                                              Primary m/
                  Labeled compound                    Analog      z's
------------------------------------------------------------------------
Acetone............................................       d6       58/64
Acrolein...........................................       d2       56/58
Acrylonitrile......................................       d3       53/56
Benzene............................................       d6       78/84
Bromodichloromethane...............................      13C       83/86
Bromoform..........................................      13C     173/176
Bromomethale.......................................       d3       96/99
Carbon tetrachloride...............................      13C       47/48
Chlorobenzene......................................       d5     112/117
Chloroethane.......................................       d5       64/71
2-chloroethylvinyl ether...........................       d7     106/113
Chloroform.........................................      13C       85/86
Chloromethane......................................       d3       50/53
Dibromochloromethane...............................      13C     129/130
1,1-dichloroethane.................................       d3       63/66
1,2-dichloroethane.................................       d4       62/67
1,1-dichloroethene.................................       d2       61/65
Trans-1,2-dichloroethene...........................       d2       61/65
1,2-dichloropropane................................       d6       63/67
Cis-1,3-dichloropropene............................       d4       75/79
Trans-1,3-dichloropropene..........................       d4       75/79
Diethyl ether......................................      d10       74/84
p-dioxane..........................................       d8       88/96
Ethylbenzene.......................................      d10     106/116
Methylene chloride.................................       d2       84/88
Methyl ethyl ketone................................       d3       72/75
1,1,2,2-tetrachloroethane..........................       d2       83/84
Tetrachloroethene..................................     13C2     166/172
Toluene............................................       d8       92/99
1,1,1-trichloroethane..............................       d3      97/102
1,1,2-trichloroethane..............................     13C2       83/84
Trichloroethene....................................      13C      95/133
Vinyl chloride.....................................       d3       62/65
------------------------------------------------------------------------


                               Table 5--Acceptance Criteria for Performance Tests
----------------------------------------------------------------------------------------------------------------
                                                                    Acceptance criteria at 20 [micro]g/L
                                                          ------------------------------------------------------
                                                              Initial precision and       Labeled      On-going
                                                              accuracy section 8.2.3      compound     accuracy
                         Compound                         -----------------------------   recovery    sec. 11.5
                                                                                          sec. 8.3  ------------
                                                           s ([micro]g/                   and 14.2
                                                                L)      X ([micro]g/L) ------------- R ([micro]g/
                                                                                        P (percent)       L)
----------------------------------------------------------------------------------------------------------------
Acetone..................................................                          Note 1
Acrolein.................................................                          Note 2
Acrylonitrile............................................                          Note 2
Benzene..................................................          9.0       13.0-28.2       ns-196         4-33
Bromodichloromethane.....................................          8.2        6.5-31.5       ns-199         4-34
Bromoform................................................          7.0        7.4-35.1       ns-214         6-36
Bromomethane.............................................         25.0          d-54.3       ns-414         d-61
Carbon tetrachloride.....................................          6.9       15.9-24.8       42-165        12-30
Chlorobenzene............................................          8.2       14.2-29.6       ns-205         4-35
Chloroethane.............................................         14.8        2.1-46.7       ns-308         d-51
2-chloroethylvinyl ether.................................         36.0          d-69.8       ns-554         d-79
Chloroform...............................................          7.9       11.6-26.3       18-172         8-30
Chloromethane............................................         26.0          d-55.5       ns-410         d-64
Dibromochloromethane.....................................          7.9       11.2-29.1       16-185         8-32
1,1-dichloroethane.......................................          6.7       11.4-31.4       23-191         9-33
1,2-dichloroethane.......................................          7.7       11.6-30.1       12-192         8-33
1,1-dichloroethene.......................................         11.7          d-49.8       ns-315         d-52
Trans-1,2-dichloroethene.................................          7.4       10.5-31.5       15-195         8-34

[[Page 360]]

 
1,2-dichloropropane......................................         19.2          d-46.8       ns-343         d-51
Cis-1,3-dichloropropene..................................         22.1          d-51.0       ns-381         d-56
Trans-1,3-dichloropropene................................         14.5          d-40.2       ns-284         d-44
Diethyl ether............................................                          Note 1
P-dioxane................................................                          Note 1
Ethyl benzene............................................          9.6       15.6-28.5       ns-203         5-35
Methylene chloride.......................................          9.7          d-49.8       ns-316         d-50
Methyl ethyl ketone......................................                          Note 1
1,1,2,2-tetrachloroethane................................          9.6       10.7-30.0        5-199         7-34
Tetrachloroethene........................................          6.6       15.1-28.5       31-181        11-32
Toluene..................................................          6.3       14.5-28.7        4-193         6-33
1,1,1-trichloroethane....................................          5.9       10.5-33.4       12-200         8-35
1,1,2-trichloroethane....................................          7.1       11.8-29.7       21-184         9-32
Trichloroethene..........................................          8.9       16.6-29.5       35-196        12-34
Vinyl chloride...........................................         27.9          d-58.5       ns-452         d-65
----------------------------------------------------------------------------------------------------------------
d = detected; result must be greater than zero.
ns = no specification; limit would be below detection limit.
 
 Specifications not available for these compounds at time of release of this method.
 Specifications not developed for these compounds; use method 603.


[[Page 361]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.055


[[Page 362]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.056

   Method 1625 Revision B--Semivolatile Organic Compounds by Isotope 
                             Dilution GC/MS

                        1. Scope and Application

    1.1 This method is designed to determine the semivolatile toxic 
organic pollutants associated with the 1976 Consent Decree and 
additional compounds amenable to extraction and analysis by capillary 
column gas chromatography-mass spectrometry (GC/MS).
    1.2 The chemical compounds listed in Tables 1 and 2 may be 
determined in municipal and industrial discharges by this method. The 
method is designed to meet the survey

[[Page 363]]

requirements of Effluent Guidelines Division (EGD) and the National 
Pollutants Discharge Elimination System (NPDES) under 40 CFR 136.1. Any 
modifications of this method, beyond those expressly permitted, shall be 
considered as major modifications subject to application and approval of 
alternate test procedures under 40 CFR 136.4 and 136.5.
    1.3 The detection limit of this method is usually dependent on the 
level of interferences rather than instrumental limitations. The limits 
listed in Tables 3 and 4 represent the minimum quantity that can be 
detected with no interferences present.
    1.4 The GC/MS portions of this method are for use only by analysts 
experienced with GC/MS or under the close supervision of such qualified 
persons. Laboratories unfamiliar with analyses of environmental samples 
by GC/MS should run the performance tests in reference 1 before 
beginning.

                          2. Summary of Method

    2.1 Stable isotopically labeled analogs of the compounds of interest 
are added to a one liter wastewater sample. The sample is extracted at 
pH 12-13, then at pH <2 with methylene chloride using continuous 
extraction techniques. The extract is dried over sodium sulfate and 
concentrated to a volume of one mL. An internal standard is added to the 
extract, and the extract is injected into the gas chromatograph (GC). 
The compounds are separated by GC and detected by a mass spectrometer 
(MS). The labeled compounds serve to correct the variability of the 
analytical technique.
    2.2 Identification of a compound (qualitative analysis) is performed 
by comparing the GC retention time and background corrected 
characteristic spectral masses with those of authentic standards.
    2.3 Quantitative analysis is performed by GC/MS using extracted ion 
current profile (EICP) areas. Isotope dilution is used when labeled 
compounds are available; otherwise, an internal standard method is used.
    2.4 Quality is assured through reproducible calibration and testing 
of the extraction and GC/MS systems.

                   3. Contamination and Interferences

    3.1 Solvents, reagents, glassware, and other sample processing 
hardware may yield artifacts and/or elevated baselines causing 
misinterpretation of chromatograms and spectra. All materials shall be 
demonstrated to be free from interferences under the conditions of 
analysis by running method blanks initially and with each sample lot 
(samples started through the extraction process on a given 8 hr shift, 
to a maximum of 20). Specific selection of reagents and purification of 
solvents by distillation in all-glass systems may be required. Glassware 
and, where possible, reagents are cleaned by solvent rinse and baking at 
450 [deg]C for one hour minimum.
    3.2 Interferences coextracted from samples will vary considerably 
from source to source, depending on the diversity of the industrial 
complex or municipality being samples.

                                4. Safety

    4.1 The toxicity or carcinogenicity of each compound or reagent used 
in this method has not been precisely determined; however, each chemical 
compound should be treated as a potential health hazard. Exposure to 
these compounds should be reduced to the lowest possible level. The 
laboratory is responsible for maintaining a current awareness file of 
OSHA regulations regarding the safe handling of the chemicals specified 
in this method. A reference file of data handling sheets should also be 
made available to all personnel involved in these analyses. Additional 
information on laboratory safety can be found in references 2-4.
    4.2 The following compounds covered by this method have been 
tentatively classified as known or suspected human or mammalian 
carcinogens: benzidine benzo(a)anthracene, 3,3'-dichlorobenzidine, 
benzo(a)pyrene, dibenzo(a,h)anthracene, N-nitrosodimethylamine, and 
[beta]-naphtylamine. Primary standards of these compounds shall be 
prepared in a hood, and a NIOSH/MESA approved toxic gas respirator 
should be worn when high concentrations are handled.

                       5. Apparatus and Materials

    5.1 Sampling equipment for discrete or composite sampling.
    5.1.1 Sample bottle, amber glass, 1.1 liters minimum. If amber 
bottles are not available, samples shall be protected from light. 
Bottles are detergent water washed, then solvent rinsed or baked at 450 
[deg]C for one hour minimum before use.
    5.1.2 Bottle caps--threaded to fit sample bottles. Caps are lined 
with Teflon. Aluminum foil may be substituted if the sample is not 
corrosive. Liners are detergent water washed, then reagent water 
(Section 6.5) and solvent rinsed, and baked at approximately 200 [deg]C 
for one hour minimum before use.
    5.1.3 Compositing equipment--automatic or manual compositing system 
incorporating glass containers for collection of a minimum 1.1 liters. 
Sample containers are kept at 0 to 4 [deg]C during sampling. Glass or 
Teflon tubing only shall be used. If the sampler uses a peristaltic 
pump, a minimum length of compressible silicone rubber tubing may be 
used in the pump only. Before use, the tubing is thoroughly rinsed with 
methanol, followed by repeated rinsings with reagent water (Section 6.5) 
to minimize sample contamination. An integrating flow meter is used to 
collect proportional composite samples.

[[Page 364]]

    5.2 Continuous liquid-liquid extractor--Teflon or glass conncecting 
joints and stopcocks without lubrication (Hershberg-Wolf Extractor) one 
liter capacity, Ace Glass 6841-10, or equivalent.
    5.3 Drying column--15 to 20 mm i.d. Pyrex chromatographic column 
equipped with coarse glass frit or glass wool plug.
    5.4 Kuderna-Danish (K-D) apparatus
    5.4.1 Concentrator tube--10mL, graduated (Kontes K-570050-1025, or 
equivalent) with calibration verified. Ground glass stopper (size 19/22 
joint) is used to prevent evaporation of extracts.
    5.4.2 Evaporation flask--500 mL (Kontes K-570001-0500, or 
equivalent), attached to concentrator tube with springs (Kontes K-
662750-0012).
    5.4.3 Snyder column--three ball macro (Kontes K-503000-0232, or 
equivalent).
    5.4.4 Snyder column--two ball micro (Kontes K-469002-0219, or 
equivalent).
    5.4.5 Boiling chips--approx 10/40 mesh, extracted with methylene 
chloride and baked at 450 [deg]C for one hr minimum.
    5.5 Water bath--heated, with concentric ring cover, capable of 
temperature control 2 [deg]C, installed in a fume 
hood.
    5.6 Sample vials--amber glass, 2-5 mL with Teflon-lined screw cap.
    5.7 Analytical balance--capable of weighing 0.1 mg.
    5.8 Gas chromatograph--shall have splitless or on-column injection 
port for capillary column, temperature program with 30 [deg]C hold, and 
shall meet all of the performance specifications in Section 12.
    5.8.1 Column--30 5 m x 0.25 0.02 mm i.d. 5% phenyl, 94% methyl, 1% vinyl silicone 
bonded phase fused silica capillary column (J & W DB-5, or equivalent).
    5.9 Mass spectrometer--70 eV electron impact ionization, shall 
repetitively scan from 35 to 450 amu in 0.95 to 1.00 second, and shall 
produce a unit resolution (valleys between m/z 441-442 less than 10 
percent of the height of the 441 peak), backgound corrected mass 
spectrum from 50 ng decafluorotriphenylphosphine (DFTPP) introduced 
through the GC inlet. The spectrum shall meet the mass-intensity 
criteria in Table 5 (reference 5). The mass spectrometer shall be 
interfaced to the GC such that the end of the capillary column 
terminates within one centimeter of the ion source but does not 
intercept the electron or ion beams. All portions of the column which 
connect the GC to the ion source shall remain at or above the column 
temperature during analysis to preclude condensation of less volatile 
compounds.
    5.10 Data system--shall collect and record MS data, store mass-
intensity data in spectral libraries, process GC/MS data, generate 
reports, and shall compute and record response factors.
    5.10.1 Data acquisition--mass spectra shall be collected 
continuously throughout the analysis and stored on a mass storage 
device.
    5.10.2 Mass spectral libraries--user created libraries containing 
mass spectra obtained from analysis of authentic standards shall be 
employed to reverse search GC/MS runs for the compounds of interest 
(Section 7.2).
    5.10.3 Data processing--the data system shall be used to search, 
locate, identify, and quantify the compounds of interest in each GC/MS 
analysis. Software routines shall be employed to compute retention times 
and peak areas. Displays of spectra, mass chromatograms, and library 
comparisons are required to verify results.
    5.10.4 Response factors and multipoint calibrations--the data system 
shall be used to record and maintain lists of response factors (response 
ratios for isotope dilution) and multipoint calibration curves (Section 
7). Computations of relative standard deviation (coefficient of 
variation) are useful for testing calibration linearity. Statistics on 
initial (Section 8.2) and on-going (Section 12.7) performance shall be 
computed and maintained.

                        6. Reagents and Standards

    6.1 Sodium hydroxide--reagent grade, 6N in reagent water.
    6.2 Sulfuric acid--reagent grade, 6N in reagent water.
    6.3 Sodium sulfate--reagent grade, granular anhydrous, rinsed with 
methylene chloride (20 mL/g) and conditioned at 450 [deg]C for one hour 
minimum.
    6.4 Methylene chloride--distilled in glass (Burdick and Jackson, or 
equivalent).
    6.5 Reagent water--water in which the compounds of interest and 
interfering compounds are not detected by this method.
    6.6 Standard solutions--purchased as solutions or mixtures with 
certification to their purity, concentration, and authenticity, or 
prepared from materials of known purity and composition. If compound 
purity is 96 percent or greater, the weight may be used without 
correction to compute the concentration of the standard. When not being 
used, standards are stored in the dark at -20 to -10 [deg]C in screw-
capped vials with Teflon-lined lids. A mark is placed on the vial at the 
level of the solution so that solvent evaporation loss can be detected. 
The vials are brought to room temperature prior to use. Any precipitate 
is redissolved and solvent is added if solvent loss has occurred.
    6.7 Preparation of stock solutions--prepare in methylene chloride, 
benzene, p-dioxane, or a mixture of these solvents per the steps below. 
Observe the safety precautions in Section 4. The large number of labeled 
and unlabeled acid, base/neutral, and Appendix C compounds used for 
combined

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calibration (Section 7) and calibration verification (12.5) require high 
concentratimns (approx 40 mg/mL) when individual stock solutions are 
prepared, so that dilutions of mixtures will permit calibration with all 
compounds in a single set of solutions. The working range for most 
compounds is 10-200 [micro]g/mL. Compounds with a reduced MS response 
may be prepared at higher concentrations.
    6.7.1 Dissolve an appropriate amount of assayed reference material 
in a suitable solvent. For example, weigh 400 mg naphthalene in a 10 mL 
ground glass stoppered volumetric flask and fill to the mark with 
benzene. After the naphthalene is completely dissolved, transfer the 
solution to a 15 mL vial with Teflon-lined cap.
    6.7.2 Stock standard solutions should be checked for signs of 
degradation prior to the preparation of calibration or performance test 
standards. Quality control check samples that can be used to determine 
the accuracy of calibration standards are available from the US 
Environmental Protection Agency, Environmental Monitoring and Support 
Laboratory, Cincinnati, Ohio 45268.
    6.7.3 Stock standard solutions shall be replaced after six months, 
or sooner if comparison with quality control check samples indicates a 
change in concentration.
    6.8 Labeled compound spiking solution--from stock standard solutions 
prepared as above, or from mixtures, prepare the spiking solution at a 
concentration of 200 [micro]g/mL, or at a concentration appropriate to 
the MS response of each compound.
    6.9 Secondary standard--using stock solutions (Section 6.7), prepare 
a secondary standard containing all of the compounds in Tables 1 and 2 
at a concentration of 400 [micro]g/mL, or higher concentration 
appropriate to the MS response of the compound.
    6.10 Internal standard solution--prepare 2,2'-difluorobiphenyl (DFB) 
at a concentration of 10 mg/mL in benzene.
    6.11 DFTPP solution--prepare at 50 [micro]g/mL in acetone.
    6.12 Solutions for obtaining authentic mass spectra (Section 7.2)--
prepare mixtures of compounds at concentrations which will assure 
authentic spectra are obtained for storage in libraries.
    6.13 Calibration solutions--combine 0.5 mL of the solution in 
Section 6.8 with 25, 50, 125, 250, and 500 uL of the solution in section 
6.9 and bring to 1.00 mL total volume each. This will produce 
calibration solutions of nominal 10, 20, 50, 100, and 200 [micro]g/mL of 
the pollutants and a constant nominal 100 [micro]g/mL of the labeled 
compounds. Spike each solution with 10 [micro]L of the internal standard 
solution (Section 6.10). These solutions permit the relative response 
(labeled to unlabeled) to be measured as a function of concentration 
(Section 7.4).
    6.14 Precision and recovery standard--used for determination of 
initial (Section 8.2) and on-going (Section 12.7) precision and 
recovery. This solution shall contain the pollutants and labeled 
compounds at a nominal concentration of 100 [micro]g/mL.
    6.15 Stability of solutions--all standard solutions (Sections 6.8-
6.14) shall be analyzed within 48 hours of preparation and on a monthly 
basis thereafter for signs of degradation. Standards will remain 
acceptable if the peak area at the quantitation mass relative to the DFB 
internal standard remains within 15 percent of the 
area obtained in the initial analysis of the standard.

                             7. Calibration

    7.1 Assemble the GC/MS and establish the operating conditions in 
Table 3. Analyze standards per the procedure in Section 11 to 
demonstrate that the analytical system meets the detection limits in 
Tables 3 and 4, and the mass-intensity criteria in Table 5 for 50 ng 
DFTPP.
    7.2 Mass spectral libraries--detection and identification of 
compounds of interest are dependent upon spectra stored in user created 
libraries.
    7.2.1 Obtain a mass spectrum of each pollutant, labeled compound, 
and the internal standard by analyzing an authentic standard either 
singly or as part of a mixture in which there is no interference between 
closely eluted components. That only a single compound is present is 
determined by examination of the spectrum. Fragments not attributable to 
the compound under study indicate the presence of an interfering 
compound.
    7.2.2 Adjust the analytical conditions and scan rate (for this test 
only) to produce an undistorted spectrum at the GC peak maximum. An 
undistorted spectrum will usually be obtained if five complete spectra 
are collected across the upper half of the GC peak. Software algorithms 
designed to ``enhance'' the spectrum may eliminate distortion, but may 
also eliminate authentic masses or introduce other distortion.
    7.2.3 The authentic reference spectrum is obtained under DFTPP 
tuning conditions (Section 7.1 and Table 5) to normalize it to spectra 
from other instruments.
    7.2.4 The spectrum is edited by saving the 5 most intense mass 
spectral peaks and all other mass spectral peaks greater than 10 percent 
of the base peak. This edited spectrum is stored for reverse search and 
for compound confirmation.
    7.3 Analytical range--demonstrate that 20 ng anthracene or 
phenanthrene produces an area at m/z 178 approx one-tenth that required 
to exceed the linear range of the system. The exact value must be 
determined by experience for each instrument. It is used to match the 
calibration range of the instrument to the analytical range and 
detection limits required, and to diagnose instrument

[[Page 366]]

sensitivity problems (Section 15.4). The 20 ug/mL calibration standard 
(Section 6.13) can be used to demonstrate this performance.
    7.3.1 Polar compound detection--demonstrate that unlabeled 
pentachlorophenol and benzidine are detectable at the 50 [micro]g/mL 
level (per all criteria in Section 13). The 50 [micro]g/mL calibration 
standard (Section 6.13) can be used to demonstrate this performance.
    7.4 Calibration with isotope dilution--isotope dilution is used when 
(1) labeled compounds are available, (2) interferences do not preclude 
its use, and (3) the quantitation mass extracted ion current profile 
(EICP) area for the compound is in the calibration range. If any of 
these conditions preclude isotope dilution, internal standard methods 
(Section 7.5 or 7.6) are used.
    7.4.1 A calibration curve encompassing the concentration range is 
prepared for each compound to be determined. The relative response 
(pollutant to labeled) vs concentration in standard solutions is plotted 
or computed using a linear regression. The example in Figure 1 shows a 
calibration curve for phenol using phenol-d5 as the isotopic diluent. 
Also shown are the 10 percent error limits (dotted 
lines). Relative Reponse (RR) is determined according to the procedures 
described below. A minimum of five data points are employed for 
calibration.
    7.4.2 The relative response of a pollutant to its labeled analog is 
determined from isotope ratio values computed from acquired data. Three 
isotope ratios are used in this process:

    RX = the isotope ratio measured for the pure pollutant.
    Ry = the isotope ratio measured for the labeled compound.
    Rm = the isotope ratio of an analytical mixture of 
pollutant and labeled compounds.

    The m/z's are selected such that 
RXRy. If Rm is not between 
2Ry and 0.5RX, the method does not apply and the 
sample is analyzed by internal or external standard methods.
    7.4.3 Capillary columns usually separate the pollutant-labeled pair, 
with the labeled compound eluted first (Figure 2). For this case, 
RX = [area m1/z]/1, at the retention time of the 
pollutant (RT2). Ry = 1/[area m2/z, at 
the retention time of the labeled compound RT1). 
Rm = [area at m1/z (at RT2)]/[area at 
RT1)], as measured in the mixture of the pollutant and 
labeled compounds (Figure 2), and RR = Rm.
    7.4.4 Special precautions are taken when the pollutant-labeled pair 
is not separated, or when another labeled compound with interfering 
spectral masses overlaps the pollutant (a case which can occur with 
isomeric compounds). In this case, it is necessary to determine the 
respective contributions of the pollutant and labeled compounds to the 
respective EICP areas. If the peaks are separated well enough to permit 
the data system or operator to remove the contributions of the compounds 
to each other, the equations in Section 7.4.3 apply. This usually occurs 
when the height of the valley between the two GC peaks at the same m/z 
is less than 10 percent of the height of the shorter of the two peaks. 
If significant GC and spectral overlap occur, RR is computed using the 
following equation:

    RR = (Ry - Rm) (RX + 1)/
(Rm - RX) (Ry + 1), where RX 
is measured as shown in Figure 3A, Ry is measured as shown in 
Figure 3B, and Rm is measured as shown in Figure 3C. For 
example, RX = 46100/4780 = 9.644, Ry = 2650/43600 
= 0.0608, Rm = 49200/48300 = 1.019. amd RR = 1.114.

    7.4.5 To calibrate the analytical system by isotope dilution, 
analyze a 1.0 [micro]L aliquot of each of the calibration standards 
(Section 6.13) using the procedure in Section 11. Compute the RR at each 
concentration.
    7.4.6 Linearity--if the ratio of relative response to concentration 
for any compound is constant (less than 20 percent coefficient of 
variation) over the 5 point calibration range, and averaged relative 
response/concentration ratio may be used for that compound; otherwise, 
the complete calibration curve for that compound shall be used over the 
5 point calibration range.
    7.5 Calibration by internal standard--used when criteria for istope 
dilution (Section 7.4) cannot be met. The internal standard to be used 
for both acid and base/neutral analyses is 2,2'-difluorobiphenyl. The 
internal standard method is also applied to determination of compounds 
having no labeled analog, and to measurement of labeled compounds for 
intra-laboratory statistics (Sections 8.4 and 12.7.4).
    7.5.1 Response factors--calibration requires the determination of 
response factors (RF) which are defined by the following equation:

    RF = (As x Cis)/(Ais x 
Cs), where
    As is the area of the characteristic mass for the 
compmund in the daily standard
    Ais is the area of the characteristic mass for the 
internal standard
    Cis is the concentration of the internal standard 
([micro]g/mL)
    Cs is the concentration of the compound in the daily 
standard ([micro]g/mL)

    7.5.1.1 The response factor is determined for at least five 
concentrations appropriate to the response of each compound (Section 
6.13); nominally, 10, 20, 50, 100, and 200 [micro]g/mL. The amount of 
internal standard added to each extract is the same (100 [micro]g/mL) so 
that Cis remains constant. The RF is plotted vs concentration 
for each compound in the standard (Cs) to produce a 
calibration curve.
    7.5.1.2 Linearity--if the response factor (RF) for any compound is 
constant (less than 35 percent coefficient of variation) over the 5

[[Page 367]]

point calibration range, an averaged response factor may be used for 
that compound; otherwise, the complete calibration curve for that 
compound shall be used over the 5 point range.
    7.6 Combined calibration--by using calibration solutions (Section 
6.13) containing the pollutants, labeled compounds, and the internal 
standard, a single set of analyses can be used to produce calibration 
curves for the isotope dilution and internal standard methods. These 
curves are verified each shift (Section 12.5) by analyzing the 100 
[micro]g/mL calibration standard (Section 6.13). Recalibration is 
required only if calibration verification (Section 12.5) criteria cannot 
be met.

                  8. Quality Assurance/Quality Control

    8.1 Each laboratory that uses this method is required to operate a 
formal quality assurance program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability, 
analysis of samples spiked with labeled compounds to evaluate and 
document data quality, and analysis of standards and blanks as tests of 
continued performance. Laboratory performance is compared to established 
performance criteria to determine if the results of analyses meet the 
performance characteristics of the method.
    8.1.1 The analyst shall make an initial demonstration of the ability 
to generate acceptable accuracy and precision with this method. This 
ability is established as described in Section 8.2.
    8.1.2 The analyst is permitted to modify this method to improve 
separations or lower the costs of measurements, provided all performance 
specifications are met. Each time a modification is made to the method, 
the analyst is required to repeat the procedure in Section 8.2 to 
demonstrate method performance.
    8.1.3 Analyses of blanks are required to demonstrate freedom from 
contamination. The procedures and criteria for analysis of a blank are 
described in Section 8.5.
    8.1.4 The laboratory shall spike all samples with labeled compounds 
to monitor method performance. This test is described in Section 8.3. 
When results of these spikes indicate atypical method performance for 
samples, the samples are diluted to bring method performance within 
acceptable limits (Section 15).
    8.1.5 The laboratory shall, on an on-going basis, demonstrate 
through calibration verification and the analysis of the precision and 
recovery standard (Section 6.14) that the analysis system is in control. 
These procedures are described in Sections 12.1, 12.5, and 12.7.
    8.1.6 The laboratory shall maintain records to define the quality of 
data that is generated. Development of accuracy statements is described 
in Section 8.4.
    8.2 Initial precision and accuracy--to establish the ability to 
generate acceptable precision and accuracy, the analyst shall perform 
the following operations:
    8.2.1 Extract, concentrate, and analyze two sets of four one-liter 
aliquots (8 aliquots total) of the precision and recovery standard 
(Section 6.14) according to the procedure in Section 10.
    8.2.2 Using results of the first set of four analyses, compute the 
average recovery (X) in [micro]g/mL and the standard deviation of the 
recovery (s) in [thetas]g/[micro]L for each compound, by isotope 
dilution for pollutants with a labeled analog, and by internal standard 
for labeled compounds and pollutants with no labeled analog.
    8.2.3 For each compound, compare s and X with the corresponding 
limits for initial precision and accuracy in Table 8. If s and X for all 
compounds meet the acceptance criteria, system performance is acceptable 
and analysis of blanks and samples may begin. If, however, any 
individual s exceeds the precision limit or any individual X falls 
outside the range for accuracy, system performance is unacceptable for 
that compound.
    Note: The large number of compounds in Table 8 present a substantial 
probability that one or more will fail the acceptance criteria when all 
compounds are analyzed. To determine if the analytical system is out of 
control, or if the failure can be attributed to probability, proceed as 
follows:
    8.2.4 Using the results of the second set of four analyses, compute 
s and X for only those compounds which failed the test of the first set 
of four analyses (Section 8.2.3). If these compounds now pass, system 
performance is acceptable for all compounds and analysis of blanks and 
samples may begin. If, however, any of the same compoulds fail again, 
the analysis system is not performing properly for these compounds. In 
this event, correct the problem and repeat the entire test (Section 
8.2.1).
    8.3 The laboratory shall spike all samples with labeled compounds to 
assess method performance on the sample matrix.
    8.3.1 Analyze each sample according to the method in Section 10.
    8.3.2 Compute the percent recovery (P) of the labeled compounds 
using the internal standard methmd (Section 7.5).
    8.3.3 Compare the labeled compound recovery for each compound with 
the corresponding limits in Table 8. If the recovery of any compounds 
falls outside its warning limit, method performance is unacceptable for 
that compound in that sample, Therefore, the sample is complex and is to 
be diluted and reanalyzed per Section 15.4.
    8.4 As part of the QA program for the laboratory, method accuracy 
for wastewater samples shall be assessed and records shall

[[Page 368]]

be maintained. After the analysis of five wastewater samples for which 
the labeled compounds pass the tests in Section 8.3, compute the average 
percent recovery (P) and the standard deviation of the percent recovery 
(sp) for the labeled compounds only. Express the accuracy 
assessment as a percent recovery interval from P--2 sp to P + 
2sp. For example, if P = 90% and sp = 10%, the 
accuracy interval is expressed as 70-100%. Update the accuracy 
assessment for each compound on a regular basis (e.g. after each 5-10 
new accuracy measurements).
    8.5 Blanks--reagent water blanks are analyzed to demonstrate freedom 
from contamination.
    8.5.1 Extract and concentrate a blank with each sample lot (samples 
started through the extraction process on the same 8 hr shift, to a 
maximum of 20 samples). Analyze the blank immediately after analysis of 
the precision and recovery standard (Section 6.14) to demonstrate 
freedom from contamination.
    8.5.2 If any of the compounds of interest (Tables 1 and 2) or any 
potentially interfering compound is found in a blank at greater than 10 
[micro]g/L (assuming a response factor of 1 relative to the internal 
standard for compounds not listed in Tables 1 and 2), analysis of 
samples is halted until the source of contamination is eliminated and a 
blank shows no evidence of contamination at this level.
    8.6 The specifications contained in this method can be met if the 
apparatus used is calibrated properly, then maintained in a calibrated 
state. The standards used for calibration (Section 7), calibration 
verification (Section 12.5), and for initial (Section 8.2) and on-going 
(Section 12.7) precision and recovery should be identical, so that the 
most precise results will be obtained. The GC/MS instrument in 
particular will provide the most reproducible results if dedicated to 
the settings and conditions required for the analysis of semi-volatiles 
by this method.
    8.7 Depending on specific program requirements, field replicates may 
be collected to determine the precision of the sampling technique, and 
spiked samples may be required to determine the accuracy of the analysis 
when internal or external standard methods are used.

            9. Sample Collection, Preservation, and Handling

    9.1 Collect samples in glass containers following conventional 
sampling practices (Reference 7). Composite samples are collected in 
refrigerated glass containers (Section 5.1.3) in accordance with the 
requirements of the sampling program.
    9.2 Maintain samples at 0-4 [deg]C from the time collectimn until 
extraction. If residual chlorine is present, add 80 mg sodium 
thiosulfate per liter of water. EPA Methods 330.4 and 330.5 may be used 
to measure residual chlorine (Reference 8).
    9.3 Begin sample extraction within seven days of collection, and 
analyze all extracts within 40 days of extraction.

         10. Sample Extraction and Concentration (See Figure 4)

    10.1 Labeled compound spiking--measure 1.00 0.01 liter of sample into a glass container. For 
untreated effluents, and samples which are expected to be difficult to 
extract and/or concentrate, measure an additional 10.0 0.1 mL and dilute to a final volume of 1.00 0.01 liter with reagent water in a glass container.
    10.1.1 For each sample or sample lot (to a maximum of 20) to be 
extracted at the same time, place three 1.00 0.10 
liter aliquots of reagent water in glass containers.
    10.1.2 Spike 0.5 mL of the labeled compound spiking solution 
(Section 6.8) into all samples and one reagant water aliquot.
    10.1.3 Spike 1.0 mL of the precision and recovery standard (Section 
6.14) into the two remaining reagent water aliquots.
    10.1.4 Stir and equilibrate all solutions for 1-2 hr.
    10.2 Base/neutral extraction--place 100-150 mL methylene chloride in 
each continuous extractor and 200-300 in each distilling flask.
    10.2.1 Pour the sample(s), blank, and standard aliquots into the 
extractors. Rinse the glass containers with 50-100 mL methylene chloride 
and add to the respective extractor.
    10.2.2 Adjust the pH of the waters in the extractors to 12-13 with 
6N NaOH while monitoring with a pH meter. Begin the extraction by 
heating the flask until the methylene chloride is boiling. When properly 
adjusted, 1-2 drops of methylene chloride per second will fall from the 
condensor tip into the water. After 1-2 hours of extraction, test the pH 
and readjust to 12-13 if required. Extract for 18-24 hours.
    10.2.3 Remove the distilling flask, estimate and record the volume 
of extract (to the nearest 100 mL), and pour the contents through a 
drying column containing 7 to 10 cm anhydrous sodium sulfate. Rinse the 
distilling flask with 30-50 mL of methylene chloride and pour through 
the drying column. Collect the solution in a 500 mL K-D evaporator flask 
equipped with a 10 mL concentrator tube. Seal, label as the base/neutral 
fraction, and concentrate per Sections 10.4 to 10.5.
    10.3 Acid extraction--adjust the pH of the waters in the extractors 
to 2 or less using 6N sulfuric acid. Charge clean distilling flasks with 
300-400 mL of methylene chloride. Test and adjust the pH of the waters 
after the first 1-2 hr of extraction. Extract for 18-24 hours.
    10.3.1 Repeat Section 10.2.3, except label as the acid fraction.

[[Page 369]]

    10.4 Concentration--concentrate the extracts in separate 500 mL K-D 
flasks equipped with 10 mL concentrator tubes.
    10.4.1 Add 1 to 2 clean boiling chips to the flask and attach a 
three-ball macro Snyder column. Prewet the column by adding 
approximately one mL of methylene chloride through the top. Place the K-
D apparatus in a hot water bath so that the entire lower rounded surface 
of the flask is bathed with steam. Adjust the vertical position of the 
apparatus and the water temperature as required to complete the 
concentration in 15 to 20 minutes. At the proper rate of distillation, 
the balls of the column will actively chatter but the chambers will not 
flood. When the liquid has reached an apparent volume of 1 mL, remove 
the K-D apparatus from the bath and allow the solvent to drain and cool 
for at least 10 minutes. Remove the Snyder column and rinse the flask 
and its lower joint into the concentrator tube with 1-2 mL of methylene 
chloride. A 5-mL syringe is recommended for this operation.
    10.4.2 For performance standards (Sections 8.2 and 12.7) and for 
blanks (Section 8.5), combine the acid and base/neutral extracts for 
each at this point. Do not combine the acid and base/neutral extracts 
for samples.
    10.5 Add a clean boiling chip and attach a two ball micro Snyder 
column to the concentrator tube. Prewet the column by adding approx 0.5 
mL methylene chloride through the top. Place the apparatus in the hot 
water bath. Adjust the vertical position and the water temperature as 
required to complete the concentration in 5-10 minutes. At the proper 
rate of distillation, the balls of the column will actively chatter but 
the chambers will not flood. When the liquid reaches an apparent volume 
of approx 0.5 mL, remove the apparatus from the water bath and allow to 
drain and cool for at least 10 minutes. Remove the micro Snyder column 
and rinse its lower joint into the concentrator tube with approx 0.2 mL 
of methylene chloride. Adjust the final volume to 1.0 mL.
    10.6 Transfer the concentrated extract to a clean screw-cap vial. 
Seal the vial with a Teflon-lined lid, and mark the level on the vial. 
Label with the sample number and fraction, and store in the dark at -20 
to -10 [deg]C until ready for analysis.

                           11. GC/MS Analysis

    11.1 Establish the operating conditions given in Table 3 or 4 for 
analysis of the base/neutral or acid extracts, respectively. For 
analysis of combined extracts (Section 10.4.2), use the operating 
conditions in Table 3.
    11.2 Bring the concentrated extract (Section 10.6) or standard 
(Sections 6.13 through 6.14) to room temperature and verify that any 
precipitate has redissolved. Verify the level on the extract (Sections 
6.6 and 10.6) and bring to the mark with solvent if required.
    11.3 Add the internal standard solution (Section 6.10) to the 
extract (use 1.0 uL of solution per 0.1 mL of extract) immediately prior 
to injection to minimize the possibility of loss by evaporation, 
adsorption, or reaction. Mix thoroughly.
    11.4 Inject a volume of the standard solution or extract such that 
100 ng of the internal standard will be injected, using on-column or 
splitless injection. For 1 mL extracts, this volume will be 1.0 uL. 
Start the GC column initial isothermal hold upon injection. Start MS 
data collection after the solvent peak elutes. Stop data collection 
after the benzo (ghi) perylene or pentachlorophenol peak elutes for the 
base/neutral or acid fraction, respectively. Return the column to the 
initial temperature for analysis of the next sample.

                  12. System and Laboratory Performance

    12.1 At the beginning of each 8 hr shift during which analyses are 
performed, GC/MS system performance and calibration are verified for all 
pollutants and labeled compounds. For these tests, analysis of the 100 
[micro]g/mL calibration standard (Section 6.13) shall be used to verify 
all performance criteria. Adjustment and/or recalibration (per Section 
7) shall be performed until all performance criteria are met. Only after 
all performance criteria are met may samples, blanks, and precision and 
recovery standards be analyzed.
    12.2 DFTPP spectrum validity--inject 1 [micro]L of the DFTPP 
solution (Section 6.11) either separately or within a few seconds of 
injection of the standard (Section 12.1) analyzed at the beginning of 
each shift. The criteria in Table 5 shall be met.
    12.3 Retention times--the absolute retention time of 2,2'-
difluorobiphenyl shall be within the range of 1078 to 1248 seconds and 
the relative retention times of all pollutants and labeled compounds 
shall fall within the limits given in Tables 3 and 4.
    12.4 GC resolution--the valley height between anthracene and 
phenanthrene at m/z 178 (or the analogs at m/z 188) shall not exceed 10 
percent of the taller of the two peaks.
    12.5 Calibration verification--compute the concentration of each 
pollutant (Tables 1 and 2) by isotope dilution (Section 7.4) for those 
compounds which have labeled analogs. Compute the concentration of each 
pollutant which has no labeled analog by the internal standard method 
(Section 7.5). Compute the concentration of the labeled compounds by the 
internal standard method. These concentrations are computed based on the 
calibration data determined in Section 7.
    12.5.1 For each pollutant and labeled compound being tested, compare 
the concentration with the calibration verification limit

[[Page 370]]

in Table 8. If all compounds meet the acceptance criteria, calibration 
has been verified and analysis of blanks, samples, and precision and 
recovery standards may proceed. If, however, any compound fails, the 
measurement system is not performing properly for that compound. In this 
event, prepare a fresh calibration standard or correct the problem 
causing the failure and repeat the test (Section 12.1), or recalibrate 
(Section 7).
    12.6 Multiple peaks--each compound injected shall give a single, 
distinct GC peak.
    12.7 On-going precision and accuracy.
    12.7.1 Analyze the extract of one of the pair of precision and 
recovery standards (Section 10.1.3) prior to analysis of samples from 
the same lot.
    12.7.2 Compute the concentration of each pollutant (Tables 1 and 2) 
by isotope dilution (Section 7.4) for those compounds which have labeled 
analogs. Compute the concentration of each pollutant which has no 
labeled analog by the internal standard method (Section 7.5). Compute 
the concentration of the labeled compounds by the internal standard 
method.
    12.7.3 For each pollutant and labeled compound, compare the 
concentration with the limits for on-going accuracy in Table 8. If all 
compounds meet the acceptance criteria, system performance is acceptable 
and analysis of blanks and samples may proceed. If, however, any 
individual concentration falls outside of the range given, system 
performance is unacceptable for that compound.
    Note: The large number of compounds in Table 8 present a substantial 
probability that one or more will fail when all compounds are analyzed. 
To determine if the extraction/concentration system is out of control or 
if the failure is caused by probability, proceed as follows:
    12.7.3.1 Analyze the second aliquot of the pair of precision and 
recovery standard (Section 10.1.3).
    12.7.3.2 Compute the concentration of only those pollutants or 
labeled compounds that failed the previous test (Section 12.7.3). If 
these compounds now pass, the extraction/concentration processes are in 
control and analysis of blanks and samples may proceed. If, however, any 
of the same compounds fail again, the extraction/concentration processes 
are not being performed properly for these compounds. In this event, 
correct the problem, re-extract the sample lot (Section 10) and repeat 
the on-going precision and recovery test (Section 12.7).
    12.7.4 Add results which pass the specifications in Section 12.7.2 
to initial and previous on-going data. Update QC charts to perform a 
graphic representation of continued laboratory performance (Figure 5). 
Develop a statement of laboratory accuracy for each pollutant and 
labeled compound by calculating the average percent recovery (R) and the 
standard deviation of percent recovery (sr). Express the 
accuracy as a recovery interval from R-2sr to R + 
2sr. For example, if R = 95% and sr = 5%, the 
accuracy is 85-105%.

                      13. Qualitative Determination

    13.1 Qualititative determination is accomplished by comparison of 
data from analysis of a sample or blank with data from analysis of the 
shift standard (Section 12.1) and with data stored in the spectral 
libraries (Section 7.2.4). Identification is confirmed when spectra and 
retention times agree per the criteria below.
    13.2 Labeled compounds and pollutants having no labeled analog:
    13.2.1 The signals for all characteristic masses stored in the 
spectral library (Section 7.2.4) shall be present and shall maximize 
within the same two consecutive scans.
    13.2.2 Either (1) the background corrected EICP areas, or (2) the 
corrected relative intensities of the mass spectral peaks at the GC peak 
maximum shall agree within a factor of two (0.5 to 2 times) for all 
masses stored in the library.
    13.2.3 The retention time relative to the nearest eluted internal 
standard shall be within 15 scans or 15 seconds, whichever is greater of this difference in 
the shift standard (Section 12.1).
    13.3 Pollutants having a labled analog:
    13.3.1 The signals for all characteristic masses stored in the 
spectral library (Section 7.2.4) shall be present and shall maximize 
within the same two consecutive scans.
    13.3.2. Either (1) the background corrected EICP areas, or (2) the 
corrected relative intensities of the mass spectral peaks at the GC peak 
maximum shall agree within a factor of two for all masses stored in the 
spectral library.
    13.3.3. The retention time difference between the pollutant and its 
labeled analog shall agree within 6 scans or 
6 seconds (whichever is greater) of this 
difference in the shift standard (Section 12.1).
    13.4 Masses present in the experimental mass spectrum that are not 
present in the reference mass spectrum shall be accounted for by 
contaminant or background ions. If the experimental mass spectrum is 
contaminated, an experienced spectrometrist (Section 1.4) is to 
determine the presence or absence of the cmmpound.

                     14. Quantitative Determination

    14.1 Isotope dilution--by adding a known amount of a labeled 
compound to every sample prior to extraction, correction for recovery of 
the pollutant can be made because the pollutant and its labeled analog 
exhibit the same effects upon extraction, concentration, and gas 
chromatography. Relative response (RR) values for mixtures are used in 
conjunction with calibration curves described in

[[Page 371]]

Section 7.4 to determine concentrations directly, so long as labeled 
compound spiking levels are constant. For the phenml example given in 
Figure 1 (Section 7.4.1), RR would be equal to 1.114. For this RR value, 
the phenol calibration curve given in Figure 1 indicates a concentration 
of 27 [micro]g/mL in the sample extract (Cex).
    14.2 Internal standard--compute the concentration in the extract 
using the response factor determined from calibration data (Section 7.5) 
and the following equation: Cex([micro]g/mL) = (As 
x Cis/(Ais x RF) where Cex is the 
concentration of the compound in the extract, and the other terms are as 
defined in Section 7.5.1.
    14.3 The concentration of the pollutant in water is computed using 
the volumes of the original water sample (Section 10.1) and the final 
extract volume (Section 10.5), as follows: Concentration in water 
([micro]g/L) = (Cex x Vex)/Vs where 
Vex is the extract volume in mL, and Vs is the 
sample volume in liters.
    14.4 If the EICP area at the quantitiation mass for any compound 
exceeds the calibration range of the system, the extract of the dilute 
aliquot (Section 10.1) is analyzed by isotope dilution; otherwise, the 
extract is diluted by a factor of 10, 9 [micro]L of internal standard 
solution (Section 6.10) are added to a 1.0 mL aliquot, and this diluted 
extract is analyzed by the internal standard method (Section 14.2). 
Quantify each compound at the highest concentration level within the 
calibration range.
    14.5 Report results for all pollutants and labeled compounds (Tables 
1 and 2) found in all standards, blanks, and samples in [micro]g/L, to 
three significant figures. Results for samples which have been diluted 
are reported at the least dilute level at which the area at the 
quantitation mass is within the calibration range (Section 14.4) and the 
labeled compound recovery is within the normal range for the method 
(Section 15.4).

                     15. Analysis of Complex Samples

    15.1 Untreated effluents and other samples frequently contain high 
levels (1000 [micro]g/L) of the compounds of interest, 
interfering compounds, and/or polymeric materials. Some samples will not 
concentrate to one mL (Section 10.5); others will overload the GC column 
and/or mass spectrometer.
    15.2 Analyze the dilute aliquot (Section 10.1) when the sample will 
not concentrate to 1.0 mL. If a dilute aliquot was not extracted, and 
the sample holding time (Section 9.3) has not been exceeded, dilute an 
aliquot of the sample with reagent water and re-extract (Section 10.1); 
otherwise, dilute the extract (Section 14.4) and analyze by the internal 
standard method (Section 14.2).
    15.3 Recovery of internal standard--the EICP area of the internal 
standard should be within a factor of two of the area in the shift 
standard (Section 12.1). If the absolute areas of the labeled compounds 
are within a factor of two of the respective areas in the shift 
standard, and the internal standard area is less than one-half of its 
respective area, then internal standard loss in the extract has 
occurred. In this case, use one of the labeled compounds (perferably a 
polynuclear aromatic hydrocarbon) to compute the concentration of a 
pollutant with no labeled analog.
    15.4 Recovery of labeled compounds--in most samples, labeled 
compound recoveries will be similar to those from reagent water (Section 
12.7). If the labeled compound recovery is outside the limits given in 
Table 8, the dilute extract (Section 10.1) is analyzed as in Section 
14.4. If the recoveries of all labeled compounds and the internal 
staldard are low (per the criteria above), then a loss in instrument 
sensitivity is the most likely cause. In this case, the 100 [micro]g/mL 
calibration standard (Section 12.1) shall be analyzed and calibration 
verified (Section 12.5). If a loss in sensitivity has occurred, the 
instrument shall be repaired, the performance specifications in Section 
12 shall be met, and the extract reanalyzed. If a loss in instrument 
sensitivity has not occurred, the method does not work on the sample 
being analyzed and the result may not be reported for regulatory 
compliance purposes.

                         16. Method Performance

    16.1 Interlaboratory performance for this method is detailed in 
references 9 and 10.
    16.2 A chromatogram of the 100 [micro]g/mL acid/base/neutral 
calibration standard (Section 6.13) is shown in Figure 6.

                               References

    1. ``Performance Tests for the Evaluation of Computerized Gas 
Chromatography/Mass Spectrometry Equipment and Laboratories'' USEPA, 
EMSL/Cincinnati, OH 45268, EPA-600/4-80-025 (April 1980).
    2. ``Working with Carcinogens,'' DHEW, PHS, CDC, NIOSH, Publication 
77-206, (August 1977).
    3. ``OSHA Safety and Health Standards, General Industry'' OSHA 2206, 
29 CFR part 1910 (January 1976).
    4. ``Safety in Academic Chemistry Laboratories, '' ACS Committee on 
Chemical Safety (1979).
    5. ``Reference Compound to Calibrate Ion Abundance Measurement in 
Gas Chromatography-Mass Spectrometry Systems,'' J.W. Eichelberger, L.E. 
Harris, and W.L. Budde, Anal. Chem., 47, 955 (1975).
    6. ``Handbook of Analytical Quality Control in Water and Wastewater 
Laboratories,'' USEPA, EMSL/Cincinnati, OH 45268, EPA-600/4-79-019 
(March 1979).
    7. ``Standard Practice for Sampling Water,'' ASTM Annual Book of 
Standards, ASTM, Philadelphia, PA, 76 (1980).

[[Page 372]]

    8. ``Methods 330.4 and 330.5 for Total Residual Chlorine,'' USEPA, 
EMSL/ Cincinnati, OH 45268, EPA 600/4-70-020 (March 1979).
    9. Colby, B.N., Beimer, R.G., Rushneck, D.R., and Telliard, W.A., 
``Isotope Dilution Gas Chromatography-Mass Spectrometry for the 
determination of Priority Pollutants in Industrial Effluents.'' USEPA, 
Effluent Guidelines Division, Washington, DC 20460 (1980).
    10. ``Inter-laboratory Validation of US Environmental Protection 
Agency Method 1625,'' USEPA, Effluent Guidelines Division, Washington, 
DC 20460 (June 15, 1984).

               Table 1--Base/Neutral Extractable Compounds
------------------------------------------------------------------------
                                             CAS
           Compound             STORET     registry    EPA-EGD    NPDES
------------------------------------------------------------------------
Acenaphthene.................     34205      83-32-9     001 B     001 B
Acenaphthylene...............     34200     208-96-8     077 B     002 B
Anthracene...................     34220     120-12-7     078 B     003 B
Benzidine....................     39120      92-87-5     005 B     004 B
Benzo(a)anthracene...........     34526      56-55-3     072 B     005 B
Benzo(b)fluoranthene.........     34230     205-99-2     074 B     007 B
Benzo(k)fluoranthene.........     34242     207-08-9     075 B     009 B
Benzo(a)pyrene...............     34247      50-32-8     073 B     006 B
Benzo(ghi)perylene...........     34521     191-24-2     079 B     008 B
Biphenyl (Appendix C)........     81513      92-52-4     512 B
Bis(2-chloroethyl) ether.....     34273     111-44-4     018 B     011 B
Bis(2-chloroethyoxy)methane..     34278     111-91-1     043 B     010 B
Bis(2-chloroisopropyl) ether.     34283     108-60-1     042 B     012 B
Bis(2-ethylhexyl) phthalate..     39100     117-81-7     066 B     013 B
4-bromophenyl phenyl ether...     34636     101-55-3     041 B     014 B
Butyl benzyl phthalate.......     34292      85-68-7     067 B     015 B
n-C10 (Appendix C)...........     77427     124-18-5     517 B
n-C12 (Appendix C)...........     77588     112-40-2     506 B
n-C14 (Appendix C)...........     77691     629-59-4     518 B
n-C16 (Appendix C)...........     77757     544-76-3     519 B
n-C18 (Appendix C)...........     77804     593-45-3     520 B
n-C20 (Appendix C)...........     77830     112-95-8     521 B
n-C22 (Appendix C)...........     77859     629-97-0     522 B
n-C24 (Appendix C)...........     77886     646-31-1     523 B
n-C26 (Appendix C)...........     77901     630-01-3     524 B
n-C28 (Appendix C)...........     78116     630-02-4     525 B
n-C30 (Appendix C)...........     78117     638-68-6     526 B
Carbazole (4c)...............     77571      86-74-8     528 B
2-chloronaphthalene..........     34581      91-58-7     020 B     016 B
4-chlorophenyl phenyl ether..     34641    7005-72-3     040 B     017 B
Chrysene.....................     34320     218-01-9     076 B     018 B
P-cymene (Appendix C)........     77356      99-87-6     513 B
Dibenzo(a,h)anthracene.......     34556      53-70-3     082 B     019 B
Dibenzofuran (Appendix C and      81302     132-64-9     505 B
 4c).........................
Dibenzothiophene (Synfuel)...     77639     132-65-0     504 B
Di-n-butyl phthalate.........     39110      84-74-2     068 B     026 B
1,2-dichlorobenzene..........     34536      95-50-1     025 B     020 B
1,3-dichlorobenzene..........     34566     541-73-1     026 B     021 B
1,4-dichlorobenzene..........     34571     106-46-7     027 B     022 B
3,3'-dichlorobenzidine.......     34631      91-94-1     028 B     023 B
Diethyl phthalate............     34336      84-66-2     070 B     024 B
2,4-dimethylphenol...........     34606     105-67-9     034 A     003 A
Dimethyl phthalate...........     34341     131-11-3     071 B     025 B
2,4-dinitrotoluene...........     34611     121-14-2     035 B     027 B
2,6-dinitrotoluene...........     34626     606-20-2     036 B     028 B
Di-n-octyl phthalate.........     34596     117-84-0     069 B     029 B
Diphenylamine (Appendix C)...     77579     122-39-4     507 B
Diphenyl ether (Appendix C)..     77587     101-84-8     508 B
1,2-diphenylhydrazine........     34346     122-66-7     037 B     030 B
Fluoranthene.................     34376     206-44-0     039 B     031 B
Fluorene.....................     34381      86-73-7     080 B     032 B
Hexachlorobenzene............     39700     118-74-1     009 B     033 B
Hexachlorobutadiene..........     34391      87-68-3     052 B     034 B
Hexachloroethane.............     34396      67-72-1     012 B     036 B
Hexachlorocyclopentadiene....     34386      77-47-4     053 B     035 B
Indeno(1,2,3-cd)pyrene.......     34403     193-39-5     083 B     037 B
Isophorone...................     34408      78-59-1     054 B     038 B
Naphthalene..................     34696      91-20-3     055 B     039 B
B-naphthylamine (Appendix C).     82553      91-59-8     502 B
Nitrobenzene.................     34447      98-95-3     056 B     040 B
N-nitrosodimethylamine.......     34438      62-75-9     061 B     041 B
N-nitrosodi-n-propylamine....     34428     621-64-7     063 B     042 B
N-nitrosodiphenylamine.......     34433      86-30-3     062 B     043 B

[[Page 373]]

 
Phenanthrene.................     34461      85-01-8     081 B     044 B
Phenol.......................     34694     108-95-2     065 A     010 A
a-Picoline (Synfuel).........     77088    109-06-89     503 B
Pyrene.......................     34469     129-00-0     084 B     045 B
styrene (Appendix C).........     77128     100-42-5     510 B
a-terpineol (Appendix C).....     77493      98-55-5     509 B
1,2,3-trichlorobenzene (4c)..     77613      87-61-6     529 B
1,2,4-trichlorobenzene.......     34551     120-82-1     008 B     046 B
------------------------------------------------------------------------


                   Table 2--Acid Extractable Compounds
------------------------------------------------------------------------
                                             CAS
           Compound             STORET     registry    EPA-EGD    NPDES
------------------------------------------------------------------------
4-chloro-3-methylphenol......     34452      59-50-7     022 A     008 A
2-chlorophenol...............     34586      95-57-8     024 A     001 A
2,4-dichlorophenol...........     34601     120-83-2     031 A     002 A
2,4-dinitrophenol............     34616      51-28-5     059 A     005 A
2-methyl-4,6-dinitrophenol...     34657     534-52-1     060 A     004 A
2-nitrophenol................     34591      88-75-5     057 A     006 A
4-nitrophenol................     34646     100-02-7     058 A     007 A
Pentachlorophenol............     39032      87-86-5     064 A     009 A
2,3,6-trichlorophenol (4c)...     77688     93-37-55     530 A
2,4,5-trichlorophenol (4c)...  ........      95-95-4     531 A
2,4,6-trichlorophenol........     34621      88-06-2     021 A     011 A
------------------------------------------------------------------------


    Table 3--Gas Chromatography of Base/Neutral Extractable Compounds
------------------------------------------------------------------------
                                    Retention time             Detection
  EGD                    ------------------------------------  limit \2\
  No.       Compound        Mean                              ([micro]g/
  \1\                       (sec)    EGD Ref     Relative         L)
------------------------------------------------------------------------
   164  2,2'-                 1163       164     1.000-1.000         10
         difluorobipheny
         l (int std)....
   061  N-                     385       164        ns               50
         nitrosodimethyl
         amine..........
   603  alpha picoline-        417       164     0.326-0.393         50
         d7.............
   703  alpha picoline..       426       603     1.006-1.028         50
   610  styrene-d5......       546       164     0.450-0.488         10
   710  styrene.........       549       610     1.002-1.009         10
   613  p-cymene-d14....       742       164     0.624-0.652         10
   713  p-cymene........       755       613     1.008-1.023         10
   265  phenol-d5.......       696       164     0.584-0.613         10
   365  phenol..........       700       265     0.995-1.010         10
   218  bis(2-                 696       164     0.584-0.607         10
         chloroethyl)
         ether-d8.......
   318  bis(2-                 704       218     1.007-1.016         10
         chloroethyl)
         ether..........
   617  n-decane-d22....       698       164     0.585-0.615         10
   717  n-decane........       720       617     1.022-1.038         10
   226  1,3-                   722       164     0.605-0.636         10
         dichlorobenzene-
         d4.............
   326  1,3-                   724       226     0.998-1.008         10
         dichlorobenzene
   227  1,4-                   737       164     0.601-0.666         10
         dichlorobenzene-
         d4.............
   327  1,4-                   740       227     0.997-1.009         10
         dichlorobenzene
   225  1,2-                   758       164     0.632-0.667         10
         dichlorobenzene-
         d4.............
   325  1,2-                   760       225     0.995-1.008         10
         dichlorobenzene
   242  bis(2-                 788       164     0.664-0.691         10
         chloroisopropyl
         ) ether-d12....
   342  bis(2-                 799       242     1.010-1.016         10
         chloroisopropyl
         ) ether........
   212  hexachloroethane-      819       164     0.690-0.717         10
         13C............
   312  hexachloroethane       823       212     0.999-1.001         10
   063  N-nitrosodi-n-         830       164        ns               20
         propylamine....
   256  nitrobenzene-d5.       845       164     0.706-0.727         10
   356  nitrobenzene....       849       256     1.002-1.007         10
   254  isophorone-d8...       881       164     0.747-0.767         10
   354  isophorone......       889       254     0.999-1.017         10
   234  2,4-dimethyl           921       164     0.781-0.803         10
         phenol-d3......
   334  2,4-                   924       234     0.999-1.003         10
         dimethylphenol.
   043  bis(2-                 939       164        ns               10
         chloroethoxy)
         methane........
   208  1,2,4-                 955       164     0.813-0.830         10
         trichlorobenzen
         e-d3...........
   308  1,2,4-                 958       208     1.000-1.005         10
         trichlorobenzen
         e..............
   255  naphthalene-d8..       963       164     0.819-0.836         10
   355  naphthalene.....       967       255     1.001-1.006         10
   609  alpha-terpineol-       973       164     0.829-0.844         10
         d3.............

[[Page 374]]

 
   709  alpha-terpineol.       975       609     0.998-1.008         10
   606  n-dodecane-d26..       953       164     0.730-0.908         10
   706  n-dodecane......       981       606     0.986-1.051         10
   529  1,2,3-                1003       164        ns               10
         trichlorobenzen
         e..............
   252  hexachlorobutadi      1005       164     0.856-0.871         10
         ene-13C4.......
   352  hexachlorobutadi      1006       252     0.999-1.002         10
         ene............
   253  hexachlorocyclop      1147       164     0.976-0.986         10
         entadiene-13C4.
   353  hexachlorocyclop      1142       253     0.999-1.001         10
         entadiene......
   220  2-                    1185       164     1.014-1.024         10
         chloronaphthale
         ne-d7..........
   320  2-                    1200       220     0.997-1.007         10
         chloronaphthale
         ne.............
   518  n-tetradecane...      1203       164        ns               10
   612  Biphenyl-d10....      1205       164     1.016-1.027         10
   712  Biphenyl........      1195       612     1.001-1.006         10
   608  Diphenyl ether-       1211       164     1.036-1.047         10
         d10............
   708  Diphenyl ether..      1216       608     0.997-1.009         10
   277  Acenaphthylene-       1265       164     1.080-1.095         10
         d8.............
   377  Acenaphthylene..      1247       277     1.000-1.004         10
   271  Dimethyl              1269       164     1.083-1.102         10
         phthalate-d4...
   371  Dimethyl              1273       271     0.998-1.005         10
         phthalate......
   236  2,6-                  1283       164     1.090-1.112         10
         dinitrotoluene-
         d3.............
   336  2,6-                  1300       236     1.001-1.005         10
         dinitrotoluene.
   201  Acenaphthene-d10      1298       164     1.107-1.125         10
   301  Acenaphthene....      1304       201     0.999-1.009         10
   605  Dibenzofuran-d8.      1331       164     1.134-1.155         10
   705  Dibenzofuran....      1335       605     0.998-1.007         10
   602  Beta-                 1368       164     1.163-1.189         50
         naphthylamine-
         d7.............
   702  Beta-                 1371       602     0.996-1.007         50
         naphthylamine..
   280  Fluorene-d10....      1395       164     1.185-1.214         10
   380  Fluorene........      1401       281     0.999-1.008         10
   240  4-chlorophenyl        1406       164     1.194-1.223         10
         phenyl ether-d5
   340  4-chlorophenyl        1409       240     0.990-1.015         10
         phenyl ether...
   270  Diethyl               1409       164     1.197-1.229         10
         phthalate-d4...
   370  Diethyl               1414       270     0.996-1.006         10
         phthalate......
   619  n-hexadecane-d34      1447       164     1.010-1.478         10
   719  n-hexadecane....      1469       619     1.013-1.020         10
   235  2,4-                  1359       164     1.152-1.181         10
         dinitrotoluene-
         d3.............
   335  2,4-                  1344       235     1.000-1.002         10
         dinitrotoluene.
   237  1,2-                  1433       164     1.216-1.248         20
         diphenylhydrazi
         ne-d8..........
   337  1,2-                  1439       237     0.999-1.009         20
         diphenylhydrazi
         ne (\3\).......
   607  Diphenylamine-        1437       164     1.213-1.249         20
         d10............
   707  Diphenylamine...      1439       607     1.000-1.007         20
   262  N-                    1447       164     1.225-1.252         20
         nitrosodiphenyl
         amine-d6.......
   362  N-                    1464       262     1.000-1.002         20
         nitrosodiphenyl
         amine (\4\)....
   041  4-bromophenyl         1498       164     1.271-1.307         10
         phenyl ether...
   209  Hexachlorobenzen      1521       164     1.288-1.327         10
         e-13C6.........
   309  Hexachlorobenzen      1522       209     0.999-1.001         10
         e..............
   281  Phenanthrene-d10      1578       164     1.334-1.380         10
   520  n-octadecane....      1580       164        ns               10
   381  Phenanthrene....      1583       281     1.000-1.005         10
   278  Anthracene-d10..      1588       164     1.342-1.388         10
   378  Anthracene......      1592       278     0.998-1.006         10
   604  Dibenzothiophene-     1559       164     1.314-1.361         10
         d8.............
   704  Dibenzothiophene      1564       604     1.000-1.006         10
   528  Carbazole.......      1650       164        ns               20
   621  n-eicosane-d42..      1655       164     1.184-1.662         10
   721  n-eicosane......      1677       621     1.010-1.021         10
   268  Di-n-butyl            1719       164     1.446-1.510         10
         phthalate-d4...
   368  Di-n-butyl            1723       268     1.000-1.003         10
         phthalate......
   239  Fluoranthene-d10      1813       164     1.522-1.596         10
   339  Fluoranthene....      1817       239     1.000-1.004         10
   284  Pyrene-d10......      1844       164     1.523-1.644         10
   384  Pyrene..........      1852       284     1.001-1.003         10
   205  Benzidine-d8....      1854       164     1.549-1.632         50
   305  Benzidine.......      1853       205     1.000-1.002         50
   522  n-docosane......      1889       164        ns               10
   623  n-tetracosane-        1997       164     1.671-1.764         10
         d50............
   723  n-tetracosane...      2025       612     1.012-1.015         10
   067  Butylbenzyl           2060       164        ns               10
         phthalate......
   276  Chrysene-d12....      2081       164     1.743-1.837         10
   376  Chrysene........      2083       276     1.000-1.004         10

[[Page 375]]

 
   272  Benzo(a)anthrace      2082       164     1.735-1.846         10
         ne-d12.........
   372  Benzo(a)anthrace      2090       272     0.999-1.007         10
         ne.............
   228  3,3'-                 2088       164     1.744-1.848         50
         dichlorobenzidi
         ne-d6..........
   328  3,3'-                 2086       228     1.000-1.001         50
         dichlorobenzidi
         ne.............
   266  Bis(2-                2123       164     1.771-1.880         10
         ethylhexyl)
         phthalate-d4...
   366  Bis(2-                2124       266     1.000-1.002         10
         ethylhexyl)
         phthalate......
   524  n-hexacosane....      2147       164        ns               10
   269  di-n-octyl            2239       164     1.867-1.982         10
         phthalate-d4...
   369  di-n-octyl            2240       269     1.000-1.002         10
         phthalate......
   525  n-octacosane....      2272       164        ns               10
   274  Benzo(b)fluorant      2281       164     1.902-2.025         10
         hene-d12.......
   354  Benzo(b)fluorant      2293       274     1.000-1.005         10
         hene...........
   275  Benzo(k)fluorant      2287       164     1.906-2.033         10
         hene-d12.......
   375  Benzo(k)fluorant      2293       275     1.000-1.005         10
         hene...........
   273  Benzo(a)pyrene-       2351       164     1.954-2.088         10
         d12............
   373  Benzo(a)pyrene..      2350       273     1.000-1.004         10
   626  N-triacontane-        2384       164     1.972-2.127         10
         d62............
   726  N-triacontane...      2429       626     1.011-1.028         10
   083  Indeno(1,2,3-         2650       164        ns               20
         cd)pyrene......
   082  Dibenzo(a,h)anth      2660       164        ns               20
         racene.........
   279  Benzo(ghi)peryle      2741       164     2.187-2.524         20
         ne-d12.........
   379  Benzo(ghi)peryle      2750       279     1.001-1.006         20
         ne.............
------------------------------------------------------------------------
\1\ Reference numbers beginning with 0, 1 or 5 indicate a pollutant
  quantified by the internal standard method; reference numbers
  beginning with 2 or 6 indicate a labeled compound quantified by the
  internal standard method; reference numbers beginning with 3 or 7
  indicate a pollutant quantified by isotope dilution.
\2\ This is a minimum level at which the entire GC/MS system must give
  recognizable mass spectra (background corrected) and acceptable
  calibration points.
\3\ Detected as azobenzene.
\4\ Detected as diphenylamine.
ns = specification not available at time of release of method.
Column: 30 2 m x 0.25 0.02
  mm i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase fused silica
  capillary.
Temperature program: 5 min at 30 [deg]C; 30 - 280 [deg]C at 8 [deg]C per
  min; isothermal at 280 [deg]C until benzo(ghi)perylene elutes.
Gas velocity: 30 5 cm/sec.


        Table 4--Gas Chromatography of Acid Extractable Compounds
------------------------------------------------------------------------
                                    Retention time             Detection
  EGD                    ------------------------------------  limit \2\
  No.       Compound        Mean                              ([micro]g/
  \1\                       (sec)    EGD Ref     Relative         L)
------------------------------------------------------------------------
   164  2,2'-                 1163       164     1.000-1.000         10
         difluorobipheny
         l (int std)....
   224  2-chlorophenol-        701       164     0.587-0.618         10
         d4.............
   324  2-chlorophenol..       705       224     0.997-1.010         10
   257  2-nitrophenol-d4       898       164     0.761-0.783         20
   357  2-nitrophenol...       900       257     0.994-1.009         20
   231  2,4-                   944       164     0.802-0.822         10
         dichlorophenol-
         d3.............
   331  2,4-                   947       231     0.997-1.006         10
         dichlorophenol.
   222  4-chloro-3-           1086       164     0.930-0.943         10
         methylphenol-d2
   322  4-chloro-3-           1091       222     0.998-1.003         10
         methylphenol...
   221  2,4,6-                1162       164     0.994-1.005         10
         trichlorophenol-
         d2.............
   321  2,4,6-                1165       221     0.998-1.004         10
         trichlorophenol
   531  2,4,5-                1170       164        ns               10
         trichlorophenol
   530  2,3,6-                1195       164        ns               10
         trichlorophenol
   259  2,4-                  1323       164     1.127-1.149         50
         dinitrophenol-
         d3.............
   359  2,4-                  1325       259     1.000-1.005         50
         dinitrophenol..
   258  4-nitrophenol-d4      1349       164     1.147-1.175         50
   358  4-nitrophenol...      1354       258     0.997-1.006         50
   260  2-methyl-4,6-         1433       164     1.216-1.249         20
         dinitrophenol-
         d2.............
   360  2-methyl-4,6-         1435       260     1.000-1.002         20
         dinitrophenol..
   264  Pentachloropheno      1559       164     1.320-1.363         50
         l-13C6.........
   364  Pentachloropheno      1561       264     0.998-1.002         50
         l..............
------------------------------------------------------------------------
\1\ Reference numbers beginning with 0, 1 or 5 indicate a pollutant
  quantified by the internal standard method; reference numbers
  beginning with 2 or 6 indicate a labeled compound quantified by the
  internal standard method; reference numbers beginning with 3 or 7
  indicate a pollutant quantified by isotope dilution.
\2\ This is a minimum level at which the entire GC/MS system must give
  recognizable mass spectra (background corrected) and acceptable
  calibration points.
ns = specification not available at time of release of method.
Column: 30 2m x 0.25 0.02mm
  i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase fused silica
  capillary.
Temperature program: 5 min at 30 [deg]C; 8 [deg]C/min. to 250 [deg]C or
  until pentachlorophenol elutes.
Gas velocity: 30 5 cm/sec.


[[Page 376]]


              Table 5--DFTPP Mass Intensity Specifications
------------------------------------------------------------------------
 Mass                          Intensity required
------------------------------------------------------------------------
    51  30-60 percent of mass 198.
    68  Less than 2 percent of mass 69.
    70  Less than 2 percent of mass 69.
   127  40-60 percent of mass 198.
   197  Less than 1 percent of mass 198.
   199  5-9 percent of mass 198.
   275  10-30 percent of mass 198.
   365  greater than 1 percent of mass 198
   441  present and less than mass 443
   442  40-100 percent of mass 198.
   443  17-23 percent of mass 442.
------------------------------------------------------------------------


    Table 6--Base/Neutral Extractable Compound Characteristic Masses
------------------------------------------------------------------------
                                                    Labeled   Primary m/
                     Compound                        analog        z
------------------------------------------------------------------------
Acenaphthene.....................................        d10    154/164
Acenaphthylene...................................         d8    152/160
Anthracene.......................................        d10    178/188
Benzidine........................................         d8    184/192
Benzo(a)anthracene...............................        d12    228/240
Benzo(b)fluoranthene.............................        d12    252/264
Benzo(k)fluoranthene.............................        d12    252/264
Benzo(a)pyrene...................................        d12    252/264
Benzo(ghi)perylene...............................        d12    276/288
Biphenyl.........................................        d10    154/164
Bis(2-chloroethyl) ether.........................         d8     93/101
Bis(2-chloroethoxy)methane.......................  .........     93
Bis(2-chloroisopropyl) ether.....................        d12    121/131
Bis(2-ethylhexyl) phthalate......................         d4    149/153
4-bromophenyl phenyl ether.......................  .........    248
Butyl benzyl phthalate...........................  .........    149
n-C10............................................        d22     55/66
n-C12............................................        d26     55/66
n-C14............................................  .........     55
n-C16............................................        d34     55/66
n-C18............................................  .........     55
n-C20............................................        d42     55/66
n-C22............................................  .........     55
n-C24............................................        d50     55/66
n-C26............................................  .........     55
n-C28............................................  .........     55
n-C30............................................        d62     55/66
Carbazole........................................         d8    167/175
2-chloronaphthalene..............................         d7    162/169
4-chlorophenyl phenyl ether......................         d5    204/209
Chrysene.........................................        d12    228/240
p-cymene.........................................        d14    114/130
Dibenzo(a,h)anthracene...........................  .........    278
Dibenzofuran.....................................         d8    168/176
Dibenzothiophene.................................         d8    184/192
Di-n-butyl phthalate.............................         d4    149/153
1,2-dichlorobenzene..............................         d4    146/152
1,3-dichlorobenzene..............................         d4    146/152
1,4-dichlorobenzene..............................         d4    146/152
3,3'-dichlorobenzidine...........................         d6    252/258
Diethyl phthalate................................         d4    149/153
2,4-dimethylphenol...............................         d3    122/125
Dimethyl phthalate...............................         d4    163/167
2,4-dinitrotoluene...............................         d3    164/168
2,6-dinitrotoluene...............................         d3    165/167
Di-n-octyl phthalate.............................         d4    149/153
Diphenylamine....................................        d10    169/179
Diphenyl ether...................................        d10    170/180
1,2-diphenylhydrazine \1\........................        d10     77/82
Fluoranthene.....................................        d10    202/212
Fluorene.........................................        d10    166/176
Hexachlorobenzene................................       13C6    284/292
Hexachlorobutadiene..............................       13C4    225/231
Hexachloroethane.................................        13C    201/204
Hexachlorocyclopentadiene........................       13C4    237/241
Ideno(1,2,3-cd)pyrene............................  .........    276
Isophorone.......................................         d8     82/88
Naphthalene......................................         d8    128/136
B-naphthylamine..................................         d7    143/150
Nitrobenzene.....................................         d5    123/128
N-nitrosodimethylamine...........................  .........     74
N-nitrosodi-n-propylamine........................  .........     70
N-nitrosodiphenylamile \2\.......................         d6    169/175
Phenanthrene.....................................        d10    178/188
Phenol...........................................         d5     94/71
a-picoline.......................................         d7     93/100
Pyrene...........................................        d10    202/212
Styrene..........................................         d5    104/109
a-terpineol......................................         d3     59/62
1,2,3-trichlorobenzene...........................         d3    180/183
1,2,4-trichlorobenzene...........................         d3    180/183
------------------------------------------------------------------------
\1\ Detected as azobenzene.
\2\ Detected as diphenylamine.


        Table 7--Acid Extractable Compound Characteristic Masses
------------------------------------------------------------------------
                                                    Labeled   Primary m/
                     Compound                        analog        z
------------------------------------------------------------------------
4-chloro-3-methylphenol..........................         d2    107/109
2-chlorophenol...................................         d4    128/132
2,4-dichlorophenol...............................         d3    162/167
2,4-dinitrophenol................................         d3    184/187
2-methyl-4,6-dinitrophenol.......................         d2    198/200
2-nitrophenol....................................         d4    139/143
4-nitrophenol....................................         d4    139/143
Pentachlorophenol................................       13C6    266/272
2,3,6-trichlorophenol............................         d2    196/200
2,4,5-trichlorophenol............................         d2    196/200
2,4,6-trichlorophenol............................         d2    196/200
------------------------------------------------------------------------


                               Table 8--Acceptance Criteria for Performance Tests
----------------------------------------------------------------------------------------------------------------
                                                                       Acceptance criteria
                                               -----------------------------------------------------------------
  EGD                                           Initial precision and      Labeled      Calibration    On-going
  No.                  Compound                    accuracy section       compound     verification    accuracy
  \1\                                             8.2.3 ([micro]g/L)    recovery sec.    sec. 12.5   sec. 11.6 R
                                               ----------------------- 8.3 and 14.2 P   ([micro]g/    ([micro]g/
                                                    s          X          (percent)         mL)           L)
----------------------------------------------------------------------------------------------------------------
   301  Acenaphthene..........................        21       79-134  ..............        80-125       72-144
   201  Acenaphthene-d10......................        38       38-147          20-270        71-141       30-180
   377  Acenaphtylene.........................        38       69-186  ..............        60-166       61-207
   277  Acenaphthylene-d8.....................        31       38-146          23-239        66-152       33-168

[[Page 377]]

 
   378  Anthracene............................        41       58-174  ..............        60-168       50-199
   278  Anthracene-d10........................        49       31-194          14-419        58-171       23-242
   305  Benzidine.............................       119       16-518  ..............        34-296       11-672
   205  Benzidine-d8..........................       269        ns-ns           ns-ns         ns-ns        ns-ns
   372  Benzo(a)anthracene....................        20       65-168  ..............        70-142       62-176
   272  Benzo(a)anthracene-d12................        41       25-298          12-605        28-357       22-329
   374  Benzo(b)fluoranthene..................       183       32-545  ..............        61-164        20-ns
   274  Benzo(b)fluoranthene-d12..............       168       11-577           ns-ns         14-ns        ns-ns
   375  Benzo(k)fluoranthene..................        26       59-143  ..............         13-ns       53-155
   275  Benzo(k)fluoranthene-d12..............       114       15-514           ns-ns         13-ns       ns-685
   373  Benzo(a)pyrene........................        26       62-195  ..............        78-129       59-206
   273  Benzo(a)pyrene-d12....................        24       35-181          21-290         12-ns       32-194
   379  Benzo(ghi)perylene....................        21       72-160  ..............        69-145       58-168
   279  Benzo(ghi)perylene-d12................        45       29-268          14-529         13-ns       25-303
   712  Biphenyl (Appendix C).................        41       75-148  ..............        58-171       62-176
   612  Biphenyl-d12..........................        43       28-165           ns-ns        52-192       17-267
   318  Bis(2-chloroethyl) ether..............        34       55-196  ..............        61-164       50-213
   218  Bis(2-chloroethyl) ether-d8...........        33       29-196          15-372        52-194       25-222
   043  Bis(2-chloroethoxy)methane*...........        27       43-153  ..............        44-228       39-166
   342  Bis(2-chloroisopropyl) ether..........        17       81-138  ..............        67-148       77-145
   242  Bis(2-chloroisopropyl)ether-d12.......        27       35-149          20-260        44-229       30-169
   366  Bis(2-ethylhexyl) phthalate...........        31       69-220  ..............        76-131       64-232
   266  Bis(2-ethylhexyl) phthalate-d4........        29       32-205          18-364        43-232       28-224
   041  4-bromophenyl phenyl ether*...........        44       44-140  ..............        52-193       35-172
   067  Butyl benzyl phthalate*...............        31       19-233  ..............        22-450       35-170
   717  n-C10 (Appendix C)....................        51       24-195  ..............        42-235       19-237
   617  n-C10-d22.............................        70       ns-298           ns-ns        44-227       ns-504
   706  n-C12 (Appendix C)....................        74       35-369  ..............        60-166       29-424
   606  n-C12-d26.............................        53       ns-331           ns-ns        41-242       ns-408
   518  n-C14 (Appendix C)*...................       109       ns-985  ..............        37-268        ns-ns
   719  n-C16 (Appendix C)....................        33       80-162  ..............        72-138       71-181
   619  n-C16-d34.............................        46       37-162          18-308        54-186       28-202
   520  n-C18 (Appendix C)*...................        39       42-131  ..............        40-249       35-167
   721  n-C20 (Appendix C)....................        59       53-263  ..............        54-184       46-301
   621  n-C20-d42.............................        34       34-172          19-306        62-162       29-198
   522  n-C22 (Appendix C)*...................        31       45-152  ..............        40-249       39-195
   723  n-C24 (Appendix C)....................        11       80-139  ..............        65-154       78-142
   623  n-C24-d50.............................        28       27-211          15-376        50-199       25-229
   524  n-C26 (Appendix C)*...................        35       35-193  ..............        26-392       31-212
   525  n-C28 (Appendix C)*...................        35       35-193  ..............        26-392       31-212
   726  n-C30 (Appendix C)....................        32       61-200  ..............        66-152       56-215
   626  n-C30-d62.............................        41       27-242          13-479        24-423       23-274
   528  Carbazole (4c)*.......................        38       36-165  ..............        44-227       31-188
   320  2-chloronaphthalene...................       100       46-357  ..............        58-171       35-442
   220  2-chloronaphthalene-d7................        41       30-168          15-324        72-139       24-204
   322  4-chloro-3-methylphenol...............        37       76-131  ..............        85-115       62-159
   222  4-chloro-3-methylphenol-d2............       111       30-174          ns-613        68-147       14-314
   324  2-chlorophenol........................        13       79-135  ..............        78-129       76-138
   224  2-chlorophenol-d4.....................        24       36-162          23-255        55-180       33-176
   340  4-chlorophenyl phenyl ether...........        42       75-166  ..............        71-142       63-194
   240  4-chlorophenyl phenyl ether-d5........        52       40-161          19-325        57-175       29-212
   376  Chrysene..............................        51       59-186  ..............        70-142       48-221
   276  Chrysene-d12..........................        69       33-219          13-512        24-411       23-290
   713  p-cymene (Appendix C).................        18       76-140  ..............        79-127       72-147
   613  p-cymene-d14..........................        67       ns-359           ns-ns        66-152       ns-468
   082  Dibenzo(a,h)anthracene*...............        55       23-299  ..............        13-761       19-340
   705  Dibenzofuran (Appendix C).............        20       85-136  ..............        73-136       79-146
   605  Dibenzofuran-d8.......................        31       47-136          28-220        66-150       39-160
   704  Dibenzothiophene (Synfuel)............        31       79-150  ..............        72-140       70-168
   604  Dibenzothiophene-d8...................        31       48-130          29-215        69-145       40-156
   368  Di-n-butyl phthalate..................        15       76-165  ..............        71-142       74-169
   268  Di-n-butyl phthalate-d4...............        23       23-195          13-346        52-192       22-209
   325  1,2-dichlorobenzene...................        17       73-146  ..............        74-135       70-152
   225  1,2-dichlorobenzene-d4................        35       14-212          ns-494        61-164       11-247
   326  1,3-dichlorobenzene...................        43       63-201  ..............        65-154       55-225
   226  1,3-dichlorobenzene-d4................        48       13-203          ns-550        52-192       ns-260
   327  1,4-dichlorobenzene...................        42       61-194  ..............        62-161       53-219

[[Page 378]]

 
   227  1,4-dichlorobenzene-d4................        48       15-193          ns-474        65-153       11-245
   328  3,3'-dichlorobenzidine................        26       68-174  ..............        77-130       64-185
   228  3,3'-dichlorobenzidine-d6.............        80       ns-562           ns-ns        18-558        ns-ns
   331  2,4-dichlorophenol....................        12       85-131  ..............        67-149       83-135
   231  2,4-dichlorophenol-d3.................        28       38-164          24-260        64-157       34-182
   370  Diethyl phthalate.....................        44       75-196  ..............        74-135       65-222
   270  Diethyl phthalate-d4..................        78       ns-260           ns-ns        47-211        ns-ns
   334  2,4-dimethylphenol....................        13       62-153  ..............        67-150       60-156
   234  2,4-dimethylphenol-d3.................        22       15-228          ns-449        58-172       14-242
   371  Dimethyl phthalate....................        36       74-188  ..............        73-137       67-207
   271  Dimethyl phthalate-d4.................       108       ns-640           ns-ns        50-201        ns-ns
   359  2,4-dinitrophenol.....................        18       72-134  ..............        75-133       68-141
   259  2,4-dinitrophenol-d3..................        66       22-308           ns-ns        39-256       17-378
   335  2,4-dinitrotoluene....................        18       75-158  ..............        79-127       72-164
   235  2,4-dinitrotoluene-d3.................        37       22-245          10-514        53-187       19-275
   336  2,6-dinitrotoluene....................        30       80-141  ..............        55-183       70-159
   236  2,6-dinitrotoluene-d3.................        59       44-184          17-442        36-278       31-250
   369  Di-n-octyl phthalate..................        16       77-161  ..............        71-140       74-166
   269  Di-n-octyl phthalate-d4...............        46       12-383           ns-ns        21-467       10-433
   707  Diphenylamine (Appendix C)............        45       58-205  ..............        57-176       51-231
   607  Diphenylamine-d10.....................        42       27-206          11-488        59-169       21-249
   708  Diphenyl ether (Appendix C)...........        19       82-136  ..............        83-120       77-144
   608  Diphenyl ether-d10....................        37       36-155          19-281        77-129       29-186
   337  1,2-diphenylhydrazine.................        73       49-308  ..............        75-134       40-360
   237  1,2-diphenylhydrazine-d10.............        35       31-173          17-316        58-174       26-200
   339  Fluoranthene..........................        33       71-177  ..............        67-149       64-194
   239  Fluoranthene-d10......................        35       36-161          20-278        47-215       30-187
   380  Fluorene..............................        29       81-132  ..............        74-135       70-151
   280  Fluorene-d10..........................        43       51-131          27-238        61-164       38-172
   309  Hexachlorobenzene.....................        16       90-124  ..............        78-128       85-132
   209  Hexachlorobenzene-13C6................        81       36-228          13-595        38-265       23-321
   352  hexachlorobutadiene...................        56       51-251  ..............        74-135       43-287
   252  hexachlorobutadiene-13C4..............        63       ns-316           ns-ns        68-148       ns-413
   312  hexachloroethane......................       227        21-ns  ..............        71-141        13-ns
   212  hexachloroethane-13C1.................        77       ns-400           ns-ns        47-212       ns-563
   353  hexachlorocyclopentadiene.............        15       69-144  ..............        77-129       67-148
   253  hexachlorocyclopentadiene-13C4........        60        ns-ns           ns-ns        47-211        ns-ns
   083  ideno(1,2,3-cd)pyrene*................        55       23-299  ..............        13-761       19-340
   354  isophorone............................        25       76-156  ..............        70-142       70-168
   254  isophorone-d8.........................        23       49-133          33-193        52-194       44-147
   360  2-methyl-4,6-dinitrophenol............        19       77-133  ..............        69-145       72-142
   260  2-methyl-4,6-dinitrophenol-d2.........        64       36-247          16-527        56-177       28-307
   355  naphthalene...........................        20       80-139  ..............        73-137       75-149
   255  naphthalene-d8........................        39       28-157          14-305        71-141       22-192
   702  B-naphthylamine (Appendix C)..........        49        10-ns  ..............        39-256        ns-ns
   602  B-naphthylamine-d7....................        33        ns-ns           ns-ns        44-230        ns-ns
   356  nitrobenzene..........................        25       69-161  ..............        85-115       65-169
   256  nitrobenzene-d5.......................        28       18-265           ns-ns        46-219       15-314
   357  2-nitrophenol.........................        15       78-140  ..............        77-129       75-145
   257  2-nitrophenol-d4......................        23       41-145          27-217        61-163       37-158
   358  4-nitrophenol.........................        42       62-146  ..............        55-183       51-175
   258  4-nitrophenol-d4......................       188       14-398           ns-ns        35-287        ns-ns
   061  N-nitrosodimethylamile*...............       198       21-472  ..............        40-249       12-807
   063  N-nitrosodi-n-proplyamine*............       198       21-472  ..............        40-249       12-807
   362  N-nitrosodiphenylamine................        45       65-142  ..............        68-148       53-173
   262  N-nitrosodiphenylamine-d6.............        37       54-126          26-256        59-170       40-166
   364  pentachlorophenol.....................        21       76-140  ..............        77-130       71-150
   264  pentachlorophenol-13C6................        49       37-212          18-412        42-237       29-254
   381  phenanthrene..........................        13       93-119  ..............        75-133       87-126
   281  phenanthrene-d10......................        40       45-130          24-241        67-149       34-168
   365  phenol................................        36       77-127  ..............        65-155       62-154
   265  phenol-d5.............................       161       21-210           ns-ns        48-208        ns-ns
   703  a-picoline (Synfuel)..................        38       59-149  ..............        60-165       50-174
   603  a-picoline-d7.........................       138       11-380           ns-ns        31-324       ns-608
   384  pyrene................................        19       76-152  ..............        76-132       72-159
   284  pyrene-d10............................        29       32-176          18-303        48-210       28-196
   710  styrene (Appendix C)..................        42       53-221  ..............        65-153       48-244

[[Page 379]]

 
   610  styrene-d5............................        49       ns-281           ns-ns        44-228       ns-348
   709  a-terpineol (Appendix C)..............        44       42-234  ..............        54-186       38-258
   609  a-terpineol-d3........................        48       22-292          ns-672        20-502       18-339
   529  1,2,3-trichlorobenzene (4c)*..........        69       15-229  ..............        60-167       11-297
   308  1,2,4-trichlorobenzene................        19       82-136  ..............        78-128       77-144
   208  1,2,4-trichlorobenzene-d3.............        57       15-212          ns-592        61-163       10-282
   530  2,3,6-trichlorophenol (4c)*...........        30       58-137  ..............        56-180       51-153
   531  2,4,5-trichlorophenol (4c)*...........        30       58-137  ..............        56-180       51-153
   321  2,4,6-trichlorophenol.................        57       59-205  ..............        81-123       48-244
   221  2,4,6-trichlorophenol-d2..............        47       43-183          21-363        69-144       34-226
----------------------------------------------------------------------------------------------------------------
\1\ Reference numbers beginning with 0, 1 or 5 indicate a pollutant quantified by the internal standard method;
  reference numbers beginning with 2 or 6 indicate a labeled compound quantified by the internal standard
  method; reference numbers beginning with 3 or 7 indicate a pollutant quantified by isotope dilution.
 
* Measured by internal standard; specification derived from related compound.
ns = no specification; limit is outside the range that can be measured reliably.


[[Page 380]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.057


[[Page 381]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.058


[[Page 382]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.059


[[Page 383]]

                       Attachment 1 to Method 1625

                              Introduction

    To support measurement of several semivolatile pollutants, EPA has 
developed this attachment to EPA Method 1625B. \1\ The modifications 
listed in this attachment are approved only for monitoring wastestreams 
from the Centralized Waste Treatment Point Source Category (40 CFR part 
437) and the Landfills Point Source Category (40 CFR part 445). EPA 
Method 1625B (the Method) employs sample extraction with methylene 
chloride followed by analysis of the extract using capillary column gas 
chromatography-mass spectrometry (GC/MS). This attachment addresses the 
addition of the semivolatile pollutants listed in Tables 1 and 2 to all 
applicable standard, stock, and spiking solutions utilized for the 
determination of semivolatile organic compounds by EPA Method 1625B.
---------------------------------------------------------------------------

    \1\ EPA Method 1625 Revision B, Semivolatile Organic Compounds by 
Isotope Dilution GC/MS, 40 CFR part 136, appendix A.
---------------------------------------------------------------------------

           1.0 EPA METHOD 1625 REVISION B MODIFICATION SUMMARY

    The additional semivolatile organic compounds listed in Tables 1 and 
2 are added to all applicable calibration, spiking, and other solutions 
utilized in the determination of semivolatile compounds by EPA Method 
1625. The instrument is to be calibrated with these compounds, and all 
procedures and quality control tests described in the Method must be 
performed.

                        2.0 SECTION MODIFICATIONS

    Note: All section and figure numbers in this Attachment reference 
section and figure numbers in EPA Method 1625 Revision B unless noted 
otherwise. Sections not listed here remain unchanged.
Section 6.7 The stock standard solutions described in this section are 
          modified such that the analytes in Tables 1 and 2 of this 
          attachment are required in addition to those specified in the 
          Method.
Section 6.8 The labeled compound spiking solution in this section is 
          modified to include the labeled compounds listed in Tables 5 
          and 6 of this attachment.
Section 6.9 The secondary standard is modified to include the additional 
          analytes listed in Tables 1 and 2 of this attachment.
Section 6.12 The solutions for obtaining authentic mass spectra are to 
          include all additional analytes listed in Tables 1 and 2 of 
          this attachment.
Section 6.13 The calibration solutions are modified to include the 
          analytes listed in Tables 1 and 2 and the labeled compounds 
          listed in Tables 5 and 6 of this attachment.
Section 6.14 The precision and recovery standard is modified to include 
          the analytes listed in Tables 1 and 2 and the labeled 
          compounds listed in Tables 5 and 6 of this attachment.
Section 6.15 The solutions containing the additional analytes listed in 
          Tables 1 and 2 of this attachment are to be analyzed for 
          stability.
Section 7.2.1 This section is modified to include the analytes listed in 
          Tables 1 and 2 and the labeled compounds listed in Tables 5 
          and 6 of this attachment.
Section 7.4.5 This section is modified to include the analytes listed in 
          Tables 1 and 2 and the labeled compounds listed in Tables 5 
          and 6 in the calibration.
Section 8.2 The initial precision and recovery (IPR) requirements are 
          modified to include the analytes listed in Tables 1 and 2 and 
          the labeled compounds listed in Tables 5 and 6 of this 
          attachment. Additional IPR performance criteria are supplied 
          in Table 7 of this attachment.
Section 8.3 The labeled compounds listed in Tables 3 and 4 of this 
          attachment are to be included in the method performance tests. 
          Additional method performance criteria are supplied in Table 7 
          of this attachment.
Section 8.5.2 The acceptance criteria for blanks includes the analytes 
          listed in Tables 1 and 2 of this attachment.
Section 10.1.2 The labeled compound solution must include the labeled 
          compounds listed in Tables 5 and 6 of this attachment.
Section 10.1.3 The precision and recovery standard must include the 
          analytes listed in Tables 1 and 2 and the labeled compounds 
          listed in Tables 5 and 6 of this attachment.
Section 12.5 Additional QC requirements for calibration verification are 
          supplied in Table 7 of this attachment.
Section 12.7 Additional QC requirements for ongoing precision and 
          recovery are supplied in Table 7 of this attachment.

[[Page 384]]



               Table 1--Base/Neutral Extractable Compounds
------------------------------------------------------------------------
                                                         Pollutant
                                                 -----------------------
                    Compound                          CAS
                                                   Registry     EPA-EGD
------------------------------------------------------------------------
acetophenone \1\................................     98-86-2         758
aniline \2\.....................................     62-53-3         757
-2,3-dichloroaniline \1\........................    608-27-5         578
-o-cresol \1\...................................     95-48-7         771
pyridine \2\....................................    110-86-1       1330
------------------------------------------------------------------------
CAS = Chemical Abstracts Registry.
EGD = Effluent Guidelines Division.
\1\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment industry.
\2\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment and Landfills industries.


                   Table 2--Acid Extractable Compounds
------------------------------------------------------------------------
                                                        Pollutant
                                               -------------------------
                   Compound                         CAS
                                                  Registry     EPA-EGD
------------------------------------------------------------------------
p-cresol \1\..................................    106-44-5        1744
------------------------------------------------------------------------
CAS = Chemical Abstracts Registry.
EGD = Effluent Guidelines Division.
\1\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment and Landfills industries.


                                          Table 3--Gas Chromatography \1\ of Base/Neutral Extractable Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                   Retention time \2\                                                Retention time \2\
                                                    ------------------------------------------------  Minimum level  EGD           ----------------------
         EGD No.                   Compound                                                          \3\ ([micro]g/  No.  Compound   Mean  EGD
                                                       Mean (sec)        EGD Ref        Relative           L)                       (sec)  Ref  Relative
------------------------------------------------------------------------------------------------------------------- -------------------------------------------------
758......................  acetophenone \4\........             818             658     1.003-1.005              10
757......................  aniline \5\.............             694             657     0.994-1.023              10
578......................  2,3-dichloroaniline \4\.            1160             164     1.003-1.007              10
771......................  o-cresol \4\............             814             671     1.005-1.009              10
1330.....................  pyridine \5\............             378            1230     1.005-1.011             10
--------------------------------------------------------------------------------------------------------------------------------------------------------
EGD = Effluent Guidelines Division.
\1\ The data presented in this table were obtained under the chromatographic conditions given in the footnote to Table 3 of EPA Method 1625B.
\2\ Retention times are approximate and are intended to be consistent with the retention times for the analytes in EPA Method 1625B.
\3\ See the definition in footnote 2 to Table 3 of EPA Method 1625B.
\4\ Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
\5\ Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.


                          Table 4--Gas Chromatography \1\ of Acid Extractable Compounds
----------------------------------------------------------------------------------------------------------------
                                                                Retention time \2\                 Minimum level
         EGD No.                 Compound        ------------------------------------------------   ([micro]/L)
                                                    Mean (sec)        EGD Ref        Relative           \3\
----------------------------------------------------------------------------------------------------------------
1744....................  p-cresol \4\..........             834            1644     1.004-1.008             20
----------------------------------------------------------------------------------------------------------------
EGD = Effluent Guidelines Division.
\1\ The data presented in this table were obtained under the chromatographic conditions given in the footnote to
  Table 4 of EPA Method 1625B.
\2\ Retention times are approximate and are intended to be consistent with the retention times for the analytes
  in EPA Method 1625B.
\3\ See the definition in footnote 2 to Table 4 of EPA Method 1625B.
\4\ Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.


     Table 5--Base/Neutral Extractable Compound Characteristic m/z's
------------------------------------------------------------------------
                                                             Primary m/z
                 Compound                    Labeled Analog      \1\
------------------------------------------------------------------------
acetophenone \2\..........................  d5                   105/110
aniline \3\...............................  d7                    93/100
o-cresol \2\..............................  d7                   108/116
2,3-dichloroaniline \2\...................  n/a                      161
pyridine \3\..............................  d5                    79/84
------------------------------------------------------------------------
m/z = mass to charge ratio.

[[Page 385]]

 
\1\ Native/labeled.
\2\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment industry.
\3\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment and Landfills industries.


         Table 6--Acid Extractable Compound Characteristic m/z's
------------------------------------------------------------------------
                                                             Primary m/z
                 Compound                    Labeled Analog      \1\
------------------------------------------------------------------------
p-cresol \2\..............................  d7                  108/116
------------------------------------------------------------------------
m/z = mass to charge ratio.
\1\ Native/labeled.
\2\ Analysis of this pollutant is approved only for the Centralized
  Waste Treatment and Landfills industries.


                               Table 7--Acceptance Criteria for Performance Tests
----------------------------------------------------------------------------------------------------------------
                                                         Acceptance criteria
                                               ---------------------------------------
                                                  Initial precision and     Labeled     Calibration    On-going
                                                  accuracy section 8.2      compound   verification    accuracy
        EGD No.                 Compound              ([micro]g/L)          recovery     sec. 12.5   sec. 12.7 R
                                               --------------------------   sec. 8.3    ([micro]g/    ([micro]g/
                                                s ([micro]g/               and 14.2 P       mL)           L)
                                                     L)           X        (percent)
----------------------------------------------------------------------------------------------------------------
758....................  acetophenone \1\.....           34       44-167  ...........        85-115       45-162
658....................  acetophenone-d 5 \1\.           51       23-254       45-162        85-115       22-264
757....................  aniline \2\..........           32       30-171  ...........        85-115       33-154
657....................  aniline-d 7 \2\......           71       15-278       33-154        85-115       12-344
771....................  o-cresol \1\.........           40       31-226  ...........        85-115       35-196
671....................  o-cresol-d 7 \1\.....           23       30-146       35-196        85-115       31-142
1744...................  p-cresol \2\.........           59       54-140  ...........        85-115       37-203
1644...................  p-cresol-d7 \2\......           22       11-618       37-203        85-115       16-415
578....................  2,3-dichloroaniline             13       40-160  ...........        85-115       44-144
                          \1\.
1330...................  pyridine \2\.........           28       10-421  ...........        83-117       18-238
1230...................  pyridine-d 5 \2\.....           ns        7-392       19-238        85-115       4-621
----------------------------------------------------------------------------------------------------------------
s = Standard deviation of four recovery measurements.
X = Average recovery for four recovery measurements.
EGD = Effluent Guidelines Division.
ns = no specification; limit is outside the range that can be measured reliably.
\1\ Analysis of this pollutant is approved only for the Centralized Waste Treatment industry.
\2\ Analysis of this pollutant is approved only for the Centralized Waste Treatment and Landfills industries.


[49 FR 43261, Oct. 26, 1984; 50 FR 692, 695, Jan. 4, 1985, as amended at 
51 FR 23702, June 30, 1986; 62 FR 48405, Sept. 15, 1997; 65 FR 3044, 
Jan. 19, 2000; 65 FR 81295, 81298, Dec. 22, 2000; 82 FR 40875, Aug. 28, 
2017]



     Sec. Appendix B to Part 136--Definition and Procedure for the 
         Determination of the Method Detection Limit--Revision 2

                               Definition

    The method detection limit (MDL) is defined as the minimum measured 
concentration of a substance that can be reported with 99% confidence 
that the measured concentration is distinguishable from method blank 
results.

                        I. Scope and Application

    (1) The MDL procedure is designed to be a straightforward technique 
for estimation of the detection limit for a broad variety of physical 
and chemical methods. The procedure requires a complete, specific, and 
well-defined analytical method. It is essential that all sample 
processing steps used by the laboratory be included in the determination 
of the method detection limit.
    (2) The MDL procedure is not applicable to methods that do not 
produce results with a continuous distribution, such as, but not limited 
to, methods for whole effluent toxicity, presence/absence methods, and 
microbiological methods that involve counting colonies. The MDL 
procedure also is not applicable to measurements such as, but not 
limited to, biochemical oxygen demand, color, pH, specific conductance, 
many titration methods, and any method where low-level spiked samples 
cannot be prepared. Except as described in the addendum, for the 
purposes of this procedure, ``spiked samples'' are prepared from a clean 
reference matrix, such as reagent water, spiked with a known and 
consistent quantity of the analyte. MDL determinations using spiked 
samples may not be appropriate for all gravimetric methods (e.g., 
residue or total suspended solids), but an MDL based on method blanks 
can be determined in such instances.

[[Page 386]]

                              II. Procedure

    (1) Estimate the initial MDL using one or more of the following:
    (a) The mean determined concentration plus three times the standard 
deviation of a set of method blanks.
    (b) The concentration value that corresponds to an instrument 
signal-to-noise ratio in the range of 3 to 5.
    (c) The concentration equivalent to three times the standard 
deviation of replicate instrumental measurements of spiked blanks.
    (d) That region of the calibration where there is a significant 
change in sensitivity, i.e., a break in the slope of the calibration.
    (e) Instrumental limitations.
    (f) Previously determined MDL.

    Note: It is recognized that the experience of the analyst is 
important to this process. However, the analyst should include some or 
all of the above considerations in the initial estimate of the MDL.

    (2) Determine the initial MDL.

    Note: The Initial MDL is used when the laboratory does not have 
adequate data to perform the Ongoing Annual Verification specified in 
Section (4), typically when a new method is implemented or if a method 
was rarely used in the last 24 months.

    (a) Select a spiking level, typically 2--10 times the estimated MDL 
in Section 1. Spiking levels in excess of 10 times the estimated 
detection limit may be required for analytes with very poor recovery 
(e.g., for an analyte with 10% recovery, spiked at 100 micrograms/L, 
with mean recovery of 10 micrograms/L; the calculated MDL may be around 
3 micrograms/L. Therefore, in this example, the spiking level would be 
33 times the MDL, but spiking lower may result in no recovery at all).
    (b) Process a minimum of seven spiked samples and seven method blank 
samples through all steps of the method. The samples used for the MDL 
must be prepared in at least three batches on three separate calendar 
dates and analyzed on three separate calendar dates. (Preparation and 
analysis may be on the same day.) Existing data may be used, if 
compliant with the requirements for at least three batches, and 
generated within the last twenty four months. The most recent available 
data for method blanks and spiked samples must be used. Statistical 
outlier removal procedures should not be used to remove data for the 
initial MDL determination, since the total number of observations is 
small and the purpose of the MDL procedure is to capture routine method 
variability. However, documented instances of gross failures (e.g., 
instrument malfunctions, mislabeled samples, cracked vials) may be 
excluded from the calculations, provided that at least seven spiked 
samples and seven method blanks are available. (The rationale for 
removal of specific outliers must be documented and maintained on file 
with the results of the MDL determination.)
    (i) If there are multiple instruments that will be assigned the same 
MDL, then the sample analyses must be distributed across all of the 
instruments.
    (ii) A minimum of two spiked samples and two method blank samples 
prepared and analyzed on different calendar dates is required for each 
instrument. Each analytical batch may contain one spiked sample and one 
method blank sample run together. A spiked sample and a method blank 
sample may be analyzed in the same batch, but are not required to be.
    (iii) The same prepared extract may be analyzed on multiple 
instruments so long as the minimum requirement of seven preparations in 
at least three separate batches is maintained.
    (c) Evaluate the spiking level: If any result for any individual 
analyte from the spiked samples does not meet the method qualitative 
identification criteria or does not provide a numerical result greater 
than zero, then repeat the spiked samples at a higher concentration. 
(Qualitative identification criteria are a set of rules or guidelines 
for establishing the identification or presence of an analyte using a 
measurement system. Qualitative identification does not ensure that 
quantitative results for the analyte can be obtained.)
    (d) Make all computations as specified in the analytical method and 
express the final results in the method-specified reporting units.
    (i) Calculate the sample standard deviation (S) of the replicate 
spiked sample measurements and the sample standard deviation of the 
replicate method blank measurements from all instruments to which the 
MDL will be applied.
    (ii) Compute the MDLs (the MDL based on spiked samples) 
as follows:

MDLS = t(n -1, 1-[alpha] = 0.99)Ss

Where:

MDLs = the method detection limit based on spiked samples
t(n-1, 1-[alpha] = 0.99) = the Student's t-value 
          appropriate for a single-tailed 99th percentile t statistic 
          and a standard deviation estimate with n-1 degrees of freedom. 
          See Addendum Table 1.
Ss = sample standard deviation of the replicate spiked sample 
          analyses.

    (iii) Compute the MDLb (the MDL based on method blanks) 
as follows:
    (A) If none of the method blanks give numerical results for an 
individual analyte, the MDLb does not apply. A numerical 
result includes both positive and negative results, including results 
below the current MDL, but not results of ``ND'' (not detected) commonly

[[Page 387]]

observed when a peak is not present in chromatographic analysis.
    (B) If some (but not all) of the method blanks for an individual 
analyte give numerical results, set the MDLb equal to the 
highest method blank result. If more than 100 method blanks are 
available, set MDLb to the level that is no less than the 
99th percentile of the method blank results. For ``n'' method blanks 
where n = 100, sort the method blanks in rank order. The (n * 
0.99) ranked method blank result (round to the nearest whole number) is 
the MDLb. For example, to find MDLb from a set of 
164 method blanks where the highest ranked method blank results are . . 
. 1.5, 1.7, 1.9, 5.0, and 10, then 164 x 0.99 = 162.36 which rounds to 
the 162nd method blank result. Therefore, MDLb is 1.9 for n = 
164 (10 is the 164th result, 5.0 is the 163rd result, and 1.9 is the 
162nd result). Alternatively, you may use spreadsheet algorithms to 
calculate the 99th percentile to interpolate between the ranks more 
precisely.
    (C) If all of the method blanks for an individual analyte give 
numerical results, then calculate the MDLb as:

MDLb = X + tn-1,1-[alpha] = (0.99)Sb
Where:

MDLb = the MDL based on method blanks
X = mean of the method blank results (use zero in place of the mean if 
          the mean is negative)
t(n-1, 1[alpha] = 0.99) = the Student's t-value 
          appropriate for the single-tailed 99th percentile t statistic 
          and a standard deviation estimate with n-1 degrees of freedom. 
          See Addendum Table 1.
Sb = sample standard deviation of the replicate method blank 
sample analyses.

    Note: If 100 or more method blanks are available, as an option, 
MDLb may be set to the concentration that is greater than or 
equal to the 99th percentile of the method blank results, as described 
in Section (2)(d)(iii)(B).

    (e) Select the greater of MDLs or MDLb as the 
initial MDL.
    (3) Ongoing Data Collection.
    (a) During any quarter in which samples are being analyzed, prepare 
and analyze a minimum of two spiked samples on each instrument, in 
separate batches, using the same spiking concentration used in Section 
2. If any analytes are repeatedly not detected in the quarterly spiked 
sample analyses, or do not meet the qualitative identification criteria 
of the method (see section 2(c) of this procedure), then this is an 
indication that the spiking level is not high enough and should be 
adjusted upward. Note that it is not necessary to analyze additional 
method blanks together with the spiked samples, the method blank 
population should include all of the routine method blanks analyzed with 
each batch during the course of sample analysis.
    (b) Ensure that at least seven spiked samples and seven method 
blanks are completed for the annual verification. If only one instrument 
is in use, a minimum of seven spikes are still required, but they may be 
drawn from the last two years of data collection.
    (c) At least once per year, re-evaluate the spiking level.
    (i) If more than 5% of the spiked samples do not return positive 
numerical results that meet all method qualitative identification 
criteria, then the spiking level must be increased and the initial MDL 
re-determined following the procedure in section 2.
    (ii) [Reserved]
    (d) If the method is altered in a way that can be reasonably 
expected to change its sensitivity, then re-determine the initial MDL 
according to section 2, and the restart the ongoing data collection.
    (e) If a new instrument is added to a group of instruments whose 
data are being pooled to create a single MDL, analyze a minimum of two 
spiked replicates and two method blank replicates on the new instrument. 
If both method blank results are below the existing MDL, then the 
existing MDLb is validated. Combine the new spiked sample 
results to the existing spiked sample results and recalculate the 
MDLs as in Section 4. If the recalculated MDLs 
does not vary by more than the factor specified in section 4(f) of this 
procedure, then the existing MDLs is validated. If either of 
these two conditions is not met, then calculate a new MDL following the 
instructions in section 2.
    (4) Ongoing Annual Verification.
    (a) At least once every thirteen months, re-calculate 
MDLs and MDLb from the collected spiked samples 
and method blank results using the equations in section 2.
    (b) Include data generated within the last twenty four months, but 
only data with the same spiking level. Only documented instances of 
gross failures (e.g., instrument malfunctions, mislabeled samples, 
cracked vials) may be excluded from the calculations. (The rationale for 
removal of specific outliers must be documented and maintained on file 
with the results of the MDL determination.) If the laboratory believes 
the sensitivity of the method has changed significantly, then the most 
recent data available may be used, maintaining compliance with the 
requirement for at least seven replicates in three separate batches on 
three separate days (see section 2b).
    (c) Include the initial MDL spiked samples, if the data were 
generated within twenty four months.
    (d) Only use data associated with acceptable calibrations and batch 
QC. Include all routine data, with the exception of batches that are 
rejected and the associated samples reanalyzed. If the method has been 
altered in a way that can be reasonably expected to

[[Page 388]]

change its sensitivity, then use only data collected after the change.
    (e) Ideally, use all method blank results from the last 24 months 
for the MDLb calculation. The laboratory has the option to 
use only the last six months of method blank data or the fifty most 
recent method blanks, whichever criteria yields the greater number of 
method blanks.
    (f) The verified MDL is the greater of the MDLs or 
MDLb. If the verified MDL is within 0.5 to 2.0 times the 
existing MDL, and fewer than 3% of the method blank results (for the 
individual analyte) have numerical results above the existing MDL, then 
the existing MDL may optionally be left unchanged. Otherwise, adjust the 
MDL to the new verification MDL. (The range of 0.5 to 2.0 approximates 
the 95th percentile confidence interval for the initial MDL 
determination with six degrees of freedom.)

 Addendum to Section II: Determination of the MDL for a Specific Matrix

    The MDL may be determined in a specific sample matrix as well as in 
reagent water.
    (1) Analyze the sample matrix to determine the native (background) 
concentration of the analyte(s) of interest.
    (2) If the response for the native concentration is at a signal-to-
noise ratio of approximately 5-20, determine the matrix-specific MDL 
according to Section 2 but without spiking additional analyte.
    (3) Calculate MDLb using the method blanks, not the 
sample matrix.
    (4) If the signal-to-noise ratio is less than 5, then the analyte(s) 
should be spiked into the sample matrix to obtain a concentration that 
will give results with a signal-to-noise ratio of approximately 10-20.
    (5) If the analytes(s) of interest have signal-to-noise ratio(s) 
greater than approximately 20, then the resulting MDL is likely to be 
biased high.

           Table 1--Single-Tailed 99th Percentile t Statistic
------------------------------------------------------------------------
                                            Degrees of
          Number of replicates             freedom (n-1)   t (n-1, 0.99)
------------------------------------------------------------------------
7.......................................               6           3.143
8.......................................               7           2.998
9.......................................               8           2.896
10......................................               9           2.821
11......................................              10           2.764
16......................................              15           2.602
21......................................              20           2.528
26......................................              25           2.485
31......................................              30           2.457
32......................................              31           2.453
48......................................              47           2.408
50......................................              49           2.405
61......................................              60           2.390
64......................................              63           2.387
80......................................              79           2.374
96......................................              95           2.366
100.....................................              99           2.365
------------------------------------------------------------------------

                           III. Documentation

    The analytical method used must be specifically identified by number 
or title and the MDL for each analyte expressed in the appropriate 
method reporting units. Data and calculations used to establish the MDL 
must be able to be reconstructed upon request. The sample matrix used to 
determine the MDL must also be identified with MDL value. Document the 
mean spiked and recovered analyte levels with the MDL. The rationale for 
removal of outlier results, if any, must be documented and maintained on 
file with the results of the MDL determination.

[82 FR 40939, Aug. 28, 2017]



Sec. Appendix C to Part 136--Determination of Metals and Trace Elements 
   in Water and Wastes by Inductively Coupled Plasma-Atomic Emission 
                        Spectrometry Method 200.7

                        1.0 Scope and Application

    1.1 Inductively coupled plasma-atomic emission spectrometry (ICP-
AES) is used to determine metals and some nonmetals in solution. This 
method is a consolidation of existing methods for water, wastewater, and 
solid wastes.1-4 (For analysis of petroleum products see 
References 5 and 6, Section 16.0). This method is applicable to the 
following analytes:

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------------------------------------------------------------------------
                                                      Chemical abstract
                      Analyte                         services registry
                                                       number (CASRN)
------------------------------------------------------------------------
Aluminum (Al).....................................             7429-90-5
Antimony (Sb).....................................             7440-36-0
Arsenic (As)......................................             7440-38-2
Barium (Ba).......................................             7440-39-3
Beryllium (Be)....................................             7440-41-7
Boron (B).........................................             7440-42-8
Cadmium (Cd)......................................             7440-43-9
Calcium (Ca)......................................             7440-70-2
Cerium \a\ (Cr)...................................             7440-45-1
Chromium (Cr).....................................             7440-47-3
Cobalt (Co).......................................             7440-48-4
Copper (Cu).......................................             7440-50-8
Iron (Fe).........................................             7439-89-6
Lead (Pb).........................................             7439-92-1
Lithium (Li)......................................             7439-93-2
Magnesium (Mg)....................................             7439-95-4
Manganese (Mn)....................................             7439-96-5
Mercury (Hg)......................................             7439-97-6
Molybdenum (Mo)...................................             7439-98-7
Nickel (Ni).......................................             7440-02-0
Phosphorus (P)....................................             7723-14-0
Potassium (K).....................................             7440-09-7
Selenium (Se).....................................             7782-49-2
Silica \b\ (Si02).................................             7631-86-9
Silver (Ag).......................................             7440-22-4
Sodium (Na).......................................             7440-23-5
Strontium (Sr)....................................             7440-24-6
Thallium (Tl).....................................             7440-28-0
Tin (Sn)..........................................             7440-31-5
Titanium (Ti).....................................             7440-32-6
Vanadium (V)......................................             7440-62-2
Zinc (Zn).........................................             7440-66-6
------------------------------------------------------------------------
\a\ Cerium has been included as method analyte for correction of
  potential interelement spectral interference.
\b\ This method is not suitable for the determination of silica in
  solids.

    1.2 For reference where this method is approved for use in 
compliance monitoring programs [e.g., Clean Water Act (NPDES) or Safe 
Drinking Water Act (SDWA)] consult both the appropriate sections of the 
Code of Federal Regulation (40 CFR Part 136 Table 1B for NPDES, and Part 
141 Sec.  141.23 for drinking water), and the latest Federal Register 
announcements.
    1.3 ICP-AES can be used to determine dissolved analytes in aqueous 
samples after suitable filtration and acid preservation. To reduce 
potential interferences, dissolved solids should be <0.2% (w/v) (Section 
4.2).
    1.4 With the exception of silver, where this method is approved for 
the determination of certain metal and metalloid contaminants in 
drinking water, samples may be analyzed directly by pneumatic 
nebulization without acid digestion if the sample has been properly 
preserved with acid and has turbidity of <1 NTU at the time of analysis. 
This total recoverable determination procedure is referred to as 
``direct analysis''. However, in the determination of some primary 
drinking water metal contaminants, preconcentration of the sample may be 
required prior to analysis in order to meet drinking water acceptance 
performance criteria (Sections 11.2.2 through 11.2.7).
    1.5 For the determination of total recoverable analytes in aqueous 
and solid samples a digestion/extraction is required prior to analysis 
when the elements are not in solution (e.g., soils, sludges, sediments 
and aqueous samples that may contain particulate and suspended solids). 
Aqueous samples containing suspended or particulate material 1% (w/v) 
should be extracted as a solid type sample.
    1.6 When determining boron and silica in aqueous samples, only 
plastic, PTFE or quartz labware should be used from time of sample 
collection to completion of analysis. For accurate determination of 
boron in solid samples only quartz or PTFE beakers should be used during 
acid extraction with immediate transfer of an extract aliquot to a 
plastic centrifuge tube following dilution of the extract to volume. 
When possible, borosilicate glass should be avoided to prevent 
contamination of these analytes.
    1.7 Silver is only slightly soluble in the presence of chloride 
unless there is a sufficient chloride concentration to form the soluble 
chloride complex. Therefore, low recoveries of silver may occur in 
samples, fortified sample matrices and even fortified blanks if 
determined as a dissolved analyte or by ``direct analysis'' where the 
sample has not been processed using the total recoverable mixed acid 
digestion. For this reason it is recommended that samples be digested 
prior to the determination of silver. The total recoverable sample 
digestion procedure given in this method is suitable for the 
determination of silver in aqueous samples containing concentrations up 
to 0.1 mg/L. For the analysis of wastewater samples containing higher 
concentrations of silver, succeeding smaller volume, well mixed aliquots 
should be prepared until the analysis solution contains <0.1 mg/L 
silver. The extraction of solid samples containing concentrations of 
silver 50 mg/kg should be treated in a similar manner. Also, 
the extraction of tin from solid samples should be prepared again using 
aliquots <1 g when determined sample concentrations exceed 1%.
    1.8 The total recoverable sample digestion procedure given in this 
method will solubilize and hold in solution only minimal concentrations 
of barium in the presence of free sulfate. For the analysis of barium in 
samples having varying and unknown concentrations of sulfate, analysis 
should be completed as soon as possible after sample preparation.
    1.9 The total recoverable sample digestion procedure given in this 
method is not suitable for the determination of volatile organo-mercury 
compounds. However, if digestion is not required (turbidity <1 NTU), the 
combined concentrations of inorganic and organo-mercury in solution can 
be determined by ``direct analysis'' pneumatic nebulization provided the 
sample solution is adjusted to contain the same mixed acid

[[Page 390]]

(HNO3 + HCl) matrix as the total recoverable calibration 
standards and blank solutions.
    1.10 Detection limits and linear ranges for the elements will vary 
with the wavelength selected, the spectrometer, and the matrices. Table 
1 provides estimated instrument detection limits for the listed 
wavelengths.\7\ However, actual method detection limits and linear 
working ranges will be dependent on the sample matrix, instrumentation, 
and selected operating conditions.
    1.11 Users of the method data should state the data-quality 
objectives prior to analysis. Users of the method must document and have 
on file the required initial demonstration performance data described in 
Section 9.2 prior to using the method for analysis.

                          2.0 Summary of Method

    2.1 An aliquot of a well mixed, homogeneous aqueous or solid sample 
is accurately weighed or measured for sample processing. For total 
recoverable analysis of a solid or an aqueous sample containing 
undissolved material, analytes are first solubilized by gentle refluxing 
with nitric and hydrochloric acids. After cooling, the sample is made up 
to volume, is mixed and centrifuged or allowed to settle overnight prior 
to analysis. For the determination of dissolved analytes in a filtered 
aqueous sample aliquot, or for the ``direct analysis'' total recoverable 
determination of analytes in drinking water where sample turbidity is <1 
NTU, the sample is made ready for analysis by the appropriate addition 
of nitric acid, and then diluted to a predetermined volume and mixed 
before analysis.
    2.2 The analysis described in this method involves multielemental 
determinations by ICP-AES using sequential or simultaneous instruments. 
The instruments measure characteristic atomic-line emission spectra by 
optical spectrometry. Samples are nebulized and the resulting aerosol is 
transported to the plasma torch. Element specific emission spectra are 
produced by a radio-frequency inductively coupled plasma. The spectra 
are dispersed by a grating spectrometer, and the intensities of the line 
spectra are monitored at specific wavelengths by a photosensitive 
device. Photocurrents from the photosensitive device are processed and 
controlled by a computer system. A background correction technique is 
required to compensate for variable background contribution to the 
determination of the analytes. Background must be measured adjacent to 
the analyte wavelength during analysis. Various interferences must be 
considered and addressed appropriately as discussed in Sections 4.0, 
7.0, 9.0, 10.0, and 11.0.

                             3.0 Definitions

    3.1 Calibration Blank--A volume of reagent water acidified with the 
same acid matrix as in the calibration standards. The calibration blank 
is a zero standard and is used to calibrate the ICP instrument (Section 
7.10.1).
    3.2 Calibration Standard (CAL)--A solution prepared from the 
dilution of stock standard solutions. The CAL solutions are used to 
calibrate the instrument response with respect to analyte concentration 
(Section 7.9).
    3.3 Dissolved Analyte--The concentration of analyte in an aqueous 
sample that will pass through a 0.45 [micro]m membrane filter assembly 
prior to sample acidification (Section 11.1).
    3.4 Field Reagent Blank (FRB)--An aliquot of reagent water or other 
blank matrix that is placed in a sample container in the laboratory and 
treated as a sample in all respects, including shipment to the sampling 
site, exposure to the sampling site conditions, storage, preservation, 
and all analytical procedures. The purpose of the FRB is to determine if 
method analytes or other interferences are present in the field 
environment (Section 8.5).
    3.5 Instrument Detection Limit (IDL)--The concentration equivalent 
to the analyte signal which is equal to three times the standard 
deviation of a series of 10 replicate measurements of the calibration 
blank signal at the same wavelength (Table 1.).
    3.6 Instrument Performance Check (IPC) Solution--A solution of 
method analytes, used to evaluate the performance of the instrument 
system with respect to a defined set of method criteria (Sections 7.11 
and 9.3.4).
    3.7 Internal Standard--Pure analyte(s) added to a sample, extract, 
or standard solution in known amount(s) and used to measure the relative 
responses of other method analytes that are components of the same 
sample or solution. The internal standard must be an analyte that is not 
a sample component (Section 11.5).
    3.8 Laboratory Duplicates (LD1 and LD2)--Two aliquots of the same 
sample taken in the laboratory and analyzed separately with identical 
procedures. Analyses of LD1 and LD2 indicate precision associated with 
laboratory procedures, but not with sample collection, preservation, or 
storage procedures.
    3.9 Laboratory Fortified Blank (LFB)--An aliquot of LRB to which 
known quantities of the method analytes are added in the laboratory. The 
LFB is analyzed exactly like a sample, and its purpose is to determine 
whether the methodology is in control and whether the laboratory is 
capable of making accurate and precise measurements (Sections 7.10.3 and 
9.3.2).
    3.10 Laboratory Fortified Sample Matrix (LFM)--An aliquot of an 
environmental sample to which known quantities of the method analytes 
are added in the laboratory. The

[[Page 391]]

LFM is analyzed exactly like a sample, and its purpose is to determine 
whether the sample matrix contributes bias to the analytical results. 
The background concentrations of the analytes in the sample matrix must 
be determined in a separate aliquot and the measured values in the LFM 
corrected for background concentrations (Section 9.4).
    3.11 Laboratory Reagent Blank (LRB)--An aliquot of reagent water or 
other blank matrices that are treated exactly as a sample including 
exposure to all glassware, equipment, solvents, reagents, and internal 
standards that are used with other samples. The LRB is used to determine 
if method analytes or other interferences are present in the laboratory 
environment, reagents, or apparatus (Sections 7.10.2 and 9.3.1).
    3.12 Linear Dynamic Range (LDR)--The concentration range over which 
the instrument response to an analyte is linear (Section 9.2.2).
    3.13 Method Detection Limit (MDL)--The minimum concentration of an 
analyte that can be identified, measured, and reported with 99% 
confidence that the analyte concentration is greater than zero (Section 
9.2.4 and Table 4.).
    3.14 Plasma Solution--A solution that is used to determine the 
optimum height above the work coil for viewing the plasma (Sections 7.15 
and 10.2.3).
    3.15 Quality Control Sample (QCS)--A solution of method analytes of 
known concentrations which is used to fortify an aliquot of LRB or 
sample matrix. The QCS is obtained from a source external to the 
laboratory and different from the source of calibration standards. It is 
used to check either laboratory or instrument performance (Sections 7.12 
and 9.2.3).
    3.16 Solid Sample--For the purpose of this method, a sample taken 
from material classified as soil, sediment or sludge.
    3.17 Spectral Interference Check (SIC) Solution--A solution of 
selected method analytes of higher concentrations which is used to 
evaluate the procedural routine for correcting known interelement 
spectral interferences with respect to a defined set of method criteria 
(Sections 7.13, 7.14 and 9.3.5).
    3.18 Standard Addition--The addition of a known amount of analyte to 
the sample in order to determine the relative response of the detector 
to an analyte within the sample matrix. The relative response is then 
used to assess either an operative matrix effect or the sample analyte 
concentration (Sections 9.5.1 and 11.5).
    3.19 Stock Standard Solution--A concentrated solution containing one 
or more method analytes prepared in the laboratory using assayed 
reference materials or purchased from a reputable commercial source 
(Section 7.8).
    3.20 Total Recoverable Analyte--The concentration of analyte 
determined either by ``direct analysis'' of an unfiltered acid preserved 
drinking water sample with turbidity of <1 NTU (Section 11.2.1), or by 
analysis of the solution extract of a solid sample or an unfiltered 
aqueous sample following digestion by refluxing with hot dilute mineral 
acid(s) as specified in the method (Sections 11.2 and 11.3).
    3.21 Water Sample--For the purpose of this method, a sample taken 
from one of the following sources: drinking, surface, ground, storm 
runoff, industrial or domestic wastewater.

                            4.0 Interferences

    4.1 Spectral interferences are caused by background emission from 
continuous or recombination phenomena, stray light from the line 
emission of high concentration elements, overlap of a spectral line from 
another element, or unresolved overlap of molecular band spectra.
    4.1.1 Background emission and stray light can usually be compensated 
for by subtracting the background emission determined by measurement(s) 
adjacent to the analyte wavelength peak. Spectral scans of samples or 
single element solutions in the analyte regions may indicate not only 
when alternate wavelengths are desirable because of severe spectral 
interference, but also will show whether the most appropriate estimate 
of the background emission is provided by an interpolation from 
measurements on both sides of the wavelength peak or by the measured 
emission on one side or the other. The location(s) selected for the 
measurement of background intensity will be determined by the complexity 
of the spectrum adjacent to the wavelength peak. The location(s) used 
for routine measurement must be free of off-line spectral interference 
(interelement or molecular) or adequately corrected to reflect the same 
change in background intensity as occurs at the wavelength peak.
    4.1.2 Spectral overlaps may be avoided by using an alternate 
wavelength or can be compensated for by equations that correct for 
interelement contributions, which involves measuring the interfering 
elements. Some potential on-line spectral interferences observed for the 
recommended wavelengths are given in Table 2. When operative and 
uncorrected, these interferences will produce false-positive 
determinations and be reported as analyte concentrations. The 
interferences listed are only those that occur between method analytes. 
Only interferences of a direct overlap nature that were observed with a 
single instrument having a working resolution of 0.035 nm are listed. 
More extensive information on interferant effects at various wavelengths 
and resolutions is available in Boumans' Tables.\8\ Users may apply 
interelement correction factors determined on their instruments within 
tested concentration ranges to compensate (off-line or

[[Page 392]]

on-line) for the effects of interfering elements.
    4.1.3 When interelement corrections are applied, there is a need to 
verify their accuracy by analyzing spectral interference check solutions 
as described in Section 7.13. Interelement corrections will vary for the 
same emission line among instruments because of differences in 
resolution, as determined by the grating plus the entrance and exit slit 
widths, and by the order of dispersion. Interelement corrections will 
also vary depending upon the choice of background correction points. 
Selecting a background correction point where an interfering emission 
line may appear should be avoided when practical. Interelement 
corrections that constitute a major portion of an emission signal may 
not yield accurate data. Users should not forget that some samples may 
contain uncommon elements that could contribute spectral 
interferences.\7 8\
    4.1.4 The interference effects must be evaluated for each individual 
instrument whether configured as a sequential or simultaneous 
instrument. For each instrument, intensities will vary not only with 
optical resolution but also with operating conditions (such as power, 
viewing height and argon flow rate). When using the recommended 
wavelengths given in Table 1, the analyst is required to determine and 
document for each wavelength the effect from the known interferences 
given in Table 2, and to utilize a computer routine for their automatic 
correction on all analyses. To determine the appropriate location for 
off-line background correction, the user must scan the area on either 
side adjacent to the wavelength and record the apparent emission 
intensity from all other method analytes. This spectral information must 
be documented and kept on file. The location selected for background 
correction must be either free of off-line interelement spectral 
interference or a computer routine must be used for their automatic 
correction on all determinations. If a wavelength other than the 
recommended wavelength is used, the user must determine and document 
both the on-line and off-line spectral interference effect from all 
method analytes and provide for their automatic correction on all 
analyses. Tests to determine the spectral interference must be done 
using analyte concentrations that will adequately describe the 
interference. Normally, 100 mg/L single element solutions are 
sufficient, however, for analytes such as iron that may be found at high 
concentration a more appropriate test would be to use a concentration 
near the upper LDR limit. See Section 10.4 for required spectral 
interference test criteria.
    4.1.5 When interelement corrections are not used, either on-going 
SIC solutions (Section 7.14) must be analyzed to verify the absence of 
interelement spectral interference or a computer software routine must 
be employed for comparing the determinative data to limits files for 
notifying the analyst when an interfering element is detected in the 
sample at a concentration that will produce either an apparent false 
positive concentration, greater than the analyte IDL, or false negative 
analyte concentration, less than the 99% lower control limit of the 
calibration blank. When the interference accounts for 10% or more of the 
analyte concentration, either an alternate wavelength free of 
interference or another approved test procedure must be used to complete 
the analysis. For example, the copper peak at 213.853 nm could be 
mistaken for the zinc peak at 213.856 nm in solutions with high copper 
and low zinc concentrations. For this example, a spectral scan in the 
213.8 nm region would not reveal the misidentification because a single 
peak near the zinc location would be observed. The possibility of this 
misidentification of copper for the zinc peak at 213.856 nm can be 
identified by measuring the copper at another emission line, e.g., 
324.754 nm. Users should be aware that, depending upon the instrumental 
resolution, alternate wavelengths with adequate sensitivity and freedom 
from interference may not be available for all matrices. In these 
circumstances the analyte must be determined using another approved test 
procedure.
    4.2 Physical interferences are effects associated with the sample 
nebulization and transport processes. Changes in viscosity and surface 
tension can cause significant inaccuracies, especially in samples 
containing high dissolved solids or high acid concentrations. If 
physical interferences are present, they must be reduced by such means 
as a high-solids nebulizer, diluting the sample, using a peristaltic 
pump, or using an appropriate internal standard element. Another problem 
that can occur with high dissolved solids is salt buildup at the tip of 
the nebulizer, which affects aerosol flow rate and causes instrumental 
drift. This problem can be controlled by a high-solids nebulizer, 
wetting the argon prior to nebulization, using a tip washer, or diluting 
the sample. Also, it has been reported that better control of the argon 
flow rates, especially for the nebulizer, improves instrument stability 
and precision; this is accomplished with the use of mass flow 
controllers.
    4.3 Chemical interferences include molecular-compound formation, 
ionization effects, and solute-vaporization effects. Normally, these 
effects are not significant with the ICP-AES technique. If observed, 
they can be minimized by careful selection of operating conditions (such 
as incident power and observation height), by buffering of the sample, 
by matrix matching, and by standard-addition

[[Page 393]]

procedures. Chemical interferences are highly dependent on matrix type 
and the specific analyte element.
    4.4 Memory interferences result when analytes in a previous sample 
contribute to the signals measured in a new sample. Memory effects can 
result from sample deposition on the uptake tubing to the nebulizer, and 
from the buildup of sample material in the plasma torch and spray 
chamber. The site where these effects occur is dependent on the element 
and can be minimized by flushing the system with a rinse blank between 
samples (Section 7.10.4). The possibility of memory interferences should 
be recognized within an analytical run and suitable rinse times should 
be used to reduce them. The rinse times necessary for a particular 
element must be estimated prior to analysis. This may be achieved by 
aspirating a standard containing elements corresponding to either their 
LDR or a concentration ten times those usually encountered. The 
aspiration time should be the same as a normal sample analysis period, 
followed by analysis of the rinse blank at designated intervals. The 
length of time required to reduce analyte signals to within a factor of 
two of the method detection limit, should be noted. Until the required 
rinse time is established, this method requires a rinse period of at 
least 60 seconds between samples and standards. If a memory interference 
is suspected, the sample must be re-analyzed after a long rinse period.

                               5.0 Safety

    5.1 The toxicity or carcinogenicity of each reagent used in this 
method have not been fully established. Each chemical should be regarded 
as a potential health hazard and exposure to these compounds should be 
as low as reasonably achievable. Each laboratory is responsible for 
maintaining a current awareness file of OSHA regulations regarding the 
safe handling of the chemicals specified in this method.9-12 
A reference file of material data handling sheets should also be made 
available to all personnel involved in the chemical analysis. 
Specifically, concentrated nitric and hydrochloric acids present various 
hazards and are moderately toxic and extremely irritating to skin and 
mucus membranes. Use these reagents in a fume hood whenever possible and 
if eye or skin contact occurs, flush with large volumes of water. Always 
wear safety glasses or a shield for eye protection, protective clothing 
and observe proper mixing when working with these reagents.
    5.2 The acidification of samples containing reactive materials may 
result in the release of toxic gases, such as cyanides or sulfides. 
Acidification of samples should be done in a fume hood.
    5.3 All personnel handling environmental samples known to contain or 
to have been in contact with human waste should be immunized against 
known disease causative agents.
    5.4 The inductively coupled plasma should only be viewed with proper 
eye protection from the ultraviolet emissions.
    5.5 It is the responsibility of the user of this method to comply 
with relevant disposal and waste regulations. For guidance see Sections 
14.0 and 15.0.

                       6.0 Equipment and Supplies

    6.1 Inductively coupled plasma emission spectrometer:
    6.1.1 Computer-controlled emission spectrometer with background-
correction capability.

The spectrometer must be capable of meeting and complying with the 
requirements described and referenced in Section 2.2.

    6.1.2 Radio-frequency generator compliant with FCC regulations.
    6.1.3 Argon gas supply--High purity grade (99.99%). When analyses 
are conducted frequently, liquid argon is more economical and requires 
less frequent replacement of tanks than compressed argon in conventional 
cylinders.
    6.1.4 A variable speed peristaltic pump is required to deliver both 
standard and sample solutions to the nebulizer.
    6.1.5 (Optional) Mass flow controllers to regulate the argon flow 
rates, especially the aerosol transport gas, are highly recommended. 
Their use will provide more exacting control of reproducible plasma 
conditions.
    6.2 Analytical balance, with capability to measure to 0.1 mg, for 
use in weighing solids, for preparing standards, and for determining 
dissolved solids in digests or extracts.
    6.3 A temperature adjustable hot plate capable of maintaining a 
temperature of 95 [deg]C.
    6.4 (Optional) A temperature adjustable block digester capable of 
maintaining a temperature of 95 [deg]C and equipped with 250 mL 
constricted digestion tubes.
    6.5 (Optional) A steel cabinet centrifuge with guard bowl, electric 
timer and brake.
    6.6 A gravity convection drying oven with thermostatic control 
capable of maintaining 180 [deg]C 5 [deg]C.
    6.7 (Optional) An air displacement pipetter capable of delivering 
volumes ranging from 0.1-2500 [micro]L with an assortment of high 
quality disposable pipet tips.
    6.8 Mortar and pestle, ceramic or nonmetallic material.
    6.9 Polypropylene sieve, 5-mesh (4 mm opening).
    6.10 Labware--For determination of trace levels of elements, 
contamination and loss are of prime consideration. Potential 
contamination sources include improperly cleaned laboratory apparatus 
and general

[[Page 394]]

contamination within the laboratory environment from dust, etc. A clean 
laboratory work area designated for trace element sample handling must 
be used. Sample containers can introduce positive and negative errors in 
the determination of trace elements by contributing contaminants through 
surface desorption or leaching, or depleting element concentrations 
through adsorption processes. All reusable labware (glass, quartz, 
polyethylene, PTFE, FEP, etc.) should be sufficiently clean for the task 
objectives. Several procedures found to provide clean labware include 
washing with a detergent solution, rinsing with tap water, soaking for 
four hours or more in 20% (v/v) nitric acid or a mixture of 
HNO3 and HCl (1 + 2 + 9), rinsing with reagent water and 
storing clean. \2 3\ Chromic acid cleaning solutions must be avoided 
because chromium is an analyte.
    6.10.1 Glassware--Volumetric flasks, graduated cylinders, funnels 
and centrifuge tubes (glass and/or metal-free plastic).
    6.10.2 Assorted calibrated pipettes.
    6.10.3 Conical Phillips beakers (Corning 1080-250 or equivalent), 
250 mL with 50 mm watch glasses.
    6.10.4 Griffin beakers, 250 mL with 75 mm watch glasses and 
(optional) 75 mm ribbed watch glasses.
    6.10.5 (Optional) PTFE and/or quartz Griffin beakers, 250 mL with 
PTFE covers.
    6.10.6 Evaporating dishes or high-form crucibles, porcelain, 100 mL 
capacity.
    6.10.7 Narrow-mouth storage bottles, FEP (fluorinated ethylene 
propylene) with screw closure, 125 mL to 1 L capacities.
    6.10.8 One-piece stem FEP wash bottle with screw closure, 125 mL 
capacity.

                       7.0 Reagents and Standards

    7.1 Reagents may contain elemental impurities which might affect 
analytical data. Only high-purity reagents that conform to the American 
Chemical Society specifications \13\ should be used whenever possible. 
If the purity of a reagent is in question, analyze for contamination. 
All acids used for this method must be of ultra high-purity grade or 
equivalent. Suitable acids are available from a number of manufacturers. 
Redistilled acids prepared by sub-boiling distillation are acceptable.
    7.2 Hydrochloric acid, concentrated (sp.gr. 1.19)--HCl.
    7.2.1 Hydrochloric acid (1 + 1)--Add 500 mL concentrated HCl to 400 
mL reagent water and dilute to 1 L.
    7.2.2 Hydrochloric acid (1 + 4)--Add 200 mL concentrated HCl to 400 
mL reagent water and dilute to 1 L.
    7.2.3 Hydrochloric acid (1 + 20)--Add 10 mL concentrated HCl to 200 
mL reagent water.
    7.3 Nitric acid, concentrated (sp.gr. 1.41)--HNO3.
    7.3.1 Nitric acid (1 + 1)--Add 500 mL concentrated HNO3 
to 400 mL reagent water and dilute to 1 L.
    7.3.2 Nitric acid (1 + 2)--Add 100 mL concentrated HNO3 
to 200 mL reagent water.
    7.3.3 Nitric acid (1 + 5)--Add 50 mL concentrated HNO3 to 
250 mL reagent water.
    7.3.4 Nitric acid (1 + 9)--Add 10 mL concentrated HNO3 to 
90 mL reagent water.
    7.4 Reagent water. All references to water in this method refer to 
ASTM Type I grade water.\14\
    7.5 Ammonium hydroxide, concentrated (sp.gr. 0.902).
    7.6 Tartaric acid, ACS reagent grade.
    7.7 Hydrogen peroxide, 50%, stabilized certified reagent grade.
    7.8 Standard Stock Solutions--Stock standards may be purchased or 
prepared from ultra-high purity grade chemicals (99.99-99.999% pure). 
All compounds must be dried for one hour at 105 [deg]C, unless otherwise 
specified. It is recommended that stock solutions be stored in FEP 
bottles. Replace stock standards when succeeding dilutions for 
preparation of calibration standards cannot be verified.
    CAUTION: Many of these chemicals are extremely toxic if inhaled or 
swallowed (Section 5.1). Wash hands thoroughly after handling.
    Typical stock solution preparation procedures follow for 1 L 
quantities, but for the purpose of pollution prevention, the analyst is 
encouraged to prepare smaller quantities when possible. Concentrations 
are calculated based upon the weight of the pure element or upon the 
weight of the compound multiplied by the fraction of the analyte in the 
compound
    From pure element,

[[Page 395]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.001

where: gravimetric factor = the weight fraction of the analyte in the 
compound

    7.8.1 Aluminum solution, stock, 1 mL = 1000 [micro]g Al: Dissolve 
1.000 g of aluminum metal, weighed accurately to at least four 
significant figures, in an acid mixture of 4.0 mL of (1 + 1) HCl and 1 
mL of concentrated HNO3 in a beaker. Warm beaker slowly to 
effect solution. When dissolution is complete, transfer solution 
quantitatively to a 1 L flask, add an additional 10.0 mL of (1 + 1) HCl 
and dilute to volume with reagent water.
    7.8.2 Antimony solution, stock, 1 mL = 1000 [micro]g Sb: Dissolve 
1.000 g of antimony powder, weighed accurately to at least four 
significant figures, in 20.0 mL (1 + 1) HNO3 and 10.0 mL 
concentrated HCl. Add 100 mL reagent water and 1.50 g tartaric acid. 
Warm solution slightly to effect complete dissolution. Cool solution and 
add reagent water to volume in a 1 L volumetric flask.
    7.8.3 Arsenic solution, stock, 1 mL = 1000 [micro]g As: Dissolve 
1.320 g of As2O3 (As fraction = 0.7574), weighed 
accurately to at least four significant figures, in 100 mL of reagent 
water containing 10.0 mL concentrated NH4OH. Warm the 
solution gently to effect dissolution. Acidify the solution with 20.0 mL 
concentrated HNO3 and dilute to volume in a 1 L volumetric 
flask with reagent water.
    7.8.4 Barium solution, stock, 1 mL = 1000 [micro]g Ba: Dissolve 
1.437 g BaCO3 (Ba fraction = 0.6960), weighed accurately to 
at least four significant figures, in 150 mL (1 + 2) HNO3 
with heating and stirring to degas and dissolve compound. Let solution 
cool and dilute with reagent water in 1 L volumetric flask.
    7.8.5 Beryllium solution, stock, 1 mL = 1000 [micro]g Be: DO NOT 
DRY. Dissolve 19.66 g BeSO44H2O (Be 
fraction = 0.0509), weighed accurately to at least four significant 
figures, in reagent water, add 10.0 mL concentrated HNO3, and 
dilute to volume in a 1 L volumetric flask with reagent water.
    7.8.6 Boron solution, stock, 1 mL = 1000 [micro]g B: DO NOT DRY. 
Dissolve 5.716 g anhydrous H3BO3 (B fraction = 
0.1749), weighed accurately to at least four significant figures, in 
reagent water and dilute in a 1 L volumetric flask with reagent water. 
Transfer immediately after mixing to a clean FEP bottle to minimize any 
leaching of boron from the glass volumetric container. Use of a nonglass 
volumetric flask is recommended to avoid boron contamination from 
glassware.
    7.8.7 Cadmium solution, stock, 1 mL = 1000 [micro]g Cd: Dissolve 
1.000 g Cd metal, acid cleaned with (1 + 9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1 + 1) 
HNO3 with heating to effect dissolution. Let solution cool 
and dilute with reagent water in a 1 L volumetric flask.
    7.8.8 Calcium solution, stock, 1 mL = 1000 [micro]g Ca: Suspend 
2.498 g CaCO3 (Ca fraction = 0.4005), dried at 180 [deg]C for 
one hour before weighing, weighed accurately to at least four 
significant figures, in reagent water and dissolve cautiously with a 
minimum amount of (1 + 1) HNO3. Add 10.0 mL concentrated 
HNO3 and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.9 Cerium solution, stock, 1 mL = 1000 [micro]g Ce: Slurry 1.228 
g CeO2 (Ce fraction = 0.8141), weighed accurately to at least 
four significant figures, in 100 mL concentrated HNO3 and 
evaporate to dryness. Slurry the residue in 20 mL H2O, add 50 
mL concentrated HNO3, with heat and stirring add 60 mL 50% 
H2O2 dropwise in 1 mL increments allowing periods 
of stirring between the 1 mL additions. Boil off excess 
H2O2 before diluting to volume in a 1 L volumetric 
flask with reagent water.
    7.8.10 Chromium solution, stock, 1 mL = 1000 [micro]g Cr: Dissolve 
1.923 g CrO3 (Cr fraction = 0.5200), weighed accurately to at 
least four significant figures, in 120 mL (1 + 5) HNO3. When 
solution is complete, dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.11 Cobalt solution, stock, 1 mL = 1000 [micro]g Co: Dissolve 
1.000 g Co metal, acid cleaned with (1 + 9) HNO3, weighed 
accurately to at least four significant figures, in 50.0 mL (1 + 1) 
HNO3. Let solution cool and dilute to volume in a 1 L 
volumetric flask with reagent water.
    7.8.12 Copper solution, stock, 1 mL = 1000 [micro]g Cu: Dissolve 
1.000 g Cu metal, acid cleaned with (1 + 9) HNO3, weighed 
accurately to at least four significant figures, in 50.0 mL (1 + 1) 
HNO3 with heating to effect dissolution. Let solution cool 
and dilute in a 1 L volumetric flask with reagent water.
    7.8.13 Iron solution, stock, 1 mL = 1000 [micro]g Fe: Dissolve 1.000 
g Fe metal, acid cleaned

[[Page 396]]

with (1 + 1) HCl, weighed accurately to four significant figures, in 100 
mL (1 + 1) HCl with heating to effect dissolution. Let solution cool and 
dilute with reagent water in a 1 L volumetric flask.
    7.8.14 Lead solution, stock, 1 mL = 1000 [micro]g Pb: Dissolve 1.599 
g Pb(NO3)2 (Pb fraction = 0.6256), weighed 
accurately to at least four significant figures, in a minimum amount of 
(1 + 1) HNO3. Add 20.0 mL (1 + 1) HNO3 and dilute 
to volume in a 1 L volumetric flask with reagent water.
    7.8.15 Lithium solution, stock, 1 mL = 1000 [micro]g Li: Dissolve 
5.324 g Li2CO3 (Li fraction = 0.1878), weighed 
accurately to at least four significant figures, in a minimum amount of 
(1 + 1) HCl and dilute to volume in a 1 L volumetric flask with reagent 
water.
    7.8.16 Magnesium solution, stock, 1 mL = 1000 [micro]g Mg: Dissolve 
1.000 g cleanly polished Mg ribbon, accurately weighed to at least four 
significant figures, in slowly added 5.0 mL (1 + 1) HCl (CAUTION: 
reaction is vigorous). Add 20.0 mL (1 + 1) HNO3 and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.17 Manganese solution, stock, 1 mL = 1000 [micro]g Mn: Dissolve 
1.000 g of manganese metal, weighed accurately to at least four 
significant figures, in 50 mL (1 + 1) HNO3 and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.18 Mercury solution, stock, 1 mL = 1000 [micro]g Hg: DO NOT DRY. 
CAUTION: highly toxic element. Dissolve 1.354 g HgCl2 (Hg 
fraction = 0.7388) in reagent water. Add 50.0 mL concentrated 
HNO3 and dilute to volume in 1 L volumetric flask with 
reagent water.
    7.8.19 Molybdenum solution, stock, 1 mL = 1000 [micro]g Mo: Dissolve 
1.500 g MoO3 (Mo fraction = 0.6666), weighed accurately to at 
least four significant figures, in a mixture of 100 mL reagent water and 
10.0 mL concentrated NH4OH, heating to effect dissolution. 
Let solution cool and dilute with reagent water in a 1 L volumetric 
flask.
    7.8.20 Nickel solution, stock, 1 mL = 1000 [micro]g Ni: Dissolve 
1.000 g of nickel metal, weighed accurately to at least four significant 
figures, in 20.0 mL hot concentrated HNO3, cool, and dilute 
to volume in a 1 L volumetric flask with reagent water.
    7.8.21 Phosphorus solution, stock, 1 mL = 1000 [micro]g P: Dissolve 
3.745 g NH4H2PO4 (P fraction = 0.2696), 
weighed accurately to at least four significant figures, in 200 mL 
reagent water and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.22 Potassium solution, stock, 1 mL = 1000 [micro]g K: Dissolve 
1.907 g KCl (K fraction = 0.5244) dried at 110 [deg]C, weighed 
accurately to at least four significant figures, in reagent water, add 
20 mL (1 + 1) HCl and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.23 Selenium solution, stock, 1 mL = 1000 [micro]g Se: Dissolve 
1.405 g SeO2 (Se fraction = 0.7116), weighed accurately to at 
least four significant figures, in 200 mL reagent water and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.24 Silica solution, stock, 1 mL = 1000 [micro]g SiO2: 
DO NOT DRY. Dissolve 2.964 g 
(NH4)2SiF6, weighed accurately to at 
least four significant figures, in 200 mL (1 + 20) HCl with heating at 
85 [deg]C to effect dissolution. Let solution cool and dilute to volume 
in a 1 L volumetric flask with reagent water.
    7.8.25 Silver solution, stock, 1 mL = 1000 [micro]g Ag: Dissolve 
1.000 g Ag metal, weighed accurately to at least four significant 
figures, in 80 mL (1 + 1) HNO3 with heating to effect 
dissolution. Let solution cool and dilute with reagent water in a 1 L 
volumetric flask. Store solution in amber bottle or wrap bottle 
completely with aluminum foil to protect solution from light.
    7.8.26 Sodium solution, stock, 1 mL = 1000 [micro]g Na: Dissolve 
2.542 g NaCl (Na fraction = 0.3934), weighed accurately to at least four 
significant figures, in reagent water. Add 10.0 mL concentrated 
HNO3 and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.27 Strontium solution, stock, 1 mL = 1000 [micro]g Sr: Dissolve 
1.685 g SrCO3 (Sr fraction = 0.5935), weighed accurately to 
at least four significant figures, in 200 mL reagent water with dropwise 
addition of 100 mL (1 + 1) HCl. Dilute to volume in a 1 L volumetric 
flask with reagent water.
    7.8.28 Thallium solution, stock, 1 mL = 1000 [micro]g Tl: Dissolve 
1.303 g TlNO3 (Tl fraction = 0.7672), weighed accurately to 
at least four significant figures, in reagent water. Add 10.0 mL 
concentrated HNO3 and dilute to volume in a 1 L volumetric 
flask with reagent water.
    7.8.29 Tin solution, stock, 1 mL = 1000 [micro]g Sn: Dissolve 1.000 
g Sn shot, weighed accurately to at least four significant figures, in 
an acid mixture of 10.0 mL concentrated HCl and 2.0 mL (1 + 1) 
HNO3 with heating to effect dissolution. Let solution cool, 
add 200 mL concentrated HCl, and dilute to volume in a 1 L volumetric 
flask with reagent water.
    7.8.30 Titanium solution, stock, 1 mL = 1000 [micro]g Ti: DO NOT 
DRY. Dissolve 6.138 g 
(NH4)2TiO(C2O4)2
H2O (Ti fraction = 0.1629), weighed accurately to at least 
four significant figures, in 100 mL reagent water. Dilute to volume in a 
1 L volumetric flask with reagent water.
    7.8.31 Vanadium solution, stock, 1 mL = 1000 [micro]g V: Dissolve 
1.000 g V metal, acid cleaned with (1 + 9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1 + 1) 
HNO3 with heating to effect dissolution. Let solution cool 
and dilute with reagent water to volume in a 1 L volumetric flask.
    7.8.32 Yttrium solution, stock 1 mL = 1000 [micro]g Y: Dissolve 
1.270 g Y2O3 (Y fraction = 0.7875), weighed 
accurately to at least four significant figures, in 50 mL (1 + 1) 
HNO3, heating to effect dissolution. Cool and dilute

[[Page 397]]

to volume in a 1 L volumetric flask with reagent water.
    7.8.33 Zinc solution, stock, 1 mL = 1000 [micro]g Zn: Dissolve 1.000 
g Zn metal, acid cleaned with (1 + 9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1 + 1) 
HNO3 with heating to effect dissolution. Let solution cool 
and dilute with reagent water to volume in a 1 L volumetric flask.
    7.9 Mixed Calibration Standard Solutions--For the analysis of total 
recoverable digested samples prepare mixed calibration standard 
solutions (see Table 3) by combining appropriate volumes of the stock 
solutions in 500 mL volumetric flasks containing 20 mL (1 + 1) 
HNO3 and 20 mL (1 + 1) HCl and dilute to volume with reagent 
water. Prior to preparing the mixed standards, each stock solution 
should be analyzed separately to determine possible spectral 
interferences or the presence of impurities. Care should be taken when 
preparing the mixed standards to ensure that the elements are compatible 
and stable together. To minimize the opportunity for contamination by 
the containers, it is recommended to transfer the mixed-standard 
solutions to acid-cleaned, never-used FEP fluorocarbon (FEP) bottles for 
storage. Fresh mixed standards should be prepared, as needed, with the 
realization that concentrations can change on aging. Calibration 
standards not prepared from primary standards must be initially verified 
using a certified reference solution. For the recommended wavelengths 
listed in Table 1 some typical calibration standard combinations are 
given in Table 3.

    Note: If the addition of silver to the recommended mixed-acid 
calibration standard results in an initial precipitation, add 15 mL of 
reagent water and warm the flask until the solution clears. For this 
acid combination, the silver concentration should be limited to 0.5 mg/
L.

    7.10 Blanks--Four types of blanks are required for the analysis. The 
calibration blank is used in establishing the analytical curve, the 
laboratory reagent blank is used to assess possible contamination from 
the sample preparation procedure, the laboratory fortified blank is used 
to assess routine laboratory performance and a rinse blank is used to 
flush the instrument uptake system and nebulizer between standards, 
check solutions, and samples to reduce memory interferences.
    7.10.1 The calibration blank for aqueous samples and extracts is 
prepared by acidifying reagent water to the same concentrations of the 
acids as used for the standards. The calibration blank should be stored 
in a FEP bottle.
    7.10.2 The laboratory reagent blank (LRB) must contain all the 
reagents in the same volumes as used in the processing of the samples. 
The LRB must be carried through the same entire preparation scheme as 
the samples including sample digestion, when applicable.
    7.10.3 The laboratory fortified blank (LFB) is prepared by 
fortifying an aliquot of the laboratory reagent blank with all analytes 
to a suitable concentration using the following recommended criteria: Ag 
0.1 mg/L, K 5.0 mg/L and all other analytes 0.2 mg/L or a concentration 
approximately 100 times their respective MDL, whichever is greater. The 
LFB must be carried through the same entire preparation scheme as the 
samples including sample digestion, when applicable.
    7.10.4 The rinse blank is prepared by acidifying reagent water to 
the same concentrations of acids as used in the calibration blank and 
stored in a convenient manner.
    7.11 Instrument Performance Check (IPC) Solution--The IPC solution 
is used to periodically verify instrument performance during analysis. 
It should be prepared in the same acid mixture as the calibration 
standards by combining method analytes at appropriate concentrations. 
Silver must be limited to <0.5 mg/L; while potassium and phosphorus 
because of higher MDLs and silica because of potential contamination 
should be at concentrations of 10 mg/L. For other analytes a 
concentration of 2 mg/L is recommended. The IPC solution should be 
prepared from the same standard stock solutions used to prepare the 
calibration standards and stored in an FEP bottle. Agency programs may 
specify or request that additional instrument performance check 
solutions be prepared at specified concentrations in order to meet 
particular program needs.
    7.12 Quality Control Sample (QCS)--Analysis of a QCS is required for 
initial and periodic verification of calibration standards or stock 
standard solutions in order to verify instrument performance. The QCS 
must be obtained from an outside source different from the standard 
stock solutions and prepared in the same acid mixture as the calibration 
standards. The concentration of the analytes in the QCS solution should 
be 1 mg/L, except silver, which must be limited to a concentration of 
0.5 mg/L for solution stability. The QCS solution should be stored in a 
FEP bottle and analyzed as needed to meet data-quality needs. A fresh 
solution should be prepared quarterly or more frequently as needed.
    7.13 Spectral Interference Check (SIC) Solutions--When interelement 
corrections are applied, SIC solutions are needed containing 
concentrations of the interfering elements at levels that will provide 
an adequate test of the correction factors.
    7.13.1 SIC solutions containing (a) 300 mg/L Fe; (b) 200 mg/L AL; 
(c) 50 mg/L Ba; (d) 50 mg/L Be; (e) 50 mg/L Cd; (f) 50 mg/L Ce; (g) 50 
mg/L Co; (h) 50 mg/L Cr; (i) 50 mg/L Cu; (j) 50

[[Page 398]]

mg/L Mn; (k) 50 mg/L Mo; (l) 50 mg/L Ni; (m) 50 mg/L Sn; (n) 50 mg/L 
SiO2; (o) 50 mg/L Ti; (p) 50 mg/L Tl and (q) 50 mg/L V should 
be prepared in the same acid mixture as the calibration standards and 
stored in FEP bottles. These solutions can be used to periodically 
verify a partial list of the on-line (and possible off-line) 
interelement spectral correction factors for the recommended wavelengths 
given in Table 1. Other solutions could achieve the same objective as 
well. (Multielement SIC solutions\3\ may be prepared and substituted for 
the single element solutions provided an analyte is not subject to 
interference from more than one interferant in the solution.)

    Note: If wavelengths other than those recommended in Table 1 are 
used, other solutions different from those above (a through q) may be 
required.

    7.13.2 For interferences from iron and aluminum, only those 
correction factors (positive or negative) when multiplied by 100 to 
calculate apparent analyte concentrations that exceed the determined 
analyte IDL or fall below the lower 3-sigma control limit of the 
calibration blank need be tested on a daily basis.
    7.13.3 For the other interfering elements, only those correction 
factors (positive or negative) when multiplied by 10 to calculate 
apparent analyte concentrations that exceed the determined analyte IDL 
or fall below the lower 3-sigma control limit of the calibration blank 
need be tested on a daily basis.
    7.13.4 If the correction routine is operating properly, the 
determined apparent analyte(s) concentration from analysis of each 
interference solution (a through q) should fall within a specific 
concentration range bracketing the calibration blank. This concentration 
range is calculated by multiplying the concentration of the interfering 
element by the value of the correction factor being tested and dividing 
by 10. If after subtraction of the calibration blank the apparent 
analyte concentration is outside (above or below) this range, a change 
in the correction factor of more than 10% should be suspected. The cause 
of the change should be determined and corrected and the correction 
factor should be updated.

    Note: The SIC solution should be analyzed more than once to confirm 
a change has occurred with adequate rinse time between solutions and 
before subsequent analysis of the calibration blank.

    7.13.5 If the correction factors tested on a daily basis are found 
to be within the 10% criteria for five consecutive days, the required 
verification frequency of those factors in compliance may be extended to 
a weekly basis. Also, if the nature of the samples analyzed is such 
(e.g., finished drinking water) that they do not contain concentrations 
of the interfering elements at the 10 mg/L level, daily verification is 
not required; however, all interelement spectral correction factors must 
be verified annually and updated, if necessary.
    7.13.6 If the instrument does not display negative concentration 
values, fortify the SIC solutions with the elements of interest at 1 mg/
L and test for analyte recoveries that are below 95%. In the absence of 
measurable analyte, over-correction could go undetected because a 
negative value could be reported as zero.
    7.14 For instruments without interelement correction capability or 
when interelement corrections are not used, SIC solutions (containing 
similar concentrations of the major components in the samples, e.g., 10 
mg/L) can serve to verify the absence of effects at the wavelengths 
selected. These data must be kept on file with the sample analysis data. 
If the SIC solution confirms an operative interference that is 10% of 
the analyte concentration, the analyte must be determined using a 
wavelength and background correction location free of the interference 
or by another approved test procedure. Users are advised that high salt 
concentrations can cause analyte signal suppressions and confuse 
interference tests.
    7.15 Plasma Solution--The plasma solution is used for determining 
the optimum viewing height of the plasma above the work coil prior to 
using the method (Section 10.2). The solution is prepared by adding a 5 
mL aliquot from each of the stock standard solutions of arsenic, lead, 
selenium, and thallium to a mixture of 20 mL (1 + 1) nitric acid and 20 
mL (1 + 1) hydrochloric acid and diluting to 500 mL with reagent water. 
Store in a FEP bottle.

            8.0 Sample Collection, Preservation, and Storage

    8.1 Prior to the collection of an aqueous sample, consideration 
should be given to the type of data required, (i.e., dissolved or total 
recoverable), so that appropriate preservation and pretreatment steps 
can be taken. The pH of all aqueous samples must be tested immediately 
prior to aliquoting for processing or ``direct analysis'' to ensure the 
sample has been properly preserved. If properly acid preserved, the 
sample can be held up to six months before analysis.
    8.2 For the determination of the dissolved elements, the sample must 
be filtered through a 0.45 [micro]m pore diameter membrane filter at the 
time of collection or as soon thereafter as practically possible. (Glass 
or plastic filtering apparatus are recommended to avoid possible 
contamination. Only plastic apparatus should be used when the 
determinations of boron and silica are critical.) Use a portion of the 
filtered sample to rinse the filter flask, discard this portion and 
collect the required volume of filtrate. Acidify

[[Page 399]]

the filtrate with (1 + 1) nitric acid immediately following filtration 
to pH <2.
    8.3 For the determination of total recoverable elements in aqueous 
samples, samples are not filtered, but acidified with (1 + 1) nitric 
acid to pH <2 (normally, 3 mL of (1 + 1) acid per liter of sample is 
sufficient for most ambient and drinking water samples). Preservation 
may be done at the time of collection, however, to avoid the hazards of 
strong acids in the field, transport restrictions, and possible 
contamination it is recommended that the samples be returned to the 
laboratory within two weeks of collection and acid preserved upon 
receipt in the laboratory. Following acidification, the sample should be 
mixed, held for 16 hours, and then verified to be pH <2 just prior 
withdrawing an aliquot for processing or ``direct analysis''. If for 
some reason such as high alkalinity the sample pH is verified to be 
2, more acid must be added and the sample held for 16 hours 
until verified to be pH <2. See Section 8.1.

    Note: When the nature of the sample is either unknown or is known to 
be hazardous, acidification should be done in a fume hood. See Section 
5.2.

    8.4 Solid samples require no preservation prior to analysis other 
than storage at 4 [deg]C. There is no established holding time 
limitation for solid samples.
    8.5 For aqueous samples, a field blank should be prepared and 
analyzed as required by the data user. Use the same container and acid 
as used in sample collection.

                           9.0 Quality Control

    9.1 Each laboratory using this method is required to operate a 
formal quality control (QC) program. The minimum requirements of this 
program consist of an initial demonstration of laboratory capability, 
and the periodic analysis of laboratory reagent blanks, fortified blanks 
and other laboratory solutions as a continuing check on performance. The 
laboratory is required to maintain performance records that define the 
quality of the data thus generated.
    9.2 Initial Demonstration of Performance (mandatory).
    9.2.1 The initial demonstration of performance is used to 
characterize instrument performance (determination of linear dynamic 
ranges and analysis of quality control samples) and laboratory 
performance (determination of method detection limits) prior to analyses 
conducted by this method.
    9.2.2 Linear dynamic range (LDR)--The upper limit of the LDR must be 
established for each wavelength utilized. It must be determined from a 
linear calibration prepared in the normal manner using the established 
analytical operating procedure for the instrument. The LDR should be 
determined by analyzing succeedingly higher standard concentrations of 
the analyte until the observed analyte concentration is no more than 10% 
below the stated concentration of the standard. Determined LDRs must be 
documented and kept on file. The LDR which may be used for the analysis 
of samples should be judged by the analyst from the resulting data. 
Determined sample analyte concentrations that are greater than 90% of 
the determined upper LDR limit must be diluted and reanalyzed. The LDRs 
should be verified annually or whenever, in the judgment of the analyst, 
a change in analytical performance caused by either a change in 
instrument hardware or operating conditions would dictate they be 
redetermined.
    9.2.3 Quality control sample (QCS)--When beginning the use of this 
method, on a quarterly basis, after the preparation of stock or 
calibration standard solutions or as required to meet data-quality 
needs, verify the calibration standards and acceptable instrument 
performance with the preparation and analyses of a QCS (Section 7.12). 
To verify the calibration standards the determined mean concentrations 
from three analyses of the QCS must be within 5% of the stated values. 
If the calibration standard cannot be verified, performance of the 
determinative step of the method is unacceptable. The source of the 
problem must be identified and corrected before either proceeding on 
with the initial determination of method detection limits or continuing 
with on-going analyses.
    9.2.4 Method detection limit (MDL)--MDLs must be established for all 
wavelengths utilized, using reagent water (blank) fortified at a 
concentration of two to three times the estimated instrument detection 
limit.\15\ To determine MDL values, take seven replicate aliquots of the 
fortified reagent water and process through the entire analytical 
method. Perform all calculations defined in the method and report the 
concentration values in the appropriate units. Calculate the MDL as 
follows:

MDL = (t) x (S)

where:

t = students' t value for a 99% confidence level and a standard 
          deviation estimate with n-1 degrees of freedom [t = 3.14 for 
          seven replicates]
S = standard deviation of the replicate analyses

    Note: If additional confirmation is desired, reanalyze the seven 
replicate aliquots on two more nonconsecutive days and again calculate 
the MDL values for each day. An average of the three MDL values for each 
analyte may provide for a more appropriate MDL estimate. If the relative 
standard deviation (RSD) from the analyses of the seven aliquots is 
<10%, the concentration used to determine the analyte MDL may have been 
inappropriately high for the determination. If so, this could result in 
the calculation of

[[Page 400]]

an unrealistically low MDL. Concurrently, determination of MDL in 
reagent water represents a best case situation and does not reflect 
possible matrix effects of real world samples. However, successful 
analyses of LFMs (Section 9.4) and the analyte addition test described 
in Section 9.5.1 can give confidence to the MDL value determined in 
reagent water. Typical single laboratory MDL values using this method 
are given in Table 4.
    The MDLs must be sufficient to detect analytes at the required 
levels according to compliance monitoring regulation (Section 1.2). MDLs 
should be determined annually, when a new operator begins work or 
whenever, in the judgment of the analyst, a change in analytical 
performance caused by either a change in instrument hardware or 
operating conditions would dictate they be redetermined.

    9.3 Assessing Laboratory Performance (mandatory)
    9.3.1 Laboratory reagent blank (LRB)--The laboratory must analyze at 
least one LRB (Section 7.10.2) with each batch of 20 or fewer samples of 
the same matrix. LRB data are used to assess contamination from the 
laboratory environment. LRB values that exceed the MDL indicate 
laboratory or reagent contamination should be suspected. When LRB values 
constitute 10% or more of the analyte level determined for a sample or 
is 2.2 times the analyte MDL whichever is greater, fresh aliquots of the 
samples must be prepared and analyzed again for the affected analytes 
after the source of contamination has been corrected and acceptable LRB 
values have been obtained.
    9.3.2 Laboratory fortified blank (LFB)--The laboratory must analyze 
at least one LFB (Section 7.10.3) with each batch of samples. Calculate 
accuracy as percent recovery using the following equation:
[GRAPHIC] [TIFF OMITTED] TR18MY12.002

where:

R = percent recovery
LFB = laboratory fortified blank
LRB = laboratory reagent blank
s = concentration equivalent of analyte added to fortify the LBR 
          solution

    If the recovery of any analyte falls outside the required control 
limits of 85-115%, that analyte is judged out of control, and the source 
of the problem should be identified and resolved before continuing 
analyses.
    9.3.3 The laboratory must use LFB analyses data to assess laboratory 
performance against the required control limits of 85-115% (Section 
9.3.2). When sufficient internal performance data become available 
(usually a minimum of 20-30 analyses), optional control limits can be 
developed from the mean percent recovery (x) and the standard deviation 
(S) of the mean percent recovery. These data can be used to establish 
the upper and lower control limits as follows:

UPPER CONTROL LIMIT = x + 3S
LOWER CONTROL LIMIT = x - 3S

    The optional control limits must be equal to or better than the 
required control limits of 85-115%. After each five to 10 new recovery 
measurements, new control limits can be calculated using only the most 
recent 20-30 data points. Also, the standard deviation (S) data should 
be used to establish an on-going precision statement for the level of 
concentrations included in the LFB. These data must be kept on file and 
be available for review.
    9.3.4 Instrument performance check (IPC) solution--For all 
determinations the laboratory must analyze the IPC solution (Section 
7.11) and a calibration blank immediately following daily calibration, 
after every 10th sample (or more frequently, if required) and at the end 
of the sample run. Analysis of the calibration blank should always be 
s = fortified sample concentration
C = sample background concentration
s = concentration equivalent of analyte added to fortify the sample

    9.4.4 If the recovery of any analyte falls outside the designated 
LFM recovery range, and the laboratory performance for that analyte is 
shown to be in control (Section 9.3), the recovery problem encountered 
with the fortified sample is judged to be matrix related, not system 
related. The data user should be informed that the result for that 
analyte in the unfortified sample is suspect due to either the 
heterogeneous nature of the sample or matrix effects and analysis by 
method of standard addition or the use of an internal standard(s) 
(Section 11.5) should be considered.
    9.4.5 Where reference materials are available, they should be 
analyzed to provide additional performance data. The analysis of 
reference samples is a valuable tool for demonstrating the ability to 
perform the method acceptably. Reference materials containing high 
concentrations of analytes can provide additional information on the 
performance of the spectral interference correction routine.
    9.5 Assess the possible need for the method of standard additions 
(MSA) or internal standard elements by the following tests. Directions 
for using MSA or internal standard(s) are given in Section 11.5.
    9.5.1 Analyte addition test: An analyte(s) standard added to a 
portion of a prepared sample, or its dilution, should be recovered to 
within 85% to 115% of the known value. The analyte(s) addition should 
produce a

[[Page 402]]

minimum level of 20 times and a maximum of 100 times the method 
detection limit. If the analyte addition is <20% of the sample analyte 
concentration, the following dilution test should be used. If recovery 
of the analyte(s) is not within the specified limits, a matrix effect 
should be suspected, and the associated data flagged accordingly. The 
method of additions or the use of an appropriate internal standard 
element may provide more accurate data.
    9.5.2 Dilution test: If the analyte concentration is sufficiently 
high (minimally, a factor of 50 above the instrument detection limit in 
the original solution but <90% of the linear limit), an analysis of a 1 
+ 4 dilution should agree (after correction for the fivefold dilution) 
within 10% of the original determination. If not, a chemical or physical 
interference effect should be suspected and the associated data flagged 
accordingly. The method of standard additions or the use of an internal-
standard element may provide more accurate data for samples failing this 
test.

                  10.0 Calibration and Standardization

    10.1 Specific wavelengths are listed in Table 1. Other wavelengths 
may be substituted if they can provide the needed sensitivity and are 
corrected for spectral interference. However, because of the difference 
among various makes and models of spectrometers, specific instrument 
operating conditions cannot be given. The instrument and operating 
conditions utilized for determination must be capable of providing data 
of acceptable quality to the program and data user. The analyst should 
follow the instructions provided by the instrument manufacturer unless 
other conditions provide similar or better performance for a task. 
Operating conditions for aqueous solutions usually vary from 1100-1200 
watts forward power, 15-16 mm viewing height, 15-19 L/min. argon coolant 
flow, 0.6-1 L/min. argon aerosol flow, 1-1.8 mL/min. sample pumping rate 
with a one minute preflush time and measurement time near 1 s per 
wavelength peak (for sequential instruments) and near 10 s per sample 
(for simultaneous instruments). Use of the Cu/Mn intensity ratio at 
324.754 nm and 257.610 nm (by adjusting the argon aerosol flow) has been 
recommended as a way to achieve repeatable interference correction 
factors.\17\
    10.2 Prior to using this method optimize the plasma operating 
conditions. The following procedure is recommended for vertically 
configured plasmas. The purpose of plasma optimization is to provide a 
maximum signal-to-background ratio for the least sensitive element in 
the analytical array. The use of a mass flow controller to regulate the 
nebulizer gas flow rate greatly facilitates the procedure.
    10.2.1 Ignite the plasma and select an appropriate incident rf power 
with minimum reflected power. Allow the instrument to become thermally 
stable before beginning. This usually requires at least 30 to 60 minutes 
of operation. While aspirating the 1000 [micro]g/mL solution of yttrium 
(Section 7.8.32), follow the instrument manufacturer's instructions and 
adjust the aerosol carrier gas flow rate through the nebulizer so a 
definitive blue emission region of the plasma extends approximately from 
5-20 mm above the top of the work coil.\18\ Record the nebulizer gas 
flow rate or pressure setting for future reference.
    10.2.2 After establishing the nebulizer gas flow rate, determine the 
solution uptake rate of the nebulizer in mL/min. by aspirating a known 
volume calibration blank for a period of at least three minutes. Divide 
the spent volume by the aspiration time (in minutes) and record the 
uptake rate. Set the peristaltic pump to deliver the uptake rate in a 
steady even flow.
    10.2.3 After horizontally aligning the plasma and/or optically 
profiling the spectrometer, use the selected instrument conditions from 
Sections 10.2.1 and 10.2.2, and aspirate the plasma solution (Section 
7.15), containing 10 [micro]g/mL each of As, Pb, Se and Tl. Collect 
intensity data at the wavelength peak for each analyte at 1 mm intervals 
from 14-18 mm above the top of the work coil. (This region of the plasma 
is commonly referred to as the analytical zone.)\19\ Repeat the process 
using the calibration blank. Determine the net signal to blank intensity 
ratio for each analyte for each viewing height setting. Choose the 
height for viewing the plasma that provides the largest intensity ratio 
for the least sensitive element of the four analytes. If more than one 
position provides the same ratio, select the position that provides the 
highest net intensity counts for the least sensitive element or accept a 
compromise position of the intensity ratios of all four analytes.
    10.2.4 The instrument operating condition finally selected as being 
optimum should provide the lowest reliable instrument detection limits 
and method detection limits. Refer to Tables 1 and 4 for comparison of 
IDLs and MDLs, respectively.
    10.2.5 If either the instrument operating conditions, such as 
incident power and/or nebulizer gas flow rate are changed, or a new 
torch injector tube having a different orifice i.d. is installed, the 
plasma and plasma viewing height should be reoptimized.
    10.2.6 Before daily calibration and after the instrument warmup 
period, the nebulizer gas flow must be reset to the determined optimized 
flow. If a mass flow controller is being used, it should be reset to the 
recorded optimized flow rate. In order to maintain valid spectral 
interelement correction routines the nebulizer gas flow rate should be

[[Page 403]]

the same from day-to-day (<2% change). The change in signal intensity 
with a change in nebulizer gas flow rate for both ``hard'' (Pb 220.353 
nm) and ``soft'' (Cu 324.754) lines is illustrated in Figure 1.
    10.3 Before using the procedure (Section 11.0) to analyze samples, 
there must be data available documenting initial demonstration of 
performance. The required data and procedure is described in Section 
9.2. This data must be generated using the same instrument operating 
conditions and calibration routine (Section 11.4) to be used for sample 
analysis. These documented data must be kept on file and be available 
for review by the data user.
    10.4 After completing the initial demonstration of performance, but 
before analyzing samples, the laboratory must establish and initially 
verify an interelement spectral interference correction routine to be 
used during sample analysis. A general description concerning spectral 
interference and the analytical requirements for background correction 
and for correction of interelement spectral interference in particular 
are given in Section 4.1. To determine the appropriate location for 
background correction and to establish the interelement interference 
correction routine, repeated spectral scan about the analyte wavelength 
and repeated analyses of the single element solutions may be required. 
Criteria for determining an interelement spectral interference is an 
apparent positive or negative concentration on the analyte that is 
outside the 3-sigma control limits of the calibration blank for the 
analyte. (The upper-control limit is the analyte IDL.) Once established, 
the entire routine must be initially and periodically verified annually, 
or whenever there is a change in instrument operating conditions 
(Section 10.2.5). Only a portion of the correction routine must be 
verified more frequently or on a daily basis. Test criteria and required 
solutions are described in Section 7.13. Initial and periodic 
verification data of the routine should be kept on file. Special cases 
where on-going verification are required is described in Section 7.14.

                             11.0 Procedure

           11.1 Aqueous Sample Preparation--Dissolved Analytes

    11.1.1 For the determination of dissolved analytes in ground and 
surface waters, pipet an aliquot (20 mL) of the filtered, acid preserved 
sample into a 50 mL polypropylene centrifuge tube. Add an appropriate 
volume of (1 + 1) nitric acid to adjust the acid concentration of the 
aliquot to approximate a 1% (v/v) nitric acid solution (e.g., add 0.4 mL 
(1 + 1) HNO3 to a 20 mL aliquot of sample). Cap the tube and 
mix. The sample is now ready for analysis (Section 1.3). Allowance for 
sample dilution should be made in the calculations. (If mercury is to be 
determined, a separate aliquot must be additionally acidified to contain 
1% (v/v) HCl to match the signal response of mercury in the calibration 
standard and reduce memory interference effects. Section 1.9).

    Note: If a precipitate is formed during acidification, transport, or 
storage, the sample aliquot must be treated using the procedure 
described in Sections 11.2.2 through 11.2.7 prior to analysis.

       11.2 Aqueous Sample Preparation--Total Recoverable Analytes

    11.2.1 For the ``direct analysis'' of total recoverable analytes in 
drinking water samples containing turbidity <1 NTU, treat an unfiltered 
acid preserved sample aliquot using the sample preparation procedure 
described in Section 11.1.1 while making allowance for sample dilution 
in the data calculation (Section 1.2). For the determination of total 
recoverable analytes in all other aqueous samples or for 
preconcentrating drinking water samples prior to analysis follow the 
procedure given in Sections 11.2.2 through 11.2.7.
    11.2.2 For the determination of total recoverable analytes in 
aqueous samples (other than drinking water with <1 NTU turbidity), 
transfer a 100 mL (1 mL) aliquot from a well mixed, acid preserved 
sample to a 250 mL Griffin beaker (Sections 1.2, 1.3, 1.6, 1.7, 1.8, and 
1.9). (When necessary, smaller sample aliquot volumes may be used.)

    Note: If the sample contains undissolved solids 1%, a 
well mixed, acid preserved aliquot containing no more than 1 g 
particulate material should be cautiously evaporated to near 10 mL and 
extracted using the acid-mixture procedure described in Sections 11.3.3 
through 11.3.6.

    11.2.3 Add 2 mL (1 + 1) nitric acid and 1.0 mL of (1 + 1) 
hydrochloric acid to the beaker containing the measured volume of 
sample. Place the beaker on the hot plate for solution evaporation. The 
hot plate should be located in a fume hood and previously adjusted to 
provide evaporation at a temperature of approximately but no higher than 
85 [deg]C. (See the following note.) The beaker should be covered with 
an elevated watch glass or other necessary steps should be taken to 
prevent sample contamination from the fume hood environment.

    Note: For proper heating adjust the temperature control of the hot 
plate such that an uncovered Griffin beaker containing 50 mL of water 
placed in the center of the hot plate can be maintained at a temperature 
approximately but no higher than 85 [deg]C. (Once the beaker is covered 
with a watch glass the temperature of the water will rise to 
approximately 95 [deg]C.)


[[Page 404]]


    11.2.4 Reduce the volume of the sample aliquot to about 20 mL by 
gentle heating at 85 [deg]C. DO NOT BOIL. This step takes about two 
hours for a 100 mL aliquot with the rate of evaporation rapidly 
increasing as the sample volume approaches 20 mL. (A spare beaker 
containing 20 mL of water can be used as a gauge.)
    11.2.5 Cover the lip of the beaker with a watch glass to reduce 
additional evaporation and gently reflux the sample for 30 minutes. 
(Slight boiling may occur, but vigorous boiling must be avoided to 
prevent loss of the HCl-H2O azeotrope.)
    11.2.6 Allow the beaker to cool. Quantitatively transfer the sample 
solution to a 50 mL volumetric flask, make to volume with reagent water, 
stopper and mix.
    11.2.7 Allow any undissolved material to settle overnight, or 
centrifuge a portion of the prepared sample until clear. (If after 
centrifuging or standing overnight the sample contains suspended solids 
that would clog the nebulizer, a portion of the sample may be filtered 
for their removal prior to analysis. However, care should be exercised 
to avoid potential contamination from filtration.) The sample is now 
ready for analysis. Because the effects of various matrices on the 
stability of diluted samples cannot be characterized, all analyses 
should be performed as soon as possible after the completed preparation.

        11.3 Solid Sample Preparation--Total Recoverable Analytes

    11.3.1 For the determination of total recoverable analytes in solid 
samples, mix the sample thoroughly and transfer a portion (20 
g) to tared weighing dish, weigh the sample and record the wet weight 
(WW). (For samples with <35% moisture a 20 g portion is sufficient. For 
samples with moisture 35% a larger aliquot 50-100 g is 
required.) Dry the sample to a constant weight at 60 [deg]C and record 
the dry weight (DW) for calculation of percent solids (Section 12.6). 
(The sample is dried at 60 [deg]C to prevent the loss of mercury and 
other possible volatile metallic compounds, to facilitate sieving, and 
to ready the sample for grinding.)
    11.3.2 To achieve homogeneity, sieve the dried sample using a 5-mesh 
polypropylene sieve and grind in a mortar and pestle. (The sieve, mortar 
and pestle should be cleaned between samples.) From the dried, ground 
material weigh accurately a representative 1.0 0.01 g aliquot (W) of the sample and transfer to a 250 
mL Phillips beaker for acid extraction (Sections 1.6, 1.7, 1.8, and 
1.9).
    11.3.3 To the beaker add 4 mL of (1 + 1) HNO3 and 10 mL 
of (1 + 4) HCl. Cover the lip of the beaker with a watch glass. Place 
the beaker on a hot plate for reflux extraction of the analytes. The hot 
plate should be located in a fume hood and previously adjusted to 
provide a reflux temperature of approximately 95 [deg]C. (See the 
following note.)

    Note: For proper heating adjust the temperature control of the hot 
plate such that an uncovered Griffin beaker containing 50 mL of water 
placed in the center of the hot plate can be maintained at a temperature 
approximately but no higher than 85 [deg]C. (Once the beaker is covered 
with a watch glass the temperature of the water will rise to 
approximately 95 [deg]C.) Also, a block digester capable of maintaining 
a temperature of 95 [deg]C and equipped with 250 mL constricted 
volumetric digestion tubes may be substituted for the hot plate and 
conical beakers in the extraction step.

    11.3.4 Heat the sample and gently reflux for 30 minutes. Very slight 
boiling may occur, however vigorous boiling must be avoided to prevent 
loss of the HCl-H2O azeotrope. Some solution evaporation will 
occur (3-4 mL).
    11.3.5 Allow the sample to cool and quantitatively transfer the 
extract to a 100 mL volumetric flask. Dilute to volume with reagent 
water, stopper and mix.
    11.3.6 Allow the sample extract solution to stand overnight to 
separate insoluble material or centrifuge a portion of the sample 
solution until clear. (If after centrifuging or standing overnight the 
extract solution contains suspended solids that would clog the 
nebulizer, a portion of the extract solution may be filtered for their 
removal prior to analysis. However, care should be exercised to avoid 
potential contamination from filtration.) The sample extract is now 
ready for analysis. Because the effects of various matrices on the 
stability of diluted samples cannot be characterized, all analyses 
should be performed as soon as possible after the completed preparation.

                          11.4 Sample Analysis

    11.4.1 Prior to daily calibration of the instrument inspect the 
sample introduction system including the nebulizer, torch, injector tube 
and uptake tubing for salt deposits, dirt and debris that would restrict 
solution flow and affect instrument performance. Clean the system when 
needed or on a daily basis.
    11.4.2 Configure the instrument system to the selected power and 
operating conditions as determined in Sections 10.1 and 10.2.
    11.4.3 The instrument must be allowed to become thermally stable 
before calibration and analyses. This usually requires at least 30 to 60 
minutes of operation. After instrument warmup, complete any required 
optical profiling or alignment particular to the instrument.

[[Page 405]]

    11.4.4 For initial and daily operation calibrate the instrument 
according to the instrument manufacturer's recommended procedures, using 
mixed calibration standard solutions (Section 7.9) and the calibration 
blank (Section 7.10.1). A peristaltic pump must be used to introduce all 
solutions to the nebulizer. To allow equilibrium to be reached in the 
plasma, aspirate all solutions for 30 seconds after reaching the plasma 
before beginning integration of the background corrected signal to 
accumulate data. When possible, use the average value of replicate 
integration periods of the signal to be correlated to the analyte 
concentration. Flush the system with the rinse blank (Section 7.10.4) 
for a minimum of 60 seconds (Section 4.4) between each standard. The 
calibration line should consist of a minimum of a calibration blank and 
a high standard. Replicates of the blank and highest standard provide an 
optimal distribution of calibration standards to minimize the confidence 
band for a straight-line calibration in a response region with uniform 
variance.\20\
    11.4.5 After completion of the initial requirements of this method 
(Sections 10.3 and 10.4), samples should be analyzed in the same 
operational manner used in the calibration routine with the rinse blank 
also being used between all sample solutions, LFBs, LFMs, and check 
solutions (Section 7.10.4).
    11.4.6 During the analysis of samples, the laboratory must comply 
with the required quality control described in Sections 9.3 and 9.4. 
Only for the determination of dissolved analytes or the ``direct 
analysis'' of drinking water with turbidity of <1 NTU is the sample 
digestion step of the LRB, LFB, and LFM not required.
    11.4.7 Determined sample analyte concentrations that are 90% or more 
of the upper limit of the analyte LDR must be diluted with reagent water 
that has been acidified in the same manner as calibration blank and 
reanalyzed (see Section 11.4.8). Also, for the interelement spectral 
interference correction routines to remain valid during sample analysis, 
the interferant concentration must not exceed its LDR. If the 
interferant LDR is exceeded, sample dilution with acidified reagent 
water and reanalysis is required. In these circumstances analyte 
detection limits are raised and determination by another approved test 
procedure that is either more sensitive and/or interference free is 
recommended.
    11.4.8 When it is necessary to assess an operative matrix 
interference (e.g., signal reduction due to high dissolved solids), the 
tests described in Section 9.5 are recommended.
    11.4.9 Report data as directed in Section 12.0.
    11.5 If the method of standard additions (MSA) is used, standards 
are added at one or more levels to portions of a prepared sample. This 
technique \21\ compensates for enhancement or depression of an analyte 
signal by a matrix. It will not correct for additive interferences such 
as contamination, interelement interferences, or baseline shifts. This 
technique is valid in the linear range when the interference effect is 
constant over the range, the added analyte responds the same as the 
endogenous analyte, and the signal is corrected for additive 
interferences. The simplest version of this technique is the single-
addition method. This procedure calls for two identical aliquots of the 
sample solution to be taken. To the first aliquot, a small volume of 
standard is added; while to the second aliquot, a volume of acid blank 
is added equal to the standard addition. The sample concentration is 
calculated by the following:
[GRAPHIC] [TIFF OMITTED] TR18MY12.004

where:

C = Concentration of the standard solution (mg/L)
S1 = Signal for fortified aliquot
S2 = Signal for unfortified aliquot
V1 = Volume of the standard addition (L)
V2 = Volume of the sample aliquot (L) used for MSA

    For more than one fortified portion of the prepared sample, linear 
regression analysis can be applied using a computer or calculator 
program to obtain the concentration of the sample solution. An 
alternative to using the method of standard additions is use of the 
internal standard technique by adding one or more elements (not in the 
samples and verified not to cause an uncorrected interelement spectral 
interference) at the same concentration (which is sufficient for optimum 
precision) to the prepared samples (blanks and standards) that are 
affected the same as the analytes by the sample matrix. Use the ratio of 
analyte signal to the internal standard signal for calibration and 
quantitation.

                   12.0 Data Analysis and Calculations

    12.1 Sample data should be reported in units of mg/L for aqueous 
samples and mg/kg dry weight for solid samples.

[[Page 406]]

    12.2 For dissolved aqueous analytes (Section 11.1) report the data 
generated directly from the instrument with allowance for sample 
dilution. Do not report analyte concentrations below the IDL.
    12.3 For total recoverable aqueous analytes (Section 11.2), multiply 
solution analyte concentrations by the dilution factor 0.5, when 100 mL 
aliquot is used to produce the 50 mL final solution, and report data as 
instructed in Section 12.4. If a different aliquot volume other than 100 
mL is used for sample preparation, adjust the dilution factor 
accordingly. Also, account for any additional dilution of the prepared 
sample solution needed to complete the determination of analytes 
exceeding 90% or more of the LDR upper limit. Do not report data below 
the determined analyte MDL concentration or below an adjusted detection 
limit reflecting smaller sample aliquots used in processing or 
additional dilutions required to complete the analysis.
    12.4 For analytes with MDLs <0.01 mg/L, round the data values to the 
thousandth place and report analyte concentrations up to three 
significant figures. For analytes with MDLs <0.01 mg/L round the data 
values to the 100th place and report analyte concentrations up to three 
significant figures. Extract concentrations for solids data should be 
rounded in a similar manner before calculations in Section 12.5 are 
performed.
    12.5 For total recoverable analytes in solid samples (Section 11.3), 
round the solution analyte concentrations (mg/L) as instructed in 
Section 12.4. Report the data up to three significant figures as mg/kg 
dry-weight basis unless specified otherwise by the program or data user. 
Calculate the concentration using the equation below:
[GRAPHIC] [TIFF OMITTED] TR18MY12.005

where:

C = Concentration in extract (mg/L)
V = Volume of extract (L, 100 mL = 0.1L)
D = Dilution factor (undiluted = 1)
W = Weight of sample aliquot extracted (g x 0.001 = kg)

    Do not report analyte data below the estimated solids MDL or an 
adjusted MDL because of additional dilutions required to complete the 
analysis.
    12.6 To report percent solids in solid samples (Section 11.3) 
calculate as follows:
[GRAPHIC] [TIFF OMITTED] TR18MY12.006

where:

DW = Sample weight (g) dried at 60 [ordm]C
WW = Sample weight (g) before drying

    Note: If the data user, program or laboratory requires that the 
reported percent solids be determined by drying at 105 [deg]C, repeat 
the procedure given in Section 11.3 using a separate portion 
(20 g) of the sample and dry to constant weight at 103-105 
[deg]C.

    12.7 The QC data obtained during the analyses provide an indication 
of the quality of the sample data and should be provided with the sample 
results.

                         13.0 Method Performance

    13.1 Listed in Table 4 are typical single laboratory total 
recoverable MDLs determined for the recommended wavelengths using 
simultaneous ICP-AES and the operating conditions given in Table 5. The 
MDLs were determined in reagent blank matrix (best case situation). PTFE 
beakers were used to avoid boron and silica contamination from glassware 
with the final dilution to 50 mL completed in polypropylene centrifuged 
tubes. The listed MDLs for solids are estimates and were calculated from 
the aqueous MDL determinations.
    13.2 Data obtained from single laboratory method testing are 
summarized in Table 6 for five types of water samples consisting of 
drinking water, surface water, ground water, and two wastewater 
effluents. The data presented cover all analytes except cerium and 
titanium. Samples were prepared using the procedure described in Section 
11.2. For each matrix, five replicate aliquots were prepared, analyzed 
and the average of the five determinations used to define the sample 
background concentration of each analyte. In addition, two pairs of 
duplicates were fortified at different concentration levels. For each 
method analyte, the sample background concentration, mean percent 
recovery, standard

[[Page 407]]

deviation of the percent recovery, and relative percent difference 
between the duplicate fortified samples are listed in Table 6. The 
variance of the five replicate sample background determinations is 
included in the calculated standard deviation of the percent recovery 
when the analyte concentration in the sample was greater than the MDL. 
The tap and well waters were processed in Teflon and quartz beakers and 
diluted in polypropylene centrifuged tubes. The nonuse of borosilicate 
glassware is reflected in the precision and recovery data for boron and 
silica in those two sample types.
    13.3 Data obtained from single laboratory method testing are 
summarized in Table 7 for three solid samples consisting of EPA 884 
Hazardous Soil, SRM 1645 River Sediment, and EPA 286 Electroplating 
Sludge. Samples were prepared using the procedure described in Section 
11.3. For each method analyte, the sample background concentration, mean 
percent recovery of the fortified additions, the standard deviation of 
the percent recovery, and relative percent difference between duplicate 
additions were determined as described in Section 13.2. Data presented 
are for all analytes except cerium, silica, and titanium. Limited 
comparative data to other methods and SRM materials are presented in 
Reference 23 of Section 16.0.
    13.4 Performance data for aqueous solutions independent of sample 
preparation from a multilaboratory study are provided in Table 8.\22\
    13.5 Listed in Table 9 are regression equations for precision and 
bias for 25 analytes abstracted from EPA Method Study 27, a 
multilaboratory validation study of Method 200.7.\1\ These equations 
were developed from data received from 12 laboratories using the total 
recoverable sample preparation procedure on reagent water, drinking 
water, surface water and three industrial effluents. For a complete 
review and description of the study, see Reference 16 of Section 16.0.

                        14.0 Pollution Prevention

    14.1 Pollution prevention encompasses any technique that reduces or 
eliminates the quantity or toxicity of waste at the point of generation. 
Numerous opportunities for pollution prevention exist in laboratory 
operation. The EPA has established a preferred hierarchy of 
environmental management techniques that places pollution prevention as 
the management option of first choice. Whenever feasible, laboratory 
personnel should use pollution prevention techniques to address their 
waste generation (e.g., Section 7.8). When wastes cannot be feasibly 
reduced at the source, the Agency recommends recycling as the next best 
option.
    14.2 For information about pollution prevention that may be 
applicable to laboratories and research institutions, consult ``Less is 
Better: Laboratory Chemical Management for Waste Reduction'', available 
from the American Chemical Society's Department of Government Relations 
and Science Policy, 1155 16th Street NW., Washington, DC 20036, (202) 
872-4477.

                          15.0 Waste Management

    15.1 The Environmental Protection Agency requires that laboratory 
waste management practices be conducted consistent with all applicable 
rules and regulations. The Agency urges laboratories to protect the air, 
water, and land by minimizing and controlling all releases from hoods 
and bench operations, complying with the letter and spirit of any sewer 
discharge permits and regulations, and by complying with all solid and 
hazardous waste regulations, particularly the hazardous waste 
identification rules and land disposal restrictions. For further 
information on waste management consult ``The Waste Management Manual 
for Laboratory Personnel'', available from the American Chemical Society 
at the address listed in the Section 14.2.

                             16.0 References

1. U.S. Environmental Protection Agency. Inductively Coupled Plasma--
          Atomic Emission Spectrometric Method for Trace Element 
          Analysis of Water and Wastes--Method 200.7, Dec. 1982. EPA-
          600/4-79-020, revised March 1983.
2. U.S. Environmental Protection Agency. Inductively Coupled Plasma 
          Atomic Emission Spectroscopy Method 6010, SW-846 Test Methods 
          for Evaluating Solid Waste, 3rd Edition, 1986.
3. U.S. Environmental Protection Agency. Method 200.7: Determination of 
          Metals and Trace Elements in Water and Wastes by Inductively 
          Coupled Plasma--Atomic Emission Spectrometry, revision 3.3, 
          EPA 600 4-91/010, June 1991.
4. U.S. Environmental Protection Agency. Inductively Coupled Plasma--
          Atomic Emission Spectrometry Method for the Analysis of Waters 
          and Solids, EMMC, July 1992.
5. Fassel, V.A. et al. Simultaneous Determination of Wear Metals in 
          Lubricating Oils by Inductively-Coupled Plasma Atomic Emission 
          Spectrometry. Anal. Chem. 48:516-519, 1976.
6. Merryfield, R.N. and R.C. Loyd. Simultaneous Determination of Metals 
          in Oil by Inductively Coupled Plasma Emission Spectrometry. 
          Anal. Chem. 51:1965-1968, 1979.
7. Winge, R.K. et al. Inductively Coupled Plasma--Atomic Emission 
          Spectroscopy: An Atlas of Spectral Information, Physical 
          Science Data 20. Elsevier Science Publishing, New York, New 
          York, 1985.
8. Boumans, P.W.J.M. Line Coincidence Tables for Inductively Coupled 
          Plasma

[[Page 408]]

          Atomic Emission Spectrometry, 2nd edition. Pergamon Press, 
          Oxford, United Kingdom, 1984.
9. Carcinogens--Working With Carcinogens, Department of Health, 
          Education, and Welfare, Public Health Service, Center for 
          Disease Control, National Institute for Occupational Safety 
          and Health, Publication No. 77-206, Aug. 1977. Available from 
          the National Technical Information Service (NTIS) as PB-
          277256.
10. OSHA Safety and Health Standards, General Industry, (29 CFR 1910), 
          Occupational Safety and Health Administration, OSHA 2206, 
          (Revised, January 1976).
11. Safety in Academic Chemistry Laboratories, American Chemical Society 
          Publication, Committee on Chemical Safety, 3rd Edition, 1979.
12. Proposed OSHA Safety and Health Standards, Laboratories, 
          Occupational Safety and Health Administration, Federal 
          Register, July 24, 1986.
13. Rohrbough, W.G. et al. Reagent Chemicals, American Chemical Society 
          Specifications, 7th edition. American Chemical Society, 
          Washington, DC, 1986.
14. American Society for Testing and Materials. Standard Specification 
          for Reagent Water, D1193-77. Annual Book of ASTM Standards, 
          Vol. 11.01. Philadelphia, PA, 1991.
15. Code of Federal Regulations 40, Ch. 1, Pt. 136 Appendix B.
16. Maxfield, R. and B. Mindak. EPA Method Study 27, Method 200.7 Trace 
          Metals by ICP, Nov. 1983. Available from National Technical 
          Information Service (NTIS) as PB 85-248-656.
17. Botto, R.I. Quality Assurance in Operating a Multielement ICP 
          Emission Spectrometer. Spectrochim. Acta, 39B(1):95-113, 1984.
18. Wallace, G.F., Some Factors Affecting the Performance of an ICP 
          Sample Introduction System. Atomic Spectroscopy, Vol. 4, p. 
          188-192, 1983.
19. Koirtyohann, S.R. et al. Nomenclature System for the Low-Power Argon 
          Inductively Coupled Plasma, Anal. Chem. 52:1965, 1980.
20. Deming, S.N. and S.L. Morgan. Experimental Design for Quality and 
          Productivity in Research, Development, and Manufacturing, Part 
          III, pp. 119-123. Short course publication by Statistical 
          Designs, 9941 Rowlett, Suite 6, Houston, TX 77075, 1989.
21. Winefordner, J.D., Trace Analysis: Spectroscopic Methods for 
          Elements, Chemical Analysis, Vol. 46, pp. 41-42.
22. Jones, C.L. et al. An Interlaboratory Study of Inductively Coupled 
          Plasma Atomic Emission Spectroscopy Method 6010 and Digestion 
          Method 3050. EPA-600/4-87-032, U.S. Environmental Protection 
          Agency, Las Vegas, Nevada, 1987.
23. Martin, T.D., E.R. Martin and SE. Long. Method 200.2: Sample 
          Preparation Procedure for Spectrochemical Analyses of Total 
          Recoverable Elements, EMSL ORD, USEPA, 1989.

         17.0 Tables, Diagrams, Flowcharts, and Validation Data

            Table 1--Wavelengths, Estimated Instrument Detection Limits, and Recommended Calibration
----------------------------------------------------------------------------------------------------------------
                                                                                  Estimated
                                                              Wavelength\a\       detection      Calibrate\c\ to
                          Analyte                                 (nm)            limit\b\           (mg/L)
                                                                                ([micro]g/L)
----------------------------------------------------------------------------------------------------------------
Aluminum..................................................           308.215                45                10
Antimony..................................................           206.833                32                 5
Arsenic...................................................           193.759                53                10
Barium....................................................           493.409               2.3                 1
Beryllium.................................................           313.042              0.27                 1
Boron.....................................................           249.678               5.7                 1
Cadmium...................................................           226.502               3.4                 2
Calcium...................................................           315.887                30                10
Cerium....................................................           413.765                48                 2
Chromium..................................................           205.552               6.1                 5
Cobalt....................................................           228.616               7.0                 2
Copper....................................................           324.754               5.4                 2
Iron......................................................           259.940               6.2                10
Lead......................................................           220.353                42                10
Lithium...................................................           670.784           \d\ 3.7                 5
Magnesium.................................................           279.079                30                10
Manganese.................................................           257.610               1.4                 2
Mercury...................................................           194.227               2.5                 2
Molybdenum................................................           203.844                12                10
Nickel....................................................           231.604                15                 2
Phosphorus................................................           214.914                76                10
Potassium.................................................           766.491           \e\ 700                20
Selenium..................................................           196.090                75                 5
Silica (SiO2).............................................           251.611     \d\ 26 (SiO2)                10
Silver....................................................           328.068               7.0               0.5

[[Page 409]]

 
Sodium....................................................           588.995                29                10
Strontium.................................................           421.552              0.77                 1
Thallium..................................................           190.864                40                 5
Tin.......................................................           189.980                25                 4
Titanium..................................................           334.941               3.8                10
Vanadium..................................................           292.402               7.5                 2
Zinc......................................................           213.856               1.8                 5
----------------------------------------------------------------------------------------------------------------
\a\ The wavelengths listed are recommended because of their sensitivity and overall acceptability. Other
  wavelengths may be substituted if they can provide the needed sensitivity and are treated with the same
  corrective techniques for spectral interference (see Section 4.1).
\b\ These estimated 3-sigma instrumental detection limits \16\ are provided only as a guide to instrumental
  limits. The method detection limits are sample dependent and may vary as the sample matrix varies. Detection
  limits for solids can be estimated by dividing these values by the grams extracted per liter, which depends
  upon the extraction procedure. Divide solution detection limits by 10 for 1 g extracted to 100 mL for solid
  detection limits.
\c\ Suggested concentration for instrument calibration.\2\ Other calibration limits in the linear ranges may be
  used.
\d\ Calculated from 2-sigma data.\5\
\e\ Highly dependent on operating conditions and plasma position.


TABLE 2--On-Line Method Interelement Spectral Interferances Arising From
                   Interferants at the 100 mg/L Level
------------------------------------------------------------------------
                              Wavelength
           Analyte               (nm)              Interferant*
------------------------------------------------------------------------
Ag..........................     328.068  Ce, Ti, Mn
Al..........................     308.215  V, Mo, Ce, Mn
As..........................     193.759  V, Al, Co, Fe, Ni
B...........................     249.678  None
Ba..........................     493.409  None
Be..........................     313.042  V, Ce
Ca..........................     315.887  Co, Mo, Ce
Cd..........................     226.502  Ni, Ti, Fe, Ce
Ce..........................     413.765  None
Co..........................     228.616  Ti, Ba, Cd, Ni, Cr, Mo, Ce
Cr..........................     205.552  Be, Mo, Ni
Cu..........................     324.754  Mo, Ti
Fe..........................     259.940  None
Hg..........................     194.227  V, Mo
K...........................     766.491  None
Li..........................     670.784  None
Mg..........................     279.079  Ce
Mn..........................     257.610  Ce
Mo..........................     203.844  Ce
Na..........................     588.995  None
Ni..........................     231.604  Co, Tl
P...........................     214.914  Cu, Mo
Pb..........................     220.353  Co, Al, Ce, Cu, Ni, Ti, Fe
Sb..........................     206.833  Cr, Mo, Sn, Ti, Ce, Fe
Se..........................     196.099  Fe
SiO2........................     251.611  None
Sn..........................     189.980  Mo, Ti, Fe, Mn, Si
Sr..........................     421.552  None
Tl..........................     190.864  Ti, Mo, Co, Ce, Al, V, Mn
Ti..........................     334.941  None
V...........................     292.402  Mo, Ti, Cr, Fe, Ce
Zn..........................     213.856  Ni, Cu, Fe
------------------------------------------------------------------------
* These on-line interferences from method analytes and titanium only
  were observed using an instrument with 0.035 nm resolution (see
  Section 4.1.2). Interferant ranked by magnitude of intensity with the
  most severe interferant listed first in the row.


                                        TABLE 3--Mixed Standard Solutions
----------------------------------------------------------------------------------------------------------------
                   Solution                                                 Analytes
----------------------------------------------------------------------------------------------------------------
I............................................  Ag, As, B, Ba, Ca, Cd, Cu, Mn, Sb, and Se
II...........................................  K, Li, Mo, Na, Sr, and Ti
III..........................................  Co, P, V, and Ce
IV...........................................  Al, Cr, Hg, SiO2, Sn, and Zn
V............................................  Be, Fe, Mg, Ni, Pb, and Tl
----------------------------------------------------------------------------------------------------------------


        TABLE 4--Total Recoverable Method Detection Limits (MDL)
------------------------------------------------------------------------
                                   MDLs Aqueous, mg/
             Analyte                    L\(1)\        Solids, mg/kg\(2)\
------------------------------------------------------------------------
Ag..............................               0.002                 0.3
Al..............................                0.02                   3
As..............................               0.008                   2
B...............................               0.003                  --
Ba..............................               0.001                 0.2
Be..............................              0.0003                 0.1
Ca..............................                0.01                   2
Cd..............................               0.001                 0.2
Ce..............................                0.02                   3
Co..............................               0.002                 0.4
Cr..............................               0.004                 0.8
Cu..............................               0.003                 0.5
Fe..............................               *0.03                   6
Hg..............................               0.007                   2
K...............................                 0.3                  60
Li..............................               0.001                 0.2
Mg..............................                0.02                   3
Mn..............................               0.001                 0.2
Mo..............................               0.004                   1
Na..............................                0.03                   6
Ni..............................               0.005                   1
P...............................                0.06                  12
Pb..............................                0.01                   2
Sb..............................               0.008                   2
Se..............................                0.02                   5
SiO2............................                0.02                  --
Sn..............................               0.007                   2
Sr..............................              0.0003                 0.1
Tl..............................               0.001                 0.2
Ti..............................                0.02                   3
V...............................               0.003                   1

[[Page 410]]

 
Zn..............................               0.002                 0.3
------------------------------------------------------------------------
\(1)\ MDL concentrations are computed for original matrix with allowance
  for 2x sample preconcentration during preparation. Samples were
  processed in PTFE and diluted in 50-mL plastic centrifuge tubes.
\(2)\ Estimated, calculated from aqueous MDL determinations.
-- Boron not reported because of glassware contamination. Silica not
  determined in solid samples.
* Elevated value due to fume-hood contamination.


   TABLE 5--Inductively Coupled Plasma Instrument Operating Conditions
------------------------------------------------------------------------
 
------------------------------------------------------------------------
Incident rf power........................  1100 watts
Reflected rf power.......................  <5 watts
Viewing height above work coil...........  15 mm
Injector tube orifice i.d................  1 mm
Argon supply.............................  liquid argon
Argon pressure...........................  40 psi
Coolant argon flow rate..................  19 L/min.
Aerosol carrier argon flow rate..........  620 mL/min.
Auxiliary (plasma) argon flow rate.......  300 mL/min.
Sample uptake rate controlled to.........  1.2 mL/min.
------------------------------------------------------------------------


[[Page 411]]


                                                Table 6--Precision and Recovery Data in Aqueous Matrices
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                 Average                                             Average
              Analyte                   Sample     Low spike    recovery R     S (R)         RPD       High spike   recovery R     S (R)         RPD
                                      conc. mg/L      mg/L         (%)                                    mg/L         (%)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Tap Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           95          0.7          2.1          0.2           96          0.0          0.0
Al.................................        0.185         0.05           98          8.8          1.7          0.2          105          3.0          3.1
As.................................       <0.008         0.05          108          1.4          3.7          0.2          101          0.7          2.0
B..................................        0.023          0.1           98          0.2          0.0          0.4           98          0.2          0.5
Ba.................................        0.042         0.05          102          1.6          2.2          0.2           98          0.4          0.8
Be.................................      <0.0003         0.01          100          0.0          0.0          0.1           99          0.0          0.0
Ca.................................         35.2          5.0          101          8.8          1.7         20.0          103          2.0          0.9
Cd.................................       <0.001         0.01          105          3.5          9.5          0.1           98          0.0          0.0
Co.................................       <0.002         0.02          100          0.0          0.0          0.2           99          0.5          1.5
Cr.................................       <0.004         0.01          110          0.0          0.0          0.1          102          0.0          0.0
Cu.................................       <0.003         0.02          103          1.8          4.9          0.2          101          1.2          3.5
Fe.................................        0.008          0.1          106          1.0          1.8          0.4          105          0.3          0.5
Hg.................................       <0.007         0.05          103          0.7          1.9          0.2          100          0.4          1.0
K..................................         1.98          5.0          109          1.4          2.3          20.          107          0.7          1.7
Li.................................        0.006         0.02          103          6.9          3.8          0.2          110          1.9          4.4
Mg.................................         8.08          5.0          104          2.2          1.5         20.0          100          0.7          1.1
Mn.................................       <0.001         0.01          100          0.0          0.0          0.1           99          0.0          0.0
Mo.................................       <0.004         0.02           95          3.5         10.5          0.2          108          0.5          1.4
Na.................................         10.3          5.0           99          3.0          2.0         20.0          106          1.0          1.6
Ni.................................       <0.005         0.02          108          1.8          4.7          0.2          104          1.1          2.9
P..................................        0.045          0.1          102         13.1          9.4          0.4          104          3.2          1.3
Pb.................................        <0.01         0.05           95          0.7          2.1          0.2          100          0.2          0.5
Sb.................................       <0.008         0.05           99          0.7          2.0          0.2          102          0.7          2.0
Se.................................        <0.02          0.1           87          1.1          3.5          0.4           99          0.8          2.3
SiO2...............................          6.5          5.0          104          3.3          3.4         20.0           96          1.1          2.3
Sn.................................       <0.007         0.05          103          2.1          5.8          0.2          101          1.8          5.0
Sr.................................        0.181          0.1          102          3.3          2.1          0.4          105          0.8          1.0
Tl.................................        <0.02          0.1          101          3.9         10.9          0.4          101          0.1          0.3
V..................................       <0.003         0.05          101          0.7          2.0          0.2           99          0.2          0.5
Zn.................................        0.005         0.05          101          3.7          9.0          0.2           98          0.9          2.5
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                       Pond Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           92          0.0          0.0          0.2           94          0.0          0.0
Al.................................        0.819          0.2           88         10.0          5.0          0.8          100          2.9          3.7
As.................................       <0.008         0.05          102          0.0          0.0          0.2           98          1.4          4.1
B..................................        0.034          0.1          111          8.9          6.9          0.4          103          2.0          0.0
Ba.................................        0.029         0.05           96          0.9          0.0          0.2           97          0.3          0.5
Be.................................      <0.0003         0.01           95          0.4          1.1          0.2           95          0.0          0.0
Ca.................................         53.9          5.0            *            *          0.7         20.0          100          2.0          1.5
Cd.................................       <0.001         0.01          107          0.0          0.0          0.1           97          0.0          0.0
Co.................................       <0.002         0.02          100          2.7          7.5          0.2           97          0.7          2.1
Cr.................................       <0.004         0.01          105          3.5          9.5          0.1          103          1.1          2.9

[[Page 412]]

 
Cu.................................       <0.003         0.02           98          2.1          4.4          0.2          100          0.5          1.5
Fe.................................        0.875          0.2           95          8.9          2.8          0.8           97          3.2          3.6
Hg.................................       <0.007         0.05           97          3.5         10.3          0.2           98          0.0          0.0
K..................................         2.48          5.0          106          0.3          0.1         20.0          103          0.2          0.4
Li.................................       <0.001         0.02          110          0.0          0.0          0.2          106          0.2          0.5
Mg.................................         10.8          5.0          102          0.5          0.0         20.0           96          0.7          1.3
Mn.................................        0.632         0.01            *            *          0.2          0.1           97          2.3          0.3
Mo.................................       <0.004         0.02          105          3.5          9.5          0.2          103          0.4          1.0
Na.................................         17.8          5.0          103          1.3          0.4         20.0           94          0.3          0.0
Ni.................................       <0.005         0.02           96          5.6          9.1          0.2          100          0.7          1.5
P..................................        0.196          0.1           91         14.7          0.3          0.4          108          3.9          1.3
Pb.................................        <0.01         0.05           96          2.6          7.8          0.2          100          0.7          2.0
Sb.................................       <0.008         0.05          102          2.8          7.8          0.2          104          0.4          1.0
Se.................................        <0.02          0.1          104          2.1          5.8          0.4          103          1.6          4.4
SiO2...............................         7.83          5.0          151          1.6          1.3         20.0          117          0.4          0.6
Sn.................................       <0.007         0.05           98          0.0          0.0          0.2           99          1.1          3.0
Sr.................................        0.129          0.1          105          0.4          0.0          0.4           99          0.1          0.2
Tl.................................        <0.02          0.1          103          1.1          2.9          0.4           97          1.3          3.9
V..................................        0.003         0.05           94          0.4          0.0          0.2           98          0.1          0.0
Zn.................................        0.006         0.05           97          1.6          1.8          0.2           94          0.4          0.0
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                       Well Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           97          0.7          2.1          0.2           96          0.2          0.5
Al.................................        0.036         0.05          107          7.6         10.1          0.2          101          1.1          0.8
As.................................       <0.008         0.05          107          0.7          1.9          0.2          104          0.4          1.0
B..................................        0.063          0.1           97          0.6          0.7          0.4           98          0.8          2.1
Ba.................................        0.102         0.05          102          3.0          0.0          0.2           99          0.9          1.0
Be.................................      <0.0003         0.01          100          0.0          0.0          0.1          100          0.0          0.0
Ca.................................         93.8          5.0            *            *          2.1         20.0          100          4.1          0.1
Cd.................................        0.002         0.01           90          0.0          0.0          0.1           96          0.0          0.0
Co.................................       <0.002         0.02           94          0.4          1.1          0.2           94          0.4          1.1
Cr.................................       <0.004         0.01          100          7.1         20.0          0.1          100          0.4          1.0
Cu.................................       <0.005         0.02          100          1.1          0.4          0.2           96          0.5          1.5
Fe.................................        0.042          0.1           99          2.3          1.4          0.4           97          1.4          3.3
Hg.................................       <0.007         0.05           94          2.8          8.5          0.2           93          1.2          3.8
K..................................         6.21          5.0           96          3.4          3.6         20.0          101          1.2          2.3
Li.................................        0.001         0.02          100          7.6          9.5          0.2          104          1.0          1.9
Mg.................................         24.5          5.0           95          5.6          0.3         20.0           93          1.6          1.2
Mn.................................         2.76         0.01            *            *          0.4          0.1            *            *          0.7
Mo.................................       <0.004         0.02          108          1.8          4.7          0.2          101          0.2          0.5
Na.................................         35.0          5.0          101         11.4          0.8         20.0          100          3.1          1.5
Ni.................................       <0.005         0.02          112          1.8          4.4          0.2           96          0.2          0.5
P..................................        0.197          0.1           95         12.7          1.9          0.4           98          3.4          0.9

[[Page 413]]

 
Pb.................................        <0.01         0.05           87          4.9         16.1          0.2           95          0.2          0.5
Sb.................................       <0.008         0.05           98          2.8          8.2          0.2           99          1.4          4.0
Se.................................        <0.02          0.1          102          0.4          1.0          0.4           94          1.1          3.4
SiO2...............................         13.1          5.0           93          4.8          2.8         20.0           99          0.8          0.0
Sn.................................       <0.007         0.05           98          2.8          8.2          0.2           94          0.2          0.5
Sr.................................        0.274          0.1           94          5.7          2.7          0.4           95          1.7          2.2
Tl.................................        <0.02          0.1           92          0.4          1.1          0.4           95          1.1          3.2
V..................................       <0.003         0.05           98          0.0          0.0          0.2           99          0.4          1.0
Zn.................................        0.538         0.05            *            *          0.7          0.2           99          2.5          1.1
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                Sewage Treatment Effluent
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................        0.009         0.05           92          1.5          3.6          0.2           95          0.1          0.0
Al.................................         1.19         0.05            *            *          0.9          0.2          113         12.4          2.1
As.................................       <0.008         0.05           99          2.1          6.1          0.2           93          2.1          6.5
B..................................        0.226          0.1          217         16.3          9.5          0.4          119         13.1         20.9
Ba.................................        0.189         0.05           90          6.8          1.7          0.2           99          1.6          0.5
Be.................................      <0.0003         0.01           94          0.4          1.1          0.1          100          0.4          1.0
Ca.................................         87.9          5.0            *            *          0.6         20.0          101          3.7          0.0
Cd.................................        0.009         0.01           89          2.6          2.3          0.1           97          0.4          1.0
Co.................................        0.016         0.02           95          3.1          0.0          0.2           93          0.4          0.5
Cr.................................        0.128         0.01            *            *          1.5          0.1           97          2.4          2.7
Cu.................................        0.174         0.02           98         33.1          4.7          0.2           98          3.0          1.4
Fe.................................         1.28          0.1            *            *          2.8          0.4          111          7.0          0.6
Hg.................................       <0.007         0.05          102          1.4          3.9          0.2           98          0.5          1.5
K..................................         10.6          5.0          104          2.8          1.3         20.0          101          0.6          0.0
Li.................................        0.011         0.02          103          8.5          3.2          0.2          105          0.8          0.5
Mg.................................         22.7          5.0          100          4.4          0.0         20.0           92          1.1          0.2
Mn.................................        0.199         0.01            *            *          2.0          0.1          104          1.9          0.3
Mo.................................        0.125         0.02          110         21.2          6.8          0.2          102          1.3          0.9
Na.................................        0.236          5.0            *            *          0.0         20.0            *            *          0.4
Ni.................................        0.087         0.02          122         10.7          4.5          0.2           98          0.8          1.1
P..................................         4.71          0.1            *            *          2.6          0.4            *            *          1.4
Pb.................................        0.015         0.05           91          3.5          5.0          0.2           96          1.3          2.9
Sb.................................       <0.008         0.05           97          0.7          2.1          0.2          103          1.1          2.9
Se.................................        <0.02          0.1          108          3.9         10.0          0.4          101          2.6          7.2
SiO2...............................         16.7          5.0          124          4.0          0.9         20.0          108          1.1          0.8
Sn.................................        0.016         0.05           90          3.8          0.0          0.2           95          1.0          0.0
Sr.................................        0.515          0.1          103          6.4          0.5          0.4           96          1.6          0.2
Tl.................................        <0.02          0.1          105          0.4          1.0          0.4           95          0.0          0.0
V..................................        0.003         0.05           93          0.9          2.0          0.2           97          0.2          0.5
Zn.................................        0.160         0.05           98          3.3          1.9          0.2          101          1.0          1.4
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                   Industrial Effluent
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................      <0.0003         0.05           88          0.0          0.0          0.2           84          0.9          3.0
Al.................................        0.054         0.05           88         11.7         12.2          0.2           90          3.9          8.1
As.................................        <0.02         0.05           82          2.8          9.8          0.2           88          0.5          1.7
B..................................         0.17          0.1          162         17.6         13.9          0.4           92          4.7          9.3
Ba.................................        0.083         0.05           86          8.2          1.6          0.2           85          2.3          2.4
Be.................................      <0.0006         0.01           94          0.4          1.1          0.1           82          1.4          4.9

[[Page 414]]

 
Ca.................................          500          5.0            *            *          2.8         20.0            *            *          2.3
Cd.................................        0.008         0.01           85          4.7          6.1          0.1           82          1.4          4.4
Co.................................       <0.004         0.02           93          1.8          5.4          0.2           83          0.4          1.2
Cr.................................        0.165         0.01            *            *          4.5          0.1          106          6.6          5.6
Cu.................................        0.095         0.02           93         23.3          0.9          0.2           95          2.7          2.8
Fe.................................        0.315          0.1           88         16.4          1.0          0.4           99          6.5          8.0
Hg.................................        <0.01         0.05           87          0.7          2.3          0.2           86          0.4          1.2
K..................................         2.87          5.0          101          3.4          2.4         20.0          100          0.8          0.4
Li.................................        0.069         0.02          103         24.7          5.6          0.2          104          2.5          2.2
Mg.................................         6.84          5.0           87          3.1          0.0         20.0           87          0.9          1.2
Mn.................................        0.141         0.01            *            *          1.2          0.1           89          6.6          4.8
Mo.................................         1.27         0.02            *            *          0.0          0.2          100         15.0          2.7
Na.................................         1500          5.0            *            *          2.7         20.0            *            *          2.0
Ni.................................        0.014         0.02           98          4.4          3.0          0.2           87          0.5          1.1
P..................................        0.326          0.1          105         16.0          4.7          0.4           97          3.9          1.4
Pb.................................        0.251         0.05           80         19.9          1.4          0.2           88          5.0          0.9
Sb.................................         2.81         0.05            *            *          0.4          0.2            *            *          2.0
Se.................................        0.021          0.1          106          2.6          3.2          0.4          105          1.9          4.6
SiO2...............................         6.83          5.0           99          6.8          1.7         20.0          100          2.2          3.0
Sn.................................        <0.01         0.05           87          0.7          2.3          0.2           86          0.4          1.2
Sr.................................         6.54          0.1            *            *          2.0          0.4            *            *          2.7
Tl.................................        <0.03          0.1           87          1.8          5.8          0.4           84          1.1          3.6
V..................................       <0.005         0.05           90          1.4          4.4          0.2           84          1.1          3.6
Zn.................................        0.024         0.05           89          6.0          4.4          0.2           91          3.5          8.9
--------------------------------------------------------------------------------------------------------------------------------------------------------
S (R) Standard deviation of percent recovery.
RPD Relative percent difference between duplicate spike determinations.

   Sec. Appendix D to Part 136--Precision and Recovery Statements for 
                      Methods for Measuring Metals

    Two selected methods from ``Methods for Chemical Analysis of Water 
and Wastes,'' EPA-600/4-79-020 (1979) have been subjected to 
interlaboratory method validation studies. The two selected methods are 
for Thallium and Zinc. The following precision and recovery statements 
are presented in this appendix and incorporated into Part 136:

                              Method 279.2

    For Thallium, Method 279.2 (Atomic Absorption, Furnace Technique) 
replace the Precision and Accuracy Section statement with the following:

                         Precision and Accuracy

    An interlaboratory study on metal analyses by this method was 
conducted by the Quality Assurance Branch (QAB) of the Environmental 
Monitoring Systems Laboratory--Cincinnati (EMSL-CI). Synthetic 
concentrates containing various levels of this element were added to 
reagent water, surface water, drinking water and three effluents. These 
samples were digested by the total digestion procedure, 4.1.3 in this 
manual. Results for the reagent water are given below. Results for other 
water types and study details are found in ``EPA Method Study 31, Trace 
Metals by Atomic Absorption (Furnace Techniques),'' National Technical 
Information Service, 5285 Port Royal Road, Springfield, VA 22161 Order 
No. PB 86-121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
    For a concentration range of 10.00-252 [micro]g/L

X = 0.8781(C) - 0.715
S = 0.1112(X) + 0.669
SR = 0.1005(X) + 0.241

Where:

C = True Value for the Concentration, [micro]g/L
X = Mean Recovery, [micro]g/L
S = Multi-laboratory Standard Deviation, [micro]g/L
SR = Single-analyst Standard Deviation, [micro]g/L

                              Method 289.2

    For Zinc, Method 289.2 (Atomic Absorption, Furnace Technique) 
replace the Precision and Accuracy Section statement with the following:

                         Precision and Accuracy

    An interlaboratory study on metal analyses by this method was 
conducted by the Quality Assurance Branch (QAB) of the Environmental 
Monitoring Systems Laboratory--Cincinnati (EMSL-CI). Synthetic 
concentrates containing various levels of this element were added to 
reagent water, surface water, drinking water and three effluents. These 
samples were digested by the total digestion procedure, 4.1.3 in this 
manual. Results for the reagent water are given below. Results for other 
water types and study details are found in ``EPA Method Study 31, Trace 
Metals by Atomic Absorption (Furnace Techniques),'' National Technical 
Information Service, 5285 Port Royal Road, Springfield, VA 22161 Order 
No. PB 86-121 704/AS, by Copeland, F.R. and Maney, J.P., January 1986.
    For a concentration range of 0.51-189 [micro]g/L

X = 1.6710(C) + 1.485
S = 0.6740(X) - 0.342
SR = 0.3895(X)- 0.384

Where:

C = True Value for the Concentration, [micro]g/L
X = Mean Recovery, [micro]g/L
S = Multi-laboratory Standard Deviation, [micro]g/L
SR = Single-analyst Standard Deviation, [micro]g/L

[77 FR 29833, May 18, 2012]



PART 140_MARINE SANITATION DEVICE STANDARD--Table of Contents



Sec.
140.1 Definitions.
140.2 Scope of standard.
140.3 Standard.
140.4 Complete prohibition.
140.5 Analytical procedures.

    Authority: 33 U.S.C. 1322, as amended.

    Source: 41 FR 4453, Jan. 29, 1976, unless otherwise noted.



Sec.  140.1  Definitions.

    For the purpose of these standards the following definitions shall 
apply:
    (a) Sewage means human body wastes and the wastes from toilets and 
other receptacles intended to receive or retain body wastes;
    (b) Discharge includes, but is not limited to, any spilling, 
leaking, pumping, pouring, emitting, emptying, or dumping;
    (c) Marine sanitation device includes any equipment for installation 
onboard a vessel and which is designed to receive, retain, treat, or 
discharge sewage and any process to treat such sewage;
    (d) Vessel includes every description of watercraft or other 
artificial contrivance used, or capable of being used,

[[Page 421]]

as a means of transportation on waters of the United States;
    (e) New vessel refers to any vessel on which construction was 
initiated on or after January 30, 1975;
    (f) Existing vessel refers to any vessel on which construction was 
initiated before January 30, 1975;
    (g) Fecal coliform bacteria are those organisms associated with the 
intestines of warm-blooded animals that are commonly used to indicate 
the presence of fecal material and the potential presence of organisms 
capable of causing human disease.



Sec.  140.2  Scope of standard.

    The standard adopted herein applies only to vessels on which a 
marine sanitation device has been installed. The standard does not 
require the installation of a marine sanitation device on any vessel 
that is not so equipped. The standard applies to vessels owned and 
operated by the United States unless the Secretary of Defense finds that 
compliance would not be in the interest of national security.



Sec.  140.3  Standard.

    (a) (1) In freshwater lakes, freshwater reservoirs or other 
freshwater impoundments whose inlets or outlets are such as to prevent 
the ingress or egress by vessel traffic subject to this regulation, or 
in rivers not capable of navigation by interstate vessel traffic subject 
to this regulation, marine sanitation devices certified by the U.S. 
Coast Guard (see 33 CFR part 159, published in 40 FR 4622, January 30, 
1975), installed on all vessels shall be designed and operated to 
prevent the overboard discharge of sewage, treated or untreated, or of 
any waste derived from sewage. This shall not be construed to prohibit 
the carriage of Coast Guard-certified flow-through treatment devices 
which have been secured so as to prevent such discharges.
    (2) In all other waters, Coast Guard-certified marine sanitation 
devices installed on all vessels shall be designed and operated to 
either retain, dispose of, or discharge sewage. If the device has a 
discharge, subject to paragraph (d) of this section, the effluent shall 
not have a fecal coliform bacterial count of greater than 1,000 per 100 
milliliters nor visible floating solids. Waters where a Coast Guard-
certified marine sanitation device permitting discharge is allowed 
include coastal waters and estuaries, the Great Lakes and inter-
connected waterways, fresh-water lakes and impoundments accessible 
through locks, and other flowing waters that are navigable interstate by 
vessels subject to this regulation.
    (b) This standard shall become effective on January 30, 1977 for new 
vessels and on January 30, 1980 for existing vessels (or, in the case of 
vessels owned and operated by the Department of Defense, two years and 
five years, for new and existing vessels, respectively, after 
promulgation of implementing regulations by the Secretary of Defense 
under section 312(d) of the Act).
    (c) Any vessel which is equipped as of the date of promulgation of 
this regulation with a Coast Guard-certified flow-through marine 
sanitation device meeting the requirements of paragraph (a)(2) of this 
section, shall not be required to comply with the provisions designed to 
prevent the overboard discharge of sewage, treated or untreated, in 
paragraph (a)(1) of this section, for the operable life of that device.
    (d) After January 30, 1980, subject to paragraphs (e) and (f) of 
this section, marine sanitation devices on all vessels on waters that 
are not subject to a prohibition of the overboard discharge of sewage, 
treated or untreated, as specified in paragraph (a)(1) of this section, 
shall be designed and operated to either retain, dispose of, or 
discharge sewage, and shall be certified by the U.S. Coast Guard. If the 
device has a discharge, the effluent shall not have a fecal coliform 
bacterial count of greater than 200 per 100 milliliters, nor suspended 
solids greater than 150 mg/1.
    (e) Any existing vessel on waters not subject to a prohibition of 
the overboard discharge of sewage in paragraph (a)(1) of this section, 
and which is equipped with a certified device on or before January 30, 
1978, shall not be required to comply with paragraph (d) of this 
section, for the operable life of that device.
    (f) Any new vessel on waters not subject to the prohibition of the 
overboard discharge of sewage in paragraph (a)(1)

[[Page 422]]

of this section, and on which construction is initiated before January 
31, 1980, which is equipped with a marine sanitation device before 
January 31, 1980, certified under paragraph (a)(2) of this section, 
shall not be required to comply with paragraph (d) of this section, for 
the operable life of that device.
    (g) The degrees of treatment described in paragraphs (a) and (d) of 
this section are ``appropriate standards'' for purposes of Coast Guard 
and Department of Defense certification pursuant to section 312(g)(2) of 
the Act.

[41 FR 4453, Jan. 29, 1976, as amended at 60 FR 33932, June 29, 1995]



Sec.  140.4  Complete prohibition.

    (a) Prohibition pursuant to CWA section 312(f)(3): a State may 
completely prohibit the discharge from all vessels of any sewage, 
whether treated or not, into some or all of the waters within such State 
by making a written application to the Administrator, Environmental 
Protection Agency, and by receiving the Administrator's affirmative 
determination pursuant to section 312(f)(3) of the Act. Upon receipt of 
an application under section 312(f)(3) of the Act, the Administrator 
will determine within 90 days whether adequate facilities for the safe 
and sanitary removal and treatment of sewage from all vessels using such 
waters are reasonably available. Applications made by States pursuant to 
section 312(f)(3) of the Act shall include:
    (1) A certification that the protection and enhancement of the 
waters described in the petition require greater environmental 
protection than the applicable Federal standard;
    (2) A map showing the location of commercial and recreational pump-
out facilities;
    (3) A description of the location of pump-out facilities within 
waters designated for no discharge;
    (4) The general schedule of operating hours of the pump-out 
facilities;
    (5) The draught requirements on vessels that may be excluded because 
of insufficient water depth adjacent to the facility;
    (6) Information indicating that treatment of wastes from such pump-
out facilities is in conformance with Federal law; and
    (7) Information on vessel population and vessel usage of the subject 
waters.
    (b) Prohibition pursuant to CWA section 312(f)(4)(A): a State may 
make a written application to the Administrator, Environmental 
Protection Agency, under section 312(f)(4)(A) of the Act, for the 
issuance of a regulation completely prohibiting discharge from a vessel 
of any sewage, whether treated or not, into particular waters of the 
United States or specified portions thereof, which waters are located 
within the boundaries of such State. Such application shall specify with 
particularly the waters, or portions thereof, for which a complete 
prohibition is desired. The application shall include identification of 
water recreational areas, drinking water intakes, aquatic sanctuaries, 
identifiable fish-spawning and nursery areas, and areas of intensive 
boating activities. If, on the basis of the State's application and any 
other information available to him, the Administrator is unable to make 
a finding that the waters listed in the application require a complete 
prohibition of any discharge in the waters or portions thereof covered 
by the application, he shall state the reasons why he cannot make such a 
finding, and shall deny the application. If the Administrator makes a 
finding that the waters listed in the application require a complete 
prohibition of any discharge in all or any part of the waters or 
portions thereof covered by the State's application, he shall publish 
notice of such findings together with a notice of proposed rule making, 
and then shall proceed in accordance with 5 U.S.C. 553. If the 
Administrator's finding is that applicable water quality standards 
require a complete prohibition covering a more restricted or more 
expanded area than that applied for by the State, he shall state the 
reasons why his finding differs in scope from that requested in the 
State's application.
    (1) For the following waters the discharge from a vessel of any 
sewage (whether treated or not) is completely prohibited pursuant to CWA 
section 312(f)(4)(A):

[[Page 423]]

    (i) Boundary Waters Canoe Area, formerly designated as the Superior, 
Little Indian Sioux, and Caribou Roadless Areas, in the Superior 
National Forest, Minnesota, as described in 16 U.S.C. 577-577d1.
    (ii) Waters of the State of Florida within the boundaries of the 
Florida Keys National Marine Sanctuary as delineated on a map of the 
Sanctuary at http://www.fknms.nos.noaa.gov/.
    (2)(i) For the marine waters of the State of California, the 
following vessels are completely prohibited from discharging any sewage 
(whether treated or not):
    (A) A large passenger vessel;
    (B) A large oceangoing vessel equipped with a holding tank which has 
not fully used the holding tank's capacity, or which contains more than 
de minimis amounts of sewage generated while the vessel was outside of 
the marine waters of the State of California.
    (ii) For purposes of paragraph (b)(2) of this section:
    (A) ``Marine waters of the State of California'' means the 
territorial sea measured from the baseline as determined in accordance 
with the Convention on the Territorial Sea and the Contiguous Zone and 
extending seaward a distance of three miles, and all enclosed bays and 
estuaries subject to tidal influences from the Oregon border (41.999325 
North Latitude, 124.212110 West Longitude, decimal degrees, NAD 1983) to 
the Mexican border (32.471231 North Latitude, 117.137814 West Longitude, 
decimal degrees, NAD 1983). A map illustrating these waters can be 
obtained from EPA or viewed at http://www.epa.gov/region9/water/no-
discharge/overview.html.
    (B) A ``large passenger vessel'' means a passenger vessel, as 
defined in section 2101(22) of title 46, United States Code, of 300 
gross tons or more, as measured under the International Convention on 
Tonnage Measurement of Ships, 1969, measurement system in 46 U.S.C. 
14302, or the regulatory measurement system of 46 U.S.C. 14502 for 
vessels not measured under 46 U.S.C. 14302, that has berths or overnight 
accommodations for passengers.
    (C) A ``large oceangoing vessel'' means a private, commercial, 
government, or military vessel of 300 gross tons or more, as measured 
under the International Convention on Tonnage Measurement of Ships, 
1969, measurement system in 46 U.S.C. 14302, or the regulatory 
measurement system of 46 U.S.C. 14502 for vessels not measured under 46 
U.S.C.14302, that is not a large passenger vessel.
    (D) A ``holding tank'' means a tank specifically designed, 
constructed, and fitted for the retention of treated or untreated 
sewage, that has been designated and approved by the ship's flag 
Administration on the ship's stability plan; a designated ballast tank 
is not a holding tank for this purpose.
    (c)(1) Prohibition pursuant to CWA section 312(f)(4)(B): A State may 
make written application to the Administrator of the Environmental 
Protection Agency under section 312(f)(4)(B) of the Act for the issuance 
of a regulation establishing a drinking water intake no discharge zone 
which completely prohibits discharge from a vessel of any sewage, 
whether treated or untreated, into that zone in particular waters, or 
portions thereof, within such State. Such application shall:
    (i) Identify and describe exactly and in detail the location of the 
drinking water supply intake(s) and the community served by the 
intake(s), including average and maximum expected amounts of inflow;
    (ii) Specify and describe exactly and in detail, the waters, or 
portions thereof, for which a complete prohibition is desired, and where 
appropriate, average, maximum and low flows in million gallons per day 
(MGD) or the metric equivalent;
    (iii) Include a map, either a USGS topographic quadrant map or a 
NOAA nautical chart, as applicable, clearly marking by latitude and 
longitude the waters or portions thereof to be designated a drinking 
water intake zone; and
    (iv) Include a statement of basis justifying the size of the 
requested drinking water intake zone, for example, identifying areas of 
intensive boating activities.
    (2) If the Administrator finds that a complete prohibition is 
appropriate under this paragraph, he or she shall publish notice of such 
finding together

[[Page 424]]

with a notice of proposed rulemaking, and then shall proceed in 
accordance with 5 U.S.C. 553. If the Administrator's finding is that a 
complete prohibition covering a more restricted or more expanded area 
than that applied for by the State is appropriate, he or she shall also 
include a statement of the reasons why the finding differs in scope from 
that requested in the State's application.
    (3) If the Administrator finds that a complete prohibition is 
inappropriate under this paragraph, he or she shall deny the application 
and state the reasons for such denial.
    (4) For the following waters the discharge from a vessel of any 
sewage, whether treated or not, is completely prohibited pursuant to CWA 
section 312(f)(4)(B):
    (i) Two portions of the Hudson River in New York State, the first is 
bounded by an east-west line through the most northern confluence of the 
Mohawk River which will be designated by the Troy-Waterford Bridge 
(126th Street Bridge) on the south and Lock 2 on the north, and the 
second of which is bounded on the north by the southern end of 
Houghtaling Island and on the south by a line between the Village of 
Roseton on the western shore and Low Point on the eastern shore in the 
vicinity of Chelsea, as described in Items 2 and 3 of 6 NYCRR Part 
858.4.
    (ii) [Reserved]

[41 FR 4453, Jan. 29, 1976, as amended at 42 FR 43837, Aug. 31, 1977; 60 
FR 63945, Dec. 13, 1995; 63 FR 1320, Jan. 8, 1998; 67 FR 35743, May 21, 
2002; 77 FR 11411, Feb. 27, 2012]



Sec.  140.5  Analytical procedures.

    In determining the composition and quality of effluent discharge 
from marine sanitation devices, the procedures contained in 40 CFR part 
136, ``Guidelines Establishing Test Procedures for the Analysis of 
Pollutants,'' or subsequent revisions or amendments thereto, shall be 
employed.



PART 141_NATIONAL PRIMARY DRINKING WATER REGULATIONS--Table of Contents



                            Subpart A_General

Sec.
141.1 Applicability.
141.2 Definitions.
141.3 Coverage.
141.4 Variances and exemptions.
141.5 Siting requirements.
141.6 Effective dates.

                  Subpart B_Maximum Contaminant Levels

141.11 Maximum contaminant levels for inorganic chemicals.
141.12 [Reserved]
141.13 Maximum contaminant levels for turbidity.

            Subpart C_Monitoring and Analytical Requirements

141.21 Coliform sampling.
141.22 Turbidity sampling and analytical requirements.
141.23 Inorganic chemical sampling and analytical requirements.
141.24 Organic chemicals, sampling and analytical requirements.
141.25 Analytical methods for radioactivity.
141.26 Monitoring frequency and compliance requirements for 
          radionuclides in community water systems
141.27 Alternate analytical techniques.
141.28 Certified laboratories.
141.29 Monitoring of consecutive public water systems.

Appendix A to Subpart C of Part 141--Alternative Testing Methods 
          Approved for Analyses Under the Safe Drinking Water Act

                  Subpart D_Reporting and Recordkeeping

141.31 Reporting requirements.
141.32 [Reserved]
141.33 Record maintenance.
141.34 [Reserved]
141.35 Reporting for unregulated contaminant monitoring results.

  Subpart E_Special Regulations, Including Monitoring Regulations and 
                         Prohibition on Lead Use

141.40 Monitoring requirements for unregulated contaminants.
141.41 Special monitoring for sodium.
141.42 Special monitoring for corrosivity characteristics.
141.43 Prohibition on use of lead pipes, solder, and flux.

     Subpart F_Maximum Contaminant Level Goals and Maximum Residual 
                        Disinfectant Level Goals

141.50 Maximum contaminant level goals for organic contaminants.
141.51 Maximum contaminant level goals for inorganic contaminants.

[[Page 425]]

141.52 Maximum contaminant level goals for microbiological contaminants.
141.53 Maximum contaminant level goals for disinfection byproducts.
141.54 Maximum residual disinfectant level goals for disinfectants.
141.55 Maximum contaminant level goals for radionuclides.

     Subpart G_National Primary Drinking Water Regulations: Maximum 
       Contaminant Levels and Maximum Residual Disinfectant Levels

141.60 Effective dates.
141.61 Maximum contaminant levels for organic contaminants.
141.62 Maximum contaminant levels for inorganic contaminants.
141.63 Maximum contaminant levels (MCLs) for microbiological 
          contaminants.
141.64 Maximum contaminant levels for disinfection byproducts.
141.65 Maximum residual disinfectant levels.
141.66 Maximum contaminant levels for radionuclides.

                  Subpart H_Filtration and Disinfection

141.70 General requirements.
141.71 Criteria for avoiding filtration.
141.72 Disinfection.
141.73 Filtration.
141.74 Analytical and monitoring requirements.
141.75 Reporting and recordkeeping requirements.
141.76 Recycle provisions.

                  Subpart I_Control of Lead and Copper

141.80 General requirements.
141.81 Applicability of corrosion control treatment steps to small, 
          medium-size and large water systems.
141.82 Description of corrosion control treatment requirements.
141.83 Source water treatment requirements.
141.84 Lead service line replacement requirements.
141.85 Public education and supplemental monitoring requirements.
141.86 Monitoring requirements for lead and copper in tap water.
141.87 Monitoring requirements for water quality parameters.
141.88 Monitoring requirements for lead and copper in source water.
141.89 Analytical methods.
141.90 Reporting requirements.
141.91 Recordkeeping requirements.

           Subpart J_Use of Non-Centralized Treatment Devices

141.100 Criteria and procedures for public water systems using point-of-
          entry devices.
141.101 Use of bottled water.

                     Subpart K_Treatment Techniques

141.110 General requirements.
141.111 Treatment techniques for acrylamide and epichlorohydrin.

     Subpart L_Disinfectant Residuals, Disinfection Byproducts, and 
                    Disinfection Byproduct Precursors

141.130 General requirements.
141.131 Analytical requirements.
141.132 Monitoring requirements.
141.133 Compliance requirements.
141.134 Reporting and recordkeeping requirements.
141.135 Treatment technique for control of disinfection byproduct (DBP) 
          precursors.

Subparts M-N [Reserved]

                  Subpart O_Consumer Confidence Reports

141.151 Purpose and applicability of this subpart.
141.152 Effective dates.
141.153 Content of the reports.
141.154 Required additional health information.
141.155 Report delivery and recordkeeping.

Appendix A to Subpart O of Part 141--Regulated Contaminants

Subpart P_Enhanced Filtration and Disinfection_Systems Serving 10,000 or 
                               More People

141.170 General requirements.
141.171 Criteria for avoiding filtration.
141.172 Disinfection profiling and benchmarking.
141.173 Filtration.
141.174 Filtration sampling requirements.
141.175 Reporting and recordkeeping requirements.

       Subpart Q_Public Notification of Drinking Water Violations

141.201 General public notification requirements.
141.202 Tier 1 Public Notice--Form, manner, and frequency of notice.
141.203 Tier 2 Public Notice--Form, manner, and frequency of notice.
141.204 Tier 3 Public Notice--Form, manner, and frequency of notice.
141.205 Content of the public notice.

[[Page 426]]

141.206 Notice to new billing units or new customers.
141.207 Special notice of the availability of unregulated contaminant 
          monitoring results.
141.208 Special notice for exceedance of the SMCL for fluoride.
141.209 Special notice for nitrate exceedances above MCL by non-
          community water systems (NCWS), where granted permission by 
          the primacy agency under Sec.  141.11(d).
141.210 Notice by primacy agency on behalf of the public water system.
141.211 Special notice for repeated failure to conduct monitoring of the 
          source water for Cryptosporidium and for failure to determine 
          bin classification or mean Cryptosporidium level.

Appendix A to Subpart Q of Part 141--NPDWR Violations and Situations 
          Requiring Public Notice
Appendix B to Subpart Q of Part 141--Standard Health Effects Language 
          for Public Notification
Appendix C to Subpart Q of Part 141--List of Acronyms Used in Public 
          Notification Regulation

Subpart R [Reserved]

                       Subpart S_Ground Water Rule

141.400 General requirements and applicability.
141.401 Sanitary surveys for ground water systems.
141.402 Ground water source microbial monitoring and analytical methods.
141.403 Treatment technique requirements for ground water systems.
141.404 Treatment technique violations for ground water systems.
141.405 Reporting and recordkeeping for ground water systems.

  Subpart T_Enhanced Filtration and Disinfection_Systems Serving Fewer 
                           Than 10,000 People

                          General Requirements

141.500 General requirements.
141.501 Who is subject to the requirements of subpart T?
141.502 When must my system comply with these requirements?
141.503 What does subpart T require?

                        Finished Water Reservoirs

141.510 Is my system subject to the new finished water reservoir 
          requirements?
141.511 What is required of new finished water reservoirs?

    Additional Watershed Control Requirements for Unfiltered Systems

141.520 Is my system subject to the updated watershed control 
          requirements?
141.521 What updated watershed control requirements must my unfiltered 
          system implement to continue to avoid filtration?
141.522 How does the State determine whether my system's watershed 
          control requirements are adequate?

                          Disinfection Profile

141.530 What is a disinfection profile and who must develop one?
141.531 What criteria must a State use to determine that a profile is 
          unnecessary?
141.532 How does my system develop a disinfection profile and when must 
          it begin?
141.533 What data must my system collect to calculate a disinfection 
          profile?
141.534 How does my system use this data to calculate an inactivation 
          ratio?
141.535 What if my system uses chloramines, ozone, or chlorine dioxide 
          for primary disinfection?
141.536 My system has developed an inactivation ratio; what must we do 
          now?

                         Disinfection Benchmark

141.540 Who has to develop a disinfection benchmark?
141.541 What are significant changes to disinfection practice?
141.542 What must my system do if we are considering a significant 
          change to disinfection practices?
141.543 How is the disinfection benchmark calculated?
141.544 What if my system uses chloramines, ozone, or chlorine dioxide 
          for primary disinfection?

                  Combined Filter Effluent Requirements

141.550 Is my system required to meet subpart T combined filter effluent 
          turbidity limits?
141.551 What strengthened combined filter effluent turbidity limits must 
          my system meet?
141.552 My system consists of ``alternative filtration'' and is required 
          to conduct a demonstration--what is required of my system and 
          how does the State establish my turbidity limits?
141.553 My system practices lime softening--is there any special 
          provision regarding my combined filter effluent?

                Individual Filter Turbidity Requirements

141.560 Is my system subject to individual filter turbidity 
          requirements?
141.561 What happens if my system's turbidity monitoring equipment 
          fails?

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141.562 My system only has two or fewer filters--is there any special 
          provision regarding individual filter turbidity monitoring?
141.563 What follow-up action is my system required to take based on 
          continuous turbidity monitoring?
141.564 My system practices lime softening--is there any special 
          provision regarding my individual filter turbidity monitoring?

                Reporting and Recordkeeping Requirements

141.570 What does subpart T require that my system report to the State?
141.571 What records does subpart T require my system to keep?

            Subpart U_Initial Distribution System Evaluations

141.600 General requirements.
141.601 Standard monitoring.
141.602 System specific studies.
141.603 40/30 certification.
141.604 Very small system waivers.
141.605 Subpart V compliance monitoring location recommendations.

         Subpart V_Stage 2 Disinfection Byproducts Requirements

141.620 General requirements.
141.621 Routine monitoring.
141.622 Subpart V monitoring plan.
141.623 Reduced monitoring.
141.624 Additional requirements for consecutive systems.
141.625 Conditions requiring increased monitoring.
141.626 Operational evaluation levels.
141.627 Requirements for remaining on reduced TTHM and HAA5 monitoring 
          based on subpart L results.
141.628 Requirements for remaining on increased TTHM and HAA5 monitoring 
          based on subpart L results.
141.629 Reporting and recordkeeping requirements.

            Subpart W_Enhanced Treatment for Cryptosporidium

                          General Requirements

141.700 General requirements.

                  Source Water Monitoring Requirements

141.701 Source water monitoring.
141.702 Sampling schedules.
141.703 Sampling locations.
141.704 Analytical methods.
141.705 Approved laboratories.
141.706 Reporting source water monitoring results.
141.707 Grandfathering previously collected data.

          Disinfection Profiling and Benchmarking Requirements

141.708 Requirements when making a significant change in disinfection 
          practice.
141.709 Developing the disinfection profile and benchmark.

                    Treatment Technique Requirements

141.710 Bin classification for filtered systems.
141.711 Filtered system additional Cryptosporidium treatment 
          requirements.
141.712 Unfiltered system Cryptosporidium treatment requirements.
141.713 Schedule for compliance with Cryptosporidium treatment 
          requirements.
141.714 Requirements for uncovered finished water storage facilities.

              Requirements for Microbial Toolbox Components

141.715 Microbial toolbox options for meeting Cryptosporidium treatment 
          requirements.
141.716 Source toolbox components.
141.717 Pre-filtration treatment toolbox components.
141.718 Treatment performance toolbox components.
141.719 Additional filtration toolbox components.
141.720 Inactivation toolbox components.

                Reporting and Recordkeeping Requirements

141.721 Reporting requirements.
141.722 Recordkeeping requirements.

           Requirements for Sanitary Surveys Performed by EPA

141.723 Requirements to respond to significant deficiencies identified 
          in sanitary surveys performed by EPA.

                 Subpart X_Aircraft Drinking Water Rule

141.800 Applicability and compliance date.
141.801 Definitions.
141.802 Coliform sampling plan.
141.803 Coliform sampling.
141.804 Aircraft water system operations and maintenance plan.
141.805 Notification to passengers and crew.
141.806 Reporting requirements.
141.807 Recordkeeping requirements.
141.808 Audits and inspections.
141.809 Supplemental treatment.
141.810 Violations.

                  Subpart Y_Revised Total Coliform Rule

141.851 General.

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141.852 Analytical methods and laboratory certification.
141.853 General monitoring requirements for all public water systems.
141.854 Routine monitoring requirements for non-community water systems 
          serving 1,000 or fewer people using only ground water.
141.855 Routine monitoring requirements for community water systems 
          serving 1,000 or fewer people using only ground water.
141.856 Routine monitoring requirements for subpart H public water 
          systems serving 1,000 or fewer people.
141.857 Routine monitoring requirements for public water systems serving 
          more than 1,000 people.
141.858 Repeat monitoring and E. coli requirements.
141.859 Coliform treatment technique triggers and assessment 
          requirements for protection against potential fecal 
          contamination.
141.860 Violations.
141.861 Reporting and recordkeeping.

    Authority: 42 U.S.C. 300f, 300g-1, 300g-2, 300g-3, 300g-4, 300g-5, 
300g-6, 300j-4, 300j-9, and 300j-11.

    Source: 40 FR 59570, Dec. 24, 1975, unless otherwise noted.

    Editorial Note: Nomenclature changes to part 141 appear at 69 FR 
18803, Apr. 9, 2004.

    Note: For community water systems serving 75,000 or more persons, 
monitoring must begin 1 year following promulation and the effective 
date of the MCL is 2 years following promulgation. For community water 
systems serving 10,000 to 75,000 persons, monitoring must begin within 3 
years from the date of promulgation and the effective date of the MCL is 
4 years from the date of promulgation. Effective immediately, systems 
that plan to make significant modifications to their treatment processes 
for the purpose of complying with the TTHM MCL are required to seek and 
obtain State approval of their treatment modification plans. This note 
affects Sec. Sec.  141.2, 141.6, 141.12, 141.24 and 141.30. For 
additional information see 44 FR 68641, Nov. 29, 1979.



                            Subpart A_General



Sec.  141.1  Applicability.

    This part establishes primary drinking water regulations pursuant to 
section 1412 of the Public Health Service Act, as amended by the Safe 
Drinking Water Act (Pub. L. 93-523); and related regulations applicable 
to public water systems.



Sec.  141.2  Definitions.

    As used in this part, the term:
    Act means the Public Health Service Act, as amended by the Safe 
Drinking Water Act, Public Law 93-523.
    Action level, is the concentration of lead or copper in water 
specified in Sec.  141.80(c) which determines, in some cases, the 
treatment requirements contained in subpart I of this part that a water 
system is required to complete.
    Bag filters are pressure-driven separation devices that remove 
particulate matter larger than 1 micrometer using an engineered porous 
filtration media. They are typically constructed of a non-rigid, fabric 
filtration media housed in a pressure vessel in which the direction of 
flow is from the inside of the bag to outside.
    Bank filtration is a water treatment process that uses a well to 
recover surface water that has naturally infiltrated into ground water 
through a river bed or bank(s). Infiltration is typically enhanced by 
the hydraulic gradient imposed by a nearby pumping water supply or other 
well(s).
    Best available technology or BAT means the best technology, 
treatment techniques, or other means which the Administrator finds, 
after examination for efficacy under field conditions and not solely 
under laboratory conditions, are available (taking cost into 
consideration). For the purposes of setting MCLs for synthetic organic 
chemicals, any BAT must be at least as effective as granular activated 
carbon.
    Cartridge filters are pressure-driven separation devices that remove 
particulate matter larger than 1 micrometer using an engineered porous 
filtration media. They are typically constructed as rigid or semi-rigid, 
self-supporting filter elements housed in pressure vessels in which flow 
is from the outside of the cartridge to the inside.
    Clean compliance history is, for the purposes of subpart Y, a record 
of no MCL violations under Sec.  141.63; no monitoring violations under 
Sec.  141.21 or subpart Y; and no coliform treatment technique trigger 
exceedances or treatment technique violations under subpart Y.
    Coagulation means a process using coagulant chemicals and mixing by 
which colloidal and suspended materials are

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destabilized and agglomerated into flocs.
    Combined distribution system is the interconnected distribution 
system consisting of the distribution systems of wholesale systems and 
of the consecutive systems that receive finished water.
    Community water system means a public water system which serves at 
least 15 service connections used by year-round residents or regularly 
serves at least 25 year-round residents.
    Compliance cycle means the nine-year calendar year cycle during 
which public water systems must monitor. Each compliance cycle consists 
of three three-year compliance periods. The first calendar year cycle 
begins January 1, 1993 and ends December 31, 2001; the second begins 
January 1, 2002 and ends December 31, 2010; the third begins January 1, 
2011 and ends December 31, 2019.
    Compliance period means a three-year calendar year period within a 
compliance cycle. Each compliance cycle has three three-year compliance 
periods. Within the first compliance cycle, the first compliance period 
runs from January 1, 1993 to December 31, 1995; the second from January 
1, 1996 to December 31, 1998; the third from January 1, 1999 to December 
31, 2001.
    Comprehensive performance evaluation (CPE) is a thorough review and 
analysis of a treatment plant's performance-based capabilities and 
associated administrative, operation and maintenance practices. It is 
conducted to identify factors that may be adversely impacting a plant's 
capability to achieve compliance and emphasizes approaches that can be 
implemented without significant capital improvements. For purpose of 
compliance with subparts P and T of this part, the comprehensive 
performance evaluation must consist of at least the following 
components: Assessment of plant performance; evaluation of major unit 
processes; identification and prioritization of performance limiting 
factors; assessment of the applicability of comprehensive technical 
assistance; and preparation of a CPE report.
    Confluent growth means a continuous bacterial growth covering the 
entire filtration area of a membrane filter, or a portion thereof, in 
which bacterial colonies are not discrete.
    Consecutive system is a public water system that receives some or 
all of its finished water from one or more wholesale systems. Delivery 
may be through a direct connection or through the distribution system of 
one or more consecutive systems.
    Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    Conventional filtration treatment means a series of processes 
including coagulation, flocculation, sedimentation, and filtration 
resulting in substantial particulate removal.
    Corrosion inhibitor means a substance capable of reducing the 
corrosivity of water toward metal plumbing materials, especially lead 
and copper, by forming a protective film on the interior surface of 
those materials.
    CT or CTcalc is the product of ``residual disinfectant 
concentration'' (C) in mg/1 determined before or at the first customer, 
and the corresponding ``disinfectant contact time'' (T) in minutes, 
i.e., ``C'' x ``T''. If a public water system applies disinfectants at 
more than one point prior to the first customer, it must determine the 
CT of each disinfectant sequence before or at the first customer to 
determine the total percent inactivation or ``total inactivation 
ratio.'' In determining the total inactivation ratio, the public water 
system must determine the residual disinfectant concentration of each 
disinfection sequence and corresponding contact time before any 
subsequent disinfection application point(s). ``CT99.9'' is 
the CT value required for 99.9 percent (3-log) inactivation of Giardia 
lamblia cysts. CT99.9 for a variety of disinfectants and 
conditions appear in tables 1.1-1.6, 2.1, and 3.1 of Sec.  141.74(b)(3).
[GRAPHIC] [TIFF OMITTED] TC15NO91.129


is the inactivation ratio. The sum of the inactivation ratios, or total 
inactivation ratio shown as

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[GRAPHIC] [TIFF OMITTED] TC15NO91.130


is calculated by adding together the inactivation ratio for each 
disinfection sequence. A total inactivation ratio equal to or greater 
than 1.0 is assumed to provide a 3-log inactivation of Giardia lamblia 
cysts.
    Diatomaceous earth filtration means a process resulting in 
substantial particulate removal in which (1) a precoat cake of 
diatomaceous earth filter media is deposited on a support membrance 
(septum), and (2) while the water is filtered by passing through the 
cake on the septum, additional filter media known as body feed is 
continuously added to the feed water to maintain the permeability of the 
filter cake.
    Direct filtration means a series of processes including coagulation 
and filtration but excluding sedimentation resulting in substantial 
particulate removal.
    Disinfectant means any oxidant, including but not limited to 
chlorine, chlorine dioxide, chloramines, and ozone added to water in any 
part of the treatment or distribution process, that is intended to kill 
or inactivate pathogenic microorganisms.
    Disinfectant contact time (``T'' in CT calculations) means the time 
in minutes that it takes for water to move from the point of 
disinfectant application or the previous point of disinfectant residual 
measurement to a point before or at the point where residual 
disinfectant concentration (``C'') is measured. Where only one ``C'' is 
measured, ``T'' is the time in minutes that it takes for water to move 
from the point of disinfectant application to a point before or at where 
residual disinfectant concentration (``C'') is measured. Where more than 
one ``C'' is measured, ``T'' is (a) for the first measurement of ``C'', 
the time in minutes that it takes for water to move from the first or 
only point of disinfectant application to a point before or at the point 
where the first ``C'' is measured and (b) for subsequent measurements of 
``C'', the time in minutes that it takes for water to move from the 
previous ``C'' measurement point to the ``C'' measurement point for 
which the particular ``T'' is being calculated. Disinfectant contact 
time in pipelines must be calculated based on ``plug flow'' by dividing 
the internal volume of the pipe by the maximum hourly flow rate through 
that pipe. Disinfectant contact time within mixing basins and storage 
reservoirs must be determined by tracer studies or an equivalent 
demonstration.
    Disinfection means a process which inactivates pathogenic organisms 
in water by chemical oxidants or equivalent agents.
    Disinfection profile is a summary of Giardia lamblia inactivation 
through the treatment plant. The procedure for developing a disinfection 
profile is contained in Sec.  141.172 (Disinfection profiling and 
benchmarking) in subpart P and Sec. Sec.  141.530-141.536 (Disinfection 
profile) in subpart T of this part.
    Domestic or other non-distribution system plumbing problem means a 
coliform contamination problem in a public water system with more than 
one service connection that is limited to the specific service 
connection from which the coliform-positive sample was taken.
    Dose equivalent means the product of the absorbed dose from ionizing 
radiation and such factors as account for differences in biological 
effectiveness due to the type of radiation and its distribution in the 
body as specified by the International Commission on Radiological Units 
and Measurements (ICRU).
    Dual sample set is a set of two samples collected at the same time 
and same location, with one sample analyzed for TTHM and the other 
sample analyzed for HAA5. Dual sample sets are collected for the 
purposes of conducting an IDSE under subpart U of this part and 
determining compliance with the TTHM and HAA5 MCLs under subpart V of 
this part.
    Effective corrosion inhibitor residual, for the purpose of subpart I 
of this part only, means a concentration sufficient to form a 
passivating film on the interior walls of a pipe.

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    Enhanced coagulation means the addition of sufficient coagulant for 
improved removal of disinfection byproduct precursors by conventional 
filtration treatment.
    Enhanced softening means the improved removal of disinfection 
byproduct precursors by precipitative softening.
    Filter profile is a graphical representation of individual filter 
performance, based on continuous turbidity measurements or total 
particle counts versus time for an entire filter run, from startup to 
backwash inclusively, that includes an assessment of filter performance 
while another filter is being backwashed.
    Filtration means a process for removing particulate matter from 
water by passage through porous media.
    Finished water is water that is introduced into the distribution 
system of a public water system and is intended for distribution and 
consumption without further treatment, except as treatment necessary to 
maintain water quality in the distribution system (e.g., booster 
disinfection, addition of corrosion control chemicals).
    First draw sample means a one-liter sample of tap water, collected 
in accordance with Sec.  141.86(b)(2), that has been standing in 
plumbing pipes at least 6 hours and is collected without flushing the 
tap.
    Flocculation means a process to enhance agglomeration or collection 
of smaller floc particles into larger, more easily settleable particles 
through gentle stirring by hydraulic or mechanical means.
    Flowing stream is a course of running water flowing in a definite 
channel.
    GAC10 means granular activated carbon filter beds with an empty-bed 
contact time of 10 minutes based on average daily flow and a carbon 
reactivation frequency of every 180 days, except that the reactivation 
frequency for GAC10 used as a best available technology for compliance 
with subpart V MCLs under Sec.  141.64(b)(2) shall be 120 days.
    GAC20 means granular activated carbon filter beds with an empty-bed 
contact time of 20 minutes based on average daily flow and a carbon 
reactivation frequency of every 240 days.
    Ground water under the direct influence of surface water (GWUDI) 
means any water beneath the surface of the ground with significant 
occurrence of insects or other macroorganisms, algae, or large-diameter 
pathogens such as Giardia lamblia or Cryptosporidium, or significant and 
relatively rapid shifts in water characteristics such as turbidity, 
temperature, conductivity, or pH which closely correlate to 
climatological or surface water conditions. Direct influence must be 
determined for individual sources in accordance with criteria 
established by the State. The State determination of direct influence 
may be based on site-specific measurements of water quality and/or 
documentation of well construction characteristics and geology with 
field evaluation.
    Gross alpha particle activity means the total radioactivity due to 
alpha particle emission as inferred from measurements on a dry sample.
    Gross beta particle activity means the total radioactivity due to 
beta particle emission as inferred from measurements on a dry sample.
    Haloacetic acids (five) (HAA5) mean the sum of the concentrations in 
milligrams per liter of the haloacetic acid compounds (monochloroacetic 
acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid, 
and dibromoacetic acid), rounded to two significant figures after 
addition.
    Halogen means one of the chemical elements chlorine, bromine or 
iodine.
    Initial compliance period means the first full three-year compliance 
period which begins at least 18 months after promulgation, except for 
contaminants listed at Sec.  141.61(a) (19)-(21), (c) (19)-(33), and 
Sec.  141.62(b) (11)-(15), initial compliance period means the first 
full three-year compliance period after promulgation for systems with 
150 or more service connections (January 1993-December 1995), and first 
full three-year compliance period after the effective date of the 
regulation (January 1996-December 1998) for systems having fewer than 
150 service connections.
    Lake/reservoir refers to a natural or man made basin or hollow on 
the Earth's surface in which water collects or is stored that may or may 
not have a current or single direction of flow.

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    Large water system, for the purpose of subpart I of this part only, 
means a water system that serves more than 50,000 persons.
    Lead service line means a service line made of lead which connects 
the water main to the building inlet and any lead pigtail, gooseneck or 
other fitting which is connected to such lead line.
    Legionella means a genus of bacteria, some species of which have 
caused a type of pneumonia called Legionnaires Disease.
    Level 1 assessment is an evaluation to identify the possible 
presence of sanitary defects, defects in distribution system coliform 
monitoring practices, and (when possible) the likely reason that the 
system triggered the assessment. It is conducted by the system operator 
or owner. Minimum elements include review and identification of atypical 
events that could affect distributed water quality or indicate that 
distributed water quality was impaired; changes in distribution system 
maintenance and operation that could affect distributed water quality 
(including water storage); source and treatment considerations that bear 
on distributed water quality, where appropriate (e.g., whether a ground 
water system is disinfected); existing water quality monitoring data; 
and inadequacies in sample sites, sampling protocol, and sample 
processing. The system must conduct the assessment consistent with any 
State directives that tailor specific assessment elements with respect 
to the size and type of the system and the size, type, and 
characteristics of the distribution system.
    Level 2 assessment is an evaluation to identify the possible 
presence of sanitary defects, defects in distribution system coliform 
monitoring practices, and (when possible) the likely reason that the 
system triggered the assessment. A Level 2 assessment provides a more 
detailed examination of the system (including the system's monitoring 
and operational practices) than does a Level 1 assessment through the 
use of more comprehensive investigation and review of available 
information, additional internal and external resources, and other 
relevant practices. It is conducted by an individual approved by the 
State, which may include the system operator. Minimum elements include 
review and identification of atypical events that could affect 
distributed water quality or indicate that distributed water quality was 
impaired; changes in distribution system maintenance and operation that 
could affect distributed water quality (including water storage); source 
and treatment considerations that bear on distributed water quality, 
where appropriate (e.g., whether a ground water system is disinfected); 
existing water quality monitoring data; and inadequacies in sample 
sites, sampling protocol, and sample processing. The system must conduct 
the assessment consistent with any State directives that tailor specific 
assessment elements with respect to the size and type of the system and 
the size, type, and characteristics of the distribution system. The 
system must comply with any expedited actions or additional actions 
required by the State in the case of an E. coli MCL violation.
    Locational running annual average (LRAA) is the average of sample 
analytical results for samples taken at a particular monitoring location 
during the previous four calendar quarters.
    Man-made beta particle and photon emitters means all radionuclides 
emitting beta particles and/or photons listed in Maximum Permissible 
Body Burdens and Maximum Permissible Concentration of Radionuclides in 
Air or Water for Occupational Exposure, NBS Handbook 69, except the 
daughter products of thorium-232, uranium-235 and uranium-238.
    Maximum contaminant level means the maximum permissable level of a 
contaminant in water which is delivered to any user of a public water 
system.
    Maximum contaminant level goal or MCLG means the maximum level of a 
contaminant in drinking water at which no known or anticipated adverse 
effect on the health of persons would occur, and which allows an 
adequate margin of safety. Maximum contaminant level goals are 
nonenforceable health goals.
    Maximum residual disinfectant level (MRDL) means a level of a 
disinfectant added for water treatment that may not be exceeded at the 
consumer's tap without an unacceptable possibility of

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adverse health effects. For chlorine and chloramines, a PWS is in 
compliance with the MRDL when the running annual average of monthly 
averages of samples taken in the distribution system, computed 
quarterly, is less than or equal to the MRDL. For chlorine dioxide, a 
PWS is in compliance with the MRDL when daily samples are taken at the 
entrance to the distribution system and no two consecutive daily samples 
exceed the MRDL. MRDLs are enforceable in the same manner as maximum 
contaminant levels under Section 1412 of the Safe Drinking Water Act. 
There is convincing evidence that addition of a disinfectant is 
necessary for control of waterborne microbial contaminants. 
Notwithstanding the MRDLs listed in Sec.  141.65, operators may increase 
residual disinfectant levels of chlorine or chloramines (but not 
chlorine dioxide) in the distribution system to a level and for a time 
necessary to protect public health to address specific microbiological 
contamination problems caused by circumstances such as distribution line 
breaks, storm runoff events, source water contamination, or cross-
connections.
    Maximum residual disinfectant level goal (MRDLG) means the maximum 
level of a disinfectant added for water treatment at which no known or 
anticipated adverse effect on the health of persons would occur, and 
which allows an adequate margin of safety. MRDLGs are nonenforceable 
health goals and do not reflect the benefit of the addition of the 
chemical for control of waterborne microbial contaminants.
    Maximum Total Trihalomethane Potential (MTP) means the maximum 
concentration of total trihalomethanes produced in a given water 
containing a disinfectant residual after 7 days at a temperature of 25 
[deg]C or above.
    Medium-size water system, for the purpose of subpart I of this part 
only, means a water system that serves greater than 3,300 and less than 
or equal to 50,000 persons.
    Membrane filtration is a pressure or vacuum driven separation 
process in which particulate matter larger than 1 micrometer is rejected 
by an engineered barrier, primarily through a size-exclusion mechanism, 
and which has a measurable removal efficiency of a target organism that 
can be verified through the application of a direct integrity test. This 
definition includes the common membrane technologies of microfiltration, 
ultrafiltration, nanofiltration, and reverse osmosis.
    Near the first service connection means at one of the 20 percent of 
all service connections in the entire system that are nearest the water 
supply treatment facility, as measured by water transport time within 
the distribution system.
    Non-community water system means a public water system that is not a 
community water system. A non-community water system is either a 
``transient non-community water system (TWS)'' or a ``non-transient non-
community water system (NTNCWS).''
    Non-transient non-community water system or NTNCWS means a public 
water system that is not a community water system and that regularly 
serves at least 25 of the same persons over 6 months per year.
    Optimal corrosion control treatment, for the purpose of subpart I of 
this part only, means the corrosion control treatment that minimizes the 
lead and copper concentrations at users' taps while insuring that the 
treatment does not cause the water system to violate any national 
primary drinking water regulations.
    Performance evaluation sample means a reference sample provided to a 
laboratory for the purpose of demonstrating that the laboratory can 
successfully analyze the sample within limits of performance specified 
by the Agency. The true value of the concentration of the reference 
material is unknown to the laboratory at the time of the analysis.
    Person means an individual; corporation; company; association; 
partnership; municipality; or State, Federal, or tribal agency.
    Picocurie (pCi) means the quantity of radioactive material producing 
2.22 nuclear transformations per minute.
    Plant intake refers to the works or structures at the head of a 
conduit through which water is diverted from a source (e.g., river or 
lake) into the treatment plant.

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    Point of disinfectant application is the point where the 
disinfectant is applied and water downstream of that point is not 
subject to recontamination by surface water runoff.
    Point-of-entry treatment device (POE) is a treatment device applied 
to the drinking water entering a house or building for the purpose of 
reducing contaminants in the drinking water distributed throughout the 
house or building.
    Point-of-use treatment device (POU) is a treatment device applied to 
a single tap used for the purpose of reducing contaminants in drinking 
water at that one tap.
    Presedimentation is a preliminary treatment process used to remove 
gravel, sand and other particulate material from the source water 
through settling before the water enters the primary clarification and 
filtration processes in a treatment plant.
    Public water system means a system for the provision to the public 
of water for human consumption through pipes or, after August 5, 1998, 
other constructed conveyances, if such system has at least fifteen 
service connections or regularly serves an average of at least twenty-
five individuals daily at least 60 days out of the year. Such term 
includes: any collection, treatment, storage, and distribution 
facilities under control of the operator of such system and used 
primarily in connection with such system; and any collection or 
pretreatment storage facilities not under such control which are used 
primarily in connection with such system. Such term does not include any 
``special irrigation district.'' A public water system is either a 
``community water system'' or a ``noncommunity water system.''
    Rem means the unit of dose equivalent from ionizing radiation to the 
total body or any internal organ or organ system. A ``millirem (mrem)'' 
is \1/1000\ of a rem.
    Repeat compliance period means any subsequent compliance period 
after the initial compliance period.
    Residual disinfectant concentration (``C'' in CT calculations) means 
the concentration of disinfectant measured in mg/l in a representative 
sample of water.
    Sanitary defect is a defect that could provide a pathway of entry 
for microbial contamination into the distribution system or that is 
indicative of a failure or imminent failure in a barrier that is already 
in place.
    Sanitary survey means an onsite review of the water source, 
facilities, equipment, operation and maintenance of a public water 
system for the purpose of evaluating the adequacy of such source, 
facilities, equipment, operation and maintenance for producing and 
distributing safe drinking water.
    Seasonal system is a non-community water system that is not operated 
as a public water system on a year-round basis and starts up and shuts 
down at the beginning and end of each operating season.
    Sedimentation means a process for removal of solids before 
filtration by gravity or separation.
    Service connection, as used in the definition of public water 
system, does not include a connection to a system that delivers water by 
a constructed conveyance other than a pipe if:
    (1) The water is used exclusively for purposes other than 
residential uses (consisting of drinking, bathing, and cooking, or other 
similar uses);
    (2) The State determines that alternative water to achieve the 
equivalent level of public health protection provided by the applicable 
national primary drinking water regulation is provided for residential 
or similar uses for drinking and cooking; or
    (3) The State determines that the water provided for residential or 
similar uses for drinking, cooking, and bathing is centrally treated or 
treated at the point of entry by the provider, a pass-through entity, or 
the user to achieve the equivalent level of protection provided by the 
applicable national primary drinking water regulations.
    Service line sample means a one-liter sample of water collected in 
accordance with Sec.  141.86(b)(3), that has been standing for at least 
6 hours in a service line.
    Single family structure, for the purpose of subpart I of this part 
only, means a building constructed as a single-family residence that is 
currently used as either a residence or a place of business.

[[Page 435]]

    Slow sand filtration means a process involving passage of raw water 
through a bed of sand at low velocity (generally less than 0.4 m/h) 
resulting in substantial particulate removal by physical and biological 
mechanisms.
    Small water system, for the purpose of subpart I of this part only, 
means a water system that serves 3,300 persons or fewer.
    Special irrigation district means an irrigation district in 
existence prior to May 18, 1994 that provides primarily agricultural 
service through a piped water system with only incidental residential or 
similar use where the system or the residential or similar users of the 
system comply with the exclusion provisions in section 1401(4)(B)(i)(II) 
or (III).
    Standard sample means the aliquot of finished drinking water that is 
examined for the presence of coliform bacteria.
    State means the agency of the State or Tribal government which has 
jurisdiction over public water systems. During any period when a State 
or Tribal government does not have primary enforcement responsibility 
pursuant to section 1413 of the Act, the term ``State'' means the 
Regional Administrator, U.S. Environmental Protection Agency.
    Subpart H systems means public water systems using surface water or 
ground water under the direct influence of surface water as a source 
that are subject to the requirements of subpart H of this part.
    Supplier of water means any person who owns or operates a public 
water system.
    Surface water means all water which is open to the atmosphere and 
subject to surface runoff.
    SUVA means Specific Ultraviolet Absorption at 254 nanometers (nm), 
an indicator of the humic content of water. It is a calculated parameter 
obtained by dividing a sample's ultraviolet absorption at a wavelength 
of 254 nm (UV 254) (in m \ = 1\) by its concentration of 
dissolved organic carbon (DOC) (in mg/L).
    System with a single service connection means a system which 
supplies drinking water to consumers via a single service line.
    Too numerous to count means that the total number of bacterial 
colonies exceeds 200 on a 47-mm diameter membrane filter used for 
coliform detection.
    Total Organic Carbon (TOC) means total organic carbon in mg/L 
measured using heat, oxygen, ultraviolet irradiation, chemical oxidants, 
or combinations of these oxidants that convert organic carbon to carbon 
dioxide, rounded to two significant figures.
    Total trihalomethanes (TTHM) means the sum of the concentration in 
milligrams per liter of the trihalomethane compounds (trichloromethane 
[chloroform], dibromochloromethane, bromodichloromethane and 
tribromomethane [bromoform]), rounded to two significant figures.
    Transient non-community water system or TWS means a non-community 
water system that does not regularly serve at least 25 of the same 
persons over six months per year.
    Trihalomethane (THM) means one of the family of organic compounds, 
named as derivatives of methane, wherein three of the four hydrogen 
atoms in methane are each substituted by a halogen atom in the molecular 
structure.
    Two-stage lime softening is a process in which chemical addition and 
hardness precipitation occur in each of two distinct unit clarification 
processes in series prior to filtration.
    Uncovered finished water storage facility is a tank, reservoir, or 
other facility used to store water that will undergo no further 
treatment to reduce microbial pathogens except residual disinfection and 
is directly open to the atmosphere.
    Virus means a virus of fecal origin which is infectious to humans by 
waterborne transmission.
    Waterborne disease outbreak means the significant occurrence of 
acute infectious illness, epidemiologically associated with the 
ingestion of water from a public water system which is deficient in 
treatment, as determined by the appropriate local or State agency.
    Wholesale system is a public water system that treats source water 
as necessary to produce finished water and then delivers some or all of 
that finished water to another public water

[[Page 436]]

system. Delivery may be through a direct connection or through the 
distribution system of one or more consecutive systems.

[40 FR 59570, Dec. 24, 1975]

    Editorial Note: For Federal Register citations affecting Sec.  
141.2, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  141.3  Coverage.

    This part shall apply to each public water system, unless the public 
water system meets all of the following conditions:
    (a) Consists only of distribution and storage facilities (and does 
not have any collection and treatment facilities);
    (b) Obtains all of its water from, but is not owned or operated by, 
a public water system to which such regulations apply:
    (c) Does not sell water to any person; and
    (d) Is not a carrier which conveys passengers in interstate 
commerce.



Sec.  141.4  Variances and exemptions.

    (a) Variances or exemptions from certain provisions of these 
regulations may be granted pursuant to sections 1415 and 1416 of the Act 
and subpart K of part 142 of this chapter (for small system variances) 
by the entity with primary enforcement responsibility, except that 
variances or exemptions from the MCLs for total coliforms and E. coli 
and variances from any of the treatment technique requirements of 
subpart H of this part may not be granted.
    (b) EPA has stayed the effective date of this section relating to 
the total coliform MCL of Sec.  141.63(a) for systems that demonstrate 
to the State that the violation of the total coliform MCL is due to a 
persistent growth of total coliforms in the distribution system rather 
than fecal or pathogenic contamination, a treatment lapse or deficiency, 
or a problem in the operation or maintenance of the distribution system. 
This is stayed until March 31, 2016, at which time the total coliform 
MCL is no longer effective.

    Note to paragraph (a): As provided in Sec.  142.304(a), small system 
variances are not available for rules addressing microbial contaminants, 
which would include subparts H, P, S, T, W, and Y of this part.

[78 FR 10346, Feb. 13, 2013]



Sec.  141.5  Siting requirements.

    Before a person may enter into a financial commitment for or 
initiate construction of a new public water system or increase the 
capacity of an existing public water system, he shall notify the State 
and, to the extent practicable, avoid locating part or all of the new or 
expanded facility at a site which:
    (a) Is subject to a significant risk from earthquakes, floods, fires 
or other disasters which could cause a breakdown of the public water 
system or a portion thereof; or
    (b) Except for intake structures, is within the floodplain of a 100-
year flood or is lower than any recorded high tide where appropriate 
records exist. The U.S. Environmental Protection Agency will not seek to 
override land use decisions affecting public water systems siting which 
are made at the State or local government levels.



Sec.  141.6  Effective dates.

    (a) Except as provided in paragraphs (b) through (k) of this 
section, and in Sec.  141.80(a)(2), the regulations set forth in this 
part shall take effect on June 24, 1977.
    (b) The regulations for total trihalomethanes set forth in Sec.  
141.12(c) shall take effect 2 years after the date of promulgation of 
these regulations for community water systems serving 75,000 or more 
individuals, and 4 years after the date of promulgation for communities 
serving 10,000 to 74,999 individuals.
    (c) The regulations set forth in Sec. Sec.  141.11(d); 141.21(a), 
(c) and (i); 141.22(a) and (e); 141.23(a)(3) and (a)(4); 141.23(f); 
141.24(e) and (f); 141.25(e); 141.27(a); 141.28(a) and (b); 141.31(a), 
(d) and (e); 141.32(b)(3); and 141.32(d) shall take effect immediately 
upon promulgation.
    (d) The regulations set forth in Sec.  141.41 shall take effect 18 
months from the date of promulgation. Suppliers

[[Page 437]]

must complete the first round of sampling and reporting within 12 months 
following the effective date.
    (e) The regulations set forth in Sec.  141.42 shall take effect 18 
months from the date of promulgation. All requirements in Sec.  141.42 
must be completed within 12 months following the effective date.
    (f) The regulations set forth in Sec.  141.11(c) and Sec.  141.23(g) 
are effective May 2, 1986. Section 141.23(g)(4) is effective October 2, 
1987.
    (g) The regulations contained in Sec.  141.6, paragraph (c) of the 
table in 141.12, and 141.62(b)(1) are effective July 1, 1991. The 
regulations contained in Sec. Sec.  141.11(b), 141.23, 141.24, 
142.57(b), 143.4(b)(12) and (b)(13), are effective July 30, 1992. The 
regulations contained in the revisions to Sec. Sec.  141.32(e) (16), 
(25) through (27) and (46); 141.61(c)(16); and 141.62(b)(3) are 
effective January 1, 1993. The effective date of regulations contained 
in Sec.  141.61(c) (2), (3), and (4) is postponed.
    (h) Regulations for the analytic methods listed at Sec.  
141.23(k)(4) for measuring antimony, beryllium, cyanide, nickel, and 
thallium are effective August 17, 1992. Regulations for the analytic 
methods listed at Sec.  141.24(f)(16) for dichloromethane, 1,2,4-
trichlorobenzene, and 1,1,2-trichloroethane are effective August 17, 
1992. Regulations for the analytic methods listed at Sec.  141.24(h)(12) 
for measuring dalapon, dinoseb, diquat, endothall, endrin, glyphosate, 
oxamyl, picloram, simazine, benzo(a)pyrene, di(2-ethylhexyl)adipate, 
di(2-ethylhexyl)phthalate, hexachlorobenzene, hexachlorocyclopentadiene, 
and 2,3,7,8-TCDD are effective August 17, 1992. The revision to Sec.  
141.12(a) promulgated on July 17, 1992 is effective on August 17, 1992.
    (i) [Reserved]
    (j) The arsenic maximum contaminant levels (MCL) listed in Sec.  
141.62 is effective for the purpose of compliance on January 23, 2006. 
Requirements relating to arsenic set forth in Sec. Sec.  141.23(i)(4), 
141.23(k)(3) introductory text, 141.23(k)(3)(ii), 141.51(b), 141.62(b), 
141.62(b)(16), 141.62(c), 141.62(d), and 142.62(b) revisions in Appendix 
A of subpart O for the consumer confidence rule, and Appendices A and B 
of subpart Q for the public notification rule are effective for the 
purpose of compliance on January 23, 2006. However, the consumer 
confidence rule reporting requirements relating to arsenic listed in 
Sec.  141.154(b) and (f) are effective for the purpose of compliance on 
February 22, 2002.
    (k) Regulations set forth in Sec. Sec.  141.23(i)(1), 141.23(i)(2), 
141.24(f)(15), 141.24(f)(22), 141.24(h)(11), 141.24(h)(20), 142.16(e), 
142.16(j), and 142.16(k) are effective for the purpose of compliance on 
January 22, 2004.

[44 FR 68641, Nov. 29, 1979, as amended at 45 FR 57342, Aug. 27, 1980; 
47 FR 10998, Mar. 12, 1982; 51 FR 11410, Apr. 2, 1986; 56 FR 30274, July 
1, 1991; 57 FR 22178, May 27, 1992; 57 FR 31838, July 17, 1992; 59 FR 
34322, July 1, 1994; 61 FR 24368, May 14, 1996; 66 FR 7061, Jan. 22, 
2001; 66 FR 28350, May 22, 2001]



                  Subpart B_Maximum Contaminant Levels



Sec.  141.11  Maximum contaminant levels for inorganic chemicals.

    (a) The maximum contaminant level for arsenic applies only to 
community water systems. The analyses and determination of compliance 
with the 0.05 milligrams per liter maximum contaminant level for arsenic 
use the requirements of Sec.  141.23.
    (b) The maximum contaminant level for arsenic is 0.05 milligrams per 
liter for community water systems until January 23, 2006.
    (c) [Reserved]
    (d) At the discretion of the State, nitrate levels not to exceed 20 
mg/l may be allowed in a non-community water system if the supplier of 
water demonstrates to the satisfaction of the State that:
    (1) Such water will not be available to children under 6 months of 
age; and
    (2) The non-community water system is meeting the public 
notification requirements under Sec.  141.209, including continuous 
posting of the fact that nitrate levels exceed 10 mg/l and the potential 
health effects of exposure; and
    (3) Local and State public health authorities will be notified 
annually of nitrate levels that exceed 10 mg/l; and

[[Page 438]]

    (4) No adverse health effects shall result.

[40 FR 59570, Dec. 24, 1975, as amended at 45 FR 57342, Aug. 27, 1980; 
47 FR 10998, Mar. 12, 1982; 51 FR 11410, Apr. 2, 1986; 56 FR 3578, Jan. 
30, 1991; 56 FR 26548, June 7, 1991; 56 FR 30274, July 1, 1991; 56 FR 
32113, July 15, 1991; 60 FR 33932, June 29, 1995; 65 FR 26022, May 4, 
2000; 66 FR 7061, Jan. 22, 2001]



Sec.  141.12  [Reserved]



Sec.  141.13  Maximum contaminant levels for turbidity.

    The maximum contaminant levels for turbidity are applicable to both 
community water systems and non-community water systems using surface 
water sources in whole or in part. The maximum contaminant levels for 
turbidity in drinking water, measured at a representative entry point(s) 
to the distribution system, are:
    (a) One turbidity unit (TU), as determined by a monthly average 
pursuant to Sec.  141.22, except that five or fewer turbidity units may 
be allowed if the supplier of water can demonstrate to the State that 
the higher turbidity does not do any of the following:
    (1) Interfere with disinfection;
    (2) Prevent maintenance of an effective disinfectant agent 
throughout the distribution system; or
    (3) Interfere with microbiological determinations.
    (b) Five turbidity units based on an average for two consecutive 
days pursuant to Sec.  141.22.

[40 FR 59570, Dec. 24, 1975]

    Editorial Note: At 54 FR 27527, June 29, 1989, Sec.  141.13 was 
amended by adding introductory text; however, the amendment could not be 
incorporated because introductory text already exists.



            Subpart C_Monitoring and Analytical Requirements



Sec.  141.21  Coliform sampling.

    (a) Routine monitoring. (1) Public water systems must collect total 
coliform samples at sites which are representative of water throughout 
the distribution system according to a written sample siting plan. These 
plans are subject to State review and revision.
    (2) The monitoring frequency for total coliforms for community water 
systems is based on the population served by the system, as follows:

     Total Coliform Monitoring Frequency for Community Water Systems
------------------------------------------------------------------------
                                                                Minimum
                                                               number of
                      Population served                         samples
                                                               per month
------------------------------------------------------------------------
25 to 1,000 \1\..............................................          1
1,001 to 2,500...............................................          2
2,501 to 3,300...............................................          3
3,301 to 4,100...............................................          4
4,101 to 4,900...............................................          5
4,901 to 5,800...............................................          6
5,801 to 6,700...............................................          7
6,701 to 7,600...............................................          8
7,601 to 8,500...............................................          9
8,501 to 12,900..............................................         10
12,901 to 17,200.............................................         15
17,201 to 21,500.............................................         20
21,501 to 25,000.............................................         25
25,001 to 33,000.............................................         30
33,001 to 41,000.............................................         40
41,001 to 50,000.............................................         50
50,001 to 59,000.............................................         60
59,001 to 70,000.............................................         70
70,001 to 83,000.............................................         80
83,001 to 96,000.............................................         90
96,001 to 130,000............................................        100
130,001 to 220,000...........................................        120
220,001 to 320,000...........................................        150
320,001 to 450,000...........................................        180
450,001 to 600,000...........................................        210
600,001 to 780,000...........................................        240
780,001 to 970,000...........................................        270
970,001 to 1,230,000.........................................        300
1,230,001 to 1,520,000.......................................        330
1,520,001 to 1,850,000.......................................        360
1,850,001 to 2,270,000.......................................        390
2,270,001 to 3,020,000.......................................        420
3,020,001 to 3,960,000.......................................        450
3,960,001 or more............................................        480
------------------------------------------------------------------------
\1\ Includes public water systems which have at least 15 service
  connections, but serve fewer than 25 persons.


If a community water system serving 25 to 1,000 persons has no history 
of total coliform contamination in its current configuration and a 
sanitary survey conducted in the past five years shows that the system 
is supplied solely by a protected groundwater source and is free of 
sanitary defects, the State may reduce the monitoring frequency 
specified above, except that in no case may the State reduce the 
monitoring frequency to less than one sample per quarter. The State must 
approve the reduced monitoring frequency in writing.
    (3) The monitoring frequency for total coliforms for non-community 
water systems is as follows:

[[Page 439]]

    (i) A non-community water system using only ground water (except 
ground water under the direct influence of surface water, as defined in 
Sec.  141.2) and serving 1,000 persons or fewer must monitor each 
calendar quarter that the system provides water to the public, except 
that the State may reduce this monitoring frequency, in writing, if a 
sanitary survey shows that the system is free of sanitary defects. 
Beginning June 29, 1994, the State cannot reduce the monitoring 
frequency for a non-community water system using only ground water 
(except ground water under the direct influence of surface water, as 
defined in Sec.  141.2) and serving 1,000 persons or fewer to less than 
once/year.
    (ii) A non-community water system using only ground water (except 
ground water under the direct influence of surface water, as defined in 
Sec.  141.2) and serving more than 1,000 persons during any month must 
monitor at the same frequency as a like-sized community water system, as 
specified in paragraph (a)(2) of this section, except the State may 
reduce this monitoring frequency, in writing, for any month the system 
serves 1,000 persons or fewer. The State cannot reduce the monitoring 
frequency to less than once/year. For systems using ground water under 
the direct influence of surface water, paragraph (a)(3)(iv) of this 
section applies.
    (iii) A non-community water system using surface water, in total or 
in part, must monitor at the same frequency as a like-sized community 
water system, as specified in paragraph (a)(2) of this section, 
regardless of the number of persons it serves.
    (iv) A non-community water system using ground water under the 
direct influence of surface water, as defined in Sec.  141.2, must 
monitor at the same frequency as a like-sized community water system, as 
specified in paragraph (a)(2) of this section. The system must begin 
monitoring at this frequency beginning six months after the State 
determines that the ground water is under the direct influence of 
surface water.
    (4) The public water system must collect samples at regular time 
intervals throughout the month, except that a system which uses only 
ground water (except ground water under the direct influence of surface 
water, as defined in Sec.  141.2), and serves 4,900 persons or fewer, 
may collect all required samples on a single day if they are taken from 
different sites.
    (5) A public water system that uses surface water or ground water 
under the direct influence of surface water, as defined in Sec.  141.2, 
and does not practice filtration in compliance with Subpart H must 
collect at least one sample near the first service connection each day 
the turbidity level of the source water, measured as specified in Sec.  
141.74(b)(2), exceeds 1 NTU. This sample must be analyzed for the 
presence of total coliforms. When one or more turbidity measurements in 
any day exceed 1 NTU, the system must collect this coliform sample 
within 24 hours of the first exceedance, unless the State determines 
that the system, for logistical reasons outside the system's control, 
cannot have the sample analyzed within 30 hours of collection. Sample 
results from this coliform monitoring must be included in determining 
compliance with the MCL for total coliforms in Sec.  141.63.
    (6) Special purpose samples, such as those taken to determine 
whether disinfection practices are sufficient following pipe placement, 
replacement, or repair, shall not be used to determine compliance with 
the MCL for total coliforms in Sec.  141.63. Repeat samples taken 
pursuant to paragraph (b) of this section are not considered special 
purpose samples, and must be used to determine compliance with the MCL 
for total coliforms in Sec.  141.63.
    (b) Repeat monitoring. (1) If a routine sample is total coliform-
positive, the public water system must collect a set of repeat samples 
within 24 hours of being notified of the positive result. A system which 
collects more than one routine sample/month must collect no fewer than 
three repeat samples for each total coliform-positive sample found. A 
system which collects one routine sample/month or fewer must collect no 
fewer than four repeat samples for each total coliform-positive sample 
found. The State may extend the 24-hour limit on a case-by-case basis if 
the system has a logistical

[[Page 440]]

problem in collecting the repeat samples within 24 hours that is beyond 
its control. In the case of an extension, the State must specify how 
much time the system has to collect the repeat samples.
    (2) The system must collect at least one repeat sample from the 
sampling tap where the original total coliform-positive sample was 
taken, and at least one repeat sample at a tap within five service 
connections upstream and at least one repeat sample at a tap within five 
service connections downstream of the original sampling site. If a total 
coliform-positive sample is at the end of the distribution system, or 
one away from the end of the distribution system, the State may waive 
the requirement to collect at least one repeat sample upstream or 
downstream of the original sampling site.
    (3) The system must collect all repeat samples on the same day, 
except that the State may allow a system with a single service 
connection to collect the required set of repeat samples over a four-day 
period or to collect a larger volume repeat sample(s) in one or more 
sample containers of any size, as long as the total volume collected is 
at least 400 ml (300 ml for systems which collect more than one routine 
sample/month).
    (4) If one or more repeat samples in the set is total coliform-
positive, the public water system must collect an additional set of 
repeat samples in the manner specified in paragraphs (b) (1)-(3) of this 
section. The additional samples must be collected within 24 hours of 
being notified of the positive result, unless the State extends the 
limit as provided in paragraph (b)(1) of this section. The system must 
repeat this process until either total coliforms are not detected in one 
complete set of repeat samples or the system determines that the MCL for 
total coliforms in Sec.  141.63 has been exceeded and notifies the 
State.
    (5) If a system collecting fewer than five routine samples/month has 
one or more total coliform-positive samples and the State does not 
invalidate the sample(s) under paragraph (c) of this section, it must 
collect at least five routine samples during the next month the system 
provides water to the public, except that the State may waive this 
requirement if the conditions of paragraph (b)(5) (i) or (ii) of this 
section are met. The State cannot waive the requirement for a system to 
collect repeat samples in paragraphs (b) (1)-(4) of this section.
    (i) The State may waive the requirement to collect five routine 
samples the next month the system provides water to the public if the 
State, or an agent approved by the State, performs a site visit before 
the end of the next month the system provides water to the public. 
Although a sanitary survey need not be performed, the site visit must be 
sufficiently detailed to allow the State to determine whether additional 
monitoring and/or any corrective action is needed. The State cannot 
approve an employee of the system to perform this site visit, even if 
the employee is an agent approved by the State to perform sanitary 
surveys.
    (ii) The State may waive the requirement to collect five routine 
samples the next month the system provides water to the public if the 
State has determined why the sample was total coliform-positive and 
establishes that the system has corrected the problem or will correct 
the problem before the end of the next month the system serves water to 
the public. In this case, the State must document this decision to waive 
the following month's additional monitoring requirement in writing, have 
it approved and signed by the supervisor of the State official who 
recommends such a decision, and make this document available to the EPA 
and public. The written documentation must describe the specific cause 
of the total coliform-positive sample and what action the system has 
taken and/or will take to correct this problem. The State cannot waive 
the requirement to collect five routine samples the next month the 
system provides water to the public solely on the grounds that all 
repeat samples are total coliform-negative. Under this paragraph, a 
system must still take at least one routine sample before the end of the 
next month it serves water to the public and use it to determine 
compliance with the MCL for total coliforms in Sec.  141.63, unless the 
State has

[[Page 441]]

determined that the system has corrected the contamination problem 
before the system took the set of repeat samples required in paragraphs 
(b) (1)-(4) of this section, and all repeat samples were total coliform-
negative.
    (6) After a system collects a routine sample and before it learns 
the results of the analysis of that sample, if it collects another 
routine sample(s) from within five adjacent service connections of the 
initial sample, and the initial sample, after analysis, is found to 
contain total coliforms, then the system may count the subsequent 
sample(s) as a repeat sample instead of as a routine sample.
    (7) Results of all routine and repeat samples not invalidated by the 
State must be included in determining compliance with the MCL for total 
coliforms in Sec.  141.63.
    (c) Invalidation of total coliform samples. A total coliform-
positive sample invalidated under this paragraph (c) does not count 
towards meeting the minimum monitoring requirements of this section.
    (1) The State may invalidate a total coliform-positive sample only 
if the conditions of paragraph (c)(1) (i), (ii), or (iii) of this 
section are met.
    (i) The laboratory establishes that improper sample analysis caused 
the total coliform-positive result.
    (ii) The State, on the basis of the results of repeat samples 
collected as required by paragraphs (b) (1) through (4) of this section, 
determines that the total coliform-positive sample resulted from a 
domestic or other non-distribution system plumbing problem. The State 
cannot invalidate a sample on the basis of repeat sample results unless 
all repeat sample(s) collected at the same tap as the original total 
coliform-positive sample are also total coliform-positive, and all 
repeat samples collected within five service connections of the original 
tap are total coliform-negative (e.g., a State cannot invalidate a total 
coliform-positive sample on the basis of repeat samples if all the 
repeat samples are total coliform-negative, or if the public water 
system has only one service connection).
    (iii) The State has substantial grounds to believe that a total 
coliform-positive result is due to a circumstance or condition which 
does not reflect water quality in the distribution system. In this case, 
the system must still collect all repeat samples required under 
paragraphs (b) (1)-(4) of this section, and use them to determine 
compliance with the MCL for total coliforms in Sec.  141.63. To 
invalidate a total coliform-positive sample under this paragraph, the 
decision with the rationale for the decision must be documented in 
writing, and approved and signed by the supervisor of the State official 
who recommended the decision. The State must make this document 
available to EPA and the public. The written documentation must state 
the specific cause of the total coliform-positive sample, and what 
action the system has taken, or will take, to correct this problem. The 
State may not invalidate a total coliform-positive sample solely on the 
grounds that all repeat samples are total coliform-negative.
    (2) A laboratory must invalidate a total coliform sample (unless 
total coliforms are detected) if the sample produces a turbid culture in 
the absence of gas production using an analytical method where gas 
formation is examined (e.g., the Multiple-Tube Fermentation Technique), 
produces a turbid culture in the absence of an acid reaction in the 
Presence-Absence (P-A) Coliform Test, or exhibits confluent growth or 
produces colonies too numerous to count with an analytical method using 
a membrane filter (e.g., Membrane Filter Technique). If a laboratory 
invalidates a sample because of such interference, the system must 
collect another sample from the same location as the original sample 
within 24 hours of being notified of the interference problem, and have 
it analyzed for the presence of total coliforms. The system must 
continue to re-sample within 24 hours and have the samples analyzed 
until it obtains a valid result. The State may waive the 24-hour time 
limit on a case-by-case basis.
    (d) Sanitary surveys. (1)(i) Public water systems which do not 
collect five or more routine samples/month must undergo an initial 
sanitary survey by June 29, 1994, for community public water systems and 
June 29, 1999, for

[[Page 442]]

non-community water systems. Thereafter, systems must undergo another 
sanitary survey every five years, except that non-community water 
systems using only protected and disinfected ground water, as defined by 
the State, must undergo subsequent sanitary surveys at least every ten 
years after the initial sanitary survey. The State must review the 
results of each sanitary survey to determine whether the existing 
monitoring frequency is adequate and what additional measures, if any, 
the system needs to undertake to improve drinking water quality.
    (ii) In conducting a sanitary survey of a system using ground water 
in a State having an EPA-approved wellhead protection program under 
section 1428 of the Safe Drinking Water Act, information on sources of 
contamination within the delineated wellhead protection area that was 
collected in the course of developing and implementing the program 
should be considered instead of collecting new information, if the 
information was collected since the last time the system was subject to 
a sanitary survey.
    (2) Sanitary surveys must be performed by the State or an agent 
approved by the State. The system is responsible for ensuring the survey 
takes place.
    (3) Sanitary surveys conducted by the State under the provisions of 
Sec.  142.16(o)(2) of this chapter may be used to meet the sanitary 
survey requirements of this section.
    (e) Fecal coliforms/Escherichia coli (E. coli) testing. (1) If any 
routine or repeat sample is total coliform-positive, the system must 
analyze that total coliform-positive culture medium to determine if 
fecal coliforms are present, except that the system may test for E. coli 
in lieu of fecal coliforms. If fecal coliforms or E. coli are present, 
the system must notify the State by the end of the day when the system 
is notified of the test result, unless the system is notified of the 
result after the State office is closed, in which case the system must 
notify the State before the end of the next business day.
    (2) The State has the discretion to allow a public water system, on 
a case-by-case basis, to forgo fecal coliform or E. coli testing on a 
total coliform-positive sample if that system assumes that the total 
coliform-positive sample is fecal coliform-positive or E. coli-positive. 
Accordingly, the system must notify the State as specified in paragraph 
(e)(1) of this section and the provisions of Sec.  141.63(b) apply.
    (f) Analytical methodology. (1) The standard sample volume required 
for total coliform analysis, regardless of analytical method used, is 
100 ml.
    (2) Public water systems need only determine the presence or absence 
of total coliforms; a determination of total coliform density is not 
required.
    (3) Public water systems must conduct total coliform analyses in 
accordance with one of the analytical methods in the following table or 
one of the alternative methods listed in appendix A to subpart C of this 
part.

----------------------------------------------------------------------------------------------------------------
               Organism                             Methodology \12\                       Citation \1\
----------------------------------------------------------------------------------------------------------------
Total Coliforms \2\...................  Total Coliform Fermentation Technique \3  9221A, B.
                                         4 5\.
                                        Total Coliform Membrane Filter Technique  9222A, B, C.
                                         \6\.
                                        Presence-Absence (P-A) Coliform Test \5   9221D.
                                         7\.
                                        ONPG-MUG Test \8\.......................  9223.
                                        Colisure Test. \9\
                                        E*Colite [supreg] Test. \10\
                                        m-ColiBlue24 [supreg] Test. \11\
                                        Readycult [supreg] Coliforms 100
                                         Presence/Absence Test. \13\
                                        Membrane Filter Technique using
                                         Chromocult [supreg] Coliform Agar. \14\
                                        Colitag [supreg] Test. \15\
----------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of
  the following documents listed in footnotes 1, 6, 8, 9, 10 , 11, 13, 14 and 15 was approved by the Director of
  the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be
  obtained from the sources listed below. Information regarding obtaining these documents can be obtained from
  the Safe Drinking Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket,
  EPA West, 1301 Constitution Avenue, NW., EPA West, Room B102, Washington DC 20460 (Telephone: 202-566-2426);
  or at the National Archives and Records Administration (NARA). For information on the availability of this
  material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/
  code_of_federal_regulations/ibr_locations.html.

[[Page 443]]

 
\1\ Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or
  20th edition (1998). American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The
  cited methods published in any of these three editions may be used. In addition, the following online versions
  may also be used: 9221 A, B, D-99, 9222 A, B, C-97, and 9223 B-97. Standard Methods Online are available at
  http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee
  is designated by the last two digits in the method number. The methods listed are the only Online versions
  that may be used.
\2\ The time from sample collection to initiation of analysis may not exceed 30 hours. Systems are encouraged
  but not required to hold samples below 10 deg. C during transit.
\3\ Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system
  conducts at least 25 parallel tests between this medium and lauryl tryptose broth using the water normally
  tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total
  coliform, using lactose broth, is less than 10 percent.
\4\ If inverted tubes are used to detect gas production, the media should cover these tubes at least one-half to
  two-thirds after the sample is added.
\5\ No requirement exists to run the completed phase on 10 percent of all total coliform-positive confirmed
  tubes.
\6\ MI agar also may be used. Preparation and use of MI agar is set forth in the article, ``New medium for the
  simultaneous detection of total coliform and Escherichia coli in water'' by Brenner, K.P., et. al., 1993,
  Appl. Environ. Microbiol. 59:3534-3544. Also available from the Office of Water Resource Center (RC-4100T),
  1200 Pennsylvania Avenue, NW., Washington, DC 20460, EPA/600/J-99/225. Verification of colonies is not
  required.
\7\ Six-times formulation strength may be used if the medium is filter-sterilized rather than autoclaved.
\8\ The ONPG-MUG Test is also known as the Autoanalysis Collect System.
\9\ A description of the Colisure Test, Feb 28, 1994, may be obtained from IDEXX Laboratories, Inc., One IDEXX
  Drive, Westbrook, Maine 04092. The Colisure Test may be read after an incubation time of 24 hours.
\10\ A description of the E*Colite [supreg] Test, ``Presence/Absence for Coliforms and E. Coli in Water,'' Dec
  21, 1997, is available from Charm Sciences, Inc., 36 Franklin Street, Malden, MA 02148-4120.
\11\ A description of the m-ColiBlue24 [supreg] Test, Aug 17, 1999, is available from the Hach Company, 100
  Dayton Avenue, Ames, IA 50010.
\12\ EPA strongly recommends that laboratories evaluate the false-positive and negative rates for the method(s)
  they use for monitoring total coliforms. EPA also encourages laboratories to establish false-positive and
  false-negative rates within their own laboratory and sample matrix (drinking water or source water) with the
  intent that if the method they choose has an unacceptable false-positive or negative rate, another method can
  be used. The Agency suggests that laboratories perform these studies on a minimum of 5% of all total coliform-
  positive samples, except for those methods where verification/confirmation is already required, e.g., the M-
  Endo and LES Endo Membrane Filter Tests, Standard Total Coliform Fermentation Technique, and Presence-Absence
  Coliform Test. Methods for establishing false-positive and negative-rates may be based on lactose
  fermentation, the rapid test for [beta]-galactosidase and cytochrome oxidase, multi-test identification
  systems, or equivalent confirmation tests. False-positive and false-negative information is often available in
  published studies and/or from the manufacturer(s).
\13\ The Readycult [supreg] Coliforms 100 Presence/Absence Test is described in the document, ``Readycult
  [supreg] Coliforms 100 Presence/Absence Test for Detection and Identification of Coliform Bacteria and
  Escherichla coli in Finished Waters'', November 2000, Version 1.0, available from EM Science (an affiliate of
  Merck KGgA, Darmstadt Germany), 480 S. Democrat Road, Gibbstown, NJ 08027-1297. Telephone number is (800) 222-
  0342, e-mail address is: [email protected].
\14\ Membrane Filter Technique using Chromocult [supreg] Coliform Agar is described in the document,
  ``Chromocult [supreg] Coliform Agar Presence/Absence Membrane Filter Test Method for Detection and
  Identification of Coliform Bacteria and Escherichla coli in Finished Waters'', November 2000, Version 1.0,
  available from EM Science (an affiliate of Merck KGgA, Darmstadt Germany), 480 S. Democrat Road, Gibbstown, NJ
  08027-1297. Telephone number is (800) 222-0342, e-mail address is: [email protected].
\15\ Colitag [supreg] product for the determination of the presence/absence of total coliforms and E. coli is
  described in ``Colitag [supreg] Product as a Test for Detection and Identification of Coliforms and E. coli
  Bacteria in Drinking Water and Source Water as Required in National Primary Drinking Water Regulations,''
  August 2001, available from CPI International, Inc., 5580 Skylane Blvd., Santa Rosa, CA, 95403, telephone
  (800) 878-7654, Fax (707) 545-7901, Internet address http://www.cpiinternational.com.

    (4) [Reserved]
    (5) Public water systems must conduct fecal coliform analysis in 
accordance with the following procedure. When the MTF Technique or 
Presence-Absence (PA) Coliform Test is used to test for total coliforms, 
shake the lactose-positive presumptive tube or P-A vigorously and 
transfer the growth with a sterile 3-mm loop or sterile applicator stick 
into brilliant green lactose bile broth and EC medium to determine the 
presence of total and fecal coliforms, respectively. For EPA-approved 
analytical methods which use a membrane filter, transfer the total 
coliform-positive culture by one of the following methods: remove the 
membrane containing the total coliform colonies from the substrate with 
a sterile forceps and carefully curl and insert the membrane into a tube 
of EC medium (the laboratory may first remove a small portion of 
selected colonies for verification), swab the entire membrane filter 
surface with a sterile cotton swab and transfer the inoculum to EC 
medium (do not leave the cotton swab in the EC medium), or inoculate 
individual total coliform-positive colonies into EC Medium. Gently shake 
the inoculated tubes of EC medium to insure adequate mixing and incubate 
in a waterbath at 44.5 0.2 [deg]C for 24 2 hours. Gas production of any amount in the inner 
fermentation tube of the EC medium indicates a positive fecal coliform 
test. The preparation of EC medium is described in Method 9221E 
(paragraph 1a) in Standard Methods for the Examination of Water and 
Wastewater, 18th edition (1992), 19th edition (1995), and 20th edition 
(1998); the cited method in any one of these three editions may be used. 
Public water systems need only determine the presence or absence of 
fecal coliforms; a determination of fecal coliform density is not 
required.

[[Page 444]]

    (6) Public water systems must conduct analysis of Escherichia coli 
in accordance with one of the following analytical methods or one of the 
alternative methods listed in appendix A to subpart C of this part.
    (i) EC medium supplemented with 50 [micro]g/mL of 4-
methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration), as 
described in Method 9222G in Standard Methods for the Examination of 
Water and Wastewater, 19th edition (1995) and 20th edition (1998). 
Either edition may be used. Alternatively, the 18th edition (1992) may 
be used if at least 10 mL of EC medium, as described in paragraph (f)(5) 
of this section, is supplemented with 50 [micro]g/mL of MUG before 
autoclaving. The inner inverted fermentation tube may be omitted. If the 
18th edition is used, apply the procedure in paragraph (f)(5) of this 
section for transferring a total coliform-positive culture to EC medium 
supplemented with MUG, incubate the tube at 44.5 0.2 [deg]C for 24 2 hours, and 
then observe fluorescence with an ultraviolet light (366 nm) in the 
dark. If fluorescence is visible, E. coli are present.
    (ii) Nutrient agar supplemented with 100 [micro]g/mL of 4-
methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration), as 
described in Method 9222G in Standard Methods for the Examination of 
Water and Wastewater, 19th edition (1995) and 20th edition (1998). 
Either edition may be used for determining if a total coliform-positive 
sample, as determined by a membrane filter technique, contains E. coli. 
Alternatively, the 18th edition (1992) may be used if the membrane 
filter containing a total coliform-positive colony(ies) is transferred 
to nutrient agar, as described in Method 9221B (paragraph 3) of Standard 
Methods (18th edition), supplemented with 100 [micro]g/mL of MUG. If the 
18th edition is used, incubate the agar plate at 35 [deg]C for 4 hours 
and then observe the colony(ies) under ultraviolet light (366 nm) in the 
dark for fluorescence. If fluorescence is visible, E. coli are present.
    (iii) Minimal Medium ONPG-MUG (MMO-MUG) Test, as set forth in the 
article ``National Field Evaluation of a Defined Substrate Method for 
the Simultaneous Detection of Total Coliforms and Escherichia coli from 
Drinking Water: Comparison with Presence-Absence Techniques'' (Edberg et 
al.), Applied and Environmental Microbiology, Volume 55, pp. 1003-1008, 
April 1989. (Note: The Autoanalysis Colilert System is an MMO-MUG test). 
If the MMO-MUG test is total coliform-positive after a 24-hour 
incubation, test the medium for fluorescence with a 366-nm ultraviolet 
light (preferably with a 6-watt lamp) in the dark. If fluorescence is 
observed, the sample is E. coli-positive. If fluorescence is 
questionable (cannot be definitively read) after 24 hours incubation, 
incubate the culture for an additional four hours (but not to exceed 28 
hours total), and again test the medium for fluorescence. The MMO-MUG 
Test with hepes buffer in lieu of phosphate buffer is the only approved 
formulation for the detection of E. coli.
    (iv) The Colisure Test. A description of the Colisure Test may be 
obtained from the Millipore Corporation, Technical Services Department, 
80 Ashby Road, Bedford, MA 01730.
    (v) The membrane filter method with MI agar, a description of which 
is cited in footnote 6 to the table in paragraph (f)(3) of this section.
    (vi) E*Colite [supreg] Test, a description of which is cited in 
footnote 10 to the table at paragraph (f)(3) of this section.
    (vii) m-ColiBlue24 [supreg] Test, a description of which is cited in 
footnote 11 to the table in paragraph (f)(3) of this section.
    (viii) Readycult [supreg] Coliforms 100 Presence/Absence Test, a 
description of which is cited in footnote 13 to the table at paragraph 
(f)(3) of this section.
    (ix) Membrane Filter Technique using Chromocult [supreg] Coliform 
Agar, a description of which is cited in footnote 14 to the table at 
paragraph (f)(3) of this section.
    (x) Colitag [supreg], a description of which is cited in footnote 15 
to the table at paragraph (f)(3) of this section.
    (7) As an option to paragraph (f)(6)(iii) of this section, a system 
with a total coliform-positive, MUG-negative, MMO-MUG test may further 
analyze the culture for the presence of E. coli by transferring a 0.1 
ml, 28-hour MMO-MUG culture to EC Medium + MUG with a pipet. The 
formulation and incubation conditions of EC Medium +

[[Page 445]]

MUG, and observation of the results are described in paragraph (f)(6)(i) 
of this section.
    (8) The following materials are incorporated by reference in this 
section with the approval of the Director of the Federal Register in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the 
analytical methods cited in Standard Methods for the Examination of 
Water and Wastewater (18th, 19th, and 20th editions) may be obtained 
from the American Public Health Association et al.; 1015 Fifteenth 
Street, NW., Washington, DC 20005-2605. Copies of the MMO-MUG Test, as 
set forth in the article ``National Field Evaluation of a Defined 
Substrate Method for the Simultaneous Enumeration of Total Coliforms and 
Escherichia coli from Drinking Water: Comparison with the Standard 
Multiple Tube Fermentation Method'' (Edberg et al.) may be obtained from 
the American Water Works Association Research Foundation, 6666 West 
Quincy Avenue, Denver, CO 80235. Copies of the MMO-MUG Test as set forth 
in the article ``National Field Evaluation of a Defined Substrate Method 
for the Simultaneous Enumeration of Total Coliforms and Escherichia coli 
from Drinking Water: Comparison with the Standard Multiple Tube 
Fermentation Method'' (Edberg et al.) may be obtained from the American 
Water Works Association Research Foundation, 6666 West Quincy Avenue, 
Denver, CO 80235. A description of the Colisure Test may be obtained 
from the Millipore Corp., Technical Services Department, 80 Ashby Road, 
Bedford, MA 01730. Copies may be inspected at EPA's Drinking Water 
Docket; 401 M St., SW.; Washington, DC 20460, or at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (g) Response to violation. (1) A public water system which has 
exceeded the MCL for total coliforms in Sec.  141.63 must report the 
violation to the State no later than the end of the next business day 
after it learns of the violation, and notify the public in accordance 
with subpart Q.
    (2) A public water system which has failed to comply with a coliform 
monitoring requirement, including the sanitary survey requirement, must 
report the monitoring violation to the State within ten days after the 
system discovers the violation, and notify the public in accordance with 
subpart Q.
    (h) The provisions of paragraphs (a) and (d) of this section are 
applicable until March 31, 2016. The provisions of paragraphs (b), (c), 
(e), (f), and (g) of this section are applicable until all required 
repeat monitoring under paragraph (b) of this section and fecal coliform 
or E. coli testing under paragraph (e) of this section that was 
initiated by a total coliform-positive sample taken before April 1, 2016 
is completed, as well as analytical method, reporting, recordkeeping, 
public notification, and consumer confidence report requirements 
associated with that monitoring and testing. Beginning April 1, 2016, 
the provisions of subpart Y of this part are applicable, with systems 
required to begin regular monitoring at the same frequency as the 
system-specific frequency required on March 31, 2016.

[54 FR 27562, June 29, 1989]

    Editorial Note: For Federal Register citations affecting Sec.  
141.21, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  141.22  Turbidity sampling and analytical requirements.

    The requirements in this section apply to unfiltered systems until 
December 30, 1991, unless the State has determined prior to that date, 
in writing pursuant to section 1412(b)(7)(iii), that filtration is 
required. The requirements in this section apply to filtered systems 
until June 29, 1993. The requirements in this section apply to 
unfiltered systems that the State has determined, in writing pursuant to 
section 1412(b)(7)(C)(iii), must install filtration, until June 29, 
1993, or until filtration is installed, whichever is later.
    (a) Samples shall be taken by suppliers of water for both community 
and non-community water systems at a representative entry point(s) to 
the water distribution system at least once

[[Page 446]]

per day, for the purposes of making turbidity measurements to determine 
compliance with Sec.  141.13. If the State determines that a reduced 
sampling frequency in a non-community will not pose a risk to public 
health, it can reduce the required sampling frequency. The option of 
reducing the turbidity frequency shall be permitted only in those public 
water systems that practice disinfection and which maintain an active 
residual disinfectant in the distribution system, and in those cases 
where the State has indicated in writing that no unreasonable risk to 
health existed under the circumstances of this option. Turbidity 
measurements shall be made as directed in Sec.  141.74(a)(1).
    (b) If the result of a turbidity analysis indicates that the maximum 
allowable limit has been exceeded, the sampling and measurement shall be 
confirmed by resampling as soon as practicable and preferably within one 
hour. If the repeat sample confirms that the maximum allowable limit has 
been exceeded, the supplier of water shall report to the State within 48 
hours. The repeat sample shall be the sample used for the purpose of 
calculating the monthly average. If the monthly average of the daily 
samples exceeds the maximum allowable limit, or if the average of two 
samples taken on consecutive days exceeds 5 TU, the supplier of water 
shall report to the State and notify the public as directed in Sec.  
141.31 and subpart Q.
    (c) Sampling for non-community water systems shall begin within two 
years after the effective date of this part.
    (d) The requirements of this Sec.  141.22 shall apply only to public 
water systems which use water obtained in whole or in part from surface 
sources.
    (e) The State has the authority to determine compliance or initiate 
enforcement action based upon analytical results or other information 
compiled by their sanctioned representatives and agencies.

[40 FR 59570, Dec. 24, 1975, as amended at 45 FR 57344, Aug. 27, 1980; 
47 FR 8998, Mar. 3, 1982; 47 FR 10998, Mar. 12, 1982; 54 FR 27527, June 
29, 1989; 59 FR 62466, Dec. 5, 1994; 65 FR 26022, May 4, 2000]



Sec.  141.23  Inorganic chemical sampling and analytical requirements.

    Community water systems shall conduct monitoring to determine 
compliance with the maximum contaminant levels specified in Sec.  141.62 
in accordance with this section. Non-transient, non-community water 
systems shall conduct monitoring to determine compliance with the 
maximum contaminant levels specified in Sec.  141.62 in accordance with 
this section. Transient, non-community water systems shall conduct 
monitoring to determine compliance with the nitrate and nitrite maximum 
contaminant levels in Sec. Sec.  141.11 and 141.62 (as appropriate) in 
accordance with this section.
    (a) Monitoring shall be conducted as follows:
    (1) Groundwater systems shall take a minimum of one sample at every 
entry point to the distribution system which is representative of each 
well after treatment (hereafter called a sampling point) beginning in 
the initial compliance period. The system shall take each sample at the 
same sampling point unless conditions make another sampling point more 
representative of each source or treatment plant.
    (2) Surface water systems shall take a minimum of one sample at 
every entry point to the distribution system after any application of 
treatment or in the distribution system at a point which is 
representative of each source after treatment (hereafter called a 
sampling point) beginning in the initial compliance period. The system 
shall take each sample at the same sampling point unless conditions make 
another sampling point more representative of each source or treatment 
plant.

    Note: For purposes of this paragraph, surface water systems include 
systems with a combination of surface and ground sources.

    (3) If a system draws water from more than one source and the 
sources are combined before distribution, the system must sample at an 
entry point to the distribution system during periods of normal 
operating conditions (i.e., when water is representative of all sources 
being used).

[[Page 447]]

    (4) The State may reduce the total number of samples which must be 
analyzed by allowing the use of compositing. Composite samples from a 
maximum of five samples are allowed, provided that the detection limit 
of the method used for analysis is less than one-fifth of the MCL. 
Compositing of samples must be done in the laboratory.
    (i) If the concentration in the composite sample is greater than or 
equal to one-fifth of the MCL of any inorganic chemical, then a follow-
up sample must be taken within 14 days at each sampling point included 
in the composite. These samples must be analyzed for the contaminants 
which exceeded one-fifth of the MCL in the composite sample. Detection 
limits for each analytical method and MCLs for each inorganic 
contaminant are the following:

               Detection Limits for Inorganic Contaminants
------------------------------------------------------------------------
                                                             Detection
        Contaminant          MCL (mg/l)     Methodology     limit (mg/l)
------------------------------------------------------------------------
Antimony..................  0.006......  Atomic            0.003
                                          Absorption;
                                          Furnace.
                                         Atomic            0.0008 \5\
                                          Absorption;
                                          Platform.
                                         ICP-Mass          0.0004
                                          Spectrometry.
                                         Hydride-Atomic    0.001
                                          Absorption.
Arsenic...................  0.010 \6\..  Atomic            0.001
                                          Absorption;
                                          Furnace.
                                         Atomic            0.0005 \7\
                                          Absorption;
                                          Platform--Stabi
                                          lized
                                          Temperature.
                                         Atomic            0.001
                                          Absorption;
                                          Gaseous Hydride.
                                         ICP-Mass          0.0014 \8\
                                          Spectrometry.
Asbestos..................  7 MFL \1\..  Transmission      0.01 MFL
                                          Electron
                                          Microscopy.
Barium....................  2..........  Atomic            0.002
                                          Absorption;
                                          furnace
                                          technique.
                                         Atomic            0.1
                                          Absorption;
                                          direct
                                          aspiration.
                                         Inductively       0.002 (0.001)
                                          Coupled Plasma.
Beryllium.................  0.004......  Atomic            0.0002
                                          Absorption;
                                          Furnace.
                                         Atomic            0.00002 \5\
                                          Absorption;
                                          Platform.
                                         Inductively       0.0003
                                          Coupled Plasma
                                          \2\.
                                         ICP-Mass          0.0003
                                          Spectrometry.
Cadmium...................  0.005......  Atomic            0.0001
                                          Absorption;
                                          furnace
                                          technique.
                                         Inductively       0.001
                                          Coupled Plasma.
Chromium..................  0.1........  Atomic            0.001
                                          Absorption;
                                          furnace
                                          technique.
                                         Inductively       0.007 (0.001)
                                          Coupled Plasma.
Cyanide...................  0.2........  Distillation,     0.02
                                          Spectrophotomet
                                          ric \3\.
                            ...........  Distillation,     0.005
                                          Automated,
                                          Spectrophotomet
                                          ric \3\.
                            ...........  Distillation,     0.02
                                          Amenable,
                                          Spectrophotomet
                                          ric \4\.
                            ...........  Distillation,     0.05
                                          Selective
                                          Electrode\3 4\.
                            ...........  UV,               0.0005
                                          Distillation,
                                          Spectrophotomet
                                          ric \9\.
                            ...........  Micro             0.0006
                                          Distillation,
                                          Flow Injection,
                                          Spectrophotomet
                                          ric \3\.
                            ...........  Ligand Exchange   0.0005
                                          with
                                          Amperometry \4\.
Mercury...................  0.002......  Manual Cold       0.0002
                                          Vapor Technique.
                                         Automated Cold    0.0002
                                          Vapor Technique.
Nickel....................  xl.........  Atomic            0.001
                                          Absorption;
                                          Furnace.
                                         Atomic            0.0006 \5\
                                          Absorption;
                                          Platform.
                                         Inductively       0.005
                                          Coupled Plasma
                                          \2\.
                                         ICP-Mass          0.0005
                                          Spectrometry.
Nitrate...................  10 (as N)..  Manual Cadmium    0.01
                                          Reduction.
                                         Automated         0.01
                                          Hydrazine
                                          Reduction.
                                         Automated         0.05
                                          Cadmium
                                          Reduction.
                                         Ion Selective     1
                                          Electrode.
                                         Ion               0.01
                                          Chromatography.
                                         Capillary Ion     0.076
                                          Electrophoresis.
Nitrite...................  1 (as N)...  Spectrophotometr  0.01
                                          ic.
                                         Automated         0.05
                                          Cadmium
                                          Reduction.
                                         Manual Cadmium    0.01
                                          Reduction.
                                         Ion               0.004
                                          Chromatography.
                                         Capillary Ion     0.103
                                          Electrophoresis.
Selenium..................  0.05.......  Atomic            0.002
                                          Absorption;
                                          furnace.
                                         Atomic            0.002
                                          Absorption;
                                          gaseous hydride.
Thallium..................  0.002......  Atomic            0.001
                                          Absorption;
                                          Furnace.
                                         Atomic            0.0007 \5\
                                          Absorption;
                                          Platform.
                                         ICP-Mass          0.0003
                                          Spectrometry.
------------------------------------------------------------------------
\1\ MFL = million fibers per liter 10 [micro]m.
\2\ Using a 2X preconcentration step as noted in Method 200.7. Lower
  MDLs may be achieved when using a 4X preconcentration.
\3\ Screening method for total cyanides.
\4\ Measures ``free'' cyanides when distillation, digestion, or ligand
  exchange is omitted.
\5\ Lower MDLs are reported using stabilized temperature graphite
  furnace atomic absorption.

[[Page 448]]

 
\6\ The value for arsenic is effective January 23, 2006. Unit then, the
  MCL is 0.05 mg/L.
\7\ The MDL reported for EPA method 200.9 (Atomic Absorption; Platform--
  Stablized Temperature) was determined using a 2x concentration step
  during sample digestion. The MDL determined for samples analyzed using
  direct analyses (i.e., no sample digestion) will be higher. Using
  multiple depositions, EPA 200.9 is capable of obtaining MDL of 0.0001
  mg/L.
\8\ Using selective ion monitoring, EPA Method 200.8 (ICP-MS) is capable
  of obtaining a MDL of 0.0001 mg/L.
\9\ Measures total cyanides when UV-digestor is used, and ``free''
  cyanides when UV-digestor is bypassed.

    (ii) If the population served by the system is 3,300 
persons, then compositing may only be permitted by the State at sampling 
points within a single system. In systems serving <=3,300 persons, the 
State may permit compositing among different systems provided the 5-
sample limit is maintained.
    (iii) If duplicates of the original sample taken from each sampling 
point used in the composite sample are available, the system may use 
these instead of resampling. The duplicates must be analyzed and the 
results reported to the State within 14 days after completing analysis 
of the composite sample, provided the holding time of the sample is not 
exceeded.
    (5) The frequency of monitoring for asbestos shall be in accordance 
with paragraph (b) of this section: the frequency of monitoring for 
antimony, arsenic, barium, beryllium, cadmium, chromium, cyanide, 
fluoride, mercury, nickel, selenium and thallium shall be in accordance 
with paragraph (c) of this section; the frequency of monitoring for 
nitrate shall be in accordance with paragraph (d) of this section; and 
the frequency of monitoring for nitrite shall be in accordance with 
paragraph (e) of this section.
    (b) The frequency of monitoring conducted to determine compliance 
with the maximum contaminant level for asbestos specified in Sec.  
141.62(b) shall be conducted as follows:
    (1) Each community and non-transient, non-community water system is 
required to monitor for asbestos during the first three-year compliance 
period of each nine-year compliance cycle beginning in the compliance 
period starting January 1, 1993.
    (2) If the system believes it is not vulnerable to either asbestos 
contamination in its source water or due to corrosion of asbestos-cement 
pipe, or both, it may apply to the State for a waiver of the monitoring 
requirement in paragraph (b)(1) of this section. If the State grants the 
waiver, the system is not required to monitor.
    (3) The State may grant a waiver based on a consideration of the 
following factors:
    (i) Potential asbestos contamination of the water source, and
    (ii) The use of asbestos-cement pipe for finished water distribution 
and the corrosive nature of the water.
    (4) A waiver remains in effect until the completion of the three-
year compliance period. Systems not receiving a waiver must monitor in 
accordance with the provisions of paragraph (b)(1) of this section.
    (5) A system vulnerable to asbestos contamination due solely to 
corrosion of asbestos-cement pipe shall take one sample at a tap served 
by asbestos-cement pipe and under conditions where asbestos 
contamination is most likely to occur.
    (6) A system vulnerable to asbestos contamination due solely to 
source water shall monitor in accordance with the provision of paragraph 
(a) of this section.
    (7) A system vulnerable to asbestos contamination due both to its 
source water supply and corrosion of asbestos-cement pipe shall take one 
sample at a tap served by asbestos-cement pipe and under conditions 
where asbestos contamination is most likely to occur.
    (8) A system which exceeds the maximum contaminant levels as 
determined in Sec.  141.23(i) of this section shall monitor quarterly 
beginning in the next quarter after the violation occurred.
    (9) The State may decrease the quarterly monitoring requirement to 
the frequency specified in paragraph (b)(1) of this section provided the 
State has determined that the system is reliably and consistently below 
the maximum contaminant level. In no case can a State make this 
determination unless a groundwater system takes a minimum of two 
quarterly samples and a surface (or combined surface/ground)

[[Page 449]]

water system takes a minimum of four quarterly samples.
    (10) If monitoring data collected after January 1, 1990 are 
generally consistent with the requirements of Sec.  141.23(b), then the 
State may allow systems to use that data to satisfy the monitoring 
requirement for the initial compliance period beginning January 1, 1993.
    (c) The frequency of monitoring conducted to determine compliance 
with the maximum contaminant levels in Sec.  141.62 for antimony, 
arsenic, barium, beryllium, cadmium, chromium, cyanide, fluoride, 
mercury, nickel, selenium and thallium shall be as follows:
    (1) Groundwater systems shall take one sample at each sampling point 
during each compliance period. Surface water systems (or combined 
surface/ground) shall take one sample annually at each sampling point.
    (2) The system may apply to the State for a waiver from the 
monitoring frequencies specified in paragraph (c)(1) of this section. 
States may grant a public water system a waiver for monitoring of 
cyanide, provided that the State determines that the system is not 
vulnerable due to lack of any industrial source of cyanide.
    (3) A condition of the waiver shall require that a system shall take 
a minimum of one sample while the waiver is effective. The term during 
which the waiver is effective shall not exceed one compliance cycle 
(i.e., nine years).
    (4) The State may grant a waiver provided surface water systems have 
monitored annually for at least three years and groundwater systems have 
conducted a minimum of three rounds of monitoring. (At least one sample 
shall have been taken since January 1, 1990). Both surface and 
groundwater systems shall demonstrate that all previous analytical 
results were less than the maximum contaminant level. Systems that use a 
new water source are not eligible for a waiver until three rounds of 
monitoring from the new source have been completed.
    (5) In determining the appropriate reduced monitoring frequency, the 
State shall consider:
    (i) Reported concentrations from all previous monitoring;
    (ii) The degree of variation in reported concentrations; and
    (iii) Other factors which may affect contaminant concentrations such 
as changes in groundwater pumping rates, changes in the system's 
configuration, changes in the system's operating procedures, or changes 
in stream flows or characteristics.
    (6) A decision by the State to grant a waiver shall be made in 
writing and shall set forth the basis for the determination. The 
determination may be initiated by the State or upon an application by 
the public water system. The public water system shall specify the basis 
for its request. The State shall review and, where appropriate, revise 
its determination of the appropriate monitoring frequency when the 
system submits new monitoring data or when other data relevant to the 
system's appropriate monitoring frequency become available.
    (7) Systems which exceed the maximum contaminant levels as 
calculated in Sec.  141.23(i) of this section shall monitor quarterly 
beginning in the next quarter after the violation occurred.
    (8) The State may decrease the quarterly monitoring requirement to 
the frequencies specified in paragraphs (c)(1) and (c)(2) of this 
section provided it has determined that the system is reliably and 
consistently below the maximum contaminant level. In no case can a State 
make this determination unless a groundwater system takes a minimum of 
two quarterly samples and a surface water system takes a minimum of four 
quarterly samples.
    (9) All new systems or systems that use a new source of water that 
begin operation after January 22, 2004 must demonstrate compliance with 
the MCL within a period of time specified by the State. The system must 
also comply with the initial sampling frequencies specified by the State 
to ensure a system can demonstrate compliance with the MCL. Routine and 
increased monitoring frequencies shall be conducted in accordance with 
the requirements in this section.
    (d) All public water systems (community; non-transient, non-
community;

[[Page 450]]

and transient, non-community systems) shall monitor to determine 
compliance with the maximum contaminant level for nitrate in Sec.  
141.62.
    (1) Community and non-transient, non-community water systems served 
by groundwater systems shall monitor annually beginning January 1, 1993; 
systems served by surface water shall monitor quarterly beginning 
January 1, 1993.
    (2) For community and non-transient, non-community water systems, 
the repeat monitoring frequency for groundwater systems shall be 
quarterly for at least one year following any one sample in which the 
concentration is =50 percent of the MCL. The State may allow 
a groundwater system to reduce the sampling frequency to annually after 
four consecutive quarterly samples are reliably and consistently less 
than the MCL.
    (3) For community and non-transient, non-community water systems, 
the State may allow a surface water system to reduce the sampling 
frequency to annually if all analytical results from four consecutive 
quarters are <50 percent of the MCL. A surface water system shall return 
to quarterly monitoring if any one sample is =50 percent of 
the MCL.
    (4) Each transient non-community water system shall monitor annually 
beginning January 1, 1993.
    (5) After the initial round of quarterly sampling is completed, each 
community and non-transient non-community system which is monitoring 
annually shall take subsequent samples during the quarter(s) which 
previously resulted in the highest analytical result.
    (e) All public water systems (community; non-transient, non-
community; and transient, non-community systems) shall monitor to 
determine compliance with the maximum contaminant level for nitrite in 
Sec.  141.62(b).
    (1) All public water systems shall take one sample at each sampling 
point in the compliance period beginning January 1, 1993 and ending 
December 31, 1995.
    (2) After the initial sample, systems where an analytical result for 
nitrite is <50 percent of the MCL shall monitor at the frequency 
specified by the State.
    (3) For community, non-transient, non-community, and transient non-
community water systems, the repeat monitoring frequency for any water 
system shall be quarterly for at least one year following any one sample 
in which the concentration is =50 percent of the MCL. The 
State may allow a system to reduce the sampling frequency to annually 
after determining the system is reliably and consistently less than the 
MCL.
    (4) Systems which are monitoring annually shall take each subsequent 
sample during the quarter(s) which previously resulted in the highest 
analytical result.
    (f) Confirmation samples:
    (1) Where the results of sampling for antimony, arsenic, asbestos, 
barium, beryllium, cadmium, chromium, cyanide, fluoride, mercury, 
nickel, selenium or thallium indicate an exceedance of the maximum 
contaminant level, the State may require that one additional sample be 
collected as soon as possible after the initial sample was taken (but 
not to exceed two weeks) at the same sampling point.
    (2) Where nitrate or nitrite sampling results indicate an exceedance 
of the maximum contaminant level, the system shall take a confirmation 
sample within 24 hours of the system's receipt of notification of the 
analytical results of the first sample. Systems unable to comply with 
the 24-hour sampling requirement must immediately notify persons served 
by the public water system in accordance with Sec.  141.202 and meet 
other Tier 1 public notification requirements under subpart Q of this 
part. Systems exercising this option must take and analyze a 
confirmation sample within two weeks of notification of the analytical 
results of the first sample.
    (3) If a State-required confirmation sample is taken for any 
contaminant, then the results of the initial and confirmation sample 
shall be averaged. The resulting average shall be used to determine the 
system's compliance in accordance with paragraph (i) of this section. 
States have the discretion to delete results of obvious sampling errors.
    (g) The State may require more frequent monitoring than specified in

[[Page 451]]

paragraphs (b), (c), (d) and (e) of this section or may require 
confirmation samples for positive and negative results at its 
discretion.
    (h) Systems may apply to the State to conduct more frequent 
monitoring than the minimum monitoring frequencies specified in this 
section.
    (i) Compliance with Sec.  141.11 or Sec.  141.62(b) (as appropriate) 
shall be determined based on the analytical result(s) obtained at each 
sampling point.
    (1) For systems which are conducting monitoring at a frequency 
greater than annual, compliance with the maximum contaminant levels for 
antimony, arsenic, asbestos, barium, beryllium, cadmium, chromium, 
cyanide, fluoride, mercury, nickel, selenium or thallium is determined 
by a running annual average at any sampling point. If the average at any 
sampling point is greater than the MCL, then the system is out of 
compliance. If any one sample would cause the annual average to be 
exceeded, then the system is out of compliance immediately. Any sample 
below the method detection limit shall be calculated at zero for the 
purpose of determining the annual average. If a system fails to collect 
the required number of samples, compliance (average concentration) will 
be based on the total number of samples collected.
    (2) For systems which are monitoring annually, or less frequently, 
the system is out of compliance with the maximum contaminant levels for 
antimony, arsenic, asbestos, barium, beryllium, cadmium, chromium, 
cyanide, fluoride, mercury, nickel, selenium or thallium if the level of 
a contaminant is greater than the MCL. If confirmation samples are 
required by the State, the determination of compliance will be based on 
the annual average of the initial MCL exceedance and any State-required 
confirmation samples. If a system fails to collect the required number 
of samples, compliance (average concentration) will be based on the 
total number of samples collected.
    (3) Compliance with the maximum contaminant levels for nitrate and 
nitrate is determined based on one sample if the levels of these 
contaminants are below the MCLs. If the levels of nitrate and/or nitrite 
exceed the MCLs in the initial sample, a confirmation sample is required 
in accordance with paragraph (f)(2) of this section, and compliance 
shall be determined based on the average of the initial and confirmation 
samples.
    (4) Arsenic sampling results will be reported to the nearest 0.001 
mg/L.
    (j) Each public water system shall monitor at the time designated by 
the State during each compliance period.
    (k) Inorganic analysis:
    (1) Analysis for the following contaminants shall be conducted in 
accordance with the methods in the following table, or the alternative 
methods listed in appendix A to subpart C of this part, or their 
equivalent as determined by EPA. Criteria for analyzing arsenic, barium, 
beryllium, cadmium, calcium, chromium, copper, lead, nickel, selenium, 
sodium, and thallium with digestion or directly without digestion, and 
other analytical test procedures are contained in Technical Notes on 
Drinking Water Methods, EPA-600/R-94-173, October 1994. This document is 
available from the National Service Center for Environmental 
Publications (NSCEP), P.O. Box 42419, Cincinnati, OH 45242-0419 or 
http://www.epa.gov/nscep/.

[[Page 452]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                       SM \4\ (18th,     SM \4\ (20th
         Contaminant           Methodology \13\         EPA            ASTM \3\          19th ed.)           ed.)        SM Online \22\       Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alkalinity................  Titrimetric.....  ................  D1067-92, 02 B..  2320 B..........  2320 B.........  2320 B-97......
                               Electrometric     ................  ................  ................  ...............  I-1030-85 \5\..
                                titration.
2. Antimony..................  Inductively       200.8 \2\
                                Coupled Plasma
                                (ICP)--Mass
                                Spectrometry.
                               Hydride-Atomic    ................  D3697-92, 02....
                                Absorption.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Atomic            ................  ................  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
3. Arsenic \14\..............  ICP-Mass          200.8 \2\.......
                                Spectrometry.
                               Atomic            200.9 \2\.......
                                Absorption;
                                Platform.
                               Atomic            ................  D2972-97, 03 C..  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
                               Hydride Atomic    ................  D1972-97, 03 B..  3114 B..........  ...............  3114 B-97......
                                Absorption.
4. Asbestos..................  Transmission      100.1 \9\
                                Electron
                                Microscopy.
                               Transmission      100.2 \10\
                                Electron
                                Microscopy.
5. Barium....................  Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            ................  ................  3111D...........  ...............  3111 D-99......
                                Absorption;
                                Direct.
                               Atomic            ................  ................  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
6. Beryllium.................  Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Atomic            ................  D3645-97, 03 B..  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
7. Cadmium...................  Inductively       200.7 \2\
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.

[[Page 453]]

 
                               Atomic            ................  ................  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
8. Calcium...................  EDTA titrimetric  ................  D511-93, 03 A...  3500-Ca D.......  3500-Ca B......  3500-Ca B-97...
                               Atomic            ................  D511-93, 03 B...  3111 B..........  ...............  3111 B-99......
                                Absorption;
                                Direct
                                Aspiration.
                               Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               Ion               ................  D6919-03........
                                Chromatography.
9. Chromium..................  Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Atomic            ................  ................  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
10. Copper...................  Atomic            ................  D1688-95, 02 C..  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
                               Atomic            ................  D1688-95, 02 A..  3111 B..........  ...............  3111 B-99......
                                Absorption;
                                Direct
                                Aspiration.
                               Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
11. Conductivity.............  Conductance.....  ................  D1125-95          2510 B..........  2510 B.........  2510 B-97......
                                                                    (Reapproved
                                                                    1999) A.
12. Cyanide..................  Manual            ................  D2036-98 A......  4500-CN- C......  4500-CN- C.....
                                Distillation
                                followed by
                                  Spectrophotom  ................  D2036-98 B......  4500-CN- G......  4500-CN- G.....  4500-CN- G-99..
                                   etric,
                                   Amenable.
                                  Spectro-       ................  D2036-98 A......  4500-CN- E......  4500-CN- E.....  4500-CN- E-99..  I-3300-85 \5\
                                   photometric
                                   Manual.
                                  Spectro-       335.4 \6\
                                   photometric
                                   Semi-
                                   automated.
                               Selective         ................  ................  4500-CN- F......  4500-CN- F.....  4500-CN- F-99..
                                Electrode.
                               UV,               ................  ................  ................  ...............  ...............  Kelada-01 \17\
                                Distillation,
                                Spectrophotomet
                                ric.
                               Micro             ................  ................  ................  ...............  ...............  QuikChem 10-204-
                                Distillation,                                                                                             00-1-X \18\
                                Flow Injection,
                                Spectrophotomet
                                ric.
                               Ligand Exchange   ................  D6888-04........  ................  ...............  ...............  OIA-1677, DW
                                and Amperometry                                                                                           \20\
                                \21\.

[[Page 454]]

 
13. Fluoride.................  Ion               300.0 \6\, 300.1  D4327-97, 03....  4110 B..........  4110 B.........  4110 B-00......
                                Chromatography.   \19\
                               Manual Distill.;  ................  ................  4500-F- B, D....  4500-F- B, D...  4500-F- B, D-97
                                Color. SPADNS.
                               Manual Electrode  ................  D1179-93, 99 B..  4500-F- C.......  4500-F- C......  4500-F- C-97...
                               Automated         ................  ................  ................  ...............  ...............  380-75WE \11\
                                Electrode.
                               Automated         ................  ................  4500-F- E.......  4500-F- E......  4500-F- E-97...  129-71W \11\
                                Alizarin.
                               Capillary Ion     ................  ................  ................  ...............  ...............  D6508, Rev. 2
                                Electrophoresis.                                                                                          \23\
14. Lead.....................  Atomic            ................  D3559-96, 03 D..  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
                               ICP-Mass          200.8 \2\
                                spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Differential      ................  ................  ................  ...............  ...............  Method 1001
                                Pulse Anodic                                                                                              \16\
                                Stripping
                                Voltametry.
15. Magnesium................  Atomic            ................  D511-93, 03 B...  3111 B..........  ...............  3111 B-99......
                                Absorption.
                               ICP.............  200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                               Complexation      ................  D511-93, 03 A...  3500-Mg E.......  3500-Mg B......  3500-Mg B-97...
                                Titrimetric
                                Methods.
                               Ion               ................  D6919-03........
                                Chromatography.
16. Mercury..................  Manual, Cold      245.1 \2\.......  D3223-97, 02....  3112 B..........  ...............  3112 B-99......
                                Vapor.
                               Automated, Cold   245.2 \1\
                                Vapor.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
17. Nickel...................  Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Atomic            ................  ................  3111 B..........  ...............  3111 B-99......
                                Absorption;
                                Direct.
                               Atomic            ................  ................  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
18. Nitrate..................  Ion               300.0 \6\, 300.1  D4327-97, 03....  4110 B..........  4110 B.........  4110 B-00......  B-1011 \8\
                                Chromatography.   \19\
                               Automated         353.2 \6\.......  D3867-90 A......  4500-NO3- F.....  4500-NO3- F....  4500-NO3- F-00
                                Cadmium
                                Reduction.
                               Ion Selective     ................  ................  4500-NO3- D.....  4500-NO3- D....  4500-NO3- D-00.  601 \7\
                                Electrode.

[[Page 455]]

 
                               Manual Cadmium    ................  D3867-90 B......  4500-NO3- E.....  4500-NO3- E....  4500-NO3- E-00
                                Reduction.
                               Capillary Ion     ................  D6508-00.
                                Electrophoresis.
19. Nitrite..................  Ion               300.0 \6\, 300.1  D4327-97, 03....  4110 B..........  4110 B.........  4110 B-00......  B-1011 \8\
                                Chromatography.   \19\.
                               Automated         353.2 \6\.......  D3867-90 A......  4500-NO3- F.....  4500-NO3- F....  4500-NO3- F-00
                                Cadmium
                                Reduction.
                               Manual Cadmium    ................  D3867-90 B......  4500-NO3- E.....  4500-NO3- E....  4500-NO3- E-00
                                Reduction.
                               Spectrophotometr  ................  ................  4500-NO2- B.....  4500-NO2- B....  4500-NO2- B-00
                                ic.
                               Capillary Ion     ................  D6508-00
                                Electrophoresis.
20. Ortho-phosphate..........  Colorimetric,     365.1 \6\.......  ................  4500-P F........  4500-P F
                                Automated,
                                Ascorbic Acid.
                               Colorimetric,     ................  D515-88 A.......  4500-P E........  4500-P E
                                ascorbic acid,
                                single reagent.
                               Colorimetric      ................  ................  ................  ...............  ...............  I-1601-85 \5\
                                Phosphomolybdat                                                                                          I-2601-90 \5\
                                e; Automated-                                                                                            I-2598-85 \5\
                                segmented flow;
                                Automated
                                Discrete.
                               Ion               300.0 \6\, 300.1  D4327-97, 03....  4110 B..........  4110 B.........  4110 B-00
                                Chromatography.   \19\.
                               Capillary Ion     ................  D6508-00
                                Electrophoresis.
21. pH.......................  Electrometric...  150.1, 150.2 \1\  D1293-95, 99....  4500-H\ + \ B...  4500-H\ + \ B..  4500-H\ + \ B-
                                                                                                                         00.
22. Selenium.................  Hydride-Atomic    ................  D3859-98, 03 A..  3114 B..........  ...............  3114 B-97......
                                Absorption.
                               ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\
                                Absorption;
                                Platform.
                               Atomic            ................  D3859-98, 03 B..  3113 B..........  ...............  3113 B-99......
                                Absorption;
                                Furnace.
23. Silica...................  Colorimetric,     ................  ................  ................  ...............  ...............  I-1700-85 \5\
                                Molybdate Blue.
                                  Automated-     ................  ................  ................  ...............  ...............  I-2700-85 \5\
                                   segmented
                                   Flow.
                               Colorimetric....  ................  D859-94, 00.....
                               Molybdosilicate.  ................  ................  4500-Si D.......  4500-SiO2 C....  4500-SiO2 C-97.

[[Page 456]]

 
                               Heteropoly blue.  ................  ................  4500-Si E.......  4500-SiO2 D....  4500-SiO2 D-97.
                               Automated for     ................  ................  4500-Si F.......  4500-SiO2 E....  4500-SiO2 E-97.
                                Molybdate-
                                reactive Silica.
                               Inductively       200.7 \2\.......  ................  3120 B..........  3120 B.........  3120 B-99......
                                Coupled Plasma.
24. Sodium...................  Inductively       200.7 \2\
                                Coupled Plasma.
                               Atomic            ................  ................  3111 B..........  ...............  3111 B-99......
                                Absorption;
                                Direct
                                Aspiration.
                               Ion               ................  D6919-03........
                                Chromatography.
25. Temperature..............  Thermometric....  ................  ................  2550............  2550...........  2550-00........
26. Thallium.................  ICP-Mass          200.8 \2\
                                Spectrometry.
                               Atomic            200.9 \2\ ......
                                Absorption;
                                Platform.
--------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents listed in
  footnotes 1-11, 16-20, and 22-23 was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of
  the documents may be obtained from the sources listed below. Information regarding obtaining these documents can be obtained from the Safe Drinking
  Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., Room 3334,
  Washington, DC 20460 (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of
  this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' EPA/600/4-79/020, March 1983. Available at NTIS, PB84-128677.
\2\ ``Methods for the Determination of Metals in Environmental Samples--Supplement I,'' EPA/600/R-94/111, May 1994. Available at NTIS, PB95-125472.
\3\ Annual Book of ASTM Standards, ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, http://www.astm.org.; Annual Book of ASTM
  Standards 1994, Vols. 11.01 and 11.02; Annual Book of ASTM Standards 1996, Vols. 11.01 and 11.02; Annual Book of ASTM Standards 1999, Vols. 11.01 and
  11.02; Annual Book of ASTM Standards 2003, Vols. 11.01 and 11.02.
\4\ Standard Methods for the Examination of Water and Wastewater, American Public Health Association, 800 I Street NW., Washington, DC 20001-3710;
  Standard Methods for the Examination of Water and Wastewater, 18th edition (1992); Standard Methods for the Examination of Water and Wastewater, 19th
  edition (1995); Standard Methods for the Examination of Water and Wastewater, 20th edition (1998).The following methods from this edition cannot be
  used: 3111 B, 3111 D, 3113 B, and 3114 B.
\5\ U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425; Methods for Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment, Open File Report 93-125, 1993; Techniques of Water
  Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd edition, 1989.
\6\ ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93/100, August 1993. Available as Technical Report
  PB94-120821 at National Technical Information Service (NTIS), 5301 Shawnee Road, Alexandria, VA 22312. http://www.ntis.gov.
\7\ The procedure shall be done in accordance with the Technical Bulletin 601 ``Standard Method of Test for Nitrate in Drinking Water,'' July 1994, PN
  221890-001, Analytical Technology, Inc. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129.
\8\ Method B-1011. ``Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography,'' August, 1987. Copies may
  be obtained from Waters Corporation, Technical Services Division, 34 Maple Street, Milford, MA 01757, Telephone: 508/482-2963, Fax: 508/482-4056.
\9\ Method 100.1, ``Analytical Method For Determination of Asbestos Fibers in Water,'' EPA/600/4-83/043, EPA, September 1983. Available at NTIS, PB83-
  260471.
\10\ Method 100.2, ``Determination of Asbestos Structure Over 10-[mu]m In Length In Drinking Water,'' EPA/600/R-94/134, June 1994. Available at NTIS,
  PB94-201902.
\11\ Industrial Method No. 129-71W, ``Fluoride in Water and Wastewater,'' December 1972, and Method No. 380-75WE, ``Fluoride in Water and Wastewater,''
  February 1976, Technicon Industrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089.
\12\ Unfiltered, no digestion or hydrolysis.
\13\ Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2x preconcentration step during sample digestion, MDLs determined when
  samples are analyzed by direct analysis (i.e., no sample digestion) will be higher. For direct analysis of cadmium and arsenic by Method 200.7, and
  arsenic by Method 3120 B, sample preconcentration using pneumatic nebulization may be required to achieve lower detection limits. Preconcentration may
  also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and lead by Method 3113 B; and lead by Method D3559-
  90D, unless multiple in-furnace depositions are made.
\14\ If ultrasonic nebulization is used in the determination of arsenic by Method 200.8, the arsenic must be in the pentavalent state to provide uniform
  signal response. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain 1 mg/L of sodium
  hypochlorite.
\15\ [Reserved]

[[Page 457]]

 
\16\ The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018. Or from
  the Hach Company, P.O. Box 389, Loveland, CO 80539.
\17\ The description for the Kelada-01 Method, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate,'' Revision
  1.2, August 2001, EPA  821-B-01-009 for cyanide is available from the National Technical Information Service (NTIS), PB 2001-108275, 5285 Port Royal
  Road, Springfield, VA 22161. The toll free telephone number is 800-553-6847. Note: A 450-W UV lamp may be used in this method instead of the 550-W
  lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified
  flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.
\18\ The description for the QuikChem Method 10-204-00-1-X, ``Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST
  and determination of cyanide by flow injection analysis,'' Revision 2.1, November 30, 2000, for cyanide is available from Lachat Instruments, 6645 W.
  Mill Rd., Milwaukee, WI 53218. Telephone: 414-358-4200.
\19\ ``Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,'' Vol. 1, EPA 815-R-00-014, August 2000. Available as
  Technical Report PB2000-106981 at National Technical Information Service (NTIS), 5301 Shawnee Road, Alexandria, VA 22312. http://www.ntis.gov.
\20\ Method OIA-1677, DW ``Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,'' January 2004. EPA-821-R-04-001, Available from
  ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842-9010.
\21\ Sulfide levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide
  method to determine if a sulfide interference is present, and treat samples accordingly.
\22\ Standard Methods Online, American Public Health Association, 800 I Street NW., Washington, DC 20001, available at http://www.standardmethods.org.
  The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods
  listed are the only online versions that may be used.


[[Page 458]]

    (2) Sample collection for antimony, arsenic, asbestos, barium, 
beryllium, cadmium, chromium, cyanide, fluoride, mercury, nickel, 
nitrate, nitrite, selenium, and thallium under this section shall be 
conducted using the sample preservation, container, and maximum holding 
time procedures specified in the table below:

------------------------------------------------------------------------
                                                  Container
         Contaminant           Preservative \1\      \2\       Time \3\
------------------------------------------------------------------------
Antimony.....................  HNO\3\..........  P or G....  6 months
Arsenic......................  Conc HNO3 to pH   P or G....  6 months
                                <2.
Asbestos.....................  4 [deg]C........  P or G....  48 hours
                                                              \4\
Barium.......................  HNO\3\..........  P or G....  6 months
Beryllium....................  HNO\3\..........  P or G....  6 months
Cadmium......................  HNO\3\..........  P or G....  6 months
Chromium.....................  HNO\3\..........  P or G....  6 months
Cyanide......................  4 [deg]C, NaOH..  P or G....  14 days
Fluoride.....................  None............  P or G....  1 month
Mercury......................  HNO\3\..........  P or G....  28 days
Nickel.......................  HNO\3\..........  P or G....  6 months
Nitrate......................  4 [deg]C........  P or G....  48 hours
                                                              \5\
Nitrate-Nitrite \6\..........  H\2\SO\4\.......  P or G....  28 days
Nitrite......................  4 [deg]C........  P or G....  48 hours
Selenium.....................  HNO\3\..........  P or G....  6 months
Thallium.....................  HNO\3\..........  P or G....  6 months
------------------------------------------------------------------------
\1\ For cyanide determinations samples must be adjusted with sodium
  hydroxide to pH 12 at the time off collection. When chilling is
  indicated the sample must be shipped and stored at 4 [deg]C or less.
  Acidification of nitrate or metals samples may be with a concentrated
  acid or a dilute (50% by volume) solution of the applicable
  concentrated acid. Acidification of samples for metals analysis is
  encouraged and allowed at the laboratory rather than at the time of
  sampling provided the shipping time and other instructions in Section
  8.3 of EPA Methods 200.7 or 200.8 or 200.9 are followed.
\2\ P = plastic, hard or soft; G = glass, hard or soft.
\3\ In all cases samples should be analyzed as soon after collection as
  possible. Follow additional (if any) information on preservation,
  containers or holding times that is specified in method.
\4\ Instructions for containers, preservation procedures and holding
  times as specified in Method 100.2 must be adhered to for all
  compliance analyses including those conducted with Method 100.1.
\5\ If the sample is chlorinated, the holding time for an unacidified
  sample kept at 4 [deg]C is extended to 14 days.
\6\ Nitrate-Nitrite refers to a measurement of total nitrate.

    (3) Analysis under this section shall only be conducted by 
laboratories that have been certified by EPA or the State. Laboratories 
may conduct sample analysis under provisional certification until 
January 1, 1996. To receive certification to conduct analyses for 
antimony, arsenic, asbestos, barium, beryllium, cadmium, chromium, 
cyanide, fluoride, mercury, nickel, nitrate, nitrite and selenium and 
thallium, the laboratory must:
    (i) Analyze Performance Evaluation (PE) samples provided by EPA, the 
State or by a third party (with the approval of the State or EPA) at 
least once a year.
    (ii) For each contaminant that has been included in the PE sample 
and for each method for which the laboratory desires certification 
achieve quantitative results on the analyses that are within the 
following acceptance limits:

------------------------------------------------------------------------
             Contaminant                       Acceptance limit
------------------------------------------------------------------------
Antimony............................  30 at =0.006 mg/1
Arsenic.............................  30 at =0.003 mg/L
Asbestos............................  2 standard deviations based on
                                       study statistics.
Barium..............................  15% at =0.15 mg/1
Beryllium...........................  15% at =0.001 mg/1
Cadmium.............................  20% at =0.002 mg/1
Chromium............................  15% at =0.01 mg/1
Cyanide.............................  25% at =0.1 mg/1
Fluoride............................  10% at =1 to 10 mg/1
Mercury.............................  30% at =0.0005 mg/1
Nickel..............................  15% at =0.01 mg/1
Nitrate.............................  10% at =0.4 mg/1
Nitrite.............................  15% at =0.4 mg/1
Selenium............................  20% at =0.01 mg/1
Thallium............................  30% at =0.002 mg/1
------------------------------------------------------------------------

    (l) Analyses for the purpose of determining compliance with Sec.  
141.11 shall be conducted using the requirements specified in paragraphs 
(l) through (q) of this section.
    (1) Analyses for all community water systems utilizing surface water 
sources shall be completed by June 24, 1978. These analyses shall be 
repeated at yearly intervals.
    (2) Analyses for all community water systems utilizing only ground 
water sources shall be completed by June 24, 1979. These analyses shall 
be repeated at three-year intervals.
    (3) For non-community water systems, whether supplied by surface or 
ground sources, analyses for nitrate shall be completed by December 24, 
1980. These analyses shall be repeated at intervals determined by the 
State.
    (4) The State has the authority to determine compliance or initiate 
enforcement action based upon analytical results and other information 
compiled by their sanctioned representatives and agencies.
    (m) If the result of an analysis made under paragraph (l) of this 
section indicates that the level of any contaminant listed in Sec.  
141.11 exceeds the maximum contaminant level, the supplier of the water 
shall report to the State within 7 days and initiate three additional 
analyses at the same sampling point within one month.

[[Page 459]]

    (n) When the average of four analyses made pursuant to paragraph (m) 
of this section, rounded to the same number of significant figures as 
the maximum contaminant level for the substance in question, exceeds the 
maximum contaminant level, the supplier of water shall notify the State 
pursuant to Sec.  141.31 and give notice to the public pursuant to 
subpart Q. Monitoring after public notification shall be at a frequency 
designated by the State and shall continue until the maximum contaminant 
level has not been exceeded in two successive samples or until a 
monitoring schedule as a condition to a variance, exemption or 
enforcement action shall become effective.
    (o) The provisions of paragraphs (m) and (n) of this section 
notwithstanding, compliance with the maximum contaminant level for 
nitrate shall be determined on the basis of the mean of two analyses. 
When a level exceeding the maximum contaminant level for nitrate is 
found, a second analysis shall be initiated within 24 hours, and if the 
mean of the two analyses exceeds the maximum contaminant level, the 
supplier of water shall report his findings to the State pursuant to 
Sec.  141.31 and shall notify the public pursuant to subpart Q.
    (p) For the initial analyses required by paragraph (l) (1), (2) or 
(3) of this section, data for surface waters acquired within one year 
prior to the effective date and data for ground waters acquired within 3 
years prior to the effective date of this part may be substituted at the 
discretion of the State.
    (q) [Reserved]

[56 FR 3579, Jan. 30, 1991]

    Editorial Note: For Federal Register citations affecting Sec.  
141.23, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  141.24  Organic chemicals, sampling and analytical requirements.

    (a)-(d) [Reserved]
    (e) Analyses for the contaminants in this section shall be conducted 
using the methods listed in the following table, or the alternative 
methods listed in appendix A to subpart C of this part, or their 
equivalent as determined by EPA.
    (1) The following documents are incorporated by reference. This 
incorporation by reference was approved by the Director of the Federal 
Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies 
may be inspected at EPA's Drinking Water Docket, 1301 Constitution 
Avenue, NW., EPA West, Room 3334, Washington, DC 20460 (Telephone: 202-
566-2426); or at the National Archives and Records Administration 
(NARA). For information on the availability of this material at NARA, 
call 202-741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html. Method 508A and 515.1 
are in Methods for the Determination of Organic Compounds in Drinking 
Water, EPA/600/4-88-039, December 1988, Revised, July 1991. Methods 547, 
550 and 550.1 are in Methods for the Determination of Organic Compounds 
in Drinking Water--Supplement I, EPA/600-4-90-020, July 1990. Methods 
548.1, 549.1, 552.1 and 555 are in Methods for the Determination of 
Organic Compounds in Drinking Water--Supplement II, EPA/600/R-92-129, 
August 1992. Methods 502.2, 504.1, 505, 506, 507, 508, 508.1, 515.2, 
524.2 525.2, 531.1, 551.1 and 552.2 are in Methods for the Determination 
of Organic Compounds in Drinking Water--Supplement III, EPA/600/R-95-
131, August 1995. Method 1613 is titled ``Tetra-through Octa-Chlorinated 
Dioxins and Furans by Isotope-Dilution HRGC/HRMS,'' EPA/821-B-94-005, 
October 1994. These documents are available from the National Technical 
Information Service, NTIS PB91-231480, PB91-146027, PB92-207703, PB95-
261616 and PB95-104774, U.S. Department of Commerce, 5285 Port Royal 
Road, Springfield, Virginia 22161. The toll free number is: 800-553-
6847. Method 6651 shall be followed in accordance with Standard Methods 
for the Examination of Water and Wastewater, 18th edition (1992), 19th 
edition (1995), or 20th edition (1998), American Public Health 
Association (APHA); any of these three editions may be used. Method 6610 
shall be followed in accordance with Standard Methods for the 
Examination of Water and Wastewater, (18th Edition Supplement) (1994), 
or with the 19th edition (1995) or 20th edition (1998) of Standard 
Methods for the Examination of Water and Wastewater;

[[Page 460]]

any of these publications may be used. The APHA documents are available 
from APHA, 1015 Fifteenth Street NW., Washington, DC 20005. Other 
required analytical test procedures germane to the conduct of these 
analyses are contained in Technical Notes on Drinking Water Methods, 
EPA/600/R-94-173, October 1994, NTIS PB95-104766. EPA Methods 515.3 and 
549.2 are available from U.S. Environmental Protection Agency, National 
Exposure Research Laboratory (NERL)-Cincinnati, 26 West Martin Luther 
King Drive, Cincinnati, OH 45268. ASTM Method D 5317-93, 98 (Reapproved 
2003) is available in the Annual Book of ASTM Standards, (1999), Vol. 
11.02, ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 
19428, any edition containing the cited version of the method may be 
used. EPA Method 515.4, ``Determination of Chlorinated Acids in Drinking 
Water by Liquid-Liquid Microextraction, Derivatization and Fast Gas 
Chromatography with Electron Capture Detection,'' Revision 1.0, April 
2000, EPA/815/B-00/001 and EPA Method 552.3, ``Determination of 
Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid 
Microextraction, Derivatization, and Gas Chromatography with Electron 
Capture Detection,'' Revision 1.0, July 2003, EPA 815-B-03-002, can be 
accessed and downloaded directly online at http://www.epa.gov/safewater/
methods/sourcalt.html. Syngenta Method AG-625, ``Atrazine in Drinking 
Water by Immunoassay,'' February 2001, is available from Syngenta Crop 
Protection, Inc., 410 Swing Road, P.O. Box 18300, Greensboro, NC 27419. 
Telephone: 336-632-6000. Method 531.2 ``Measurement of N-
methylcarbamoyloximes and N-methylcarbamates in Water by Direct Aqueous 
Injection HPLC with Postcolumn Derivatization,'' Revision 1.0, September 
2001, EPA 815-B-01-002, can be accessed and downloaded directly online 
at http://www.epa.gov/safewater/methods/sourcalt.html.

----------------------------------------------------------------------------------------------------------------
            Contaminant                  EPA method         Standard methods          ASTM            Other
----------------------------------------------------------------------------------------------------------------
1. Benzene........................  502.2, 524.2........
2. Carbon tetrachloride...........  502.2, 524.2, 551.1.
3. Chlorobenzene..................  502.2, 524.2........
4. 1,2-Dichlorobenzene............  502.2, 524.2........
5. 1,4-Dichlorobenzene............  502.2, 524.2........
6. 1,2-Dichloroethane.............  502.2, 524.2........
7. cis-Dichloroethylene...........  502.2, 524.2........
8. trans-Dichloroethylene.........  502.2, 524.2........
9. Dichloromethane................  502.2, 524.2........
10. 1,2-Dichloropropane...........  502.2, 524.2........
11. Ethylbenzene..................  502.2, 524.2........
12. Styrene.......................  502.2, 524.2........
13. Tetrachloroethylene...........  502.2, 524.2, 551.1.
14. 1,1,1-Trichloroethane.........  502.2, 524.2, 551.1.
15. Trichloroethylene.............  502.2, 524.2, 551.1.
16. Toluene.......................  502.2, 524.2........
17. 1,2,4-Trichlorobenzene........  502.2, 524.2........
18. 1,1-Dichloroethylene..........  502.2, 524.2........
19. 1,1,2-Trichloroethane.........  502.2, 524.2, 551.1.
20. Vinyl chloride................  502.2, 524.2........
21. Xylenes (total)...............  502.2, 524.2........
22. 2,3,7,8-TCDD (dioxin).........  1613................
23. 2,4-D \4\ (as acids, salts,     515.2, 555, 515.1,    ....................  D5317-93, 98
 and esters).                        515.3, 515.4.                               (Reapproved
                                                                                 2003).
24. 2,4,5-TP \4\ (Silvex).........  515.2, 555, 515.1,    ....................  D5317-93, 98
                                     515.3, 515.4.                               (Reapproved
                                                                                 2003).
25. Alachlor \2\..................  507, 525.2, 508.1,
                                     505, 551.1.
26. Atrazine \2\..................  507, 525.2, 508.1,    ....................  ...............  Syngenta \5\ AG-
                                     505, 551.1.                                                  625
27. Benzo(a)pyrene................  525.2, 550, 550.1...
28. Carbofuran....................  531.1, 531.2........  6610................
29. Chlordane.....................  508, 525.2, 508.1,
                                     505.
30. Dalapon.......................  552.1 515.1, 552.2,
                                     515.3, 515.4, 552.3.

[[Page 461]]

 
31. Di(2-ethylhexyl)adipate.......  506, 525.2..........
32. Di(2-ethylhexyl)phthalate.....  506, 525.2..........
33. Dibromochloropropane (DBCP)...  504.1, 551.1........
34. Dinoseb \4\...................  515.2, 555, 515.1,
                                     515.3, 515.4.
35. Diquat........................  549.2...............
36. Endothall.....................  548.1...............
37. Endrin........................  508, 525.2, 508.1,
                                     505, 551.1.
38. Ethylene dibromide (EDB)......  504.1, 551.1........
39. Glyphosate....................  547.................  6651................
40. Heptachlor....................  508, 525.2, 508.1,
                                     505, 551.1.
41. Heptachlor Epoxide............  508, 525.2, 508.1,
                                     505, 551.1.
42. Hexachlorobenzene.............  508, 525.2, 508.1,
                                     505, 551.1.
43. Hexachlorocyclopentadiene.....  508, 525.2, 508.1,
                                     505, 551.1.
44. Lindane.......................  508, 525.2, 508.1,
                                     505, 551.1.
45. Methoxychlor..................  508, 525.2, 508.1,
                                     505, 551.1.
46. Oxamyl........................  531.1, 531.2........  6610................
47. PCBs \3\ (as                    508A................
 decachlorobiphenyl).
48. PCBs \3\ (as Aroclors)........  508.1, 508, 525.2,
                                     505.
49. Pentachlorophenol.............  515.2, 525.2, 555,    ....................  D5317-93, 98
                                     515.1, 515.3, 515.4.                        (Reapproved
                                                                                 2003).
50. Picloram \4\..................  515.2, 555, 515.1,    ....................  D5317-93, 98
                                     515.3, 515.4.                               (Reapproved
                                                                                 2003).
51. Simazine \2\..................  507, 525.2, 508.1,
                                     505, 551.1.
52. Toxaphene.....................  508, 508.1, 525.2,
                                     505.
53. Total Trihalomethanes.........  502.2, 524.2, 551.1.
----------------------------------------------------------------------------------------------------------------
\1\ [Reserved]
\2\ Substitution of the detector specified in Method 505, 507, 508 or 508.1 for the purpose of achieving lower
  detection limits is allowed as follows. Either an electron capture or nitrogen phosphorous detector may be
  used provided all regulatory requirements and quality control criteria are met.
\3\ PCBs are qualitatively identified as Aroclors and measured for compliance purposes as decachlorobiphenyl.
  Users of Method 505 may have more difficulty in achieving the required detection limits than users of Methods
  508.1, 525.2 or 508.
\4\ Accurate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA
  Methods 515.1, 515.2, 515.3, 515.4 and 555 and ASTM Method D5317-93.
\5\ This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for
  drinking water treatment. In samples from all other systems, any result for atrazine generated by Method AG-
  625 that is greater than one-half the maximum contaminant level (MCL) (in other words, greater than 0.0015mg/L
  or 1.5 [mu]g/L) must be confirmed using another approved method for this contaminant and should use additional
  volume of the original sample collected for compliance monitoring. In instances where a result from Method AG-
  625 triggers such confirmatory testing, the confirmatory result is to be used to determine compliance.

    (2) [Reserved]
    (f) Beginning with the initial compliance period, analysis of the 
contaminants listed in Sec.  141.61(a) (1) through (21) for the purpose 
of determining compliance with the maximum contaminant level shall be 
conducted as follows:
    (1) Groundwater systems shall take a minimum of one sample at every 
entry point to the distribution system which is representative of each 
well after treatment (hereafter called a sampling point). Each sample 
must be taken at the same sampling point unless conditions make another 
sampling point more representative of each source, treatment plant, or 
within the distribution system.
    (2) Surface water systems (or combined surface/ground) shall take a 
minimum of one sample at points in the distribution system that are 
representative of each source or at each entry point to the distribution 
system after treatment (hereafter called a sampling point). Each sample 
must be taken at the same sampling point unless conditions make another 
sampling point more representative of each source, treatment plant, or 
within the distribution system.
    (3) If the system draws water from more than one source and the 
sources are combined before distribution, the system must sample at an 
entry point to the distribution system during periods of normal 
operating conditions

[[Page 462]]

(i.e., when water representative of all sources is being used).
    (4) Each community and non-transient non-community water system 
shall take four consecutive quarterly samples for each contaminant 
listed in Sec.  141.61(a) (2) through (21) during each compliance 
period, beginning in the initial compliance period.
    (5) If the initial monitoring for contaminants listed in Sec.  
141.61(a) (1) through (8) and the monitoring for the contaminants listed 
in Sec.  141.61(a) (9) through (21) as allowed in paragraph (f)(18) has 
been completed by December 31, 1992, and the system did not detect any 
contaminant listed in Sec.  141.61(a) (1) through (21), then each ground 
and surface water system shall take one sample annually beginning with 
the initial compliance period.
    (6) After a minimum of three years of annual sampling, the State may 
allow groundwater systems with no previous detection of any contaiminant 
listed in Sec.  141.61(a) to take one sample during each compliance 
period.
    (7) Each community and non-transient non-community ground water 
system which does not detect a contaminant listed in Sec.  141.61(a) (1) 
through (21) may apply to the State for a waiver from the requirements 
of paragraphs (f)(5) and (f)(6) of this section after completing the 
initial monitoring. (For purposes of this section, detection is defined 
as =0.0005 mg/l.) A waiver shall be effective for no more 
than six years (two compliance periods). States may also issue waivers 
to small systems for the initial round of monitoring for 1,2,4-
trichlorobenzene.
    (8) A State may grant a waiver after evaluating the following 
factor(s):
    (i) Knowledge of previous use (including transport, storage, or 
disposal) of the contaminant within the watershed or zone of influence 
of the system. If a determination by the State reveals no previous use 
of the contaminant within the watershed or zone of influence, a waiver 
may be granted.
    (ii) If previous use of the contaminant is unknown or it has been 
used previously, then the following factors shall be used to determine 
whether a waiver is granted.
    (A) Previous analytical results.
    (B) The proximity of the system to a potential point or non-point 
source of contamination. Point sources include spills and leaks of 
chemicals at or near a water treatment facility or at manufacturing, 
distribution, or storage facilities, or from hazardous and municipal 
waste landfills and other waste handling or treatment facilities.
    (C) The environmental persistence and transport of the contaminants.
    (D) The number of persons served by the public water system and the 
proximity of a smaller system to a larger system.
    (E) How well the water source is protected against contamination, 
such as whether it is a surface or groundwater system. Groundwater 
systems must consider factors such as depth of the well, the type of 
soil, and wellhead protection. Surface water systems must consider 
watershed protection.
    (9) As a condition of the waiver a groundwater system must take one 
sample at each sampling point during the time the waiver is effective 
(i.e., one sample during two compliance periods or six years) and update 
its vulnerability assessment considering the factors listed in paragraph 
(f)(8) of this section. Based on this vulnerability assessment the State 
must reconfirm that the system is non-vulnerable. If the State does not 
make this reconfirmation within three years of the initial 
determination, then the waiver is invalidated and the system is required 
to sample annually as specified in paragraph (5) of this section.
    (10) Each community and non-transient non-community surface water 
system which does not detect a contaminant listed in Sec.  141.61(a) (1) 
through (21) may apply to the State for a waiver from the requirements 
of (f)(5) of this section after completing the initial monitoring. 
Composite samples from a maximum of five sampling points are allowed, 
provided that the detection limit of the method used for analysis is 
less than one-fifth of the MCL. Systems meeting this criterion must be 
determined by the State to be non-vulnerable based on a vulnerability 
assessment during each compliance period. Each system receiving a waiver 
shall sample at the frequency specified by the State (if any).

[[Page 463]]

    (11) If a contaminant listed in Sec.  141.61(a) (2) through (21) is 
detected at a level exceeding 0.0005 mg/l in any sample, then:
    (i) The system must monitor quarterly at each sampling point which 
resulted in a detection.
    (ii) The State may decrease the quarterly monitoring requirement 
speci fied in paragraph (f)(11)(i) of this section provided it has 
determined that the system is reliably and consistently below the 
maximum contaminant level. In no case shall the State make this 
determination unless a groundwater system takes a minimum of two 
quarterly samples and a surface water system takes a minimum of four 
quarterly samples.
    (iii) If the State determines that the system is reliably and 
consistently below the MCL, the State may allow the system to monitor 
annually. Systems which monitor annually must monitor during the 
quarter(s) which previously yielded the highest analytical result.
    (iv) Systems which have three consecutive annual samples with no 
detection of a contaminant may apply to the State for a waiver as 
specified in paragraph (f)(7) of this section.
    (v) Groundwater systems which have detected one or more of the 
following two-carbon organic compounds: trichloroethylene, 
tetrachloroethylene, 1,2-dichloroethane, 1,1,1-trichloroethane, cis-1,2-
dichloroethylene, trans-1,2-dichloroethylene, or 1,1-dichloroethylene 
shall monitor quarterly for vinyl chloride. A vinyl chloride sample 
shall be taken at each sampling point at which one or more of the two-
carbon organic compounds was detected. If the results of the first 
analysis do not detect vinyl chloride, the State may reduce the 
quarterly monitoring frequency of vinyl chloride monitoring to one 
sample during each compliance period. Surface water systems are required 
to monitor for vinyl chloride as specified by the State.
    (12) Systems which violate the requirements of Sec.  141.61(a) (1) 
through (21), as determined by paragraph (f)(15) of this section, must 
monitor quarterly. After a minimum of four consecutive quarterly samples 
which show the system is in compliance as specified in paragraph (f)(15) 
of this section the system and the State determines that the system is 
reliably and consistently below the maximum contaminant level, the 
system may monitor at the frequency and times specified in paragraph 
(f)(11)(iii) of this section.
    (13) The State may require a confirmation sample for positive or 
negative results. If a confirmation sample is required by the State, the 
result must be averaged with the first sampling result and the average 
is used for the compliance determination as specified by paragraph 
(f)(15). States have discretion to delete results of obvious sampling 
errors from this calculation.
    (14) The State may reduce the total number of samples a system must 
analyze by allowing the use of compositing. Composite samples from a 
maximum of five sampling points are allowed, provided that the detection 
limit of the method used for analysis is less than one-fifth of the MCL. 
Compositing of samples must be done in the laboratory and analyzed 
within 14 days of sample collection.
    (i) If the concentration in the composite sample is greater than or 
equal to 0.0005 mg/l for any contaminant listed in Sec.  141.61(a), then 
a follow-up sample must be taken within 14 days at each sampling point 
included in the composite, and be analyzed for that contaminant.
    (ii) If duplicates of the original sample taken from each sampling 
point used in the composite sample are available, the system may use 
these instead of resampling. The duplicates must be analyzed and the 
results reported to the State within 14 days after completing analysis 
of the composite sample, provided the holding time of the sample is not 
exceeded.
    (iii) If the population served by the system is 3,300 
persons, then compositing may only be permitted by the State at sampling 
points within a single system. In systems serving <=3,300 persons, the 
State may permit compositing among different systems provided the 5-
sample limit is maintained.
    (iv) Compositing samples prior to GC analysis.

[[Page 464]]

    (A) Add 5 ml or equal larger amounts of each sample (up to 5 samples 
are allowed) to a 25 ml glass syringe. Special precautions must be made 
to maintain zero headspace in the syringe.
    (B) The samples must be cooled at 4 [deg]C during this step to 
minimize volatilization losses.
    (C) Mix well and draw out a 5-ml aliquot for analysis.
    (D) Follow sample introduction, purging, and desorption steps 
described in the method.
    (E) If less than five samples are used for compositing, a 
proportionately small syringe may be used.
    (v) Compositing samples prior to GC/MS analysis.
    (A) Inject 5-ml or equal larger amounts of each aqueous sample (up 
to 5 samples are allowed) into a 25-ml purging device using the sample 
introduction technique described in the method.
    (B) The total volume of the sample in the purging device must be 25 
ml.
    (C) Purge and desorb as described in the method.
    (15) Compliance with Sec.  141.61(a) (1) through (21) shall be 
determined based on the analytical results obtained at each sampling 
point. If one sampling point is in violation of an MCL, the system is in 
violation of the MCL.
    (i) For systems monitoring more than once per year, compliance with 
the MCL is determined by a running annual average at each sampling 
point.
    (ii) Systems monitoring annually or less frequently whose sample 
result exceeds the MCL must begin quarterly sampling. The system will 
not be considered in violation of the MCL until it has completed one 
year of quarterly sampling.
    (iii) If any sample result will cause the running annual average to 
exceed the MCL at any sampling point, the system is out of compliance 
with the MCL immediately.
    (iv) If a system fails to collect the required number of samples, 
compliance will be based on the total number of samples collected.
    (v) If a sample result is less than the detection limit, zero will 
be used to calculate the annual average.
    (16) [Reserved]
    (17) Analysis under this section shall only be conducted by 
laboratories that are certified by EPA or the State according to the 
following conditions (laboratories may conduct sample analysis under 
provisional certification until January 1, 1996):
    (i) To receive certification to conduct analyses for the 
contaminants in Sec.  141.61(a) (2) through (21) the laboratory must:
    (A) Analyze Performance Evaluation (PE) samples provided by EPA, the 
State, or by a third party (with the approval of the State or EPA) at 
least once a year by each method for which the laboratory desires 
certification.
    (B) Achieve the quantitative acceptance limits under paragraphs 
(f)(17)(i)(C) and (D) of this section for at least 80 percent of the 
regulated organic contaminants included in the PE sample.
    (C) Achieve quantitative results on the analyses performed under 
paragraph (f)(17)(i)(A) of this section that are within 20% of the actual amount of the substances in the 
Performance Evaluation sample when the actual amount is greater than or 
equal to 0.010 mg/l.
    (D) Achieve quantitative results on the analyses performed under 
paragraph (f)(17)(i)(A) of this section that are within 40 percent of the actual amount of the substances in the 
Performance Evaluation sample when the actual amount is less than 0.010 
mg/l.
    (E) Achieve a method detection limit of 0.0005 mg/l, according to 
the procedures in appendix B of part 136.
    (ii) To receive certification to conduct analyses for vinyl 
chloride, the laboratory must:
    (A) Analyze Performance Evaluation (PE) samples provided by EPA, the 
State, or by a third party (with the approval of the State or EPA) at 
least once a year by each method for which the laboratory desires 
certification.
    (B) Achieve quantitative results on the analyses performed under 
paragraph (f)(17)(ii)(A) of this section that are within 40 percent of the actual amount of vinyl chloride in the 
Performance Evaluation sample.
    (C) Achieve a method detection limit of 0.0005 mg/l, according to 
the procedures in appendix B of part 136.

[[Page 465]]

    (D) Obtain certification for the contaminants listed in Sec.  
141.61(a)(2) through (21).
    (18) States may allow the use of monitoring data collected after 
January 1, 1988, required under section 1445 of the Act for purposes of 
initial monitoring compliance. If the data are generally consistent with 
the other requirements of this section, the State may use these data 
(i.e., a single sample rather than four quarterly samples) to satisfy 
the initial monitoring requirement of paragraph (f)(4) of this section. 
Systems which use grandfathered samples and did not detect any 
contaminant listed Sec.  141.61(a)(2) through (21) shall begin 
monitoring annually in accordance with paragraph (f)(5) of this section 
beginning with the initial compliance period.
    (19) States may increase required monitoring where necessary to 
detect variations within the system.
    (20) Each certified laboratory must determine the method detection 
limit (MDL), as defined in appendix B to part 136, at which it is 
capable of detecting VOCs. The acceptable MDL is 0.0005 mg/l. This 
concentration is the detection concentration for purposes of this 
section.
    (21) Each public water system shall monitor at the time designated 
by the State within each compliance period.
    (22) All new systems or systems that use a new source of water that 
begin operation after January 22, 2004 must demonstrate compliance with 
the MCL within a period of time specified by the State. The system must 
also comply with the initial sampling frequencies specified by the State 
to ensure a system can demonstrate compliance with the MCL. Routine and 
increased monitoring frequencies shall be conducted in accordance with 
the requirements in this section.
    (g) [Reserved]
    (h) Analysis of the contaminants listed in Sec.  141.61(c) for the 
purposes of determining compliance with the maximum contaminant level 
shall be conducted as follows, with the exception that no monitoring is 
required for aldicarb, aldicarb sulfoxide or aldicarb sulfone:
    (1) Groundwater systems shall take a minimum of one sample at every 
entry point to the distribution system which is representative of each 
well after treatment (hereafter called a sampling point). Each sample 
must be taken at the same sampling point unless conditions make another 
sampling point more representative of each source or treatment plant.
    (2) Surface water systems shall take a minimum of one sample at 
points in the distribution system that are representative of each source 
or at each entry point to the distribution system after treatment 
(hereafter called a sampling point). Each sample must be taken at the 
same sampling point unless conditions make another sampling point more 
representative of each source or treatment plant.
    Note: For purposes of this paragraph, surface water systems include 
systems with a combination of surface and ground sources.
    (3) If the system draws water from more than one source and the 
sources are combined before distribution, the system must sample at an 
entry point to the distribution system during periods of normal 
operating conditions (i.e., when water representative of all sources is 
being used).
    (4) Monitoring frequency: (i) Each community and non-transient non-
community water system shall take four consecutive quarterly samples for 
each contaminant listed in Sec.  141.61(c) during each compliance period 
beginning with the initial compliance period.
    (ii) Systems serving more than 3,300 persons which do not detect a 
contaminant in the initial compliance period may reduce the sampling 
frequency to a minimum of two quarterly samples in one year during each 
repeat compliance period.
    (iii) Systems serving less than or equal to 3,300 persons which do 
not detect a contaminant in the initial compliance period may reduce the 
sampling frequency to a minimum of one sample during each repeat 
compliance period.
    (5) Each community and non-transient water system may apply to the 
State for a waiver from the requirement of paragraph (h)(4) of this 
section. A system must reapply for a waiver for each compliance period.

[[Page 466]]

    (6) A State may grant a waiver after evaluating the following 
factor(s): Knowledge of previous use (including transport, storage, or 
disposal) of the contaminant within the watershed or zone of influence 
of the system. If a determination by the State reveals no previous use 
of the contaminant within the watershed or zone of influence, a waiver 
may be granted. If previous use of the contaminant is unknown or it has 
been used previously, then the following factors shall be used to 
determine whether a waiver is granted.
    (i) Previous analytical results.
    (ii) The proximity of the system to a potential point or non-point 
source of contamination. Point sources include spills and leaks of 
chemicals at or near a water treatment facility or at manufacturing, 
distribution, or storage facilities, or from hazardous and municipal 
waste landfills and other waste handling or treatment facilities. Non-
point sources include the use of pesticides to control insect and weed 
pests on agricultural areas, forest lands, home and gardens, and other 
land application uses.
    (iii) The environmental persistence and transport of the pesticide 
or PCBs.
    (iv) How well the water source is protected against contamination 
due to such factors as depth of the well and the type of soil and the 
integrity of the well casing.
    (v) Elevated nitrate levels at the water supply source.
    (vi) Use of PCBs in equipment used in the production, storage, or 
distribution of water (i.e., PCBs used in pumps, transformers, etc.).
    (7) If an organic contaminant listed in Sec.  141.61(c) is detected 
(as defined by paragraph (h)(18) of this section) in any sample, then:
    (i) Each system must monitor quarterly at each sampling point which 
resulted in a detection.
    (ii) The State may decrease the quarterly monitoring requirement 
specified in paragraph (h)(7)(i) of this section provided it has 
determined that the system is reliably and consistently below the 
maximum contaminant level. In no case shall the State make this 
determination unless a groundwater system takes a minimum of two 
quarterly samples and a surface water system takes a minimum of four 
quarterly samples.
    (iii) After the State determines the system is reliably and 
consistently below the maximum contaminant level the State may allow the 
system to monitor annually. Systems which monitor annually must monitor 
during the quarter that previously yielded the highest analytical 
result.
    (iv) Systems which have 3 consecutive annual samples with no 
detection of a contaminant may apply to the State for a waiver as 
specified in paragraph (h)(6) of this section.
    (v) If the monitoring results in detection of one or more of certain 
related contaminants (heptachlor and heptachlor epoxide), then 
subsequent monitoring shall analyze for all related contaminants.
    (8) Systems which violate the requirements of Sec.  141.61(c) as 
determined by paragraph (h)(11) of this section must monitor quarterly. 
After a minimum of four quarterly samples show the system is in 
compliance and the State determines the system is reliably and 
consistently below the MCL, as specified in paragraph (h)(11) of this 
section, the system shall monitor at the frequency specified in 
paragraph (h)(7)(iii) of this section.
    (9) The State may require a confirmation sample for positive or 
negative results. If a confirmation sample is required by the State, the 
result must be averaged with the first sampling result and the average 
used for the compliance determination as specified by paragraph (h)(11) 
of this section. States have discretion to delete results of obvious 
sampling errors from this calculation.
    (10) The State may reduce the total number of samples a system must 
analyze by allowing the use of compositing. Composite samples from a 
maximum of five sampling points are allowed, provided that the detection 
limit of the method used for analysis is less than one-fifth of the MCL. 
Compositing of samples must be done in the laboratory and analyzed 
within 14 days of sample collection.
    (i) If the concentration in the composite sample detects one or more 
contaminants listed in Sec.  141.61(c), then a follow-up sample must be 
taken within

[[Page 467]]

14 days at each sampling point included in the composite, and be 
analyzed for that contaminant.
    (ii) If duplicates of the original sample taken from each sampling 
point used in the composite sample are available, the system may use 
these instead of resampling. The duplicates must be analyzed and the 
results reported to the State within 14 days after completion of the 
composite analysis or before the holding time for the initial sample is 
exceeded whichever is sooner.
    (iii) If the population served by the system is 3,300 
persons, then compositing may only be permitted by the State at sampling 
points within a single system. In systems serving <=3,300 persons, the 
State may permit compositing among different systems provided the 5-
sample limit is maintained.
    (11) Compliance with Sec.  141.61(c) shall be determined based on 
the analytical results obtained at each sampling point. If one sampling 
point is in violation of an MCL, the system is in violation of the MCL.
    (i) For systems monitoring more than once per year, compliance with 
the MCL is determined by a running annual average at each sampling 
point.
    (ii) Systems monitoring annually or less frequently whose sample 
result exceeds the regulatory detection level as defined by paragraph 
(h)(18) of this section must begin quarterly sampling. The system will 
not be considered in violation of the MCL until it has completed one 
year of quarterly sampling.
    (iii) If any sample result will cause the running annual average to 
exceed the MCL at any sampling point, the system is out of compliance 
with the MCL immediately.
    (iv) If a system fails to collect the required number of samples, 
compliance will be based on the total number of samples collected.
    (v) If a sample result is less than the detection limit, zero will 
be used to calculate the annual average.
    (12) [Reserved]
    (13) Analysis for PCBs shall be conducted as follows using the 
methods in paragraph (e) of this section:
    (i) Each system which monitors for PCBs shall analyze each sample 
using either Method 508.1, 525.2, 508 or 505. Users of Method 505 may 
have more difficulty in achieving the required Aroclor detection limits 
than users of Methods 508.1, 525.2 or 508.
    (ii) If PCBs (as one of seven Aroclors) are detected (as designated 
in this paragraph) in any sample analyzed using Method 505 or 508, the 
system shall reanalyze the sample using Method 508A to quantitate PCBs 
(as decachlorobiphenyl).

------------------------------------------------------------------------
                                                        Detection limit
                       Aroclor                               (mg/l)
------------------------------------------------------------------------
1016.................................................        0.00008
1221.................................................        0.02
1232.................................................        0.0005
1242.................................................        0.0003
1248.................................................        0.0001
1254.................................................        0.0001
1260.................................................        0.0002
------------------------------------------------------------------------

    (iii) Compliance with the PCB MCL shall be determined based upon the 
quantitative results of analyses using Method 508A.
    (14) If monitoring data collected after January 1, 1990, are 
generally consistent with the requirements of Sec.  141.24(h), then the 
State may allow systems to use that data to satisfy the monitoring 
requirement for the initial compliance period beginning January 1, 1993.
    (15) The State may increase the required monitoring frequency, where 
necessary, to detect variations within the system (e.g., fluctuations in 
concentration due to seasonal use, changes in water source).
    (16) The State has the authority to determine compliance or initiate 
enforcement action based upon analytical results and other information 
compiled by their sanctioned representatives and agencies.
    (17) Each public water system shall monitor at the time designated 
by the State within each compliance period.
    (18) Detection as used in this paragraph shall be defined as greater 
than or equal to the following concentrations for each contaminant.

------------------------------------------------------------------------
                                                              Detection
                        Contaminant                           limit (mg/
                                                                  l)
------------------------------------------------------------------------
Alachlor...................................................   .0002
Aldicarb...................................................   .0005
Aldicarb sulfoxide.........................................   .0005
Aldicarb sulfone...........................................   .0008
Atrazine...................................................   .0001
Benzo[a]pyrene.............................................   .00002
Carbofuran.................................................   .0009

[[Page 468]]

 
Chlordane..................................................   .0002
Dalapon....................................................   .001
1,2-Dibromo-3-chloropropane (DBCP).........................   .00002
Di (2-ethylhexyl) adipate..................................   .0006
Di (2-ethylhexyl) phthalate................................   .0006
Dinoseb....................................................   .0002
Diquat.....................................................   .0004
2,4-D......................................................   .0001
Endothall..................................................   .009
Endrin.....................................................   .00001
Ethylene dibromide (EDB)...................................   .00001
Glyphosate.................................................   .006
Heptachlor.................................................   .00004
Heptachlor epoxide.........................................   .00002
Hexachlorobenzene..........................................   .0001
Hexachlorocyclopentadiene..................................   .0001
Lindane....................................................   .00002
Methoxychlor...............................................   .0001
Oxamyl.....................................................   .002
Picloram...................................................   .0001
Polychlorinated biphenyls (PCBs) (as decachlorobiphenyl)...   .0001
Pentachlorophenol..........................................   .00004
Simazine...................................................   .00007
Toxaphene..................................................   .001
2,3,7,8-TCDD (Dioxin)......................................   .000000005
2,4,5-TP (Silvex)..........................................   .0002
------------------------------------------------------------------------


    (19) Anaylsis under this section shall only be conducted by 
laboratories that have received certification by EPA or the State and 
have met the following conditions:
    (i) To receive certification to conduct analyses for the 
contaminants in Sec.  141.61(c) the laboratory must:
    (A) Analyze Performance Evaluation (PE) samples provided by EPA, the 
State, or by a third party (with the approval of the State or EPA) at 
least once a year by each method for which the laboratory desires 
certification.
    (B) For each contaminant that has been included in the PE sample 
achieve quantitative results on the analyses that are within the 
following acceptance limits:

------------------------------------------------------------------------
                Contaminant                  Acceptance limits (percent)
------------------------------------------------------------------------
DBCP......................................  40
EDB.......................................  40.
Alachlor..................................  45.
Atrazine..................................  45.
Benzo[a]pyrene............................  2 standard deviations.
Carbofuran................................  45.
Chlordane.................................  45.
Dalapon...................................  2 standard deviations.
Di(2-ethylhexyl)adipate...................  2 standard deviations.
Di(2-ethylhexyl)phthalate.................  2 standard deviations.
Dinoseb...................................  2 standard deviations.
Diquat....................................  2 standard deviations.
Endothall.................................  2 standard deviations.
Endrin....................................  30.
Glyphosate................................  2 standard deviations.
Heptachlor................................  45.
Heptachlor epoxide........................  45.
Hexachlorobenzene.........................  2 standard deviations.
Hexachloro- cyclopentadiene                 2 standard deviations.
Lindane...................................  45.
Methoxychlor..............................  45.
Oxamyl....................................  2 standard deviations.
PCBs (as Decachlorobiphenyl)                0-200.
Picloram..................................  2 standard deviations.
Simazine..................................  2 standard deviations.
Toxaphene.................................  45.
Aldicarb..................................  2 standard deviations.
Aldicarb sulfoxide........................  2 standard deviations.
Aldicarb sulfone..........................  2 standard deviations.
Pentachlorophenol.........................  50.
2,3,7,8-TCDD (Dioxin).....................  2 standard deviations.
2,4-D.....................................  50.
2,4,5-TP (Silvex).........................  50.
------------------------------------------------------------------------

    (ii) [Reserved]
    (20) All new systems or systems that use a new source of water that 
begin operation after January 22, 2004 must demonstrate compliance with 
the MCL within a period of time specified by the State. The system must 
also comply with the initial sampling frequencies specified by the State 
to ensure a system can demonstrate compliance with the MCL. Routine and 
increased monitoring frequencies shall be conducted in accordance with 
the requirements in this section.

(Approved by the Office of Management and Budget under control number 
2040-0090)

[40 FR 59570, Dec. 24, 1975]

    Editorial Note: For Federal Register citations affecting Sec.  
141.24, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  141.25  Analytical methods for radioactivity.

    (a) Analysis for the following contaminants shall be conducted to 
determine compliance with Sec.  141.66 (radioactivity) in accordance 
with the methods in the following table, or the alternative methods 
listed in appendix A to subpart C this part, or their equivalent 
determined by EPA in accordance with Sec.  141.27.

[[Page 469]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                    Reference (Method of Page Number)
                                               ---------------------------------------------------------------------------------------------------------
         Contaminant             Methodology                 EPA
                                                 EPA \1\     \2\    EPA \3\    EPA \4\       SM \5\       ASTM \6\      USGS \7\      DOE \8\     Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Naturally Occurring:
    Gross alpha \11\ and beta  Evaporation....      900.0  p. 1..  00-01...  p. 1......  302, 7110 B,    ..........  R-1120-76....
                                                                                          7110 B-00.
    Gross alpha \11\.........  Coprecipitation  .........  ......  00-02...  ..........  7110 C, 7110 C-
                                                                                          00.
    Radium 226...............  Radon emanation      903.1  p. 16.  Ra-04...  p. 19.....  305, 7500-Ra    D3454-97..  R-1141-76....  Ra-04.....  NY \9\,
                                                                                          C, 7500-Ra C-
                                                                                          01.
                               Radiochemical..      903.0  p. 13.  Ra-03...  ..........  304, 7500-Ra    D2460-97..  R-1140-76....  ..........  GA \14\
                                                                                          B, 7500-Ra B-
                                                                                          01.
    Radium 228...............  Radiochemical..      904.0  p. 24.  Ra-05...  p. 19.....  7500-Ra D,      ..........  R-1142-76....  ..........  NY \9\,
                                                                                          7500-Ra D-01.                                         NJ \10\,
                                                                                                                                                GA \14\
    Uranium \12\.............  Radiochemical..      908.0  ......  ........  ..........  7500-U B, 7500-
                                                                                          U B-00.
                               Fluorometric...      908.1  ......  ........  ..........  7500-U C (17th  D2907-97..  R-1180-76, R-  U-04......
                                                                                          Ed.).                       1181-76.
                               ICP-MS.........      200.8  ......  ........  ..........  3125..........  D5673-03..
                                                     \13\
                               Alpha            .........  ......  00-07...  p. 33.....  7500-U C        D3972-97,   R-1182-76....  U-02......
                                Spectrometry.                                             (18th, 19th,    02.
                                                                                          or 20th Ed.),
                                                                                          7500-U C-00.
                               Laser            .........  ......  ........  ..........  ..............  D5174-97,
                                Phosphorimetry.                                                           02.
Man-Made:
    Radioactive Cesium.......  Radiochemical..      901.0  p. 4..  ........  ..........  7500-Cs B,      D2459-72..  R-1111-76....
                                                                                          7500-Cs B-00.
                               Gamma Ray            901.1  ......  ........  p. 92.....  7120, 7120-97.  D3649-91,   R-1110-76....  4.5.2.3...
                                Spectrometry.                                                             98a.
    Radioactive Iodine.......  Radiochemical..      902.0  p. 6..  ........  ..........  7500-I B, 7500-
                                                                                          I B-00.
                                                           p. 9..  ........  ..........  7500-I C, 7500-
                                                                                          I C-00.

[[Page 470]]

 
                                                                                         7500-I D, 7500- D3649-91,
                                                                                          I D-00.         98a.
                               Gamma Ray            901.1  ......  ........  p. 92.....  7120, 7120-97.  D4785-93,   .............  4.5.2.3...
                                Spectrometry.                                                             00a.
    Radioactive Strontium 89,  Radiochemical..      905.0  p. 29.  Sr-04...  p. 65.....  303, 7500-Sr    ..........  R-1160-76....  Sr-01, Sr-
     90.                                                                                  B, 7500-Sr B-                              02.
                                                                                          01.
    Tritium..................  Liquid               906.0  p. 34.  H-02....  p. 87.....  306, 7500-\3\   D4107-91,   R-1171-76....
                                Scintillation.                                            H B, 7500-\3\   98
                                                                                          H B-00.         (Reapprov
                                                                                                          ed 2002).
    Gamma Emitters...........  Gamma Ray            901.1  ......  ........  p. 92.....  7120, 7120-97.  D3649-91,   R-1110-76....  Ga-01-R...
                                Spectrometry.                                                             98a.
                                                    902.0  ......  ........  ..........  7500-Cs B,      D4785-93,
                                                                                          7500-Cs B-00.   00a.
                                                    901.0  ......  ........  ..........  7500-I B, 7500-
                                                                                          I B-00.
--------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 and 13 through 14
  was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained
  from the sources listed below. Information regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791.
  Documents may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., Room 3334 , Washington, DC 20460 (Telephone: 202-
  566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-
  6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
\1\ ``Prescribed Procedures for the Measurement of Radioactivity in Drinking Water,'' EPA 600/4-80-032, August 1980. Available at the U.S. Department of
  Commerce, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800-553-6847), PB 80-224744.
\2\ ``Interim Radiochemical Methodology for Drinking Water,'' EPA 600/4-75-008 (revised), March 1976. Available NTIS, ibid.
\3\ ``Radiochemistry Procedures Manual,'' EPA 520/5-84-006, December 1987. Available NTIS, ibid.
\4\ ``Radiochemical Analytical Procedures for Analysis of Environmental Samples,'' March 1979. Available at NTIS, ibid. EMSL LV 053917.
\5\ ``Standard Methods for the Examination of Water and Wastewater,'' 13th, 17th, 18th, 19th or 20th edition, 1971, 1989, 1992, 1995, 1998. Available at
  American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. Methods 302, 303, 304, 305 and 306 are only in the 13th edition.
  Methods 7110B, 7500-Ra B, 7500-Ra C, 7500-Ra D, 7500-U B, 7500-Cs B, 7500-I B, 7500-I C, 7500-I D, 7500-Sr B, and 7500-\3\H B are in the 17th, 18th,
  19th and 20th editions. Method 7110 C is in the 18th, 19th and 20th editions. Method 7500-U C Fluorometric Uranium is only in the 17th Edition, and
  7500-U C Alpha spectrometry is only in the 18th, 19th and 20th editions. Method 7120 is only in the 19th and 20th editions. Method 3125 is only in the
  20th edition. Methods 7110 B-00, 7110 C-00, 7500-Ra B-01, 7500-Ra C-01, 7500-Ra D-01, 7500-U B-00, 7500-U C-00, 7500-I B-00, 7500-I C-00, 7500-I D-00,
  7120-97, 7500-Sr B-01, and 7500-\3\H B-00 are available online at http://www.standardmethods.org. The year in which each method was approved by the
  Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be
  used.
\6\ Annual Book of ASTM Standards, Vol. 11.01 and 11.02, 2002; ASTM International; any year containing the cited version of the method may be used.
  Copies of these two volumes and the 2003 version of D 5673-03 may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West
  Conshohocken, PA 19428-2959.
\7\ ``Methods for Determination of Radioactive Substances in Water and Fluvial Sediments,'' Chapter A5 in Book 5 of Techniques of Water-Resources
  Investigations of the United States Geological Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal
  Center, Denver, CO 80225-0425.
\8\ ``EML Procedures Manual,'' 28th (1997) or 27th (1990) Editions, Volumes 1 and 2; either edition may be used. In the 27th Edition Method Ra-04 is
  listed as Ra-05 and Method Ga-01-R is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S. Department of Energy
  (DOE), 376 Hudson Street, New York, NY 10014-3621.

[[Page 471]]

 
\9\ ``Determination of Ra-226 and Ra-228 (Ra-02),'' January 1980, Revised June 1982. Available at Radiological Sciences Institute for Laboratories and
  Research, New York State Department of Health, Empire State Plaza, Albany, NY 12201.
\10\ ``Determination of Radium 228 in Drinking Water,'' August 1980. Available at State of New Jersey, Department of Environmental Protection, Division
  of Environmental Quality, Bureau of Radiation and Inorganic Analytical Services, 9 Ewing Street, Trenton, NJ 08625.
\11\ Natural uranium and thorium-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods;
  americium-241 is approved with co-precipitation methods.
\12\ If uranium (U) is determined by mass, a 0.67 pCi/[mu]g of uranium conversion factor must be used. This conversion factor is based on the 1:1
  activity ratio of U-234 and U-238 that is characteristic of naturally occurring uranium.
\13\ ``Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry,'' Revision 5.4, which is published in
  ``Methods for the Determination of Metals in Environmental Samples--Supplement I,'' ' EPA 600-R-94-111, May 1994. Available at NTIS, PB 95-125472.
\14\ ``The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors,'' Revision 1.2,
  December 2004. Available from the Environmental Resources Center, Georgia Institute of Technology, 620 Cherry Street, Atlanta, GA 30332-0335, USA,
  Telephone: 404-894-3776. This method may be used to analyze for radium-226 and radium-228 in samples collected after January 1, 2005 to satisfy the
  radium-226 and radium-228 monitoring requirements specified at 40 CFR 141.26.


[[Page 472]]

    (b) When the identification and measurement of radionuclides other 
than those listed in paragraph (a) of this section is required, the 
following references are to be used, except in cases where alternative 
methods have been approved in accordance with Sec.  141.27.
    (1) Procedures for Radiochemical Analysis of Nuclear Reactor Aqueous 
Solutions, H. L. Krieger and S. Gold, EPA-R4-73-014. USEPA, Cincinnati, 
Ohio, May 1973.
    (2) HASL Procedure Manual, Edited by John H. Harley. HASL 300, ERDA 
Health and Safety Laboratory, New York, NY., 1973.
    (c) For the purpose of monitoring radioactivity concentrations in 
drinking water, the required sensitivity of the radioanalysis is defined 
in terms of a detection limit. The detection limit shall be that 
concentration which can be counted with a precision of plus or minus 100 
percent at the 95 percent confidence level (1.96[sigma] where [sigma] is 
the standard deviation of the net counting rate of the sample).
    (1) To determine compliance with Sec.  141.66(b), (c), and (e) the 
detection limit shall not exceed the concentrations in Table B to this 
paragraph.

Table B--Detection Limits for Gross Alpha Particle Activity, Radium 226,
                         Radium 228, and Uranium
------------------------------------------------------------------------
                Contaminant                        Detection limit
------------------------------------------------------------------------
Gross alpha particle activity..............  3 pCi/L.
Radium 226.................................  1 pCi/L.
Radium 228.................................  1 pCi/L.
Uranium....................................  1 [micro]g/L
------------------------------------------------------------------------

    (2) To determine compliance with Sec.  141.66(d) the detection 
limits shall not exceed the concentrations listed in Table C to this 
paragraph.

Table C--Detection Limits for Man-made Beta Particle and Photon Emitters
------------------------------------------------------------------------
               Radionuclide                        Detection limit
------------------------------------------------------------------------
Tritium...................................  1,000 pCi/1.
Strontium-89..............................  10 pCi/1.
Strontium-90..............................  2 pCi/1.
Iodine-131................................  1 pCi/1.
Cesium-134................................  10 pCi/1.
Gross beta................................  4 pCi/1.
Other radionuclides.......................  \1/10\ of the applicable
                                             limit.
------------------------------------------------------------------------

    (d) To judge compliance with the maximum contaminant levels listed 
in Sec.  141.66, averages of data shall be used and shall be rounded to 
the same number of significant figures as the maximum contaminant level 
for the substance in question.
    (e) The State has the authority to determine compliance or initiate 
enforcement action based upon analytical results or other information 
compiled by their sanctioned representatives and agencies.

[41 FR 28404, July 9, 1976, as amended at 45 FR 57345, Aug. 27, 1980; 62 
FR 10173, Mar. 5, 1997; 65 FR 76745, Dec. 7, 2000; 67 FR 65250, Oct. 23, 
2002; 69 FR 38855, June 29, 2004; 69 FR 52180, Aug. 25, 2004; 72 FR 
11245, Mar. 12, 2007; 74 FR 30958, June 29, 2009]



Sec.  141.26  Monitoring frequency and compliance requirements 
for radionuclides in community water systems.

    (a) Monitoring and compliance requirements for gross alpha particle 
activity, radium-226, radium-228, and uranium. (1) Community water 
systems (CWSs) must conduct initial monitoring to determine compliance 
with Sec.  141.66(b), (c), and (e) by December 31, 2007. For the 
purposes of monitoring for gross alpha particle activity, radium-226, 
radium-228, uranium, and beta particle and photon radioactivity in 
drinking water, ``detection limit'' is defined as in Sec.  141.25(c).
    (i) Applicability and sampling location for existing community water 
systems or sources. All existing CWSs using ground water, surface water 
or systems using both ground and surface water (for the purpose of this 
section hereafter referred to as systems) must sample at every entry 
point to the distribution system that is representative of all sources 
being used (hereafter called a sampling point) under normal operating 
conditions. The system must take each sample at the same sampling point 
unless conditions make another sampling point more representative of 
each source or the State has designated a distribution system location, 
in accordance with paragraph (a)(2)(ii)(C) of this section.
    (ii) Applicability and sampling location for new community water 
systems or sources. All new CWSs or CWSs that use a new source of water 
must begin to conduct initial monitoring for the new source within the 
first quarter after

[[Page 473]]

initiating use of the source. CWSs must conduct more frequent monitoring 
when ordered by the State in the event of possible contamination or when 
changes in the distribution system or treatment processes occur which 
may increase the concentration of radioactivity in finished water.
    (2) Initial monitoring: Systems must conduct initial monitoring for 
gross alpha particle activity, radium-226, radium-228, and uranium as 
follows:
    (i) Systems without acceptable historical data, as defined below, 
must collect four consecutive quarterly samples at all sampling points 
before December 31, 2007.
    (ii) Grandfathering of data: States may allow historical monitoring 
data collected at a sampling point to satisfy the initial monitoring 
requirements for that sampling point, for the following situations.
    (A) To satisfy initial monitoring requirements, a community water 
system having only one entry point to the distribution system may use 
the monitoring data from the last compliance monitoring period that 
began between June 2000 and December 8, 2003.
    (B) To satisfy initial monitoring requirements, a community water 
system with multiple entry points and having appropriate historical 
monitoring data for each entry point to the distribution system may use 
the monitoring data from the last compliance monitoring period that 
began between June 2000 and December 8, 2003.
    (C) To satisfy initial monitoring requirements, a community water 
system with appropriate historical data for a representative point in 
the distribution system may use the monitoring data from the last 
compliance monitoring period that began between June 2000 and December 
8, 2003, provided that the State finds that the historical data 
satisfactorily demonstrate that each entry point to the distribution 
system is expected to be in compliance based upon the historical data 
and reasonable assumptions about the variability of contaminant levels 
between entry points. The State must make a written finding indicating 
how the data conforms to the these requirements.
    (iii) For gross alpha particle activity, uranium, radium-226, and 
radium-228 monitoring, the State may waive the final two quarters of 
initial monitoring for a sampling point if the results of the samples 
from the previous two quarters are below the detection limit.
    (iv) If the average of the initial monitoring results for a sampling 
point is above the MCL, the system must collect and analyze quarterly 
samples at that sampling point until the system has results from four 
consecutive quarters that are at or below the MCL, unless the system 
enters into another schedule as part of a formal compliance agreement 
with the State.
    (3) Reduced monitoring: States may allow community water systems to 
reduce the future frequency of monitoring from once every three years to 
once every six or nine years at each sampling point, based on the 
following criteria.
    (i) If the average of the initial monitoring results for each 
contaminant (i.e., gross alpha particle activity, uranium, radium-226, 
or radium-228) is below the detection limit specified in Table B, in 
Sec.  141.25(c)(1), the system must collect and analyze for that 
contaminant using at least one sample at that sampling point every nine 
years.
    (ii) For gross alpha particle activity and uranium, if the average 
of the initial monitoring results for each contaminant is at or above 
the detection limit but at or below \1/2\ the MCL, the system must 
collect and analyze for that contaminant using at least one sample at 
that sampling point every six years. For combined radium-226 and radium-
228, the analytical results must be combined. If the average of the 
combined initial monitoring results for radium-226 and radium-228 is at 
or above the detection limit but at or below \1/2\ the MCL, the system 
must collect and analyze for that contaminant using at least one sample 
at that sampling point every six years.
    (iii) For gross alpha particle activity and uranium, if the average 
of the initial monitoring results for each contaminant is above \1/2\ 
the MCL but at or below the MCL, the system must collect and analyze at 
least one sample at that sampling point every three years. For combined 
radium-226 and radium-

[[Page 474]]

228, the analytical results must be combined. If the average of the 
combined initial monitoring results for radium-226 and radium-228 is 
above \1/2\ the MCL but at or below the MCL, the system must collect and 
analyze at least one sample at that sampling point every three years.
    (iv) Systems must use the samples collected during the reduced 
monitoring period to determine the monitoring frequency for subsequent 
monitoring periods (e.g., if a system's sampling point is on a nine year 
monitoring period, and the sample result is above \1/2\ MCL, then the 
next monitoring period for that sampling point is three years).
    (v) If a system has a monitoring result that exceeds the MCL while 
on reduced monitoring, the system must collect and analyze quarterly 
samples at that sampling point until the system has results from four 
consecutive quarters that are below the MCL, unless the system enters 
into another schedule as part of a formal compliance agreement with the 
State.
    (4) Compositing: To fulfill quarterly monitoring requirements for 
gross alpha particle activity, radium-226, radium-228, or uranium, a 
system may composite up to four consecutive quarterly samples from a 
single entry point if analysis is done within a year of the first 
sample. States will treat analytical results from the composited as the 
average analytical result to determine compliance with the MCLs and the 
future monitoring frequency. If the analytical result from the 
composited sample is greater than \1/2\ MCL, the State may direct the 
system to take additional quarterly samples before allowing the system 
to sample under a reduced monitoring schedule.
    (5) A gross alpha particle activity measurement may be substituted 
for the required radium-226 measurement provided that the measured gross 
alpha particle activity does not exceed 5 pCi/l. A gross alpha particle 
activity measurement may be substituted for the required uranium 
measurement provided that the measured gross alpha particle activity 
does not exceed 15 pCi/l. The gross alpha measurement shall have a 
confidence interval of 95% (1.65[sigma], where [sigma] is the standard 
deviation of the net counting rate of the sample) for radium-226 and 
uranium. When a system uses a gross alpha particle activity measurement 
in lieu of a radium-226 and/or uranium measurement, the gross alpha 
particle activity analytical result will be used to determine the future 
monitoring frequency for radium-226 and/or uranium. If the gross alpha 
particle activity result is less than detection, \1/2\ the detection 
limit will be used to determine compliance and the future monitoring 
frequency.
    (b) Monitoring and compliance requirements for beta particle and 
photon radioactivity. To determine compliance with the maximum 
contaminant levels in Sec.  141.66(d) for beta particle and photon 
radioactivity, a system must monitor at a frequency as follows:
    (1) Community water systems (both surface and ground water) 
designated by the State as vulnerable must sample for beta particle and 
photon radioactivity. Systems must collect quarterly samples for beta 
emitters and annual samples for tritium and strontium-90 at each entry 
point to the distribution system (hereafter called a sampling point), 
beginning within one quarter after being notified by the State. Systems 
already designated by the State must continue to sample until the State 
reviews and either reaffirms or removes the designation.
    (i) If the gross beta particle activity minus the naturally 
occurring potassium-40 beta particle activity at a sampling point has a 
running annual average (computed quarterly) less than or equal to 50 
pCi/L (screening level), the State may reduce the frequency of 
monitoring at that sampling point to once every 3 years. Systems must 
collect all samples required in paragraph (b)(1) of this section during 
the reduced monitoring period.
    (ii) For systems in the vicinity of a nuclear facility, the State 
may allow the CWS to utilize environmental surveillance data collected 
by the nuclear facility in lieu of monitoring at the system's entry 
point(s), where the State determines if such data is applicable to a 
particular water system. In the event that there is a release from a 
nuclear facility, systems which are using surveillance data must begin 
monitoring at the community water

[[Page 475]]

system's entry point(s) in accordance with paragraph (b)(1) of this 
section.
    (2) Community water systems (both surface and ground water) 
designated by the State as utilizing waters contaminated by effluents 
from nuclear facilities must sample for beta particle and photon 
radioactivity. Systems must collect quarterly samples for beta emitters 
and iodine-131 and annual samples for tritium and strontium-90 at each 
entry point to the distribution system (hereafter called a sampling 
point), beginning within one quarter after being notified by the State. 
Systems already designated by the State as systems using waters 
contaminated by effluents from nuclear facilities must continue to 
sample until the State reviews and either reaffirms or removes the 
designation.
    (i) Quarterly monitoring for gross beta particle activity shall be 
based on the analysis of monthly samples or the analysis of a composite 
of three monthly samples. The former is recommended.
    (ii) For iodine-131, a composite of five consecutive daily samples 
shall be analyzed once each quarter. As ordered by the State, more 
frequent monitoring shall be conducted when iodine-131 is identified in 
the finished water.
    (iii) Annual monitoring for strontium-90 and tritium shall be 
conducted by means of the analysis of a composite of four consecutive 
quarterly samples or analysis of four quarterly samples. The latter 
procedure is recommended.
    (iv) If the gross beta particle activity minus the naturally 
occurring potassium-40 beta particle activity at a sampling point has a 
running annual average (computed quarterly) less than or equal to 15 
pCi/L (screening level), the State may reduce the frequency of 
monitoring at that sampling point to every 3 years. Systems must collect 
the same type of samples required in paragraph (b)(2) of this section 
during the reduced monitoring period.
    (v) For systems in the vicinity of a nuclear facility, the State may 
allow the CWS to utilize environmental surveillance data collected by 
the nuclear facility in lieu of monitoring at the system's entry 
point(s), where the State determines if such data is applicable to a 
particular water system. In the event that there is a release from a 
nuclear facility, systems which are using surveillance data must begin 
monitoring at the community water system's entry point(s) in accordance 
with paragraph (b)(2) of this section.
    (3) Community water systems designated by the State to monitor for 
beta particle and photon radioactivity can not apply to the State for a 
waiver from the monitoring frequencies specified in paragraph (b)(1) or 
(b)(2) of this section.
    (4) Community water systems may analyze for naturally occurring 
potassium-40 beta particle activity from the same or equivalent sample 
used for the gross beta particle activity analysis. Systems are allowed 
to subtract the potassium-40 beta particle activity value from the total 
gross beta particle activity value to determine if the screening level 
is exceeded. The potassium-40 beta particle activity must be calculated 
by multiplying elemental potassium concentrations (in mg/L) by a factor 
of 0.82.
    (5) If the gross beta particle activity minus the naturally 
occurring potassium-40 beta particle activity exceeds the appropriate 
screening level, an analysis of the sample must be performed to identify 
the major radioactive constituents present in the sample and the 
appropriate doses must be calculated and summed to determine compliance 
with Sec.  141.66(d)(1), using the formula in Sec.  141.66(d)(2). Doses 
must also be calculated and combined for measured levels of tritium and 
strontium to determine compliance.
    (6) Systems must monitor monthly at the sampling point(s) which 
exceed the maximum contaminant level in Sec.  141.66(d) beginning the 
month after the exceedance occurs. Systems must continue monthly 
monitoring until the system has established, by a rolling average of 3 
monthly samples, that the MCL is being met. Systems who establish that 
the MCL is being met must return to quarterly monitoring until they meet 
the requirements set forth in paragraph (b)(1)(i) or (b)(2)(iv) of this 
section.
    (c) General monitoring and compliance requirements for 
radionuclides. (1) The

[[Page 476]]

State may require more frequent monitoring than specified in paragraphs 
(a) and (b) of this section, or may require confirmation samples at its 
discretion. The results of the initial and confirmation samples will be 
averaged for use in compliance determinations.
    (2) Each public water systems shall monitor at the time designated 
by the State during each compliance period.
    (3) Compliance: Compliance with Sec.  141.66 (b) through (e) will be 
determined based on the analytical result(s) obtained at each sampling 
point. If one sampling point is in violation of an MCL, the system is in 
violation of the MCL.
    (i) For systems monitoring more than once per year, compliance with 
the MCL is determined by a running annual average at each sampling 
point. If the average of any sampling point is greater than the MCL, 
then the system is out of compliance with the MCL.
    (ii) For systems monitoring more than once per year, if any sample 
result will cause the running average to exceed the MCL at any sample 
point, the system is out of compliance with the MCL immediately.
    (iii) Systems must include all samples taken and analyzed under the 
provisions of this section in determining compliance, even if that 
number is greater than the minimum required.
    (iv) If a system does not collect all required samples when 
compliance is based on a running annual average of quarterly samples, 
compliance will be based on the running average of the samples 
collected.
    (v) If a sample result is less than the detection limit, zero will 
be used to calculate the annual average, unless a gross alpha particle 
activity is being used in lieu of radium-226 and/or uranium. If the 
gross alpha particle activity result is less than detection, \1/2\ the 
detection limit will be used to calculate the annual average.
    (4) States have the discretion to delete results of obvious sampling 
or analytic errors.
    (5) If the MCL for radioactivity set forth in Sec.  141.66 (b) 
through (e) is exceeded, the operator of a community water system must 
give notice to the State pursuant to Sec.  141.31 and to the public as 
required by subpart Q of this part.

[65 FR 76745, Dec. 7, 2000, as amended at 69 FR 38855, June 29, 2004]



Sec.  141.27  Alternate analytical techniques.

    (a) With the written permission of the State, concurred in by the 
Administrator of the U.S. EPA, an alternate analytical technique may be 
employed. An alternate technique shall be accepted only if it is 
substantially equivalent to the prescribed test in both precision and 
accuracy as it relates to the determination of compliance with any MCL. 
The use of the alternate analytical technique shall not decrease the 
frequency of monitoring required by this part.

[45 FR 57345, Aug. 27, 1980]



Sec.  141.28  Certified laboratories.

    (a) For the purpose of determining compliance with Sec.  141.21 
through 141.27, 141.30, 141.40, 141.74, 141.89 and 141.402, samples may 
be considered only if they have been analyzed by a laboratory certified 
by the State except that measurements of alkalinity, calcium, 
conductivity, disinfectant residual, orthophosphate, pH, silica, 
temperature and turbidity may be performed by any person acceptable to 
the State.
    (b) Nothing in this part shall be construed to preclude the State or 
any duly designated representative of the State from taking samples or 
from using the results from such samples to determine compliance by a 
supplier of water with the applicable requirements of this part.

[45 FR 57345, Aug. 27, 1980; 47 FR 10999, Mar. 12, 1982, as amended at 
59 FR 34323, July 1, 1994; 64 FR 67465, Dec. 1, 1999; 71 FR 65651, Nov. 
8, 2006]



Sec.  141.29  Monitoring of consecutive public water systems.

    When a public water system supplies water to one or more other 
public water systems, the State may modify the monitoring requirements 
imposed by this part to the extent that the interconnection of the 
systems justifies treating them as a single system for monitoring 
purposes. Any modified

[[Page 477]]

monitoring shall be conducted pursuant to a schedule specified by the 
State and concurred in by the Administrator of the U.S. Environmental 
Protection Agency.



 Sec. Appendix A to Subpart C of Part 141--Alternative Testing Methods 
         Approved for Analyses Under the Safe Drinking Water Act

    Only the editions stated in the following table are approved.

                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.21(f)(3)
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Organism                    Methodology        SM 21st Edition \1\    SM 22nd Edition \28\      SM Online \3\               Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Total Coliforms...................  Total Coliform         9221 A, B............  9221 A, B............  9221 A,B-06.........
                                     Fermentation
                                     Technique.
                                    Total Coliform         9222 A, B, C.........
                                     Membrane Filter
                                     Technique.
                                    Presence-Absence (P-   9221 D...............
                                     A) Coliform Test.
                                    ONPG-MUG Test........  9223.................  9223 B...............  9223 B-04...........
                                    Colitag \TM\.........  .....................  .....................  ....................  Modified Colitag \TM\
                                                                                                                                \13\
                                    Tecta EC/TC \33\.....  .....................  .....................  ....................  .........................
--------------------------------------------------------------------------------------------------------------------------------------------------------


                   Alternative Testing Methods for Contaminants Listed at 40 CFR 141.21(f)(5)
----------------------------------------------------------------------------------------------------------------
                Organism                         Methodology            SM 22nd Edition \28\      SM Online \3\
----------------------------------------------------------------------------------------------------------------
Fecal Coliforms........................  Fecal Coliform Procedure..  9221 E....................       9221 E-06
----------------------------------------------------------------------------------------------------------------


[[Page 478]]


                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.21(f)(6)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                 SM 20th Edition  SM 21st Edition  SM 22nd Edition
           Organism               Methodology          \6\              \1\              \28\           SM Online \3\                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
E.coli.......................  ONPG-MUG Test...          9223 B           9223 B           9223 B        9223 B-97, B-04
                               Colitag \TM\....  ...............  ...............  ...............  .....................  Modified Colitag \TM\ \13\
                               Tecta EC/TC \33\  ...............  ...............  ...............  .....................  .............................
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 479]]


                   Alternative Testing Methods for Contaminants Listed at 40 CFR 141.23(k)(1)
----------------------------------------------------------------------------------------------------------------
                                                                 SM 22nd
 Contaminant     Methodology       EPA method       SM 21st      edition     SM online   ASTM \4\       Other
                                                  edition \1\      \28\         \3\
----------------------------------------------------------------------------------------------------------------
Alkalinity..  Titrimetric.....  ................  2320 B.....  2320 B.....  ..........  D1067-06
                                                                                         B, 11 B
Antimony....  Hydride--Atomic   ................  ...........  ...........  ..........  D 3697-07,
               Absorption.                                                               -12.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,
               Absorption;                                                   B-10.
               Furnace.
              Axially viewed    200.5, Revision   ...........  ...........  ..........
               inductively       4.2.\2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Arsenic.....  Atomic            ................  3113 B.....  3113 B.....  3113 B-04,  D 2972-08
               Absorption;                                                   B-10.       C, -15 C.
               Furnace.
              Hydride Atomic    ................  3114 B.....  3114 B.....  3114 B-09.  D 2972-08
               Absorption.                                                               B, -15 B.
              Axially viewed    200.5, Revision
               inductively       4.2.\2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Barium......  Inductively       ................  3120 B.....  3120 B.....
               Coupled Plasma.
              Atomic            ................  3111 D.....  3111 D.....
               Absorption;
               Direct.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,
               Absorption;                                                   B-10.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2 \2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Beryllium...  Inductively       ................  3120 B.....  3120 B.....
               Coupled Plasma.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,  D 3645-08
               Absorption;                                                   B-10.       B, -15 B.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2.\2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Cadmium.....  Atomic            ................  3113 B.....  3113 B.....  3113 B-04,
               Absorption;                                                   B-10.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2 \2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Calcium.....  EDTA Titrimetric  ................  3500-Ca B..  3500-Ca B..  ..........  D 511-09, -
                                                                                         14 A.
              Atomic            ................  3111 B.....  3111 B.....  ..........  D 511-90, -
               Absorption;                                                               14 B.
               Direct
               Aspiration.
              Inductively       ................  3120 B.....  3120 B.....  ..........
               Coupled Plasma.
              Axially viewed    200.5, Revision   ...........  ...........  ..........
               inductively       4.2.\2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
              Ion               ................  ...........  ...........  ..........  D 6919-09.
               Chromatography.
Chromium....  Inductively       ................  3120 B.....  3120 B.....
               Coupled Plasma.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,
               Absorption;                                                   B-10.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2 \2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Copper......  Atomic            ................  3113 B.....  3113 B.....  3113 B-04,  D 1688-07,
               Absorption;                                                   B-10.       -12 C.
               Furnace.

[[Page 480]]

 
              Atomic            ................  3111 B.....  3111 B.....  ..........  D 1688-07,
               Absorption;                                                               -12 A.
               Direct
               Aspiration.
              Inductively       ................  3120 B.....  3120 B.....  ..........
               Coupled Plasma.
              Axially viewed    200.5, Revision   ...........  ...........  ..........
               inductively       4.2.\2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
              Colorimetric....  ................  ...........  ...........  ..........  ..........  Hach Method
                                                                                                     8026 \35\
                                                                                                     Hach Method
                                                                                                     10272.\36\
Conductivity  Conductance.....  ................  2510 B.....  2510 B.....  ..........  D 1125-14
                                                                                         A.
Cyanide.....  Manual            ................  ...........  ...........  ..........  D 2036-06
               Distillation                                                              A
               followed by.
              Spectrophotometr  ................  4500-CN- G.  4500-CN- G.  ..........  D 2036-06
               ic, Amenable.                                                             B
              Spectrophotometr  ................  4500-CN- E.  4500-CN- E.  ..........  D2036-06 A
               ic Manual.
              Selective         ................  4500-CN- F.  4500-CN- F.
               Electrode.
              Headspace Gas     ................  ...........  ...........  ..........  ..........  ME355.01 \7\
               Chromatography/
               Mass
               Spectrometry.
Fluoride....  Ion               ................  4110 B.....  4110 B.....  ..........  D 4327-11.
               Chromatography.
              Manual            ................  4500-F- B,   4500-F- B,
               Distillation;                       D.           D.
               Colorimetric
               SPADNS.
              Manual Electrode  ................  4500-F- C..  4500-F- C..  ..........  D 1179-04,
                                                                                         10 B.
              Automated         ................  4500-F- E..  4500-F- E..
               Alizarin.
              Arsenite-Free     ................  ...........  ...........  ..........  ..........  Hach SPADNS
               Colorimetric                                                                          2 Method
               SPADNS.                                                                               10225 \22\
Lead........  Atomic            ................  3113 B.....  3113 B.....  3113 B-04,  D 3559-08
               Absorption;                                                   B-10.       D, -15 D.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2.\2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Magnesium...  Atomic            ................  3111 B.....  3111 B.....  ..........  D 511-09, -
               Absorption.                                                               14 B.
              Inductively       ................  3120 B.....  3120 B.....  ..........
               Coupled Plasma.
              Complexation      ................  3500-Mg B..  3500-Mg B..  ..........  D 511-09, -
               Titrimetric                                                               14 A.
               Methods.
              Axially viewed    200.5, Revision   ...........  ...........  ..........
               inductively       4.2.\2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
              Ion               ................  ...........  ...........  ..........  D 6919-09.
               Chromatography.
Mercury.....  Manual, Cold      ................  3112 B.....  3112 B.....  3112 B-09.  D 3223-12.
               Vapor.
Nickel......  Inductively       ................  3120 B.....  3120 B.....
               Coupled Plasma.
              Atomic            ................  3111 B.....  3111 B.....
               Absorption;
               Direct.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,
               Absorption;                                                   B-10.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2 \2\.
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Nitrate.....  Ion               ................  4110 B.....  4110 B.....  ..........  D 4327-11.
               Chromatography.

[[Page 481]]

 
              Automated         ................  4500-NO3- F  4500-NO3- F
               Cadmium
               Reduction.
              Manual Cadmium    ................  4500-NO3- E  4500-NO3- E
               Reduction.
              Ion Selective     ................  4500-NO3- D  4500-NO3- D
               Electrode.
              Reduction/        ................  ...........  ...........  ..........  ..........  Systea Easy
               Colorimetric.                                                                         (1-Reagent)
                                                                                                     \8\ NECi
                                                                                                     Nitrate-
                                                                                                     Reductase.\
                                                                                                     40\
              Colorimetric;     ................  ...........  ...........  ..........  ..........  Hach
               Direct.                                                                               TNTplus\TM\
                                                                                                     835/836
                                                                                                     Method
                                                                                                     10206.\23\
              Capillary Ion     ................  ...........  ...........  ..........  D 6508-15.
               Electrophoresis.
Nitrite.....  Ion               ................  4110 B.....  4110 B.....  ..........  D 4327-11.
               Chromatography.
              Automated         ................  4500-NO3- F  4500-NO3- F
               Cadmium
               Reduction.
              Manual Cadmium    ................  4500-NO3- E  4500-NO3- E
               Reduction.
              Spectrophotometr  ................  4500-NO2- B  4500-NO2- B
               ic.
              Reduction/        ................  ...........  ...........  ..........  ..........  Systea Easy
               Colorimetric.                                                                         (1-Reagent)
                                                                                                     \8\ NECi
                                                                                                     Nitrate-
                                                                                                     Reductase.\
                                                                                                     40\
              Capillary Ion     ................  ...........  ...........  ..........  D 6508-15.
               Electrophoresis.
Orthophospha  Ion               ................  4110 B.....  4110 B.....  ..........  D 4327-11.
 te.           Chromatography.
              Colorimetric,     ................  4500-P E...  4500-P E...  4500-P E-
               ascorbic acid,                                                99.
               single reagent.
              Colorimetric,     ................  4500-P F...  4500-P F...  4500-P F-   ..........  Thermo
               Automated,                                                    99.                     Fisher
               Ascorbic Acid.                                                                        Discrete
                                                                                                     Analyzer.\4
                                                                                                     1\
              Capillary Ion     ................  ...........  ...........  ..........  D 6508-15.
               Electrophoresis.
pH..........  Electrometric...  150.3 \48\......  4500-H\+\ B  4500-H\+\ B  ..........  D 1293-12.
Selenium....  Hydride-Atomic    ................  3114 B.....  3114 B.....  3114 B-09.  D 3859-08
               Absorption.                                                               A, --15 A.
              Atomic            ................  3113 B.....  3113 B.....  3113 B-04,  D 3859-08
               Absorption;                                                   B-10.       B, -15 B.
               Furnace.
              Axially viewed    200.5, Revision
               inductively       4.2. \2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
Silica......  Colorimetric....  ................  ...........  ...........  ..........  D859-05,
                                                                                         10
              Molybdosilicate.  ................  4500-SiO2 C  4500-SiO2
                                                                C.
              Heteropoly blue.  ................  4500-SiO2 D  4500-SiO2
                                                                D.
              Automated for     ................  4500-SiO2 E  4500-SiO2
               Molybdate-                                       E.
               reactive Silica.
              Axially viewed    200.5, Revision
               inductively       4.2 \2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
              Inductively       ................  3120 B.....  3120 B
               Coupled Plasma.
Sodium......  Atomic            ................  3111 B.....  3111 B
               Absorption;
               Direct
               Aspiration.

[[Page 482]]

 
              Axially viewed    200.5, Revision
               inductively       4.2 \2\
               coupled plasma-
               atomic emission
               spectrometry
               (AVICP-AES).
              Ion               ................  ...........  ...........  ..........  D 6919-09
               Chromatography.
Temperature.  Thermometric....  ................  2550.......  2550.......  2550-10...
----------------------------------------------------------------------------------------------------------------


[[Page 483]]


                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.24(e)(1)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                SM 21st edition     SM 22nd edition
           Contaminant                       Methodology                    EPA method                \1\                \28\            SM online \3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Benzene.........................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Carbon tetrachloride............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Chlorobenzene...................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,2-Dichlorobenzene.............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,4-Dichlorobenzene.............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,2-Dichloroethane..............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
cis-Dichloroethylene............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
trans-Dichloroethylene..........  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Dichloromethane.................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,2-Dichloropropane.............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Ethylbenzene....................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Styrene.........................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Tetrachloroethylene.............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,1,1-Trichloroethane...........  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Trichloroethylene...............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Toluene.........................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,2,4-Trichlorobenzene..........  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,1-Dichloroethylene............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
1,1,2-Trichlorethane............  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Vinyl chloride..................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
Xylenes (total).................  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
2,4-D...........................  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
2,4,5-TP (Silvex)...............  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
Alachlor........................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Atrazine........................  Liquid Chromatography                             536 \25\
                                   Electrospray Ionization Tandem
                                   Mass Spectrometry (LC/ESI-MS/MS).
                                  Solid Phase Extraction/Gas            525.3, \24\ 523 \26\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Benzo(a)pyrene..................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Carbofuran......................  High-performance liquid            .......................  6610 B............  6610 B............  6610 B-04.
                                   chromatography (HPLC) with post-
                                   column derivatization and
                                   fluorescence detection.
Chlordane.......................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Dalapon.........................  Ion Chromatography Electrospray                   557 \14\
                                   Ionization Tandem Mass
                                   Spectrometry (IC-ESI-MS/MS).
                                  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
Di(2-ethylhexyl)adipate.........  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Di(2-ethylhexyl)phthalate.......  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).

[[Page 484]]

 
Dibromochloropropane (DBCP).....  Purge & trap/Gas Chromatography/                 524.3 \9\
                                   Mass Spectrometry.
Dinoseb.........................  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
Endrin..........................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Ethyl dibromide (EDB)...........  Purge & trap/Gas Chromatography/                 524.3 \9\
                                   Mass Spectrometry.
Glyphosate......................  High-Performance Liquid            .......................  6651 B............  6651 B............  6651 B-00, B-05.
                                   Chromatography (HPLC) with Post-
                                   Column Derivatization and
                                   Fluorescence Detection.
Heptachlor......................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Heptachlor Epoxide..............  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Hexachlorobenzene...............  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Hexachlorocyclo-pentadiene......  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Lindane.........................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Methoxychlor....................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Oxamyl..........................  High-performance liquid            .......................  6610 B............  6610 B............  6610 B-04.
                                   chromatography (HPLC) with post-
                                   column derivatization and
                                   fluorescence detection.
PCBs (as Aroclors)..............  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Pentachlorophenol...............  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
                                  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Picloram........................  Gas Chromatography/Electron        .......................  6640 B............  6640 B............  6640 B-01, B-06.
                                   Capture Detection (GC/ECD).
Simazine........................  Liquid Chromatography                             536 \25\
                                   Electrospray Ionization Tandem
                                   Mass Spectrometry (LC/ESI-MS/MS).
                                  Solid Phase Extraction/Gas             525.3,\24\ 523 \26\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Toxaphene.......................  Solid Phase Extraction/Gas                      525.3 \24\
                                   Chromatography/Mass Spectrometry
                                   (GC/MS).
Total Trihalomethanes...........  Purge & trap/Gas Chromatography/      524.3,\9\ 524.4 \29\
                                   Mass Spectrometry.
--------------------------------------------------------------------------------------------------------------------------------------------------------


                                         Alternative Testing Methods for Contaminants Listed at 40 CFR 141.25(a)
--------------------------------------------------------------------------------------------------------------------------------------------------------
         Contaminant              Methodology      SM 21st edition \1\     SM 22nd edition \28\          ASTM \4\                  SM online \3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Naturally Occurring:

[[Page 485]]

 
    Gross alpha and beta.....  Evaporation.....  7110 B.................  7110 B................
                               Liquid            .......................  ......................  D 7283-17.............  7110 D-17
                                Scintillation.
    Gross alpha..............  Coprecipitation.  7110 C.................  7110 C................
    Radium 226...............  Radon emanation.  7500-Ra C..............  7500-Ra C.............  D 3454-05.............
                               Radiochemical...  7500-Ra B..............  7500-Ra B.............  D 2460-07.............
                               Gamma             .......................  7500-Ra E.............  ......................  7500-Ra E-07
                                Spectrometry.
    Radium 228...............  Radiochemical...  7500-Ra D..............  7500-Ra D.............
                               Gamma             .......................  7500-Ra E.............  ......................  7500-Ra E-07
                                Spectrometry.
    Uranium..................  Radiochemical...  7500-U B...............  7500-U B..............
                               ICP-MS..........  3125...................  ......................  D 5673-05, 10.........
                               Alpha             7500-U C...............  7500-U C..............  D 3972-09.............
                                spectrometry.
                               Laser             .......................  ......................  D 5174-07.............
                                Phosphorimetry.
                               Alpha Liquid      .......................  D 6239-09.............
                                Scintillation
                                Spectrometry.
Man-Made:
    Radioactive Cesium.......  Radiochemical...  7500-Cs B..............  7500-Cs B.............
                               Gamma Ray         7120...................  7120..................  D 3649-06.............
                                Spectrometry.
    Radioactive Iodine.......  Radiochemical...  7500-I B...............  7500-I B..............  D 3649-06.
                                                 7500-I C...............  7500-I C,.............
                                                 7500-I D...............  7500-I D..............
                               Gamma Ray         7120...................  7120..................  D 4785-08.............
                                Spectrometry.
    Radioactive Strontium 89,  Radiochemical...  7500-Sr B..............  7500-Sr B.............
     90.
    Tritium..................  Liquid            7500-\3\''H B..........  7500-\3\ H B..........  D 4107-08.............
                                Scintillation.
    Gamma Emitters...........  Gamma Ray         7120...................  7120..................  D 3649-06.
                                Spectrometry.    7500-Cs B..............  7500-Cs B.............  D 4785-08.............
                                                 7500-I B...............  7500-I B..............
--------------------------------------------------------------------------------------------------------------------------------------------------------


                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.74(a)(1)
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Organism                    Methodology        SM 21st Edition \1\  SM 22nd Edition \28\      SM Online \3\                Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Total Coliform....................  Total Coliform         9221 A, B, C........  9221 A, B, C........  9221 A,B,C-06.......
                                     Fermentation
                                     Technique.
                                    Total Coliform         9222 A, B, C........
                                     Membrane Filter
                                     Technique.
                                    ONPG-MUG Test........  9223................  9223 B..............  9223 B-04...........
Fecal Coliforms...................  Fecal Coliform         9221 E..............  9221 E..............  9221 E-06...........
                                     Procedure.
                                    Fecal Coliform Filter  9222 D..............  9222 D..............  9222 D-06...........
                                     Procedure.
Heterotrophic bacteria............  Pour Plate Method....  9215 B..............  9215 B..............  9215 B-04...........
Turbidity.........................  Nephelometric Method.  2130 B..............  2130 B..............
                                    Laser Nephelometry     ....................  ....................  ....................  Mitchell M5271.\10\
                                     (online).                                                                                Mitchell M5331, Rev.
                                                                                                                              1.2.\42\ Lovibond PTV
                                                                                                                              6000.\46\

[[Page 486]]

 
                                    LED Nephelometry       ....................  ....................  ....................  Mitchell M5331 \11\
                                     (online).                                                                                Mitchell M5331, Rev.
                                                                                                                              1.2.\42\ Lovibond PTV
                                                                                                                              2000.\45\
                                    LED Nephelometry       ....................  ....................  ....................  AMI Turbiwell.\15\ Lovibond
                                     (online).                                                                                PTV 1000.\44\
                                    LED Nephelometry       ....................  ....................  ....................  Orion AQ4500.\12\
                                     (portable).
                                    360[deg] Nephelometry  ....................  ....................  ....................  Hach Method 10258.\39\
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 487]]


                                  Alternative Testing Methods for Disinfectant Residuals Listed at 40 CFR 141.74(a)(2)
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Residual                    Methodology       SM 21st Edition \1\    SM 22nd Edition \28\         ASTM \4\                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Free Chlorine.....................  Amperometric          4500-Cl D............  4500-Cl D............  D 1253-08, -14.......
                                     Titration.
                                    DPD Ferrous           4500-Cl F............  4500-Cl F............
                                     Titrimetric.
                                    DPD Colorimetric....  4500-Cl G............  4500-Cl G............  .....................  Hach Method 10260.\31\
                                    Syringaldazine        4500-Cl H............  4500-Cl H............
                                     (FACTS).
                                    On-line Chlorine      .....................  .....................  .....................  EPA 334.0.\16\
                                     Analyzer.
                                    Amperometric Sensor.  .....................  .....................  .....................  ChloroSense.\17\
                                    Indophenol            .....................  .....................  .....................  Hach Method 10241.\34\
                                     Colorimetric.
Total Chlorine....................  Amperometric          4500-Cl D............  4500-Cl D............  D 1253-08, -14.......
                                     Titration.
                                    Amperometric          4500-Cl E............  4500-Cl E............
                                     Titration (Low
                                     level measurement).
                                    DPD Ferrous           4500-Cl F............  4500-Cl F............
                                     Titrimetric.
                                    DPD Colorimetric....  4500-Cl G............  4500-Cl G............  .....................  Hach Method 10260.\31\
                                    Iodometric Electrode  4500-Cl I............  4500-Cl I............
                                    On-line Chlorine      .....................  .....................  .....................  EPA 334.0.\16\
                                     Analyzer.
                                    Amperometric Sensor.  .....................  .....................  .....................  ChloroSense.\17\
Chlorine Dioxide..................  Amperometric          4500-ClO2 C..........  4500-ClO2 C..........
                                     Titration.
                                    Amperometric          4500-ClO2 E..........  4500-ClO2 E..........
                                     Titration.
                                    Amperometric Sensor.  .....................  .....................  .....................  ChlordioX Plus.\32\
Ozone.............................  Indigo Method.......  4500-O3 B............  4500-O3 B............
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 488]]


                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.131(b)(1)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                       SM 21st Edition  SM 22nd Edition
         Contaminant              Methodology       EPA Method         ASTM \4\        SM Online \3\         \1\              \28\            Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
TTHM.........................  P&T/GC/MS.......  524.3 \9\, 524.4
                                                  \29\.
HAA5.........................  LLE               ................  ................  6251 B-07.......  6251 B.........  6251 B.........
                                (diazomethane)/
                                GC/ECD.
                               Ion               557. \14\
                                Chromatography
                                Electrospray
                                Ionization
                                Tandem Mass
                                Spectrometry
                                (IC-ESI-MS/MS).
                               Two-Dimensional   ................  ................  ................  ...............  ...............  Thermo Fisher
                                Ion                                                                                                       557.1.\47\
                                Chromatography
                                (IC) with
                                Suppressed
                                Conductivity
                                Detection.
Bromate......................  Two-Dimensional   302.0 \18\......
                                Ion
                                Chromatography
                                (IC).
                               Ion               557 \14\........
                                Chromatography
                                Electrospray
                                Ionization
                                Tandem Mass
                                Spectrometry
                                (IC-ESI-MS/MS).
                               Chemically        ................  D 6581-08 A.....
                                Suppressed Ion
                                Chromatography.
                               Electrolytically  ................  D 6581-08 B.....
                                Suppressed Ion
                                Chromatography.
Chlorite.....................  Chemically        ................  D 6581-08 A.....
                                Suppressed Ion
                                Chromatography.
                               Electrolytically  ................  D 6581-08 B.....
                                Suppressed Ion
                                Chromatography.
Chlorite--daily monitoring as  Amperometric      ................  ................  ................  4500-ClO2 E....  4500-ClO2 E....
 prescribed in 40 CFR           Titration.
 141.132(b)(2)(i)(A).
                               Amperometric      ................  ................  ................  ...............  ...............  ChlordioX
                                Sensor.                                                                                                   Plus.\32\
--------------------------------------------------------------------------------------------------------------------------------------------------------


                                  Alternative Testing Methods for Disinfectant Residuals Listed at 40 CFR 141.131(c)(1)
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Residual                    Methodology        SM 21st Edition \1\  SM 22nd Edition \28\        ASTM \4\                   Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Free Chlorine.....................  Amperometric           4500-Cl D...........  4500-Cl D...........  D 1253-08, -14......
                                     Titration.

[[Page 489]]

 
                                    DPD Ferrous            4500-Cl F...........  4500-Cl F...........
                                     Titrimetric.
                                    DPD Colorimetric.....  4500-Cl G...........  4500-Cl G...........  ....................  Hach Method 10260.\31\
                                    Syringaldazine         4500-Cl H...........  4500-Cl H...........
                                     (FACTS).
                                    Amperometric Sensor..  ....................  ....................  ....................  ChloroSense.\17\
                                    On-line Chlorine       ....................  ....................  ....................  EPA 334.0.\16\
                                     Analyzer.
                                    Indophenol             ....................  ....................  ....................  Hach Method 10241.\34\
                                     Colorimetric.
Combined Chlorine.................  Amperometric           4500-Cl D...........  4500-Cl D...........  D 1253-08, -14......
                                     Titration.
                                    DPD Ferrous            4500-Cl F...........  4500-Cl F...........
                                     Titrimetric.
                                    DPD Colorimetric.....  4500-Cl G...........  4500-Cl G...........  ....................  Hach Method 10260.\31\
Total Chlorine....................  Amperometric           4500-Cl D...........  4500-Cl D...........  D 1253-08, -14......
                                     Titration.
                                    Low level              4500-Cl E...........  4500-Cl E...........
                                     Amperometric
                                     Titration.
                                    DPD Ferrous            4500-Cl F...........  4500-Cl F...........
                                     Titrimetric.
                                    DPD Colorimetric.....  4500-Cl G...........  4500-Cl G...........  ....................  Hach Method 10260.\31\
                                    Iodometric Electrode.  4500-Cl I...........  4500-Cl I...........
                                    Amperometric Sensor..  ....................  ....................  ....................  ChloroSense.\17\
                                    On-line Chlorine       ....................  ....................  ....................  EPA 334.0.\16\
                                     Analyzer.
Chlorine Dioxide..................  Amperometric Method    4500-ClO2 E.........  4500-ClO2 E.........
                                     II.
                                    Amperometric Sensor..  ....................  ....................  ....................  ChlordioX Plus \32\.
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 490]]


 Alternative Testing Methods for Disinfectant Residuals Listed at 40 CFR
                 141.131(c)(2), If Approved by the State
------------------------------------------------------------------------
           Residual               Methodology             Method
------------------------------------------------------------------------
Free Chlorine................  Test Strips.....  Method D99-003 \5\
------------------------------------------------------------------------


[[Page 491]]


                                         Alternative Testing Methods for Parameters Listed at 40 CFR 141.131(d)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                   SM 21st Edition  SM 22nd Edition
           Parameter               Methodology           \1\              \28\        SM Online \3\            EPA                      Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Total Organic Carbon (TOC)....  High Temperature   5310 B.........  5310 B.........  ...............  415.3, Rev 1.2.\19\..
                                 Combustion.
                                Persulfate-        5310 C.........  5310 C.........  ...............  415.3, Rev 1.2 \19\..  Hach Method 10267.\38\
                                 Ultraviolet or
                                 Heated
                                 Persulfate
                                 Oxidation.
                                Wet Oxidation....  5310 D.........  5310 D.........  ...............  415.3, Rev 1.2.\19\..
                                Ozone Oxidation..  ...............  ...............  ...............  .....................  Hach Method 10261.\37\
Specific Ultraviolet            Calculation using  ...............  ...............  ...............  415.3, Rev 1.2.\19\..
 Absorbance (SUVA).              DOC and UV254
                                 data.
Dissolved Organic Carbon (DOC)  High Temperature   5310 B.........  5310 B.........  ...............  415.3, Rev 1.2.\19\..
                                 Combustion.
                                Persulfate-        5310 C.........  5310 C.........  ...............  415.3, Rev 1.2.\19\..
                                 Ultraviolet or
                                 Heated
                                 Persulfate
                                 Oxidation.
                                Wet Oxidation....  5310 D.........  5310 D.........  ...............  415.3, Rev 1.2.\19\..
Ultraviolet absorption at 254   Spectrophotometry  5910 B.........  5910 B.........  5910 B-11......  415.3, Rev 1.2.\19\..  ...........................
 nm (UV254).
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 492]]


Alternative Testing Methods With MRL <=0.0010 mg/L for Monitoring Listed
                     at 40 CFR 141.132(b)(3)(ii)(B)
------------------------------------------------------------------------
      Contaminant              Methodology              EPA method
------------------------------------------------------------------------
Bromate................  Two-Dimensional Ion      302.0 \18\
                          Chromatography (IC).
                         Ion Chromatography       557 \14\
                          Electrospray
                          Ionization Tandem Mass
                          Spectrometry (IC-ESI-
                          MS/MS).
------------------------------------------------------------------------


                                       Alternative Testing Methods for Contaminants Listed at 40 CFR 141.402(c)(2)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                        SM 20th Edition     SM 21st Edition     SM 22nd Edition
            Organism                  Methodology             \6\                 \1\                \28\            SM Online \3\           Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
E. coli.........................  Colilert[supreg]..  ..................  9223 B............  9223 B............  9223 B-97, B-04...
                                  Colisure[supreg]..  ..................  9223 B............  9223 B............  9223 B-97, B-04...
                                  Colilert-18.......  9223 B............  9223 B............  9223 B............  9223 B-97, B-04...
                                  Readycult[supreg].  ..................  ..................  ..................  ..................  Readycult.[supreg]
                                                                                                                                       \20\
                                  Colitag...........  ..................  ..................  ..................  ..................  Modified
                                                                                                                                       Colitag.\TM\ \13\
                                  Chromocult[supreg]  ..................  ..................  ..................  ..................  Chromocult.[supreg
                                                                                                                                       ] \21\
                                  EC-MUG............  ..................  ..................  9221 F............  9221 F-06.........
                                  Tecta EC/TC. \33\
                                   \43\
 
Enterococci.....................  Multiple-Tube       ..................  ..................  ..................  9230 B-04.........
                                   Technique.
Coliphage.......................  Two-Step            ..................  ..................  ..................  ..................  Fast Phage \30\
                                   Enrichment
                                   Presence-Absence
                                   Procedure.
--------------------------------------------------------------------------------------------------------------------------------------------------------


                    Alternative Testing Methods for Contaminants Listed at 40 CFR 141.704(a)
----------------------------------------------------------------------------------------------------------------
               Organism                                Methodology                          EPA Method
----------------------------------------------------------------------------------------------------------------
Cryptosporidium.......................  Filtration/Immunomagnetic Separation/     1623.1 \27\
                                         Immunofluorescence Assay Microscopy.
----------------------------------------------------------------------------------------------------------------


                    Alternative Testing Methods for Contaminants Listed at 40 CFR 141.704(b)
----------------------------------------------------------------------------------------------------------------
                 Organism                             Methodology                     SM 20th edition \6\
----------------------------------------------------------------------------------------------------------------
E. coli..................................  Membrane Filtration, Two Step....  9222 D/9222 G
----------------------------------------------------------------------------------------------------------------


                   Alternative Testing Methods for Contaminants Listed at 40 CFR 141.852(a)(5)
----------------------------------------------------------------------------------------------------------------
                                                                    SM 20th,
                                  Methodology                         21st      SM 22nd Edition
           Organism                category           Method      editions \1\        \28\        SM Online \3\
                                                                       \6\
----------------------------------------------------------------------------------------------------------------
Total Coliforms..............  Lactose           Standard Total   ............  9221 B.1, B.2..  9221 B.1, B.2-
                                Fermentation      Coliform                                        06.
                                Methods.          Fermentation
                                                  Technique.
                               Enzyme Substrate  Colilert[supreg  ............  9223 B.........  9223 B-04.
                                Methods.          ].
                                                 Colisure[supreg  ............  9223 B.........  9223 B-04.
                                                  ].
                                                 Colilert-18....  9223 B......  9223 B.........  9223 B-04.
                                                 Tecta EC/TC. 33
                                                  43
Escherichia coli.............  Escherichia coli  EC-MUG medium..  ............  9221 F.1.......  9221 F.1-06.
                                Procedure
                                (following
                                Lactose
                                Fermentation
                                Methods).
                               Enzyme Substrate  Colilert[supreg  ............  9223 B.........  9223 B-04.
                                Methods.          ].
                                                 Colisure[supreg  ............  9223 B.........  9223 B-04.
                                                  ].
                                                 Colilert-18....  9223 B......  9223 B.........  9223 B-04.

[[Page 493]]

 
                                                 Tecta EC/TC. 33
                                                  43
----------------------------------------------------------------------------------------------------------------


[[Page 494]]


                                         Alternative Testing Methods for Contaminants Listed at 40 CFR 143.4(b)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                          SM 21st Edition     SM 22nd Edition
         Contaminant              Methodology       EPA method           ASTM \4\               \1\                \28\               SM online \3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Aluminum.....................  Axially viewed    200.5, Revision
                                inductively       4.2 \2\.
                                coupled plasma-
                                atomic emission
                                spectrometry
                                (AVICP-AES).
                               Atomic            ................  ...................  3111 D............  3111 D............
                                Absorption;
                                Direct.
                               Atomic            ................  ...................  3113 B............  3113 B............  3113 B-04, B-10.
                                Absorption;
                                Furnace.
                               Inductively       ................  ...................  3120 B............  3120 B............
                                Coupled Plasma.
Chloride.....................  Silver Nitrate    ................  D 512-04 B, 12 B...  4500-Cl- B........  4500-Cl- B........
                                Titration.
                               Ion               ................  D 4327-11..........  4110 B............  4110 B............
                                Chromatography.
                               Potentiometric    ................  ...................  4500-Cl- D........  4500-Cl- D........
                                Titration.
Color........................  Visual            ................  ...................  2120 B............  2120 B............
                                Comparison.
Foaming Agents...............  Methylene Blue    ................  ...................  5540 C............  5540 C............
                                Active
                                Substances
                                (MBAS).
Iron.........................  Axially viewed    200.5, Revision
                                inductively       4.2 \2\.
                                coupled plasma-
                                atomic emission
                                spectrometry
                                (AVICP-AES).
                               Atomic            ................  ...................  3111 B............  3111 B............
                                Absorption;
                                Direct.
                               Atomic            ................  ...................  3113 B............  3113 B............  3113 B-04, B-10.
                                Absorption;
                                Furnace.
                               Inductively       ................  ...................  3120 B............  3120 B............
                                Coupled Plasma.
Manganese....................  Axially viewed    200.5, Revision
                                inductively       4.2 \2\.
                                coupled plasma-
                                atomic emission
                                spectrometry
                                (AVICP-AES).
                               Atomic            ................  ...................  3111 B............  3111 B............
                                Absorption;
                                Direct.
                               Atomic            ................  ...................  3113 B............  3113 B............  3113 B-04, B-10.
                                Absorption;
                                Furnace.
                               Inductively       ................  ...................  3120 B............  3120 B............
                                Coupled Plasma.
Odor.........................  Threshold Odor    ................  ...................  2150 B............  2150 B............
                                Test.
Silver.......................  Axially viewed    200.5, Revision
                                inductively       4.2 \2\.
                                coupled plasma-
                                atomic emission
                                spectrometry
                                (AVICP-AES).
                               Atomic            ................  ...................  3111 B............  3111 B............
                                Absorption;
                                Direct.
                               Atomic            ................  ...................  3113 B............  3113 B............  3113 B-04, B-10.
                                Absorption;
                                Furnace.
                               Inductively       ................  ...................  3120 B............  3120 B............
                                Coupled Plasma.
Sulfate......................  Ion               ................  D 4327-11..........  4110 B............  4110 B............
                                Chromatography.
                               Gravimetric with  ................  ...................  4500-SO4 2- C.....  4500-SO4 2- C.....  4500-SO4 2- C-97
                                ignition of
                                residue.
                               Gravimetric with  ................  ...................  4500-SO4 2- D.....  4500-SO4 2- D.....  4500-SO4 2- D-97
                                drying of
                                residue.
                               Turbidimetric     ................  D 516-07, 11.......  4500-SO4 2- E.....  4500-SO4 2- E.....  4500-SO4 2- E-97
                                method.
                               Automated         ................  ...................  4500-SO4 2- F.....  4500-SO4 2- F.....  4500-SO4 2- F-97
                                methylthymol
                                blue method.
Total Dissolved Solids.......  Total Dissolved   ................  ...................  2540 C............  2540 C............
                                Solids Dried at
                                180 deg C.

[[Page 495]]

 
Zinc.........................  Axially viewed    200.5, Revision
                                inductively       4.2 \2\
                                coupled plasma-
                                atomic emission
                                spectrometry
                                (AVICP-AES).
                               Atomic            ................  ...................  3111 B............  3111 B............
                                Absorption;
                                Direct
                                Aspiration.
                               Inductively       ................  ...................  3120 B............  3120 B............
                                Coupled Plasma.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Standard Methods for the Examination of Water and Wastewater, 21st edition (2005). Available from American Public Health Association, 800 I Street,
  NW., Washington, DC 20001-3710.
\2\ EPA Method 200.5, Revision 4.2. ``Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission
  Spectrometry.'' 2003. EPA/600/R-06/115. (Available at http://www.epa.gov/water-research/epa-drinking-water-research-methods.)
\3\ Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods
  Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.
\4\ Available from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959 or http://astm.org. The methods listed are the only
  alternative versions that may be used.
\5\ Method D99-003, Revision 3.0. ``Free Chlorine Species (HOCl- and OCl-) by Test Strip,'' November 21, 2003. Available from Industrial Test Systems,
  Inc., 1875 Langston St., Rock Hill, SC 29730.
\6\ Standard Methods for the Examination of Water and Wastewater, 20th edition (1998). Available from American Public Health Association, 800 I Street,
  NW., Washington, DC 20001-3710.
\7\ Method ME355.01, Revision 1.0. ``Determination of Cyanide in Drinking Water by GC/MS Headspace,'' May 26, 2009. Available at http://www.nemi.gov or
  from James Eaton, H & E Testing Laboratory, 221 State Street, Augusta, ME 04333. (207) 287-2727.
\8\ Systea Easy (1-Reagent). ``Systea Easy (1-Reagent) Nitrate Method,'' February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific,
  LLC., 900 Jorie Blvd., Suite 35, Oak Brook, IL 60523.
\9\ EPA Method 524.3, Version 1.0. ``Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry,''
  June 2009. EPA 815-B-09-009. Available at the National Service Center for Environmental Publications (www.epa.gov/nscep). Search ``815B09009''.
\10\ Mitchell Method M5271, Revision 1.1. ``Determination of Turbidity by Laser Nephelometry,'' March 5, 2009. Available at http://www.nemi.gov or from
  Leck Mitchell, PhD, PE, 656 Independence Valley Dr., Grand Junction, CO 81507.
\11\ Mitchell Method M5331, Revision 1.1. ``Determination of Turbidity by LED Nephelometry,'' March 5, 2009. Available at http://www.nemi.gov or from
  Leck Mitchell, PhD, PE, 656 Independence Valley Dr., Grand Junction, CO 81507.
\12\ Orion Method AQ4500, Revision 1.0. ``Determination of Turbidity by LED Nephelometry,'' May 8, 2009. Available at http://www.nemi.gov or from Thermo
  Scientific, 166 Cummings Center, Beverly, MA 01915, http://www.thermo.com.
\13\ Modified Colitag \TM\ Method, ``Modified Colitag \TM\ Test Method for the Simultaneous Detection of E. coli and other Total Coliforms in Water (ATP
  D05-0035),'' August 28, 2009. Available at http://www.nemi.gov or from CPI, International, 580 Skylane Boulevard, Santa Rosa, CA 95403.
\14\ EPA Method 557. ``Determination of Haloacetic Acids, Bromate, and Dalapon in Drinking Water by Ion Chromatography Electrospray Ionization Tandem
  Mass Spectrometry (IC-ESI-MS/MS),'' September 2009. EPA 815-B-09-012. Available at the National Service Center for Environmental Publications
  (www.epa.gov/nscep). Search ``815B09012''.
\15\ AMI Turbiwell, ``Continuous Measurement of Turbidity Using a SWAN AMI Turbiwell Turbidimeter,'' August 2009. Available at http://www.nemi.gov or
  from Markus Bernasconi, SWAN Analytische Instrumente AG, Studbachstrasse 13, CH-8340 Hinwil, Switzerland.
\16\ EPA Method 334.0. ``Determination of Residual Chlorine in Drinking Water Using an On-line Chlorine Analyzer,'' September 2009. EPA 815-B-09-013.
  Available at the National Service Center for Environmental Publications (www.epa.gov/nscep). Search ``815B09013''.
\17\ ChloroSense. ``Measurement of Free and Total Chlorine in Drinking Water by Palintest ChloroSense,'' August 2009. Available at https://www.nemi.gov
  or from Palintest Ltd, 1455 Jamike Avenue (Suite 100), Erlanger, KY 41018.
\18\ EPA Method 302.0. ``Determination of Bromate in Drinking Water using Two-Dimensional Ion Chromatography with Suppressed Conductivity Detection,''
  September 2009. EPA 815-B-09-014. Available at the National Service Center for Environmental Publications (www.epa.gov/nscep). Search ``815B09014''.
\19\ EPA 415.3, Revision 1.2. ``Determination of Total Organic Carbon and Specific UV Absorbance at 254 nm in Source Water and Drinking Water,''
  September 2009. EPA/600/R-09/122. Available at http://www.epa.gov/water-research/epa-drinking-water-research-methods.
\20\ Readycult[supreg] Method, ``Readycult[supreg] Coliforms 100 Presence/Absence Test for Detection and Identification of Coliform Bacteria and
  Escherichia coli in Finished Waters,'' January, 2007. Version 1.1. Available from EMD Millipore (division of Merck KGaA, Darmstadt, Germany), 290
  Concord Road, Billerica, MA 01821.
\21\ Chromocult[supreg] Method, ``Chromocult[supreg] Coliform Agar Presence/Absence Membrane Filter Test Method for Detection and Identification of
  Coliform Bacteria and Escherichia coli in Finished Waters,'' November, 2000. Version 1.0. EMD Millipore (division of Merck KGaA, Darmstadt, Germany),
  290 Concord Road, Billerica, MA 01821.
\22\ Hach Company Method, ``Hach Company SPADNS 2 (Arsenic-free) Fluoride Method 10225--Spectrophotometric Measurement of Fluoride in Water and
  Wastewater,'' January 2011. 5600 Lindbergh Drive, P.O. Box 389, Loveland, Colorado 80539. (Available at http://www.hach.com.)
\23\ Hach Company. ``Hach Company TNTplus \TM\ 835/836 Nitrate Method 10206--Spectrophotometric Measurement of Nitrate in Water and Wastewater,''
  January 2011. 5600 Lindbergh Drive, P.O. Box 389, Loveland, Colorado 80539. (Available at http://www.hach.com.)
\24\ EPA Method 525.3. ``Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas
  Chromatography/Mass Spectrometry (GC/MS),'' February 2012. EPA/600/R-12/010. Available at http://www.epa.gov/water-research/epa-drinking-water-
  research-methods.
\25\ EPA Method 536. ``Determination of Triazine Pesticides and their Degradates in Drinking Water by Liquid Chromatography Electrospray Ionization
  Tandem Mass Spectrometry (LC/ESI-MS/MS),'' October 2007. EPA 815-B-07-002. Available at the National Service Center for Environmental Publications
  (www.epa.gov/nscep). Search ``815B07002''.

[[Page 496]]

 
\26\ EPA Method 523. ``Determination of Triazine Pesticides and their Degradates in Drinking Water by Gas Chromatography/Mass Spectrometry (GC/MS),''
  February 2011. EPA 815-R-11-002. Available at the National Service Center for Environmental Publications (www.epa.gov/nscep). Search ``815R11002''.
\27\ EPA Method 1623.1. ``Cryptosporidium and Giardia in Water by Filtration/IMS/FA,'' 2012. EPA-816-R-12-001. Available at the National Service Center
  for Environmental Publications (www.epa.gov/nscep). Search ``816R12001''.
\28\ Standard Methods for the Examination of Water and Wastewater, 22nd edition (2012). Available from American Public Health Association, 800 I Street
  NW., Washington, DC 20001-3710.
\29\ EPA Method 524.4, Version 1.0. ``Measurement of Purgeable Organic Compounds in Water by Gas Chromatography/Mass Spectrometry using Nitrogen Purge
  Gas,'' May 2013. EPA 815-R-13-002. Available at the National Service Center for Environmental Publications (www.epa.gov/nscep). Search ``815R13002''.
\30\ Charm Sciences Inc. ``Fast Phage Test Procedure. Presence/Absence for Coliphage in Ground Water with Same Day Positive Prediction''. Version 009.
  November 2012. 659 Andover Street, Lawrence, MA 01843. Available at www.charmsciences.com.
\31\ Hach Company. ``Hach Method 10260--Determination of Chlorinated Oxidants (Free and Total) in Water Using Disposable Planar Reagent-filled Cuvettes
  and Mesofluidic Channel Colorimetry,'' April 2013. 5600 Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\32\ ChlordioX Plus. ``Chlorine Dioxide and Chlorite in Drinking Water by Amperometry using Disposable Sensors,'' November 2013. Available from
  Palintest Ltd, Jamike Avenue (Suite 100), Erlanger, KY 41018.
\33\ Tecta EC/TC. ``Techta\TM\ EC/TC Medium and Techta\TM\ Instrument: A Presence/Absence Method for the Simultaneous Detection of Total Coliforms and
  Escherichia coli (E. coli) in Drinking Water,'' version 1.0, May 2014. Available from Pathogen Detection Systems, Inc., 382 King Street East,
  Kingston, Ontario, Canada, K7K 2Y2.
\34\ Hach Company. ``Hach Method 10241--Spectrophotometric Measurement of Free Chlorine (Cl2) in Finished Drinking Water,'' November 2015. Revision 1.2.
  5600 Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\35\ Hach Company. ``Hach Method 8026--Spectrophotometric Measurement of Copper in Finished Drinking Water,'' December 2015. Revision 1.2. 5600
  Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\36\ Hach Company. ``Hach Method 10272--Spectrophotometric Measurement of Copper in Finished Drinking Water,'' December 2015. Revision 1.2. 5600
  Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\37\ Hach Company. ``Hach Method 10261--Total Organic Carbon in Finished Drinking Water by Catalyzed Ozone Hydroxyl Radical Oxidation Infrared
  Analysis,'' December 2015. Revision 1.2. 5600 Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\38\ Hach Company. ``Hach Method 10267--Spectrophotometric Measurement of Total Organic Carbon (TOC) in Finished Drinking Water,'' December 2015.
  Revision 1.2. 5600 Lindbergh Drive, P.O. Box 389, Loveland, CO 80539. (Available at http://www.hach.com.)
\39\ Hach Company. ``Hach Method 10258--Determination of Turbidity by 360[deg] Nephelometry,'' January 2016. 5600 Lindbergh Drive, P.O. Box 389,
  Loveland, CO 80539. (Available at http://www.hach.com.)
\40\ Nitrate Elimination Company, Inc. (NECi). ``Method for Nitrate Reductase Nitrate-Nitrogen Analysis of Drinking Water,'' February 2016. Superior
  Enzymes, Inc., 334 Hecla Street, Lake Linden, Michigan 49945.
\41\ Thermo Fisher. ``Thermo Fisher Scientific Drinking Water Orthophosphate Method for Thermo Scientific Gallery Discrete Analyzer,'' February 2016.
  Revision 5. Thermo Fisher Scientific, Ratastie 2, 01620 Vantaa, Finland.
\42\ Mitchell Method M5331, Revision 1.2. ``Determination of Turbidity by LED or Laser Nephelometry,'' February 2016. Available from Leck Mitchell,
  Ph.D., PE, 656 Independence Valley Dr., Grand Junction, CO 81507.
\43\ Tecta EC/TC. ``TectaTM EC/TC Medium and the TectaTM Instrument: A Presence/Absence Method for the Simultaneous Detection of Total Coliforms and
  Escherichia coli (E. coli) in Drinking Water,'' version 2.0, February 2017. Available from Pathogen Detection Systems, Inc., 382 King Street East,
  Kingston, Ontario, Canada, K7K 2Y2.
\44\ Lovibond PTV 1000. ``Continuous Measurement of Drinking Water Turbidity Using a Lovibond PTV 1000 White Light LED Turbidimeter,'' December 2016.
  Revision 1.0. Available from Tintometer, Inc., 6456 Parkland Drive, Sarasota, FL 34243.
\45\ Lovibond PTV 2000. ``Continuous Measurement of Drinking Water Turbidity Using a Lovibond PTV 2000 660-nm LED Turbidimeter,'' December 2016.
  Revision 1.0. Available from Tintometer, Inc., 6456 Parkland Drive, Sarasota, FL 34243.
\46\ Lovibond PTV 6000. ``Continuous Measurement of Drinking Water Turbidity Using a Lovibond PTV 6000 Laser Turbidimeter,'' December 2016. Revision
  1.0. Available from Tintometer, Inc., 6456 Parkland Drive, Sarasota, FL 34243.
\47\ Thermo Fisher. ``Thermo Fisher Method 557.1: Determination of Haloacetic Acids in Drinking Water using Two-Dimensional Ion Chromatography with
  Suppressed Conductivity Detection,'' January 2017. Version 1.0. Available from Thermo Fisher Scientific, 490 Lakeside Dr., Sunnyvale, CA 94085
  ([email protected]).
\48\ EPA Method 150.3. ``Determination of pH in Drinking Water,'' February 2017. EPA 815-B-17-001. Available at the National Service Center for
  Environmental Publications (www.epa.gov/nscep).


[74 FR 38353, Aug. 3, 2009, as amended at 74 FR 57914, Nov. 10, 2009; 74 
FR 63069, Dec. 2, 2009; 75 FR 32299, June 8, 2010; 76 FR 37018, June 24, 
2011; 77 FR 38527, June 28, 2012; 78 FR 32565, May 31, 2013; 78 FR 
37463, June 21, 2013; 79 FR 35086, June 19, 2014; 79 FR 36428, June 27, 
2014; 81 FR 46844, July 19, 2016; 82 FR 34867, July 27, 2017]

[[Page 497]]



                  Subpart D_Reporting and Recordkeeping



Sec.  141.31  Reporting requirements.

    (a) Except where a shorter period is specified in this part, the 
supplier of water shall report to the State the results of any test 
measurement or analysis required by this part within (1) The first ten 
days following the month in which the result is received, or (2) the 
first ten days following the end of the required monitoring period as 
stipulated by the State, whichever of these is shortest.
    (b) Except where a different reporting period is specified in this 
part, the supplier of water must report to the State within 48 hours the 
failure to comply with any national primary drinking water regulation 
(including failure to comply with monitoring requirements) set forth in 
this part.
    (c) The supplier of water is not required to report analytical 
results to the State in cases where a State laboratory performs the 
analysis and reports the results to the State office which would 
normally receive such notification from the supplier.
    (d) The public water system, within 10 days of completing the public 
notification requirements under subpart Q of this part for the initial 
public notice and any repeat notices, must submit to the primacy agency 
a certification that it has fully complied with the public notification 
regulations. The public water system must include with this 
certification a representative copy of each type of notice distributed, 
published, posted, and made available to the persons served by the 
system and to the media.
    (e) The water supply system shall submit to the State within the 
time stated in the request copies of any records required to be 
maintained under Sec.  141.33 hereof or copies of any documents then in 
existence which the State or the Administrator is entitled to inspect 
pursuant to the authority of section 1445 of the Safe Drinking Water Act 
or the equivalent provisions of State law.

[40 FR 59570, Dec. 24, 1975, as amended at 45 FR 57345, Aug. 27, 1980; 
65 FR 26022, May 4, 2000]



Sec.  141.32  [Reserved]



Sec.  141.33  Record maintenance.

    Any owner or operator of a public water system subject to the 
provisions of this part shall retain on its premises or at a convenient 
location near its premises the following records:
    (a) Records of microbiological analyses and turbidity analyses made 
pursuant to this part shall be kept for not less than 5 years. Records 
of chemical analyses made pursuant to this part shall be kept for not 
less than 10 years. Actual laboratory reports may be kept, or data may 
be transferred to tabular summaries, provided that the following 
information is included:
    (1) The date, place, and time of sampling, and the name of the 
person who collected the sample;
    (2) Identification of the sample as to whether it was a routine 
distribution system sample, check sample, raw or process water sample or 
other special purpose sample;
    (3) Date of analysis;
    (4) Laboratory and person responsible for performing analysis;
    (5) The analytical technique/method used; and
    (6) The results of the analysis.
    (b) Records of action taken by the system to correct violations of 
primary drinking water regulations shall be kept for a period not less 
than 3 years after the last action taken with respect to the particular 
violation involved.
    (c) Copies of any written reports, summaries or communications 
relating to sanitary surveys of the system conducted by the system 
itself, by a private consultant, or by any local, State or Federal 
agency, shall be kept for a period not less than 10 years after 
completion of the sanitary survey involved.
    (d) Records concerning a variance or exemption granted to the system 
shall be kept for a period ending not less than 5 years following the 
expiration of such variance or exemption.
    (e) Copies of public notices issued pursuant to subpart Q of this 
part and certifications made to the primacy agency pursuant to Sec.  
141.31 must be kept for three years after issuance.
    (f) Copies of monitoring plans developed pursuant to this part shall 
be kept for the same period of time as the

[[Page 498]]

records of analyses taken under the plan are required to be kept under 
paragraph (a) of this section, except as specified elsewhere in this 
part.

[40 FR 59570, Dec. 24, 1975, as amended at 65 FR 26022, May 4, 2000; 71 
FR 478, Jan. 4, 2006]



Sec.  141.34  [Reserved]



Sec.  141.35  Reporting for unregulated contaminant monitoring results.

    (a) General applicability. This section applies to any owner or 
operator of a public water system (PWS) required to monitor for 
unregulated contaminants under Sec.  141.40(a); such owner or operator 
is referred to as ``you.'' This section specifies the information that 
must be reported to EPA prior to the commencement of monitoring and 
describes the process for reporting monitoring results to EPA. For the 
purposes of this section, PWS ``population served'' is the retail 
population served directly by the PWS as reported to the Federal Safe 
Drinking Water Information System (SDWIS/Fed); wholesale or consecutive 
populations are not included. For purposes of this section, the term 
``finished'' means water that is introduced into the distribution system 
of a PWS and is intended for distribution and consumption without 
further treatment, except the treatment necessary to maintain water 
quality in the distribution system (e.g., booster disinfection, addition 
of corrosion control chemicals). For purposes of this section, the term 
``State'' refers to the State or Tribal government entity that has 
jurisdiction over your PWS even if that government does not have primary 
enforcement responsibility for PWSs under the Safe Drinking Water Act. 
For purposes of this section, the term ``PWS Official'' refers to the 
person at your PWS who is able to function as the official spokesperson 
for the system's Unregulated Contaminant Monitoring Regulation (UCMR) 
activities; and the term ``PWS Technical Contact'' refers to the person 
at your PWS who is responsible for the technical aspects of your UCMR 
activities, such as details concerning sampling and reporting.
    (b) Reporting by all systems. You must meet the reporting 
requirements of this paragraph if you meet the applicability criteria in 
Sec.  141.40(a)(1) and (2).
    (1) Where to submit UCMR reporting requirement information. Some of 
your reporting requirements are to be fulfilled electronically and 
others by mail. Information that must be submitted using EPA's 
electronic data reporting system must be submitted through: https://
www.epa.gov/dwucmr. Documentation that is required to be mailed can be 
submitted either: To UCMR Sampling Coordinator, USEPA, Technical Support 
Center, 26 West Martin Luther King Drive (MS 140), Cincinnati, OH 45268; 
or by email at [email protected]. In addition, you must 
notify the public of the availability of unregulated contaminant 
monitoring data as provided in subpart Q (Public Notification) of this 
part (40 CFR 141.207). Community Water Systems that detect unregulated 
contaminants under this monitoring must also address such detections as 
part of their Consumer Confidence Reports, as provided in subpart O of 
this part (40 CFR 141.151).
    (2) Contacting EPA if your system does not meet applicability 
criteria or has a status change. If you have received a letter from EPA 
or your State concerning your required monitoring and your system does 
not meet the applicability criteria for UCMR established in Sec.  
141.40(a)(1) or (2), or if a change occurs at your system that may 
affect your requirements under UCMR as defined in Sec.  141.40(a)(3) 
through (5), you must mail or email a letter to EPA, as specified in 
paragraph (b)(1) of this section. The letter must be from your PWS 
Official and must include your PWS Identification (PWSID) Code along 
with an explanation as to why the UCMR requirements are not applicable 
to your PWS, or have changed for your PWS, along with the appropriate 
contact information. EPA will make an applicability determination based 
on your letter and in consultation with the State when necessary. You 
are subject to UCMR requirements unless and until you receive a letter 
from EPA agreeing that you do not meet the applicability criteria.
    (c) Reporting by large systems. If you serve a population of more 
than 10,000

[[Page 499]]

people, and meet the applicability criteria in Sec.  141.40(a)(2)(i), 
you must meet the reporting requirements in paragraphs (c)(1) through 
(8) of this section.
    (1) Contact and zip code information. You must provide contact 
information by December 31, 2017, and provide updates within 30 days if 
this information changes. The contact information must be submitted 
using EPA's electronic data reporting system, as specified in paragraph 
(b)(1) of this section, and include the name, affiliation, mailing 
address, phone number, and email address for your PWS Technical Contact 
and your PWS Official. In addition, as a one-time reporting requirement, 
you must report the U.S. Postal Service Zip Code(s) for all areas being 
served water by your PWS.
    (2) Sampling location and inventory information. You must provide 
your sampling location(s) and inventory information by December 31, 
2017, using EPA's electronic data reporting system. You must submit, 
verify or update the following information for each sampling location, 
or for each approved representative sampling location (as specified in 
paragraph (c)(3) of this section regarding representative sampling 
locations): PWSID Code; PWS Name; PWS Facility Identification Code; PWS 
Facility Name; PWS Facility Type; Water Source Type; Sampling Point 
Identification Code; Sampling Point Name; and Sampling Point Type Code; 
(as defined in Table 1 of paragraph (e) of this section). If this 
information changes, you must report updates, including new sources and 
sampling locations that are put in use before or during the PWS' UCMR 
sampling period, to EPA's electronic data reporting system within 30 
days of the change.
    (3) Proposed ground water representative sampling locations. Some 
systems that use ground water as a source and have multiple entry points 
to the distribution system (EPTDSs) may propose monitoring at 
representative entry point(s), rather than monitor at every EPTDS, as 
follows:
    (i) Qualifications. Large PWSs that have EPA- or State-approved 
alternate EPTDS sampling locations from a previous UCMR cycle, or as 
provided for under Sec.  141.23(a)(1), Sec.  141.24(f)(1), or Sec.  
141.24(h)(1), may submit a copy of documentation from their State or EPA 
that approves their alternative sampling plan for EPTDSs. PWSs that do 
not have an approved alternative EPTDS sampling plan may submit a 
proposal to sample at representative EPTDS(s) rather than at each 
individual EPTDS if: They use ground water as a source; all of their 
well sources have either the same treatment or no treatment; and they 
have multiple EPTDSs from the same source, such as an aquifer. You must 
submit a copy of the existing alternate EPTDS sampling plan or your 
representative well proposal, as appropriate, April 19, 2017, as 
specified in paragraph (b)(1) of this section.
    (ii) Demonstration. If you are submitting a proposal to sample at 
representative EPTDS(s) rather than at each individual EPTDS, you must 
demonstrate that any EPTDS that you select as representative of the 
ground water you supply from multiple wells is associated with a well 
that draws from the same aquifer as the wells it will represent. The 
proposed well must be representative of the highest annual volume 
producing and most consistently active wells in the representative 
array. If that representative well is not in use at the scheduled 
sampling time, you must select and sample an alternative representative 
well. You must submit the following information for each proposed 
representative sampling location: PWSID Code; PWS Name; PWS Facility 
Identification Code; PWS Facility Name; PWS Facility Type; Sampling 
Point Identification Code; and Sampling Point Name (as defined in Table 
1, paragraph (e) of this section). You must also include documentation 
to support your proposal that the specified wells are representative of 
other wells. This documentation can include system-maintained well logs 
or construction drawings indicating that the representative well(s) is/
are at a representative depth, and details of well casings and grouting; 
data demonstrating relative homogeneity of water quality constituents 
(e.g., pH, dissolved oxygen, conductivity, iron, manganese) in samples 
drawn from each well; and data showing that your wells are located in a 
limited geographic area (e.g., all wells within a 0.5

[[Page 500]]

mile radius) and/or, if available, the hydrogeologic data indicating the 
time of travel separating the representative well from each of the 
individual wells it represents (e.g., all wells within a five-year time 
of travel delineation). Your proposal must be sent in writing to EPA, as 
specified in paragraph (b)(1) of this section. You must also provide a 
copy of this information to the State, unless otherwise directed by the 
State. Information about the actual or potential occurrence or non-
occurrence of contaminants in an individual well, or a well's 
vulnerability to contamination, must not be used as a basis for 
selecting a representative well.
    (iii) Approval. EPA or the State (as specified in the Partnership 
Agreement reached between the State and EPA) will review your proposal, 
coordinate any necessary changes with you, and approve the final list of 
EPTDSs where you will be required to monitor. Your plan will not be 
final until you receive written approval from EPA or the State.
    (4) Contacting EPA if your PWS has not been notified of 
requirements. If you believe you are subject to UCMR requirements, as 
defined in Sec.  141.40(a)(1) and (2)(i), and you have not been notified 
by either EPA or your State by April 19, 2017, you must send a letter to 
EPA, as specified in paragraph (b)(1) of this section. The letter must 
be from your PWS Official and must include an explanation as to why the 
UCMR requirements are applicable to your system along with the 
appropriate contact information. A copy of the letter must also be 
submitted to the State, as directed by the State. EPA will make an 
applicability determination based on your letter, and in consultation 
with the State when necessary, and will notify you regarding your 
applicability status and required sampling schedule. However, if your 
PWS meets the applicability criteria specified in Sec.  141.40(a)(2)(i), 
you are subject to the UCMR monitoring and reporting requirements, 
regardless of whether you have been notified by the State or EPA.
    (5) Notifying EPA if your PWS cannot sample according to schedule--
    (i) General rescheduling notification requirements. Large systems 
may change their monitoring schedules up to December 31, 2017, using 
EPA's electronic data reporting system, as specified in paragraph (b)(1) 
of this section. After this date has passed, if your PWS cannot sample 
according to your assigned sampling schedule (e.g., because of budget 
constraints, or if a sampling location will be closed during the 
scheduled month of monitoring), you must mail or email a letter to EPA, 
as specified in paragraph (b)(1) of this section, prior to the scheduled 
sampling date. You must include an explanation of why the samples cannot 
be taken according to the assigned schedule, and you must provide the 
alternative schedule you are requesting. You must not reschedule 
monitoring specifically to avoid sample collection during a suspected 
vulnerable period. You are subject to your assigned UCMR sampling 
schedule or the schedule that you revised on or before December 31, 
2017, unless and until you receive a letter from EPA specifying a new 
schedule.
    (ii) Exceptions to the rescheduling notification requirements. For 
ground water sampling, if the second round of sampling will be completed 
five to seven months after the first sampling event, as specified in 
Table 2 of Sec.  141.40(a)(4)(i)(B), no notification to EPA is required. 
If any ground water sampling location will be non-operational for more 
than one month before and one month after the month in which the second 
sampling event is scheduled (i.e., it is not possible for you to sample 
within the five to seven month window), you must notify EPA, as 
specified in paragraph (b)(1) of this section, explaining why the 
schedule cannot be met. You must comply with any modified schedule 
provided by EPA.
    (6) Reporting monitoring results. For UCMR samples, you must report 
all data elements specified in Table 1 of paragraph (e) of this section, 
using EPA's electronic data reporting system. You also must report any 
changes, relative to what is currently posted, made to data elements 1 
through 9 to EPA in writing, explaining the nature and purpose of the 
proposed change, as specified in paragraph (b)(1) of this section.

[[Page 501]]

    (i) Electronic reporting system. You are responsible for ensuring 
that the laboratory conducting the analysis of your unregulated 
contaminant monitoring samples (your laboratory) posts the analytical 
results to EPA's electronic reporting system. You are also responsible 
for reviewing, approving, and submitting those results to EPA.
    (ii) Reporting schedule. You must ensure that your laboratory posts 
the data to EPA's electronic data reporting system within 120 days from 
the sample collection date (sample collection must occur as specified in 
Sec.  141.40(a)(4)). You have 60 days from when the laboratory posts the 
data in EPA's electronic data reporting system to review, approve, and 
submit the data to the State and EPA, at the Web address specified in 
paragraph (b)(1) of this section. If you do not electronically approve 
and submit the laboratory data to EPA within 60 days of the laboratory's 
posting data to EPA's electronic reporting system, the data will be 
considered approved by you and available for State and EPA review.
    (7) Only one set of results accepted. If you report more than one 
set of valid results for the same sampling location and the same 
sampling event (for example, because you have had more than one 
laboratory analyze replicate samples collected under Sec.  141.40(a)(5), 
or because you have collected multiple samples during a single 
monitoring event at the same sampling location), EPA will use the 
highest of the reported values as the official result.
    (8) No reporting of previously collected data. You cannot report 
previously collected data to meet the testing and reporting requirements 
for the contaminants listed in Sec.  141.40(a)(3). All analyses must be 
performed by laboratories approved by EPA to perform UCMR analyses using 
the analytical methods specified in Table 1 of Sec.  141.40(a)(3) and 
using samples collected according to Sec.  141.40(a)(4). Such 
requirements preclude the possibility of ``grandfathering'' previously 
collected data.
    (d) Reporting by small systems. If you serve a population of 10,000 
or fewer people, and you are notified that you have been selected for 
UCMR monitoring, your reporting requirements will be specified within 
the materials that EPA sends you, including a request for contact 
information, and a request for information associated with the sampling 
kit.
    (1) Contact and zip code information. EPA will send you a notice 
requesting contact information for key individuals at your system, 
including name, affiliation, mailing address, phone number and email 
address. These individuals include your PWS Technical Contact and your 
PWS Official. You are required to provide this contact information 
within 90 days of receiving the notice from EPA as specified in 
paragraph (b)(1) of this section. If this contact information changes, 
you also must provide updates within 30 days of the change, as specified 
in paragraph (b)(1) of this section. In addition, as a one-time 
reporting requirement, you must report the U.S. Postal Service Zip 
Code(s) for all areas being served water by your PWS.
    (2) Reporting sampling information. You must provide your sampling 
location(s) by December 31, 2017, using EPA's electronic data reporting 
system, as specified in paragraph (b)(1) of this section. If this 
information changes, you must report updates, including new sources and 
sampling locations that are put in use before or during the PWS' UCMR 
sampling period, to EPA's electronic data reporting system within 30 
days of the change, as specified in paragraph (b)(1) of this section. 
You must record all data elements listed in Table 1 of paragraph (e) of 
this section on each sample form and sample bottle, as appropriate, 
provided to you by the UCMR Sampling Coordinator. You must send this 
information as specified in the instructions of your sampling kit, which 
will include the due date and return address. You must report any 
changes made in data elements 1 through 9 by emailing an explanation of 
the nature and purpose of the proposed change to EPA, as specified in 
paragraph (b)(1) of this section.
    (e) Data elements. Table 1 defines the data elements that must be 
provided for UCMR monitoring.

[[Page 502]]



   Table 1--Unregulated Contaminant Monitoring Reporting Requirements
------------------------------------------------------------------------
           Data element                          Definition
------------------------------------------------------------------------
1. Public Water System              The code used to identify each PWS.
 Identification (PWSID) Code.        The code begins with the standard 2-
                                     character postal State abbreviation
                                     or Region code; the remaining 7
                                     numbers are unique to each PWS in
                                     the State. The same identification
                                     code must be used to represent the
                                     PWS identification for all current
                                     and future UCMR monitoring.
2. Public Water System Name.......  Unique name, assigned once by the
                                     PWS.
3. Public Water System Facility     An identification code established
 Identification Code.                by the State or, at the State's
                                     discretion, by the PWS, following
                                     the format of a 5-digit number
                                     unique within each PWS for each
                                     applicable facility (i.e., for each
                                     source of water, treatment plant,
                                     distribution system, or any other
                                     facility associated with water
                                     treatment or delivery). The same
                                     identification code must be used to
                                     represent the facility for all
                                     current and future UCMR monitoring.
4. Public Water System Facility     Unique name, assigned once by the
 Name.                               PWS, for every facility ID (e.g.,
                                     Treatment Plant).
5. Public Water System Facility     That code that identifies that type
 Type.                               of facility as either:
                                    CC = consecutive connection.
                                    DS = distribution system.
                                    IN = source water influent.
                                    SS = sampling station.
                                    TP = treatment plant.
                                    OT = other.
6. Water Source Type..............  The type of source water that
                                     supplies a water system facility.
                                     Systems must report one of the
                                     following codes for each sampling
                                     location:
                                    SW = surface water (to be reported
                                     for water facilities that are
                                     served entirely by a surface water
                                     source during the twelve-month
                                     period).
                                    GW = ground water (to be reported
                                     for water facilities that are
                                     served entirely by a ground water
                                     source during the twelve-month
                                     period).
                                    GU = ground water under the direct
                                     influence of surface water (to be
                                     reported for water facilities that
                                     are served all or in part by ground
                                     water under the direct influence of
                                     surface water at any time during
                                     the twelve-month sampling period),
                                     and are not served at all by
                                     surface water during this period.
                                    MX = mixed water (to be reported for
                                     water facilities that are served by
                                     a mix of surface water, ground
                                     water and/or ground water under the
                                     direct influence of surface water
                                     during the twelve-month period).
7. Sampling Point Identification    An identification code established
 Code.                               by the State, or at the State's
                                     discretion, by the PWS, that
                                     uniquely identifies each sampling
                                     point. Each sampling code must be
                                     unique within each applicable
                                     facility, for each applicable
                                     sampling location (i.e., entry
                                     point to the distribution system,
                                     source water influent or
                                     distribution system sample at
                                     maximum residence time). The same
                                     identification code must be used to
                                     represent the sampling location for
                                     all current and future UCMR
                                     monitoring.
8. Sampling Point Name............  Unique sample point name, assigned
                                     once by the PWS, for every sample
                                     point ID (e.g., Entry Point).
9. Sampling Point Type Code.......  A code that identifies the location
                                     of the sampling point as either:
                                    SR = source water taken from plant
                                     influent; untreated water entering
                                     the water treatment plant (i.e., a
                                     location prior to any treatment).
                                    EP = entry point to the distribution
                                     system.
                                    DS = distribution system sample.
10. Disinfectant Type.............  All of the disinfectants/oxidants
                                     that have been added prior to the
                                     entry point to the distribution
                                     system. Please select all that
                                     apply:
                                    PEMB = Permanganate.
                                    HPXB = Hydrogen peroxide.
                                    CLGA = Gaseous chlorine.
                                    CLOF = Offsite Generated
                                     Hypochlorite (stored as a liquid
                                     form).
                                    CLON = Onsite Generated
                                     Hypochlorite.
                                    CAGC = Chloramine (formed with
                                     gaseous chlorine).
                                    CAOF = Chloramine (formed with
                                     offsite hypochlorite).
                                    CAON = Chloramine (formed with
                                     onsite hypochlorite).
                                    CLDB = Chlorine dioxide.
                                    OZON = Ozone.
                                    ULVL = Ultraviolet light.
                                    OTHD = All other types of
                                     disinfectant/oxidant.
                                    NODU = No disinfectant/oxidant used.
11. Treatment Information.........  Treatment information associated
                                     with the sample point. Please
                                     select all that apply:
                                    CON = Conventional (non-softening,
                                     consisting of at least coagulation/
                                     sedimentation basins and
                                     filtration).
                                    SFN = Softening.
                                    RBF = River bank filtration.
                                    PSD = Pre-sedimentation.
                                    INF = In-line filtration.
                                    DFL = Direct filtration.
                                    SSF = Slow sand filtration.
                                    BIO = Biological filtration
                                     (operated with an intention of
                                     maintaining biological activity
                                     within filter).
                                    UTR = Unfiltered treatment for
                                     surface water source.

[[Page 503]]

 
                                    GWD = Groundwater system with
                                     disinfection only.
                                    PAC = Application of powder
                                     activated carbon.
                                    GAC = Granular activated carbon
                                     adsorption (not part of filters in
                                     CON, SCO, INF, DFL, or SSF).
                                    AIR = Air stripping (packed towers,
                                     diffused gas contactors).
                                    POB = Pre-oxidation with chlorine
                                     (applied before coagulation for CON
                                     or SFN plants or before filtration
                                     for other filtration plants).
                                    MFL = Membrane filtration.
                                    IEX = Ionic exchange.
                                    DAF = Dissolved air floatation.
                                    CWL = Clear well/finished water
                                     storage without aeration.
                                    CWA = Clear well/finished water
                                     storage with aeration.
                                    ADS = Aeration in distribution
                                     system (localized treatment).
                                    OTH = All other types of treatment.
                                    NTU = No treatment used.
                                    DKN = Do not know.
12. Disinfectant Residual Type....  Disinfectant residual type in the
                                     distribution system for each HAA
                                     sample.
                                    CL2 = Chlorine (i.e., originating
                                     from addition of free chlorine
                                     only).
                                    CLO2 = chlorine dioxide.
                                    CLM = Chloramines (originating from
                                     with addition of chlorine and
                                     ammonia or pre-formed chloramines).
                                    CAC = Chlorine and chloramines (if
                                     being mixed from chlorinated and
                                     chloroaminated water).
                                    NOD = No disinfectant residual.
13. Sample Collection Date........  The date the sample is collected,
                                     reported as 4-digit year, 2-digit
                                     month, and 2-digit day (YYYY/MM/
                                     DD).
14. Sample Identification Code....  An alphanumeric value up to 30
                                     characters assigned by the
                                     laboratory to uniquely identify
                                     containers, or groups of
                                     containers, containing water
                                     samples collected at the same
                                     sampling location for the same
                                     sampling date.
15. Contaminant...................  The unregulated contaminant for
                                     which the sample is being analyzed.
16. Analytical Method Code........  The identification code of the
                                     analytical method used.
17. Extraction Batch                Laboratory assigned extraction batch
 Identification Code.                ID. Must be unique for each
                                     extraction batch within the
                                     laboratory for each method. For CCC
                                     samples report the Analysis Batch
                                     Identification Code as the value
                                     for this field. For methods without
                                     an extraction batch, leave this
                                     field null.
18. Extraction Date...............  Date for the start of the extraction
                                     batch (YYYY/MM/DD). For methods
                                     without an extraction batch, leave
                                     this field null.
19. Analysis Batch Identification   Laboratory assigned analysis batch
 Code.                               ID. Must be unique for each
                                     analysis batch within the
                                     laboratory for each method.
20. Analysis Date.................  Date for the start of the analysis
                                     batch (YYYY/MM/DD).
21. Sample Analysis Type..........  The type of sample collected and/or
                                     prepared, as well as the
                                     fortification level. Permitted
                                     values include:
                                    CF = concentration fortified; the
                                     concentration of a known
                                     contaminant added to a field sample
                                     reported with sample analysis types
                                     LFSM, LFSMD, LFB, CCC and QCS.
                                    CCC = continuing calibration check;
                                     a calibration standard containing
                                     the contaminant, the internal
                                     standard, and surrogate analyzed to
                                     verify the existing calibration for
                                     those contaminants.
                                    FS = field sample; sample collected
                                     and submitted for analysis under
                                     this rule.
                                    IS = internal standard; a standard
                                     that measures the relative response
                                     of contaminants.
                                    LFB = laboratory fortified blank; an
                                     aliquot of reagent water fortified
                                     with known quantities of the
                                     contaminants and all preservation
                                     compounds.
                                    LRB = laboratory reagent blank; an
                                     aliquot of reagent water treated
                                     exactly as a field sample,
                                     including the addition of
                                     preservatives, internal standards,
                                     and surrogates to determine if
                                     interferences are present in the
                                     laboratory, reagents, or other
                                     equipment.
                                    LFSM = laboratory fortified sample
                                     matrix; a UCMR field sample with a
                                     known amount of the contaminant of
                                     interest and all preservation
                                     compounds added.
                                    LFSMD = laboratory fortified sample
                                     matrix duplicate; duplicate of the
                                     laboratory fortified sample matrix.
                                    QCS = quality control sample; a
                                     sample prepared with a source
                                     external to the one used for
                                     initial calibration and CCC. The
                                     QCS is used to check calibration
                                     standard integrity.
                                    QHS = quality HAA sample; HAA sample
                                     collected and submitted for quality
                                     control purposes.
                                    SUR = surrogate standard; a standard
                                     that assesses method performance
                                     for each extraction.
22. Analytical Results--Sign......  A value indicating whether the
                                     sample analysis result was:
                                    (<) ``less than'' means the
                                     contaminant was not detected, or
                                     was detected at a level below the
                                     Minimum Reporting Level.
                                    (=) ``equal to'' means the
                                     contaminant was detected at the
                                     level reported in ``Analytical
                                     Result-- Measured Value.''
23. Analytical Result--Measured     The actual numeric value of the
 Value.                              analytical results for: Field
                                     samples; laboratory fortified
                                     matrix samples; laboratory
                                     fortified sample matrix duplicates;
                                     and concentration fortified.
24. Additional Value..............  Represents the true value or the
                                     fortified concentration for spiked
                                     samples for QC Sample Analysis
                                     Types (CCC, EQC, LFB, LFSM and
                                     LFSMD). For Sample Analysis Type FS
                                     and LRB and for IS and surrogate QC
                                     Contaminants, leave this field
                                     null.

[[Page 504]]

 
25. Laboratory Identification Code  The code, assigned by EPA, used to
                                     identify each laboratory. The code
                                     begins with the standard two-
                                     character State postal
                                     abbreviation; the remaining five
                                     numbers are unique to each
                                     laboratory in the State.
26. Sample Event Code.............  A code assigned by the PWS for each
                                     sample event. This will associate
                                     samples with the PWS monitoring
                                     plan to allow EPA to track
                                     compliance and completeness.
                                     Systems must assign the following
                                     codes:
                                    SEC1, SEC2, SEC3, SEC4, SEC5, SEC6,
                                     SEC7 and SEC8--represent samples
                                     collected to meet UCMR Assessment
                                     Monitoring requirements for
                                     cyanotoxins; where ``SEC1''
                                     represents the first sampling
                                     period, ``SEC2'' the second period
                                     and so forth, for all eight
                                     sampling events.
                                    SEA1, SEA2, SEA3 and SEA4--represent
                                     samples collected to meet UCMR
                                     Assessment Monitoring requirements
                                     for the additional contaminants;
                                     where ``SEA1'' and ``SEA2''
                                     represent the first and second
                                     sampling period for all water
                                     types; and ``SEA3'' and ``SEA4''
                                     represent the third and fourth
                                     sampling period for SW and GU
                                     sources only.
27. Bloom Occurrence..............  A yes or no answer provided by the
                                     PWS for each cyanotoxin sample
                                     event.
                                    Question: Preceding the finished
                                     water sample collection, did you
                                     observe an algal bloom in your
                                     source waters near the intake?
                                    YES = if yes, select all the YESs
                                     that apply:
                                     YD = yes, on the day the UCMR
                                     cyanotoxin sample was collected.
                                     YW = yes, between the day the
                                     sample was taken and the past week.
                                     YM = yes, between the past week and
                                     past month.
                                     YY = yes, between the past month
                                     and past year.
                                     YP = yes, prior to the past year.
                                    NO = have never seen a bloom.
28. Cyanotoxin Occurrence.........  A yes or no answer provided by the
                                     PWS for each cyanotoxin sample
                                     event.
                                    Question: Preceding the finished
                                     water sample collection, were
                                     cyanotoxins ever detected in your
                                     source waters near the intake and
                                     prior to any treatment (based on
                                     sampling by you or another party)?
                                    YES = if yes, select all the YESs
                                     that apply:
                                     YD = yes, on the day the UCMR
                                     cyanotoxin sample was collected.
                                     YW = yes, between the day the
                                     sample was taken and the past week.
                                     YM = yes, between the past week and
                                     past month.
                                     YY = yes, between the past month
                                     and past year.
                                     YP = yes, prior to the past year.
                                    NO = have never detected cyanotoxins
                                     in source water.
                                    NS = unaware of any source water
                                     cyanotoxin sampling.
                                    Select all that apply (i.e., all
                                     that were detected) if you answered
                                     YES to detecting cyanotoxins in
                                     source water:
                                     MIC = Microcystins.
                                     CYL = Cylindrospermopsin.
                                     ANA = Anatoxin-A.
                                     SAX = Saxitoxins.
                                     OTH = Other.
                                     DK = do not know.
29. Indicator of Possible Bloom--   A yes or no answer provided by the
 Treatment.                          PWS for each cyanotoxin sample
                                     event.
                                    Question: Preceding the finished
                                     water sample collection, did you
                                     notice any changes in your
                                     treatment system operation and/or
                                     treated water quality that may
                                     indicate a bloom in the source
                                     water?
                                    YES = if yes, select all that apply:
                                     DFR = Decrease in filter runtimes.
                                     ITF = Increase in turbidity in
                                     filtered water.
                                     ICD = Need for increased coagulant
                                     dose.
                                     TOI = Increase in taste and odor
                                     issues in finished water.
                                     IOD = Need for increase in oxidant/
                                     disinfectant dose.
                                     IDB = Increase in TTHM/HAA5 in
                                     finished water.
                                     OTH = Describe other changes.
                                    NO = no changes.
30. Indicator of Possible Bloom--   A yes or no answer provided by the
 Source Water Quality Parameters.    PWS for each cyanotoxin sample
                                     event.
                                    Question: Preceding the finished
                                     water sample collection, did you
                                     observe any notable changes in
                                     source water quality parameters (if
                                     measured)?
                                    YES = if yes, select all that apply
                                     to the source water:
                                     ITP = Increase in water
                                     temperature.
                                     ITU = Increase in turbidity.
                                     IAL = Increase in alkalinity.
                                     ITO = Increase in total organic
                                     carbon.
                                     ICD = Increase in chlorine demand.
                                     IPH = Increase in pH.
                                     ICA = Increase in chlorophyll a.
                                     IPY = Increase in phycocyanin.
                                     INU = Increase in nutrients
                                     (example: nitrogen or phosphorus).
                                     OTH = Describe other changes.
                                    NO = no changes observed.
------------------------------------------------------------------------


[[Page 505]]


[72 FR 389, Jan. 4, 2007, as amended at 77 FR 26096, May 2, 2012; 81 FR 
92684, Dec. 20, 2016]



  Subpart E_Special Regulations, Including Monitoring Regulations and 
                         Prohibition on Lead Use



Sec.  141.40  Monitoring requirements for unregulated contaminants.

    (a) General applicability. This section specifies the monitoring and 
quality control requirements that must be followed if you own or operate 
a public water system (PWS) that is subject to the Unregulated 
Contaminant Monitoring Regulation (UCMR), as specified in paragraphs 
(a)(1) and (2) of this section. In addition, this section specifies the 
UCMR requirements for State and Tribal participation. For the purposes 
of this section, PWS ``population served,'' ``State,'' '' PWS 
Official,'' ``PWS Technical Contact,'' and ``finished water'' apply as 
defined in Sec.  141.35(a). The determination of whether a PWS is 
required to monitor under this rule is based on the type of system 
(e.g., community water system, non-transient non-community water system, 
etc.), and its retail population, as indicated by SDWIS/Fed on December 
31, 2015.
    (1) Applicability to transient non-community systems. If you own or 
operate a transient non-community water system, you are not subject to 
monitoring requirements in this section.
    (2) Applicability to community water systems and non-transient non-
community water systems--(i) Large systems. If you own or operate a 
retail PWS (other than a transient non-community system) that serves 
more than 10,000 people, you must monitor according to the 
specifications in this paragraph (a)(2)(i). If you believe that your 
applicability status is different than EPA has specified in the 
notification letter that you received, or if you are subject to UCMR 
requirements and you have not been notified by either EPA or your State, 
you must report to EPA, as specified in Sec.  141.35(b)(2) or (c)(4).
    (A) Assessment monitoring. You must monitor for the contaminants on 
List 1, per Table 1, UCMR Contaminant List, in paragraph (a)(3) of this 
section. If you serve a retail population of more than 10,000 people, 
you are required to perform this monitoring regardless of whether you 
have been notified by the State or EPA.
    (B) Screening Survey. You must monitor for the unregulated 
contaminants on List 2 (Screening Survey) of Table 1, as specified in 
paragraph (a)(3) of this section, if your system serves 10,001 to 
100,000 people and you are notified by EPA or your State that you are 
part of the State Monitoring Plan for Screening Survey testing. If your 
system serves more than 100,000 people, you are required to conduct this 
Screening Survey testing regardless of whether you have been notified by 
the State or EPA.
    (C) Pre-Screen Testing. You must monitor for the unregulated 
contaminants on List 3 of Table 1, in paragraph (a)(3) of this section, 
if notified by your State or EPA that you are part of the Pre-Screen 
Testing.
    (ii) Small systems. Small PWSs, as defined in this paragraph, will 
not be selected to monitor for any more than one of the three monitoring 
lists provided in Table 1, UCMR Contaminant List, in paragraph (a)(3) of 
this section. EPA will provide sample containers, provide pre-paid air 
bills for shipping the sampling materials, conduct the laboratory 
analysis, and report and review monitoring results for all small systems 
selected to conduct monitoring under paragraphs (a)(2)(ii)(A) through 
(C) of this section. If you own or operate a PWS that serves 10,000 or 
fewer people you must monitor as follows:
    (A) Assessment monitoring. You must monitor for the contaminants on 
List 1 per Table 1, in paragraph (a)(3) of this section, if you are 
notified by your State or EPA that you are part of the State Monitoring 
Plan for Assessment Monitoring.
    (B) Screening Survey. You must monitor for the unregulated 
contaminants on List 2 of Table 1, in paragraph (a)(3) of this section, 
if notified by your State or EPA that you are part of the State 
Monitoring Plan for the Screening Survey.

[[Page 506]]

    (C) Pre-screen testing. You must monitor for the contaminants on 
List 3 of Table 1, in paragraph (a)(3) of this section if you are 
notified by your State or EPA that you are part of the State Monitoring 
Plan for Pre-Screen Testing.
    (3) Analytes to be monitored. Lists 1, 2, and 3 contaminants are 
provided in the following table:

                                                             Table 1--UCMR Contaminant List
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                   4--Minimum
          1--Contaminant            2--CAS Registry No.     3--Analytical      reporting level b       5--Sampling           6--Period during which
                                                              methods a                                 location c         monitoring to be completed
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                             List 1: Assessment Monitoring Cyanotoxin Chemical Contaminants
--------------------------------------------------------------------------------------------------------------------------------------------------------
``total microcystin''............  N/A.................  EPA 546............  0.3 [micro]g/L.....  EPTDS..............  3/1/2018-11/30/2020.
anatoxin-a.......................  64285-06-9..........  EPA 545............  0.03 [micro]g/L....  EPTDS..............  3/1/2018-11/30/2020.
cylindrospermopsin...............  143545-90-8.........  EPA 545............  0.09 [micro]g/L....  EPTDS..............  3/1/2018-11/30/2020.
microcystin-LA...................  96180-79-9..........  EPA 544............  0.008 [micro]g/L...  EPTDS..............  3/1/2018-11/30/2020.
microcystin-LF...................  154037-70-4.........  EPA 544............  0.006 [micro]g/L...  EPTDS..............  3/1/2018-11/30/2020.
microcystin-LR...................  101043-37-2.........  EPA 544............  0.02 [micro]g/L....  EPTDS..............  3/1/2018-11/30/2020.
microcystin-LY...................  123304-10-9.........  EPA 544............  0.009 [micro]g/L...  EPTDS..............  3/1/2018-11/30/2020.
microcystin-RR...................  111755-37-4.........  EPA 544............  0.006 [micro]g/L...  EPTDS..............  3/1/2018-11/30/2020.
microcystin-YR...................  101064-48-6.........  EPA 544............  0.02 [micro]g/L....  EPTDS..............  3/1/2018-11/30/2020.
nodularin........................  118399-22-7.........  EPA 544............  0.005 [micro]g/L...  EPTDS..............  3/1/2018-11/30/2020.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                             List 1: Assessment Monitoring Additional Chemical Contaminants
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                         Metals
--------------------------------------------------------------------------------------------------------------------------------------------------------
germanium........................  7440-56-4...........  EPA 200.8, ASTM      0.3 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
                                                          D5673-10, SM 3125.
manganese........................  7439-96-5...........  EPA 200.8, ASTM      0.4 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
                                                          D5673-10, SM 3125.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                   Pesticides and a Pesticide Manufacturing Byproduct
--------------------------------------------------------------------------------------------------------------------------------------------------------
alpha-hexachlorocyclohexane......  319-84-6............  EPA 525.3..........  0.01 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
chlorpyrifos.....................  2921-88-2...........  EPA 525.3..........  0.03 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
dimethipin.......................  55290-64-7..........  EPA 525.3..........  0.2 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
ethoprop.........................  13194-48-4..........  EPA 525.3..........  0.03 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
oxyfluorfen......................  42874-03-3..........  EPA 525.3..........  0.05 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
profenofos.......................  41198-08-7..........  EPA 525.3..........  0.3 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
tebuconazole.....................  107534-96-3.........  EPA 525.3..........  0.2 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
total permethrin (cis- & trans-).  52645-53-1..........  EPA 525.3..........  0.04 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
tribufos.........................  78-48-8.............  EPA 525.3..........  0.07 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                       Brominated Haloacetic Acid (HAA) Groups d e
--------------------------------------------------------------------------------------------------------------------------------------------------------
HAA5.............................  N/A.................  EPA 552.3 or EPA     N/A................  D/DBPR HAA location  1/1/2018-12/31/2020.
                                                          557.
HAA6Br...........................  N/A.................  EPA 552.3 or EPA     N/A................  D/DBPR HAA location  1/1/2018-12/31/2020.
                                                          557.
HAA9.............................  N/A.................  EPA 552.3 or EPA     N/A................  D/DBPR HAA location  1/1/2018-12/31/2020.
                                                          557.
--------------------------------------------------------------------------------------------------------------------------------------------------------

[[Page 507]]

 
                                                                        Alcohols
--------------------------------------------------------------------------------------------------------------------------------------------------------
1-butanol........................  71-36-3.............  EPA 541............  2.0 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
2-methoxyethanol.................  109-86-4............  EPA 541............  0.4 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
2-propen-1-ol....................  107-18-6............  EPA 541............  0.5 [micro]g/L.....  EPTDS..............  1/1/2018-12/31/2020.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                              Other Semivolatile Chemicals
--------------------------------------------------------------------------------------------------------------------------------------------------------
butylated hydroxanisole..........  25013-16-5..........  EPA 530............  0.03 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
o-toluidine......................  95-53-4.............  EPA 530............  0.007 [micro]g/L...  EPTDS..............  1/1/2018-12/31/2020.
quinoline........................  91-22-5.............  EPA 530............  0.02 [micro]g/L....  EPTDS..............  1/1/2018-12/31/2020.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                List 2: Screening Survey
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reserved.........................  Reserved............  Reserved...........  Reserved...........  Reserved...........  Reserved.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                               List 3: Pre-Screen Testing
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reserved.........................  Reserved............  Reserved...........  Reserved...........  Reserved...........  Reserved.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Column headings are:
1--Contaminant: The name of the contaminant to be analyzed.
2--CAS (Chemical Abstract Service) Registry Number or Identification Number: A unique number identifying the chemical contaminants.
3--Analytical Methods: Method numbers identifying the methods that must be used to test the contaminants.
4--Minimum Reporting Level (MRL): The value and unit of measure at or above which the concentration of the contaminant must be measured using the
  approved analytical methods. If EPA determines, after the first six months of monitoring that the specified MRLs result in excessive resampling, EPA
  will establish alternate MRLs and will notify affected PWSs and laboratories of the new MRLs. N/A is defined as non-applicable.
5--Sampling Location: The locations within a PWS at which samples must be collected.
6--Period During Which Monitoring to be Completed: The time period during which the sampling and testing will occur for the indicated contaminant.
a The analytical procedures shall be performed in accordance with the documents associated with each method, see paragraph (c) of this section.
b The MRL is the minimum concentration of each analyte that must be reported to EPA.
c With the exception of HAA monitoring, sampling must occur at entry points to the distribution system (EPTDSs), after treatment is applied, that
  represent each non-emergency water source in routine use over the 12-month period of monitoring. Systems that purchase water with multiple connections
  from the same wholesaler may select one representative connection from that wholesaler. This EPTDS sampling location must be representative of the
  highest annual volume connections. If the connection selected as the representative EPTDS is not available for sampling, an alternate highest volume
  representative connection must be sampled. See 40 CFR 141.35(c)(3) for an explanation of the requirements related to the use of representative GW
  EPTDSs. Sampling for UCMR 4 HAA groups must be conducted at the Disinfectants and Disinfection Byproduct Rule (D/DBPR) sampling locations (40 CFR
  141.622).
d UCMR 4 HAA monitoring applies only to those PWSs that are subject to D/DBPR HAA5 monitoring requirements.
e PWSs that purchase 100 percent of their water (``consecutive systems'') are not required to collect UCMR 4 source water samples for TOC or bromide
  analyses. Sampling for TOC and bromide must otherwise occur at source water influent locations representing untreated water entering the water
  treatment plant (i.e., a location prior to any treatment). SW and GWUDI systems subject to the D/DBPR TOC monitoring must use their D/DBPR TOC source
  water sampling site(s) from 40 CFR 141.132 for UCMR 4 TOC and bromide samples. SW and GWUDI systems that are not subject to D/DBPR TOC monitoring will
  use their Long Term 2 Enhance Surface Water Treatment Rule (LT2) source water sampling site(s) (40 CFR 141.703) for UCMR 4 TOC and bromide samples.
  Ground water systems that are subject to the D/DBPRs, and therefore subject to UCMR 4 HAA monitoring, will take TOC and bromide samples at their
  influents entering their treatment train. TOC and bromide must be collected at the same time as HAA samples. These indicator samples must be collected
  at a single source water influent using methods already approved for compliance monitoring. TOC methods include: SM 5310 B, SM 5310 C, SM 5310 D (21st
  edition), or SM 5310 B-00, SM 5310 C-00, SM 5310 D-00 (SM Online), EPA Method 415.3 (Rev. 1.1 or 1.2). Bromide methods include: EPA Methods 300.0
  (Rev. 2.1), 300.1 (Rev. 1.0), 317.0 (Rev. 2.0), 326.0 (Rev. 1.0) or ASTM D 6581-12. The MRLs for the individual HAAs are discussed in paragraph
  (a)(5)(v) of this section.

    (4) Sampling requirements--(i) Large systems. If you serve more than 
10,000 people and meet the UCMR applicability criteria specified in 
paragraph (a)(2)(i) of this section, you must comply with the 
requirements specified in paragraphs (a)(4)(i)(A) through (I) of this 
section. Your samples must be collected according to the schedule that 
you are assigned by EPA or your State, or the schedule that you revised 
using EPA's electronic data reporting system on or before December 31, 
2017. Your schedule must follow both the timing and frequency of 
monitoring specified in Tables 1 and 2 of this section.
    (A) Monitoring period. You must collect the samples in one 
continuous 12-month period for List 1 Assessment Monitoring, and, if 
applicable, for List 2 Screening Survey, or List 3 Pre-Screen Testing, 
during the time frame indicated in column 6 of Table 1, in paragraph 
(a)(3) of this section. EPA or

[[Page 508]]

your State will specify the month(s) and year(s) in which your 
monitoring must occur. As specified in Sec.  141.35(c)(5), you must 
contact EPA if you believe you cannot conduct monitoring according to 
your schedule.
    (B) Frequency. You must collect the samples within the timeframe and 
according to the frequency specified by contaminant type and water 
source type for each sampling location, as specified in Table 2, in this 
paragraph. For the second or subsequent round of sampling, if a sample 
location is non-operational for more than one month before and one month 
after the scheduled sampling month (i.e., it is not possible for you to 
sample within the window specified in Table 2, in this paragraph), you 
must notify EPA as specified in Sec.  141.35(c)(5) to reschedule your 
sampling.

                       Table 2--Monitoring Frequency by Contaminant and Water Source Types
----------------------------------------------------------------------------------------------------------------
          Contaminant type              Water source type           Timeframe               Frequency \1\
----------------------------------------------------------------------------------------------------------------
List 1 Cyanotoxins Chemicals.......  Surface water or        March-November........  You must monitor twice a
                                      Ground water under                              month for four consecutive
                                      the direct influence                            months (total of eight
                                      of surface water                                sampling events). Sample
                                      (GWUDI).                                        events must occur two
                                                                                      weeks apart.
List 1 Contaminants--Additional      Surface water or GWUDI  12 months.............  You must monitor for four
 Chemicals.                                                                           consecutive quarters.
                                                                                      Sample events must occur
                                                                                      three months apart.
                                                                                      (Example: If first
                                                                                      monitoring is in January,
                                                                                      the second monitoring must
                                                                                      occur any time in April,
                                                                                      the third any time in July
                                                                                      and the fourth any time in
                                                                                      October).
                                     Ground water..........  12 months.............  You must monitor twice in a
                                                                                      consecutive 12-month
                                                                                      period. Sample events must
                                                                                      occur 5-7 months apart.
                                                                                      (Example: If the first
                                                                                      monitoring event is in
                                                                                      April, the second
                                                                                      monitoring event must
                                                                                      occur any time in
                                                                                      September, October or
                                                                                      November).
----------------------------------------------------------------------------------------------------------------
\1\ Systems must assign a sample event code for each contaminant listed in Table 1. Sample event codes must be
  assigned by the PWS for each sample event. For more information on sample event codes see Sec.   141.35(e)
  Table 1.

    (C) Location. You must collect samples for each List 1 Assessment 
Monitoring contaminant, and, if applicable, for each List 2 Screening 
Survey, or List 3 Pre-Screen Testing contaminant, as specified in Table 
1, in paragraph (a)(3) of this section. Samples must be collected at 
each sample point that is specified in column 5 and footnote c of Table 
1, in paragraph (a)(3) of this section. PWSs conducting List 1 
monitoring for the brominated HAA groups must collect TOC and bromide 
samples as specified in footnote d of Table 1, in paragraph (a)(3) of 
this section. If you are a GW system with multiple EPTDSs, and you 
request and receive approval from EPA or the State for sampling at 
representative EPTDS(s), as specified in Sec.  141.35(c)(3), you must 
collect your samples from the approved representative sampling 
location(s).
    (D) Sampling instructions. For each List 1 Assessment Monitoring 
contaminant, and, if applicable, for each List 2 Screening Survey, or 
List 3 Pre-Screen Testing contaminant, you must follow the sampling 
procedure for the method specified in column 3 of Table 1, in paragraph 
(a)(3) of this section. In addition, you must not composite (that is, 
combine, mix, or blend) the samples; you must collect and preserve each 
sample separately.
    (E) Sample collection and shipping time. If you must ship the 
samples for analysis, you must collect the samples early enough in the 
day to allow adequate time to send the samples for overnight delivery to 
the laboratory. You should not collect samples on Friday, Saturday, or 
Sunday because sampling on these days may not allow samples to be 
shipped and received at the laboratory at the required temperature, 
unless you have made special arrangements with your laboratory to 
receive the samples.
    (F) Analytical methods. For each contaminant, you must use the 
respective analytical methods for List 1, and, if applicable, for List 
2, or List 3 that are specified in column 3 of Table 1, in paragraph 
(a)(3) of this section; report values at or above the minimum reporting 
levels for List 1, and, if applicable, for List 2 Screening Survey, or 
List 3 Pre-Screen Testing, that are

[[Page 509]]

specified in column 4 of Table 1, in paragraph (a)(3) of this section; 
and conduct the quality control procedures specified in paragraph (a)(5) 
of this section.
    (G) Laboratory errors or sampling deviations. If the laboratory data 
do not meet the required QC criteria, as specified in paragraph (a)(5) 
of this section, or you do not follow the required sampling procedures, 
as specified in paragraphs (a)(4) of this section, you must resample 
within 30 days of being informed or becoming aware of these facts. This 
resampling is not for the purpose of confirming previous results, but to 
correct the sampling or laboratory error. All systems must report the 
results obtained from the first sampling for each sampling period, 
except for cases of sampling or laboratory errors. For the purposes of 
this rule, no samples are to be recollected for the purposes of 
confirming the results observed in a previous sampling.
    (H) Analysis. For the List 1 contaminants, and, if applicable, List 
2 Screening Survey, or List 3 Pre-Screen Testing contaminants, 
identified in Table 1, paragraph (a)(3) of this section, you must 
arrange for testing by a laboratory that has been approved by EPA 
according to requirements in paragraph (a)(5)(ii) of this section.
    (I) Review and reporting of results. After you have received the 
laboratory results, you must review, approve, and submit the system 
information, and sample collection data and test results. You must 
report the results as provided in Sec.  141.35(c)(6).
    (ii) Small systems. If you serve 10,000 or fewer people and are 
notified that you are part of the State Monitoring Plan for Assessment 
Monitoring, Screening Survey or Pre-Screen monitoring, you must comply 
with the requirements specified in paragraphs (a)(4)(ii)(A) through (H) 
of this section. If EPA or the State informs you that they will be 
collecting your UCMR samples, you must assist them in identifying the 
appropriate sampling locations and in collecting the samples.
    (A) Monitoring period and frequency. You must collect samples at the 
times specified for you by the State or EPA. Your schedule must follow 
both the timing of monitoring specified in Table 1, List 1, and, if 
applicable, List 2, or List 3, and the frequency of monitoring in Table 
2 of this section.
    (B) Location. You must collect samples at the locations specified 
for you by the State or EPA.
    (C) Sample kits. You must store and maintain the sample collection 
kits sent to you by the UCMR Sampling Coordinator in accordance with the 
kit's instructions. The sample kit will include all necessary 
containers, packing materials and cold packs, instructions for 
collecting the sample and sample treatment (such as dechlorination or 
preservation), report forms for each sample, contact name and telephone 
number for the laboratory, and a prepaid return shipping docket and 
return address label. If any of the materials listed in the kit's 
instructions are not included in the kit or arrive damaged, you must 
notify the UCMR Sampling Coordinator who sent you the sample collection 
kits.
    (D) Sampling instructions. You must comply with the instructions 
sent to you by the State or EPA concerning the use of containers, 
collection (how to fill the sample bottle), dechlorination and/or 
preservation, and sealing and preparation of sample and shipping 
containers for shipment. You must not composite (that is, combine, mix, 
or blend) the samples. You also must collect, preserve, and test each 
sample separately. You must also comply with the instructions sent to 
you by the UCMR Sampling Coordinator concerning the handling of sample 
containers for specific contaminants.
    (E) Sampling deviations. If you do not collect a sample according to 
the instructions provided to you for a listed contaminant, you must 
report the deviation within 7 days of the scheduled monitoring on the 
sample reporting form, as specified in Sec.  141.35(d)(2). You must 
resample following instructions that you will be sent from the UCMR 
Sampling Coordinator or State. A copy of the form must be sent to the 
laboratory with the recollected samples, and to the UCMR Sampling 
Coordinator.
    (F) [Reserved]
    (G) Sampling forms. You must completely fill out each of the 
sampling forms and bottles sent to you by the

[[Page 510]]

UCMR Sampling Coordinator, including data elements listed in Sec.  
141.35(e) for each sample, as specified in Sec.  141.35(d)(2). You must 
sign and date the sampling forms.
    (H) Sample collection and shipping. You must collect the samples 
early enough in the day to allow adequate time to send the samples for 
overnight delivery to the laboratory. You should not collect samples on 
Friday, Saturday, or Sunday because sampling on these days may not allow 
samples to be shipped and received at the laboratory at the required 
temperature unless you have made special arrangements with EPA for the 
laboratory to receive the samples. Once you have collected the samples 
and completely filled in the sampling forms, you must send the samples 
and the sampling forms to the laboratory designated on the air bill.
    (iii) Phased sample analysis for microcystins. You must collect the 
three required samples (one each for EPA Methods 544, 545 and 546 
(ELISA) at the EPTDS) for each sampling event, but not all samples may 
need to be analyzed. If the Method 546 ELISA result is less than 0.3 
[micro]g/L, report that result and do not analyze the EPA Method 544 
sample for that sample event. If the Method 546 ELISA result is greater 
than or equal to 0.3 [micro]g/L, report the value and analyze the other 
microcystin sample using EPA Method 544. You must analyze the EPA Method 
545 sample for each sample event for Cylindrospermopsin and anatoxin-a 
only.
    (5) Quality control requirements. If your system serves more than 
10,000 people, you must ensure that the quality control requirements 
listed below are met during your sampling procedures and by the 
laboratory conducting your analyses. You must also ensure that all 
method quality control procedures and all UCMR quality control 
procedures are followed.
    (i) Sample collection/preservation. You must follow the sample 
collection and preservation requirements for the specified method for 
each of the contaminants in Table 1, in paragraph (a)(3) of this 
section. These requirements specify sample containers, collection, 
dechlorination, preservation, storage, sample holding time, and extract 
storage and/or holding time that you must assure that the laboratory 
follow.
    (ii) Laboratory approval for Lists 1, List 2 and List 3. To be 
approved to conduct UCMR testing, the laboratory must be certified under 
Sec.  141.28 for one or more compliance analyses; demonstrate for each 
analytical method it plans to use for UCMR testing that it can meet the 
Initial Demonstration of Capability (IDC) requirements detailed in the 
analytical methods specified in column 3 of Table 1, in paragraph (a)(3) 
of this section; and successfully participate in the UCMR Proficiency 
Testing (PT) Program administered by EPA for each analytical method it 
plans to use for UCMR testing. UCMR laboratory approval decisions will 
be granted on an individual method basis for the methods listed in 
column 3 of Table 1 in paragraph (a)(3) of this section for List 1, List 
2, and List 3 contaminants. Laboratory approval is contingent upon the 
capability of the laboratory to post monitoring data to the EPA 
electronic data reporting system. To participate in the UCMR Laboratory 
Approval Program, the laboratory must complete and submit the necessary 
registration forms by February 21, 2017, and necessary application 
material April 19, 2017. Correspondence must be addressed to: UCMR 
Laboratory Approval Coordinator, USEPA, Technical Support Center, 26 
West Martin Luther King Drive, (MS 140), Cincinnati, OH 45268; or 
emailed to EPA at: [email protected].
    (iii) Minimum Reporting Level. The MRL is an estimate of the 
quantitation limit. Assuming good instrumentation and experienced 
analysts, an MRL is achievable, with 95% confidence, by 75% of 
laboratories nationwide.
    (A) Validation of laboratory performance. Your laboratory must be 
capable of quantifying each contaminant listed in Table 1, at or below 
the MRL specified in column 4 of Table 1, in paragraph (a)(3) of this 
section. You must ensure that the laboratory completes and has on file 
and available for your inspection, records of two distinct procedures. 
First, your laboratory must have conducted an IDC involving replicate 
analyses at or below the MRL as described in this paragraph. Second, for

[[Page 511]]

each day that UCMR analyses are conducted by your laboratory, a 
validation of its ability to quantify each contaminant, at or below the 
MRL specified in column 4 of Table 1, in paragraph (a)(3) of this 
section, following the procedure listed in paragraph (a)(5)(iii)(B) of 
this section, must be performed. The procedure for initial validation of 
laboratory performance at or below the MRL is as follows:
    (1) All laboratories performing analysis under UCMR must demonstrate 
that they are capable of meeting data quality objectives at or below the 
MRL listed in Table 1, column 4, in paragraph (a)(3) of this section.
    (2) The MRL, or any concentration below the MRL, at which 
performance is being evaluated, must be contained within the range of 
calibration. The calibration curve regression model and the range of 
calibration levels that are used in these performance validation steps 
must be used in all routine sample analyses used to comply with this 
regulation. Only straight line or quadratic regression models are 
allowed. The use of either weighted or unweighted models is permitted. 
The use of cubic regression models is not permitted.
    (3) Replicate analyses of at least seven (7) fortified samples in 
reagent water must be performed at or below the MRL for each analyte, 
and must be processed through the entire method procedure (i.e., 
including extraction, where applicable, and with all preservatives).
    (4) A prediction interval of results (PIR), which is based on the 
estimated arithmetic mean of analytical results and the estimated sample 
standard deviation of measurement results, must be determined by 
Equation 1:
[GRAPHIC] [TIFF OMITTED] TR04JA07.000

Where:

t is the Student's t value with df degrees of freedom and confidence 
          level (1-[alpha]),
s is the sample standard deviation of n replicate samples fortified at 
          the MRL,
n is the number of replicates.

    (5) The values needed to calculate the PIR using Equation 1 are: 
Number of replicates (n); Student's t value with a two-sided 99% 
confidence level for n number of replicates; the average (mean) of at 
least seven replicates; and the sample standard deviation. Factor 1 is 
referred to as the Half Range PIR (HRPIR).
[GRAPHIC] [TIFF OMITTED] TR04JA07.001


For a certain number of replicates and for a certain confidence level in 
Student's t, this factor
[GRAPHIC] [TIFF OMITTED] TR04JA07.002


is constant, and can be tabulated according to replicate number and 
confidence level for the Student's t. Table 3 in this paragraph lists 
the constant factor (C) for replicate sample numbers 7 through 10 with a 
confidence level of 99% for Student's t.

    (6) The HRPIR is calculated by Equation 2:
    [GRAPHIC] [TIFF OMITTED] TR04JA07.003
    
    (7) The PIR is calculated by Equation 3:
    [GRAPHIC] [TIFF OMITTED] TR04JA07.004
    

[[Page 512]]



Table 3--The Constant Factor (C) to be Multiplied by the Standard Deviation to Determine the Half Range Interval
                                of the PIR (Student's t 99% Confidence Level) \a\
----------------------------------------------------------------------------------------------------------------
                                                                            Constant factor (C) to be multiplied
             Replicates                        Degrees of freedom                 by the standard deviation
----------------------------------------------------------------------------------------------------------------
                               7                                     6                                 3.963
----------------------------------------------------------------------------------------------------------------
                               8                                     7                                 3.711
----------------------------------------------------------------------------------------------------------------
                               9                                     8                                 3.536
----------------------------------------------------------------------------------------------------------------
                              10                                     9                                3.409
----------------------------------------------------------------------------------------------------------------
\a\ The critical t-value for a two-sided 99% confidence interval is equivalent to the critical t-value for a one-
  sided 99.5% confidence interval, due to the symmetry of the t-distribution. PIR = Prediction Interval of
  Results.

    (8) The lower and upper result limits of the PIR must be converted 
to percent recovery of the concentration being tested. To pass criteria 
at a certain level, the PIR lower recovery limits cannot be lower than 
the lower recovery limits of the QC interval (50%), and the PIR upper 
recovery limits cannot be greater than the upper recovery limits of the 
QC interval (150%). When either of the PIR recovery limits falls outside 
of either bound of the QC interval of recovery (higher than 150% or less 
than 50%), laboratory performance is not validated at the concentration 
evaluated. If the PIR limits are contained within both bounds of the QC 
interval, laboratory performance is validated for that analyte.
    (B) Quality control requirements for validation of laboratory 
performance at or below the MRL.
    (1) You must ensure that the calibration curve regression model and 
that the range of calibration levels that are used in these performance 
validation steps are used in future routine sample analysis. Only 
straight line or quadratic regression models are allowed. The use of 
either weighted or unweighted models is permitted. The use of cubic 
regression models is not permitted.
    (2) You must ensure, once your laboratory has performed an IDC as 
specified in each analytical method (demonstrating that DQOs are met at 
or below an MRL), that a daily performance check is performed for each 
analyte and method. A single laboratory blank, fortified at or below the 
MRL for each analyte, must be processed through the entire method 
procedure. The measured concentration for each analyte must be converted 
to a percent recovery, and if the recovery is within 50%-150% 
(inclusive), the daily performance of the laboratory has been validated. 
The results for any analyte for which 50%-150% recovery cannot be 
demonstrated during the daily check are not valid. Laboratories may 
elect to re-run the daily performance check sample if the performance 
for any analyte or analytes cannot be validated. If performance is 
validated for these analytes, the laboratory performance is considered 
validated. Alternatively, the laboratory may re-calibrate and repeat the 
performance validation process for all analytes.
    (iv) Laboratory fortified sample matrix and laboratory fortified 
sample matrix duplicate. You must ensure that your laboratory prepares 
and analyzes the Laboratory Fortified Sample Matrix (LFSM) sample for 
accuracy and Laboratory Fortified Sample Matrix Duplicate (LFSMD) 
samples for precision to determine method accuracy and precision for all 
contaminants in Table 1, in paragraph (a)(3) of this section. LFSM/LFSMD 
samples must be prepared using a sample collected and analyzed in 
accordance with UCMR requirements and analyzed at a frequency of 5% (or 
1 LFSM/LFSMD set per every 20 samples) or with each sample batch, 
whichever is more frequent. In addition, the LFSM/LFSMD fortification 
concentrations must be alternated between a low-level fortification and 
mid-level fortification approximately 50% of the time. (For example: A 
set of 40 samples will require preparation and analysis of 2 LFSM/LFSMD 
paired samples. The first LFSM/LFSMD paired sample set must be fortified 
at

[[Page 513]]

either the low-level or mid-level, and the second LFSM/LFSMD paired 
sample set must be fortified with the other standard, either the low-
level or mid-level, whichever was not used for the initial LFSM/LFSMD 
paired sample set.) The low-level LFSM/LFSMD fortification concentration 
must be within 50% of the MRL for each contaminant 
(e.g., for an MRL of 1 [micro]g/L the acceptable fortification levels 
must be between 0.5 [micro]g/L and 1.5 [micro]g/L). The mid-level LFSM/
LFSMD fortification concentration must be within 20% of the mid-level calibration standard for each 
contaminant, and is to represent, where possible and where the 
laboratory has data from previously analyzed samples, an approximate 
average concentration observed in previous analyses of that analyte. 
There are no UCMR contaminant recovery acceptance criteria specified for 
LFSM/LFSMD analyses. All LFSM/LFSMD data are to be reported.
    (v) Method defined quality control. You must ensure that your 
laboratory analyzes Laboratory Fortified Blanks and conducts Laboratory 
Performance Checks, as appropriate to the method's requirements, for 
those methods listed in Table 1, column 3, in paragraph (a)(3) of this 
section. Each method specifies acceptance criteria for these QC checks. 
The following HAA results must be reported using EPA's electronic data 
reporting system for quality control purposes.

[[Page 514]]



                                                                 Table 4--HAA QC Results
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                       4--Minimum
        1--Contaminant             2--CAS            3--Analytical methods a       reporting level b   5--HAA6Br Group   6--HAA9 Group    7--HAA5 Group
                                Registry No.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                         Brominated Haloacetic Acid (HAA) Groups
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bromochloroacetic acid (BCAA)       5589-96-8  EPA 552.3 or EPA 557..............  0.3 [micro]g/L...
Bromodichloroacetic acid           71133-14-7  EPA 552.3 or EPA 557..............  0.5 [micro]g/L...
 (BDCAA).
Chlorodibromoacetic acid            5278-95-5  EPA 552.3 or EPA 557..............  0.3 [micro]g/L...  HAA6Br
 (CDBAA).
Tribromoacetic acid (TBAA)...         75-96-7  EPA 552.3 or EPA 557..............  2.0 [micro]g/L...
Monobromoacetic acid (MBAA)..         79-08-3  EPA 552.3 or EPA 557..............  0.3 [micro]g/L...
                                                                                                                                        ----------------
Dibromoacetic acid (DBAA)....        631-64-1  EPA 552.3 or EPA 557..............  0.3 [micro]g/L...  ................  HAA9
                                                                                                     ------------------
Dichloroacetic acid (DCAA)...         79-43-6  EPA 552.3 or EPA 557..............  0.2 [micro]g/L...
Monochloroacetic acid (MCAA).         79-11-8  EPA 552.3 or EPA 557..............  2.0 [micro]g/L...  ................  ...............  HAA5
Trichloroacetic acid (TCAA)..         76-03-9  EPA 552.3 or EPA 557..............  0.5 [micro]g/L...
--------------------------------------------------------------------------------------------------------------------------------------------------------
Column headings are:
1--Contaminant: The name of the contaminant to be analyzed.
2--CAS (Chemical Abstract Service) Registry Number or Identification Number: A unique number identifying the chemical contaminants.
3--Analytical Methods: Method numbers identifying the methods that must be used to test the contaminants.
4--Minimum Reporting Level (MRL): The value and unit of measure at or above which the concentration of the contaminant must be measured using the
  approved analytical methods. If EPA determines, after the first six months of monitoring that the specified MRLs result in excessive resampling, EPA
  will establish alternate MRLs and will notify affected PWSs and laboratories of the new MRLs.
5-7--HAA groups identified in paragraph (a)(3) of this section to be monitored as UCMR contaminants.
a The analytical procedures shall be performed in accordance with the documents associated with each method, see paragraph (c) of this section, and must
  meet all quality control requirements outlined paragraph (a)(5) of this section.
b The MRL is the minimum concentration of each analyte that must be reported to EPA.


[[Page 515]]

    (vi) Reporting. You must require your laboratory to submit these 
data electronically to the State and EPA using EPA's electronic data 
reporting system, accessible at https://www.epa.gov/dwucmr, within 120 
days from the sample collection date. You then have 60 days from when 
the laboratory posts the data to review, approve and submit the data to 
the State and EPA, via EPA's electronic data reporting system. If you do 
not electronically approve and submit the laboratory data to EPA within 
60 days of the laboratory posting data to EPA's electronic reporting 
system, the data will be considered approved and available for State and 
EPA review.
    (6) Violation of this rule--(i) Monitoring violations. Any failure 
to monitor in accordance with Sec.  141.40(a)(3)-(5) is a monitoring 
violation.
    (ii) Reporting violations. Any failure to report in accordance with 
Sec.  141.35 is a reporting violation.
    (b) Petitions and waivers by States--(1) Governors' petition for 
additional contaminants. The Safe Drinking Water Act allows Governors of 
seven (7) or more States to petition the EPA Administrator to add one or 
more contaminants to the UCMR Contaminant List in paragraph (a)(3) of 
this section. The petition must clearly identify the reason(s) for 
adding the contaminant(s) to the monitoring list, including the 
potential risk to public health, particularly any information that might 
be available regarding disproportional risks to the health and safety of 
children, the expected occurrence documented by any available data, any 
analytical methods known or proposed to be used to test for the 
contaminant(s), and any other information that could assist the 
Administrator in determining which contaminants present the greatest 
public health concern and should, therefore, be included on the UCMR 
Contaminant List in paragraph (a)(3) of this section.
    (2) State-wide waivers. A State can waive monitoring requirements 
only with EPA approval and under very limited conditions. Conditions and 
procedures for obtaining a waiver are as follows:
    (i) Application. A State may apply to EPA for a State-wide waiver 
from the unregulated contaminant monitoring requirements for PWSs 
serving more than 10,000 people. To apply for such a waiver, the State 
must submit an application to EPA that includes the following 
information: The list of contaminants on the UCMR Contaminant List for 
which a waiver is requested, along with documentation for each 
contaminant in the request demonstrating that the contaminants or their 
parent compounds do not occur naturally in the State, and certifying 
that during the past 15 years they have not been used, applied, stored, 
disposed of, released, or detected in the source waters or distribution 
systems in the State.
    (ii) Approval. EPA will review State applications and notify the 
State whether it accepts or rejects the request. The State must receive 
written approval from EPA before issuing a State-wide waiver.
    (c) Incorporation by reference. These standards are incorporated by 
reference into this section with the approval of the Director of the 
Federal Register under 5 U.S.C. 552(a) and 1 CFR part 51. All approved 
material is available for inspection either electronically at http://
www.regulations.gov, in hard copy at the Water Docket, EPA/DC, and from 
the sources as follows. The Public Reading Room (EPA West, Room 3334, 
1301 Constitution Ave. NW., Washington, DC) is open from 8:30 a.m. to 
4:30 p.m., Monday through Friday, excluding legal holidays. The 
telephone number for this Public Reading Room is (202) 566-1744, and the 
telephone number for the Water Docket is (202) 566-2426. The material is 
also available for inspection at the National Archives and Records 
Administration (NARA). For information on the availability of this 
material at NARA, call (202) 741-6030 or go to http://www.archives.gov/
federal-register/cfr/about.html.
    (1) U.S. Environmental Protection Agency, Water Docket, EPA/DC, EPA 
West, Room 3334, 1301 Constitution Ave. NW., Washington, DC 20004.
    (i) Method 200.8 ``Determination of Trace Elements in Waters and 
Wastes by Inductively Coupled Plasma--Mass Spectrometry,'' Revision 5.4, 
EMMC

[[Page 516]]

Version, 1994. Available on the Internet at https://www.nemi.gov.
    (ii) Method 300.0 ``Determination of Inorganic Anions by Ion 
Chromatography Samples,'' Revision 2.1, August 1993. Available on the 
Internet at https://www.nemi.gov.
    (iii) Method 300.1 ``Determination of Inorganic Anions in Drinking 
Water by Ion Chromatography,'' Revision 1.0, 1997. Available on the 
Internet at https://www.epa.gov/dwanalyticalmethods.
    (iv) Method 317.0 ``Determination of Inorganic Oxyhalide 
Disinfection By-Products in Drinking Water Using Ion Chromatography with 
the Addition of a Postcolumn Reagent for Trace Bromate Analysis,'' 
Revision 2.0, July 2001, EPA 815-B-01-001. Available on the Internet at 
https://www.epa.gov/dwanalyticalmethods.
    (v) Method 326.0 ``Determination of Inorganic Oxyhalide Disinfection 
By-Products in Drinking Water Using Ion Chromatography Incorporating the 
Addition of a Suppressor Acidified Postcolumn Reagent for Trace Bromate 
Analysis,'' Revision 1.0, June 2002, EPA 815-R-03-007. Available on the 
Internet at https://www.epa.gov/dwanalyticalmethods.
    (vi) Method 415.3 ``Determination of Total Organic Carbon and 
Specific UV Absorbance at 254 nm in Source Water and Drinking Water,'' 
Revision 1.1, February 2005, EPA/600/R-05/055. Available on the Internet 
at https://www.epa.gov/water-research/epa-drinking-water-research-
methods.
    (vii) Method 415.3 ``Determination of Total Organic Carbon and 
Specific UV Absorbance at 254 nm in Source Water and Drinking Water,'' 
Revision 1.2, September 2009, EPA/600/R-09/122. Available on the 
Internet at https://www.epa.gov/water-research/epa-drinking-water-
research-methods.
    (viii) Method 525.3 ``Determination of Semivolatile Organic 
Chemicals in Drinking Water by Solid Phase Extraction and Capillary 
Column Gas Chromatography/Mass Spectrometry (GC/MS),'' Version 1.0, 
February 2012, EPA/600/R-12/010. Available on the Internet https://
www.epa.gov/water-research/epa-drinking-water-research-methods.
    (ix) Method 530 ``Determination of Select Semivolatile Organic 
Chemicals in Drinking Water by Solid Phase Extraction and Gas 
Chromatography/Mass Spectrometry (GC/MS),'' Version 1.0, January 2015, 
EPA/600/R-14/442. Available on the Internet at https://www.epa.gov/
water-research/epa-drinking-water-research-methods.
    (x) EPA Method 541: ``Determination of 1-Butanol, 1,4-Dioxane, 2-
Methoxyethanol and 2-Propen-1-ol in Drinking Water by Solid Phase 
Extraction and Gas Chromatography/Mass Spectrometry,'' November 2015, 
EPA 815-R-15-011. Available on the Internet at https://www.epa.gov/
water-research/epa-drinking-water-research-methods.
    (xi) Method 544 ``Determination of Microcystins and Nodularin in 
Drinking Water by Solid Phase Extraction and Liquid Chromatography/
Tandem Mass Spectrometry (LC/MS/MS),'' Version 1.0, February 2015, EPA 
600-R-14/474. Available on the Internet at https://www.epa.gov/water-
research/epa-drinking-water-research-methods.
    (xii) EPA Method 545: ``Determination of Cylindrospermopsin and 
Anatoxin-a in Drinking Water by Liquid Chromatography Electrospray 
Ionization Tandem Mass Spectrometry (LC/ESI-MS/MS),'' April 2015, EPA 
815-R-15-009. Available on the Internet at https://www.epa.gov/
dwanalyticalmethods.
    (xiii) EPA Method 546: ``Determination of Total Microcystins and 
Nodularins in Drinking Water and Ambient Water by Adda Enzyme-Linked 
Immunosorbent Assay,'' August 2016, EPA-815-B-16-011. Available on the 
Internet at https://www.epa.gov/dwanalyticalmethods.
    (xiv) Method 552.3 ``Determination of Haloacetic Acids and Dalapon 
in Drinking Water by Liquid-Liquid Microextraction, Derivatization, and 
Gas Chromatography with Electron Capture Detection,'' Revision 1.0, July 
2003, EPA 815-B-03-002. Available on the Internet at https://
www.epa.gov/dwanalyticalmethods.
    (xv) EPA Method 557: ``Determination of Haloacetic Acids, Bromate, 
and Dalapon in Drinking Water by Ion Chromatography Electrospray 
Ionization Tandem Mass Spectrometry (IC-ESI-MS/MS),'' Version 1.0, 
September 2009, EPA 815-B-09-012. Available on

[[Page 517]]

the Internet at https://www.epa.gov/dwanalyticalmethods.
    (2) American Public Health Association--Standard Test Method for 
Elements in Water by Inductively Coupled Plasma-Mass Spectrometry,'' 
approved August 1, 2010. Available for purchase on the Internet at 
http://www.astm.org/Standards/D5673.htm.
    (i) ``Standard Methods for the Examination of Water & Wastewater,'' 
21st edition (2005).
    (A) SM 3125 ``Metals by Inductively Coupled Plasma/Mass 
Spectrometry.''
    (B) SM 5310B ``Total Organic Carbon (TOC): High-Temperature 
Combustion Method.''
    (C) SM 5310C ``Total Organic Carbon (TOC): Persulfate-UV or Heated-
Persulfate Oxidation Method.''
    (D) SM 5310D ``Total Organic Carbon (TOC): Wet-Oxidation Method.''
    (ii) The following methods are from ``Standard Methods Online.,'' 
approved 2000 (unless noted). Available for purchase on the Internet at 
http://www.standardmethods.org.
    (A) SM 3125 ``Metals by Inductively Coupled Plasma/Mass 
Spectrometry'' Editorial revisions, 2011 (SM 3125-09).
    (B) SM 5310B ``Total Organic Carbon: High-Temperature Combustion 
Method,'' (5310B-00).
    (C) SM 5310C ``Total Organic Carbon: Persulfate-UV or Heated-
Persulfate Oxidation Method,'' (5310C-00).
    (D) SM 5310D ``Total Organic Carbon: Wet-Oxidation Method,'' (5310D-
00).
    (3) ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 
19428-2959.
    (i) ASTM D5673-10 ``Standard Test Method for Elements in Water by 
Inductively Coupled Plasma-Mass Spectrometry,'' approved August 1, 2010. 
Available for purchase on the Internet at http://www.astm.org/Standards/
D5673.htm.
    (ii) ASTM D6581-12 ``Standard Test Methods for Bromate, Bromide, 
Chlorate, and Chlorite in Drinking Water by Suppressed Ion 
Chromatography,'' approved March 1, 2012. Available for purchase on the 
Internet at http://www.astm.org/Standards/D6581.htm.

[72 FR 393, Jan. 4, 2007; 72 FR 3916, Jan. 26, 2007, as amended at 77 FR 
26098, May 2, 2012; 81 FR 92688, Dec. 20, 2016]



Sec.  141.41  Special monitoring for sodium.

    (a) Suppliers of water for community public water systems shall 
collect and analyze one sample per plant at the entry point of the 
distribution system for the determination of sodium concentration 
levels; samples must be collected and analyzed annually for systems 
utilizing surface water sources in whole or in part, and at least every 
three years for systems utilizing solely ground water sources. The 
minimum number of samples required to be taken by the system shall be 
based on the number of treatment plants used by the system, except that 
multiple wells drawing raw water from a single aquifer may, with the 
State approval, be considered one treatment plant for determining the 
minimum number of samples. The supplier of water may be required by the 
State to collect and analyze water samples for sodium more frequently in 
locations where the sodium content is variable.
    (b) The supplier of water shall report to EPA and/or the State the 
results of the analyses for sodium within the first 10 days of the month 
following the month in which the sample results were received or within 
the first 10 days following the end of the required monitoring period as 
stipulated by the State, whichever of these is first. If more than 
annual sampling is required the supplier shall report the average sodium 
concentration within 10 days of the month following the month in which 
the analytical results of the last sample used for the annual average 
was received. The supplier of water shall not be required to report the 
results to EPA where the State has adopted this regulation and results 
are reported to the State. The supplier shall report the results to EPA 
where the State has not adopted this regulation.
    (c) The supplier of water shall notify appropriate local and State 
public health officials of the sodium levels by written notice by direct 
mail within three months. A copy of each notice required to be provided 
by this paragraph shall be sent to EPA and/or the State within 10 days 
of its issuance. The supplier of water is not required to notify 
appropriate local and State public health officials of the sodium levels

[[Page 518]]

where the State provides such notices in lieu of the supplier.
    (d) Analyses for sodium shall be conducted as directed in Sec.  
141.23(k)(1).

[45 FR 57345, Aug. 27, 1980, as amended at 59 FR 62470, Dec. 5, 1994]



Sec.  141.42  Special monitoring for corrosivity characteristics.

    (a)-(c) [Reserved]
    (d) Community water supply systems shall identify whether the 
following construction materials are present in their distribution 
system and report to the State:

Lead from piping, solder, caulking, interior lining of distribution 
mains, alloys and home plumbing.
Copper from piping and alloys, service lines, and home plumbing.
Galvanized piping, service lines, and home plumbing.
Ferrous piping materials such as cast iron and steel.
Asbestos cement pipe.


In addition, States may require identification and reporting of other 
materials of construction present in distribution systems that may 
contribute contaminants to the drinking water, such as:

Vinyl lined asbestos cement pipe.
Coal tar lined pipes and tanks.

[45 FR 57346, Aug. 27, 1980; 47 FR 10999, Mar. 12, 1982, as amended at 
59 FR 62470, Dec. 5, 1994]



Sec.  141.43  Prohibition on use of lead pipes, solder, and flux.

    (a) In general--(1) Prohibition. Any pipe, solder, or flux, which is 
used after June 19, 1986, in the installation or repair of--
    (i) Any public water system, or
    (ii) Any plumbing in a residential or nonresidential facility 
providing water for human consumption which is connected to a public 
water system shall be lead free as defined by paragraph (d) of this 
section. This paragraph (a)(1) shall not apply to leaded joints 
necessary for the repair of cast iron pipes.
    (2) [Reserved]
    (b) State enforcement--(1) Enforcement of prohibition. The 
requirements of paragraph (a)(1) of this section shall be enforced in 
all States effective June 19, 1988. States shall enforce such 
requirements through State or local plumbing codes, or such other means 
of enforcement as the State may determine to be appropriate.
    (2) [Reserved]
    (c) Penalties. If the Administrator determines that a State is not 
enforcing the requirements of paragraph (a) of this section, as required 
pursuant to paragraph (b) of this section, the Administrator may 
withhold up to 5 percent of Federal funds available to that State for 
State program grants under section 1443(a) of the Act.
    (d) Definition of lead free. For purposes of this section, the term 
lead free:
    (1) When used with respect to solders and flux refers to solders and 
flux containing not more than 0.2 percent lead;
    (2) When used with respect to pipes and pipe fittings refers to 
pipes and pipe fittings containing not more than 8.0 percent lead; and
    (3) When used with respect to plumbing fittings and fixtures 
intended by the manufacturer to dispense water for human ingestion 
refers to fittings and fixtures that are in compliance with standards 
established in accordance with 42 U.S.C. 300g-6(e).

[52 FR 20674, June 2, 1987, as amended at 65 FR 2003, Jan. 12, 2000]



     Subpart F_Maximum Contaminant Level Goals and Maximum Residual 
                        Disinfectant Level Goals



Sec.  141.50  Maximum contaminant level goals for organic contaminants.

    (a) MCLGs are zero for the following contaminants:

    (1) Benzene
    (2) Vinyl chloride
    (3) Carbon tetrachloride
    (4) 1,2-dichloroethane
    (5) Trichloroethylene
    (6) Acrylamide
    (7) Alachlor
    (8) Chlordane
    (9) Dibromochloropropane
    (10) 1,2-Dichloropropane
    (11) Epichlorohydrin
    (12) Ethylene dibromide
    (13) Heptachlor
    (14) Heptachlor epoxide
    (15) Pentachlorophenol

[[Page 519]]

    (16) Polychlorinated biphenyls (PCBs)
    (17) Tetrachloroethylene
    (18) Toxaphene
    (19) Benzo[a]pyrene
    (20) Dichloromethane (methylene chloride)
    (21) Di(2-ethylhexyl)phthalate
    (22) Hexachlorobenzene
    (23) 2,3,7,8-TCDD (Dioxin)
    (b) MCLGs for the following contaminants are as indicated:

------------------------------------------------------------------------
                                                                MCLG in
                         Contaminant                              mg/l
------------------------------------------------------------------------
(1) 1,1-Dichloroethylene.....................................     0.007
(2) 1,1,1-Trichloroethane....................................     0.20
(3) para-Dichlorobenzene.....................................     0.075
(4) Aldicarb.................................................     0.001
(5) Aldicarb sulfoxide.......................................     0.001
(6) Aldicarb sulfone.........................................     0.001
(7) Atrazine.................................................     0.003
(8) Carbofuran...............................................     0.04
(9) o-Dichlorobenzene........................................     0.6
(10) cis-1,2-Dichloroethylene................................     0.07
(11) trans-1,2-Dichloroethylene..............................     0.1
(12) 2,4-D...................................................     0.07
(13) Ethylbenzene............................................     0.7
(14) Lindane.................................................     0.0002
(15) Methoxychlor............................................     0.04
(16) Monochlorobenzene.......................................     0.1
(17) Styrene.................................................     0.1
(18) Toluene.................................................     1
(19) 2,4,5-TP................................................     0.05
(20) Xylenes (total).........................................    10
(21) Dalapon.................................................     0.2
(22) Di(2-ethylhexyl)adipate.................................      .4
(23) Dinoseb.................................................      .007
(24) Diquat..................................................      .02
(25) Endothall...............................................      .1
(26) Endrin..................................................      .002
(27) Glyphosate..............................................      .7
(28) Hexachlorocyclopentadiene...............................      .05
(29) Oxamyl (Vydate).........................................      .2
(30) Picloram................................................      .5
(31) Simazine................................................      .004
(32) 1,2,4-Trichlorobenzene..................................      .07
(33) 1,1,2-Trichloroethane...................................      .003
------------------------------------------------------------------------


[50 FR 46901, Nov. 13, 1985, as amended at 52 FR 20674, June 2, 1987; 52 
FR 25716, July 8, 1987; 56 FR 3592, Jan. 30, 1991; 56 FR 30280, July 1, 
1991; 57 FR 31846, July 17, 1992]



Sec.  141.51  Maximum contaminant level goals for inorganic contaminants.

    (a) [Reserved]
    (b) MCLGs for the following contaminants are as indicated:

------------------------------------------------------------------------
                  Contaminant                          MCLG (mg/l)
------------------------------------------------------------------------
Antimony......................................                     0.006
Arsenic.......................................                  zero \1\
Asbestos......................................    7 Million fibers/liter
                                                         (longer than 10
                                                              [micro]m).
Barium........................................                         2
Beryllium.....................................                      .004
Cadmium.......................................                     0.005
Chromium......................................                       0.1
Copper........................................                       1.3
Cyanide (as free Cyanide).....................                        .2
Fluoride......................................                       4.0
Lead..........................................                      zero
Mercury.......................................                     0.002
Nitrate.......................................         10 (as Nitrogen).
Nitrite.......................................          1 (as Nitrogen).
Total Nitrate + Nitrite.......................         10 (as Nitrogen).
Selenium......................................                      0.05
Thallium......................................                     .0005
------------------------------------------------------------------------
\1\ This value for arsenic is effective January 23, 2006. Until then,
  there is no MCLG.


[50 FR 47155, Nov. 14, 1985, as amended at 52 FR 20674, June 2, 1987; 56 
FR 3593, Jan. 30, 1991; 56 FR 26548, June 7, 1991; 56 FR 30280, July 1, 
1991; 57 FR 31846, July 17, 1992; 60 FR 33932, June 29, 1995; 66 FR 
7063, Jan. 22, 2001]



Sec.  141.52  Maximum contaminant level goals for microbiological contaminants.

    (a) MCLGs for the following contaminants are as indicated:

------------------------------------------------------------------------
                Contaminant                             MCLG
------------------------------------------------------------------------
(1) Giardia lamblia.......................  zero
(2) Viruses...............................  zero
(3) Legionella............................  zero
(4) Total coliforms (including fecal).....  zero
coliforms and Escherichia coli............
(5) Cryptosporidium.......................  zero
(6) Escherichia coli (E. coli)............  zero
------------------------------------------------------------------------

    (b) The MCLG identified in paragraph (a)(4) of this section is 
applicable until March 31, 2016. The MCLG identified in paragraph (a)(6) 
of this section is applicable beginning April 1, 2016.

[78 FR 10347, Feb. 13, 2013]



Sec.  141.53  Maximum contaminant level goals for disinfection byproducts.

    MCLGs for the following disinfection byproducts are as indicated:

------------------------------------------------------------------------
                                                                MCLG (mg/
                    Disinfection byproduct                         L)
------------------------------------------------------------------------
Bromodichloromethane..........................................   zero
Bromoform.....................................................   zero
Bromate.......................................................   zero
Chlorite......................................................      0.8
Chloroform....................................................      0.07
Dibromochloromethane..........................................      0.06
Dichloroacetic acid...........................................   zero
Monochloroacetic acid.........................................      0.07
Trichloroacetic acid..........................................      0.02
------------------------------------------------------------------------


[63 FR 69465, Dec. 16, 1998, as amended at 65 FR 34405, May 30, 2000; 71 
FR 478, Jan. 4, 2006]

[[Page 520]]



Sec.  141.54  Maximum residual disinfectant level goals for disinfectants.

    MRDLGs for disinfectants are as follows:

------------------------------------------------------------------------
          Disinfectant residual                     MRDLG(mg/L)
------------------------------------------------------------------------
Chlorine................................  4 (as Cl 2).
Chloramines.............................  4 (as Cl 2).
Chlorine dioxide........................  0.8 (as ClO2)
------------------------------------------------------------------------


[63 FR 69465, Dec. 16, 1998]



Sec.  141.55  Maximum contaminant level goals for radionuclides.

    MCLGs for radionuclides are as indicated in the following table:

------------------------------------------------------------------------
                 Contaminant                              MCLG
------------------------------------------------------------------------
1. Combined radium-226 and radium-228........  Zero.
2. Gross alpha particle activity (excluding    Zero.
 radon and uranium).
3. Beta particle and photon radioactivity....  Zero.
4. Uranium...................................  Zero.
------------------------------------------------------------------------


[65 FR 76748, Dec. 7, 2000]



     Subpart G_National Primary Drinking Water Regulations: Maximum 
       Contaminant Levels and Maximum Residual Disinfectant Levels



Sec.  141.60  Effective dates.

    (a) The effective dates for Sec.  141.61 are as follows:
    (1) The effective date for paragraphs (a)(1) through (a)(8) of Sec.  
141.61 is January 9, 1989.
    (2) The effective date for paragraphs (a)(9) through (a)(18) and 
(c)(1) through (c)(18) of Sec.  141.61 is July 30, 1992.
    (3) The effective date for paragraphs (a)(19) through (a)(21), 
(c)(19) through (c)(25), and (c)(27) through (c)(33) of Sec.  141.61 is 
January 17, 1994. The effective date of Sec.  141.61(c)(26) is August 
17, 1992.

    (b) The effective dates for Sec.  141.62 are as follows:
    (1) The effective date of paragraph (b)(1) of Sec.  141.62 is 
October 2, 1987.
    (2) The effective date for paragraphs (b)(2) and (b)(4) through 
(b)(10) of Sec.  141.62 is July 30, 1992.
    (3) The effective date for paragraphs (b)(11) through (b)(15) of 
Sec.  141.62 is January 17, 1994.
    (4) The effective date for Sec.  141.62(b)(16) is January 23, 2006.

[56 FR 3593, Jan. 30, 1991, as amended at 57 FR 31846, July 17, 1992; 59 
FR 34324, July 1, 1994; 66 FR 7063, Jan. 22, 2001]



Sec.  141.61  Maximum contaminant levels for organic contaminants.

    (a) The following maximum contaminant levels for organic 
contaminants apply to community and non-transient, non-community water 
systems.

------------------------------------------------------------------------
            CAS No.                  Contaminant           MCL (mg/l)
------------------------------------------------------------------------
 (1) 75-01-4..................  Vinyl chloride.......         0.002
 (2) 71-43-2..................  Benzene..............         0.005
 (3) 56-23-5..................  Carbon tetrachloride.         0.005
 (4) 107-06-2.................  1,2-Dichloroethane...         0.005
 (5) 79-01-6..................  Trichloroethylene....         0.005
 (6) 106-46-7.................  para-Dichlorobenzene.         0.075
 (7) 75-35-4..................  1,1-Dichloroethylene.         0.007
 (8) 71-55-6..................  1,1,1-Trichloroethane         0.2
 (9) 156-59-2.................  cis-1,2-                      0.07
                                 Dichloroethylene.
 (10) 78-87-5.................  1,2-Dichloropropane..         0.005
 (11) 100-41-4................  Ethylbenzene.........         0.7
 (12) 108-90-7................  Monochlorobenzene....         0.1
 (13) 95-50-1.................  o-Dichlorobenzene....         0.6
 (14) 100-42-5................  Styrene..............         0.1
 (15) 127-18-4................  Tetrachloroethylene..         0.005
 (16) 108-88-3................  Toluene..............         1
 (17) 156-60-5................  trans-1,2-                    0.1
                                 Dichloroethylene.
 (18) 1330-20-7...............  Xylenes (total)......        10
 (19) 75-09-2.................  Dichloromethane......         0.005
 (20) 120-82-1................  1,2,4-Trichloro-               .07
                                 benzene.
 (21) 79-00-5.................  1,1,2-Trichloro-               .005
                                 ethane.
------------------------------------------------------------------------

    (b) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies as indicated in the Table below granular activated carbon 
(GAC),

[[Page 521]]

packed tower aeration (PTA), or oxidation (OX) as the best technology 
treatment technique, or other means available for achieving compliance 
with the maximum contaminant level for organic contaminants identified 
in paragraphs (a) and (c) of this section:

                        BAT for Organic Contaminants Listed in Sec.   141.61 (a) and (c)
----------------------------------------------------------------------------------------------------------------
                   CAS No.                                 Contaminant                 GAC       PTA       OX
----------------------------------------------------------------------------------------------------------------
15972-60-8..................................  Alachlor............................      X
116-06-3....................................  Aldicarb............................      X
1646-88-4...................................  Aldicarb sulfone....................      X
1646-87-3...................................  Aldicarb sulfoxide..................      X
1912-24-9...................................  Atrazine............................      X
71-43-2.....................................  Benzene.............................      X         X
50-32-8.....................................  Benzo[a]pyrene......................      X
1563-66-2...................................  Carbofuran..........................      X
56-23-5.....................................  Carbon tetrachloride................      X         X
57-74-9.....................................  Chlordane...........................      X
75-99-0.....................................  Dalapon.............................      X
94-75-7.....................................  2,4-D...............................      X
103-23-1....................................  Di (2-ethylhexyl) adipate...........      X         X
117-81-7....................................  Di (2-ethylhexyl) phthalate.........      X
96-12-8.....................................  Dibromochloropropane (DBCP).........      X         X
95-50-1.....................................  o-Dichlorobenzene...................      X         X
106-46-7....................................  para-Dichlorobenzene................      X         X
107-06-2....................................  1,2-Dichloroethane..................      X         X
75-35-4.....................................  1,1-Dichloroethylene................      X         X
156-59-2....................................  cis-1,2-Dichloroethylene............      X         X
156-60-5....................................  trans-1,2-Dichloroethylene..........      X         X
75-09-2.....................................  Dichloromethane.....................  ........      X
78-87-5.....................................  1,2-Dichloropropane.................      X         X
88-85-7.....................................  Dinoseb.............................      X
85-00-7.....................................  Diquat..............................      X
145-73-3....................................  Endothall...........................      X
72-20-8.....................................  Endrin..............................      X
100-41-4....................................  Ethylbenzene........................      X         X
106-93-4....................................  Ethylene Dibromide (EDB)............      X         X
1071-83-6...................................  Gylphosate..........................  ........  ........      X
76-44-8.....................................  Heptachlor..........................      X
1024-57-3...................................  Heptachlor epoxide..................      X
118-74-1....................................  Hexachlorobenzene...................      X
77-47-3.....................................  Hexachlorocyclopentadiene...........      X         X
58-89-9.....................................  Lindane.............................      X
72-43-5.....................................  Methoxychlor........................      X
108-90-7....................................  Monochlorobenzene...................      X         X
23135-22-0..................................  Oxamyl (Vydate).....................      X
87-86-5.....................................  Pentachlorophenol...................      X
1918-02-1...................................  Picloram............................      X
1336-36-3...................................  Polychlorinated biphenyls (PCB).....      X
122-34-9....................................  Simazine............................      X
100-42-5....................................  Styrene.............................      X         X
1746-01-6...................................  2,3,7,8-TCDD (Dioxin)...............      X
127-18-4....................................  Tetrachloroethylene.................      X         X
108-88-3....................................  Toluene.............................      X         X
8001-35-2...................................  Toxaphene...........................      X
93-72-1.....................................  2,4,5-TP (Silvex)...................      X
120-82-1....................................  1,2,4-Trichlorobenzene..............      X         X
71-55-6.....................................  1,1,1-Trichloroethane...............      X         X
79-00-5.....................................  1,1,2-Trichloroethane...............      X         X
79-01-6.....................................  Trichloroethylene...................      X         X
75-01-4.....................................  Vinyl chloride......................  ........      X
1330-20-7...................................  Xylene..............................      X         X     ........
----------------------------------------------------------------------------------------------------------------

    (c) The following maximum contaminant levels for synthetic organic 
contaminants apply to community water systems and non-transient, non-
community water systems:

------------------------------------------------------------------------
            CAS No.                  Contaminant           MCL (mg/l)
------------------------------------------------------------------------
 (1) 15972-60-8...............  Alachlor.............         0.002

[[Page 522]]

 
 (2) 116-06-3.................  Aldicarb.............         0.003
 (3) 1646-87-3................  Aldicarb sulfoxide...         0.004
 (4) 1646-87-4................  Aldicarb sulfone.....         0.002
 (5) 1912-24-9................  Atrazine.............         0.003
 (6) 1563-66-2................  Carbofuran...........         0.04
 (7) 57-74-9..................  Chlordane............         0.002
 (8) 96-12-8..................  Dibromochloropropane.         0.0002
 (9) 94-75-7..................  2,4-D................         0.07
(10) 106-93-4.................  Ethylene dibromide...         0.00005
(11) 76-44-8..................  Heptachlor...........         0.0004
(12) 1024-57-3................  Heptachlor epoxide...         0.0002
(13) 58-89-9..................  Lindane..............         0.0002
(14) 72-43-5..................  Methoxychlor.........         0.04
(15) 1336-36-3................  Polychlorinated               0.0005
                                 biphenyls.
(16) 87-86-5..................  Pentachlorophenol....         0.001
(17) 8001-35-2................  Toxaphene............         0.003
(18) 93-72-1..................  2,4,5-TP.............         0.05
(19) 50-32-8..................  Benzo[a]pyrene.......         0.0002
(20) 75-99-0..................  Dalapon..............         0.2
(21) 103-23-1.................  Di(2-ethylhexyl)              0.4
                                 adipate.
(22) 117-81-7.................  Di(2-ethylhexyl)              0.006
                                 phthalate.
(23) 88-85-7..................  Dinoseb..............         0.007
(24) 85-00-7..................  Diquat...............         0.02
(25) 145-73-3.................  Endothall............         0.1
(26) 72-20-8..................  Endrin...............         0.002
(27) 1071-53-6................  Glyphosate...........         0.7
(28) 118-74-1.................  Hexacholorbenzene....         0.001
(29) 77-47-4..................  Hexachlorocyclopentad         0.05
                                 iene.
(30) 23135-22-0...............  Oxamyl (Vydate)......         0.2
(31) 1918-02-1................  Picloram.............         0.5
(32) 122-34-9.................  Simazine.............         0.004
(33) 1746-01-6................  2,3,7,8-TCDD (Dioxin)  3 x 10-8
------------------------------------------------------------------------


[56 FR 3593, Jan. 30, 1991, as amended at 56 FR 30280, July 1, 1991; 57 
FR 31846, July 17, 1992; 59 FR 34324, July 1, 1994]



Sec.  141.62  Maximum contaminant levels for inorganic contaminants.

    (a) [Reserved]
    (b) The maximum contaminant levels for inorganic contaminants 
specified in paragraphs (b) (2)-(6), (b)(10), and (b) (11)-(16) of this 
section apply to community water systems and non-transient, non-
community water systems. The maximum contaminant level specified in 
paragraph (b)(1) of this section only applies to community water 
systems. The maximum contaminant levels specified in (b)(7), (b)(8), and 
(b)(9) of this section apply to community water systems; non-transient, 
non-community water systems; and transient non-community water systems.

------------------------------------------------------------------------
                Contaminant                          MCL (mg/l)
------------------------------------------------------------------------
(1) Fluoride..............................  4.0
(2) Asbestos..............................  7 Million Fibers/liter
                                             (longer than 10 [micro]m).
(3) Barium................................  2
(4) Cadmium...............................  0.005
(5) Chromium..............................  0.1
(6) Mercury...............................  0.002
(7) Nitrate...............................  10 (as Nitrogen)
(8) Nitrite...............................  1 (as Nitrogen)
(9) Total Nitrate and Nitrite.............  10 (as Nitrogen)
(10) Selenium.............................  0.05
(11) Antimony.............................  0.006
(12) Beryllium............................  0.004
(13) Cyanide (as free Cyanide)............  0.2
(14) [Reserved]...........................
(15) Thallium.............................  0.002
(16) Arsenic..............................  0.010
------------------------------------------------------------------------

    (c) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment technique, or 
other means available for achieving compliance with the maximum 
contaminant levels for inorganic contaminants identified in paragraph 
(b) of this section, except fluoride:

         BAT for Inorganic Compounds Listed in Section 141.62(b)
------------------------------------------------------------------------
                      Chemical Name                           BAT(s)
------------------------------------------------------------------------
Antimony................................................             2,7
Arsenic \4\.............................................  1, 2, 5, 6, 7,
                                                               9, 12 \5\
Asbestos................................................           2,3,8
Barium..................................................         5,6,7,9

[[Page 523]]

 
Beryllium...............................................       1,2,5,6,7
Cadmium.................................................         2,5,6,7
Chromium................................................     2,5,6 \2\,7
Cyanide.................................................          5,7,13
Mercury.................................................       2 \1\,4,6
                                                               \1\,7 \1\
Nickel..................................................           5,6,7
Nitrate.................................................           5,7,9
Nitrite.................................................             5,7
Selenium................................................   1,2 \3\,6,7,9
Thallium................................................             1,5
------------------------------------------------------------------------
\1\ BAT only if influent Hg concentrations <=10[micro]g/1.
\2\ BAT for Chromium III only.
\3\ BAT for Selenium IV only.
\4\ BATs for Arsenic V. Pre-oxidation may be required to convert Arsenic
  III to Arsenic V.
\5\ To obtain high removals, iron to arsenic ratio must be at least
  20:1.

                          Key to BATS in Table

1 = Activated Alumina
2 = Coagulation/Filtration (not BAT for systems <500 service 
connections)
3 = Direct and Diatomite Filtration
4 = Granular Activated Carbon
5 = Ion Exchange
6 = Lime Softening (not BAT for systems <500 service connections)
7 = Reverse Osmosis
8 = Corrosion Control
9 = Electrodialysis
10 = Chlorine
11 = Ultraviolet
12 = Oxidation/Filtration
13 = Alkaline Chlorination (pH =8.5)
    (d) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies in the following table the affordable technology, treatment 
technique, or other means available to systems serving 10,000 persons or 
fewer for achieving compliance with the maximum contaminant level for 
arsenic:

    Small System Compliance Technologies (SSCTs) \1\ for Arsenic \2\
------------------------------------------------------------------------
                                             Affordable for listed small
    Small system compliance technology          system categories \3\
------------------------------------------------------------------------
Activated Alumina (centralized)...........  All size categories.
Activated Alumina (Point-of-Use) \4\......  All size categories.
Coagulation/Filtration \5\................  501-3,300, 3,301-10,000.
Coagulation-assisted Microfiltration......  501-3,300, 3,301-10,000.
Electrodialysis reversal \6\..............  501-3,300, 3,301-10,000.
Enhanced coagulation/filtration...........  All size categories
Enhanced lime softening (pH10.5).
Ion Exchange..............................  All size categories.
Lime Softening \5\........................  501-3,300, 3,301-10,000.
Oxidation/Filtration \7\..................  All size categories.
Reverse Osmosis (centralized) \6\.........  501-3,300, 3,301-10,000.
Reverse Osmosis (Point-of-Use) \4\........  All size categories.
------------------------------------------------------------------------
\1\ Section 1412(b)(4)(E)(ii) of SDWA specifies that SSCTs must be
  affordable and technically feasible for small systems.
\2\ SSCTs for Arsenic V. Pre-oxidation may be required to convert
  Arsenic III to Arsenic V.
\3\ The Act (ibid.) specifies three categories of small systems: (i)
  those serving 25 or more, but fewer than 501, (ii) those serving more
  than 500, but fewer than 3,301, and (iii) those serving more than
  3,300, but fewer than 10,001.
\4\ When POU or POE devices are used for compliance, programs to ensure
  proper long-term operation, maintenance, and monitoring must be
  provided by the water system to ensure adequate performance.
\5\ Unlikely to be installed solely for arsenic removal. May require pH
  adjustment to optimal range if high removals are needed.
\6\ Technologies reject a large volume of water--may not be appropriate
  for areas where water quantity may be an issue.
\7\ To obtain high removals, iron to arsenic ratio must be at least
  20:1.


[56 FR 3594, Jan. 30, 1991, as amended at 56 FR 30280, July 1, 1991; 57 
FR 31847, July 17, 1992; 59 FR 34325, July 1, 1994; 60 FR 33932, June 
29, 1995; 66 FR 7063, Jan. 22, 2001; 68 FR 14506, Mar. 25, 2003; 69 FR 
38855, June 29, 2004]



Sec.  141.63  Maximum contaminant levels (MCLs) 
for microbiological contaminants.

    (a) Until March 31, 2016, the total coliform MCL is based on the 
presence or absence of total coliforms in a sample, rather than coliform 
density.
    (1) For a system that collects at least 40 samples per month, if no 
more than 5.0 percent of the samples collected during a month are total 
coliform-positive, the system is in compliance with the MCL for total 
coliforms.
    (2) For a system that collects fewer than 40 samples per month, if 
no more than one sample collected during a month is total coliform-
positive, the system is in compliance with the MCL for total coliforms.
    (b) Until March 31, 2016, any fecal coliform-positive repeat sample 
or E. coli-positive repeat sample, or any total coliform-positive repeat 
sample following a fecal coliform-positive or E. coli-positive routine 
sample, constitutes a violation of the MCL for total coliforms. For 
purposes of the public notification requirements in subpart Q of this 
part, this is a violation that may pose an acute risk to health.
    (c) Beginning April 1, 2016, a system is in compliance with the MCL 
for E.

[[Page 524]]

coli for samples taken under the provisions of subpart Y of this part 
unless any of the conditions identified in paragraphs (c)(1) through 
(c)(4) of this section occur. For purposes of the public notification 
requirements in subpart Q of this part, violation of the MCL may pose an 
acute risk to health.
    (1) The system has an E. coli-positive repeat sample following a 
total coliform-positive routine sample.
    (2) The system has a total coliform-positive repeat sample following 
an E. coli-positive routine sample.
    (3) The system fails to take all required repeat samples following 
an E. coli-positive routine sample.
    (4) The system fails to test for E. coli when any repeat sample 
tests positive for total coliform.
    (d) Until March 31, 2016, a public water system must determine 
compliance with the MCL for total coliforms in paragraphs (a) and (b) of 
this section for each month in which it is required to monitor for total 
coliforms. Beginning April 1, 2016, a public water system must determine 
compliance with the MCL for E. coli in paragraph (c) of this section for 
each month in which it is required to monitor for total coliforms.
    (e) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
contaminant level for total coliforms in paragraphs (a) and (b) of this 
section and for achieving compliance with the maximum contaminant level 
for E. coli in paragraph (c) of this section:
    (1) Protection of wells from fecal contamination by appropriate 
placement and construction;
    (2) Maintenance of a disinfectant residual throughout the 
distribution system;
    (3) Proper maintenance of the distribution system including 
appropriate pipe replacement and repair procedures, main flushing 
programs, proper operation and maintenance of storage tanks and 
reservoirs, cross connection control, and continual maintenance of 
positive water pressure in all parts of the distribution system;
    (4) Filtration and/or disinfection of surface water, as described in 
subparts H, P, T, and W of this part, or disinfection of ground water, 
as described in subpart S of this part, using strong oxidants such as 
chlorine, chlorine dioxide, or ozone; and
    (5) For systems using ground water, compliance with the requirements 
of an EPA-approved State Wellhead Protection Program developed and 
implemented under section 1428 of the SDWA.
    (f) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the technology, treatment techniques, or other means 
available identified in paragraph (e) of this section as affordable 
technology, treatment techniques, or other means available to systems 
serving 10,000 or fewer people for achieving compliance with the maximum 
contaminant level for total coliforms in paragraphs (a) and (b) of this 
section and for achieving compliance with the maximum contaminant level 
for E. coli in paragraph (c) of this section.

[78 FR 10347, Feb. 13, 2013]



Sec.  141.64  Maximum contaminant levels for disinfection byproducts.

    (a) Bromate and chlorite. The maximum contaminant levels (MCLs) for 
bromate and chlorite are as follows:

------------------------------------------------------------------------
                   Disinfection byproduct                     MCL (mg/L)
------------------------------------------------------------------------
Bromate....................................................        0.010
Chlorite...................................................        1.0
------------------------------------------------------------------------

    (1) Compliance dates for CWSs and NTNCWSs. Subpart H systems serving 
10,000 or more persons must comply with this paragraph (a) beginning 
January 1, 2002. Subpart H systems serving fewer than 10,000 persons and 
systems using only ground water not under the direct influence of 
surface water must comply with this paragraph (a) beginning January 1, 
2004.
    (2) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
contaminant levels for bromate and chlorite identified in this paragraph 
(a):

[[Page 525]]



------------------------------------------------------------------------
         Disinfection byproduct             Best available technology
------------------------------------------------------------------------
Bromate................................  Control of ozone treatment
                                          process to reduce production
                                          of bromate
Chlorite...............................  Control of treatment processes
                                          to reduce disinfectant demand
                                          and control of disinfection
                                          treatment processes to reduce
                                          disinfectant levels
------------------------------------------------------------------------

    (b) TTHM and HAA5. (1) Subpart L--RAA compliance. (i) Compliance 
dates. Subpart H systems serving 10,000 or more persons must comply with 
this paragraph (b)(1) beginning January 1, 2002. Subpart H systems 
serving fewer than 10,000 persons and systems using only ground water 
not under the direct influence of surface water must comply with this 
paragraph (b)(1) beginning January 1, 2004. All systems must comply with 
these MCLs until the date specified for subpart V compliance in Sec.  
141.620(c).

------------------------------------------------------------------------
                   Disinfection byproduct                     MCL (mg/L)
------------------------------------------------------------------------
Total trihalomethanes (TTHM)...............................        0.080
Haloacetic acids (five) (HAA5).............................        0.060
------------------------------------------------------------------------

    (ii) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
contaminant levels for TTHM and HAA5 identified in this paragraph 
(b)(1):

------------------------------------------------------------------------
          Disinfection byproduct              Best available technology
------------------------------------------------------------------------
Total trihalomethanes (TTHM) and            Enhanced coagulation or
 Haloacetic acids (five) (HAA5).             enhanced softening or
                                             GAC10, with chlorine as the
                                             primary and residual
                                             disinfectant
------------------------------------------------------------------------

    (2) Subpart V--LRAA compliance. (i) Compliance dates. The subpart V 
MCLs for TTHM and HAA5 must be complied with as a locational running 
annual average at each monitoring location beginning the date specified 
for subpart V compliance in Sec.  141.620(c).

------------------------------------------------------------------------
                   Disinfection byproduct                     MCL (mg/L)
------------------------------------------------------------------------
Total trihalomethanes (TTHM)...............................        0.080
Haloacetic acids (five) (HAA5).............................        0.060
------------------------------------------------------------------------

    (ii) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
contaminant levels for TTHM and HAA5 identified in this paragraph (b)(2) 
for all systems that disinfect their source water:

------------------------------------------------------------------------
         Disinfection byproduct             Best available technology
------------------------------------------------------------------------
Total trihalomethanes (TTHM) and         Enhanced coagulation or
 Haloacetic acids (five) (HAA5).          enhanced softening, plus
                                          GAC10; or nanofiltration with
                                          a molecular weight cutoff
                                          <=1000 Daltons; or GAC20
------------------------------------------------------------------------

    (iii) The Administrator, pursuant to section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
contaminant levels for TTHM and HAA5 identified in this paragraph (b)(2) 
for consecutive systems and applies only to the disinfected water that 
consecutive systems buy or otherwise receive:

------------------------------------------------------------------------
         Disinfection byproduct             Best available technology
------------------------------------------------------------------------
Total trihalomethanes (TTHM) and         Systems serving =10,000: Improved
                                          distribution system and
                                          storage tank management to
                                          reduce residence time, plus
                                          the use of chloramines for
                                          disinfectant residual
                                          maintenance
                                         Systems serving <10,000:
                                          Improved distribution system
                                          and storage tank management to
                                          reduce residence time
------------------------------------------------------------------------


[71 FR 478, Jan. 4, 2006]



Sec.  141.65  Maximum residual disinfectant levels.

    (a) Maximum residual disinfectant levels (MRDLs) are as follows:

------------------------------------------------------------------------
          Disinfectant residual                     MRDL (mg/L)
------------------------------------------------------------------------
Chlorine................................  4.0 (as Cl2).
Chloramines.............................  4.0 (as Cl2).
Chlorine dioxide........................  0.8 (as ClO2).
------------------------------------------------------------------------

    (b) Compliance dates--(1) CWSs and NTNCWSs. Subpart H systems 
serving 10,000 or more persons must comply with this section beginning 
January 1, 2002. Subpart H systems serving fewer than 10,000 persons and 
systems using only ground water not under the direct influence of 
surface water must comply with this subpart beginning January 1, 2004.
    (2) Transient NCWSs. Subpart H systems serving 10,000 or more 
persons and using chlorine dioxide as a disinfectant

[[Page 526]]

or oxidant must comply with the chlorine dioxide MRDL beginning January 
1, 2002. Subpart H systems serving fewer than 10,000 persons and using 
chlorine dioxide as a disinfectant or oxidant and systems using only 
ground water not under the direct influence of surface water and using 
chlorine dioxide as a disinfectant or oxidant must comply with the 
chlorine dioxide MRDL beginning January 1, 2004.
    (c) The Administrator, pursuant to Section 1412 of the Act, hereby 
identifies the following as the best technology, treatment techniques, 
or other means available for achieving compliance with the maximum 
residual disinfectant levels identified in paragraph (a) of this 
section: control of treatment processes to reduce disinfectant demand 
and control of disinfection treatment processes to reduce disinfectant 
levels.

[63 FR 69465, Dec. 16, 1998, as amended at 66 FR 3776, Jan. 16, 2001]



Sec.  141.66  Maximum contaminant levels for radionuclides.

    (a) [Reserved]
    (b) MCL for combined radium-226 and -228. The maximum contaminant 
level for combined radium-226 and radium-228 is 5 pCi/L. The combined 
radium-226 and radium-228 value is determined by the addition of the 
results of the analysis for radium-226 and the analysis for radium-228.
    (c) MCL for gross alpha particle activity (excluding radon and 
uranium). The maximum contaminant level for gross alpha particle 
activity (including radium-226 but excluding radon and uranium) is 15 
pCi/L.
    (d) MCL for beta particle and photon radioactivity. (1) The average 
annual concentration of beta particle and photon radioactivity from man-
made radionuclides in drinking water must not produce an annual dose 
equivalent to the total body or any internal organ greater than 4 
millirem/year (mrem/year).
    (2) Except for the radionuclides listed in table A, the 
concentration of man-made radionuclides causing 4 mrem total body or 
organ dose equivalents must be calculated on the basis of 2 liter per 
day drinking water intake using the 168 hour data list in ``Maximum 
Permissible Body Burdens and Maximum Permissible Concentrations of 
Radionuclides in Air and in Water for Occupational Exposure,'' NBS 
(National Bureau of Standards) Handbook 69 as amended August 1963, U.S. 
Department of Commerce. This incorporation by reference was approved by 
the Director of the Federal Register in accordance with 5 U.S.C. 552(a) 
and 1 CFR part 51. Copies of this document are available from the 
National Technical Information Service, NTIS ADA 280 282, U.S. 
Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 
22161. The toll-free number is 800-553-6847. Copies may be inspected at 
EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or 
at the National Archives and Records Administration (NARA). For 
information on the availability of this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html. If two or more 
radionuclides are present, the sum of their annual dose equivalent to 
the total body or to any organ shall not exceed 4 mrem/year.

 Table A--Average Annual Concentrations Assumed To Produce: a Total Body
                       or Organ Dose of 4 mrem/yr
------------------------------------------------------------------------
 
------------------------------------------------------------------------
1. Radionuclide.................  Critical organ....  pCi per liter
2. Tritium......................  Total body........  20,000
3. Strontium-90.................  Bone Marrow.......  8
------------------------------------------------------------------------

    (e) MCL for uranium. The maximum contaminant level for uranium is 30 
[micro]g/L.
    (f) Compliance dates. (1) Compliance dates for combined radium-226 
and -228, gross alpha particle activity, gross beta particle and photon 
radioactivity, and uranium: Community water systems must comply with the 
MCLs listed in paragraphs (b), (c), (d), and (e) of this section 
beginning December 8, 2003 and compliance shall be determined in 
accordance with the requirements of Sec. Sec.  141.25 and 141.26. 
Compliance with reporting requirements for the radionuclides under 
appendix A to subpart O and appendices A and B to subpart Q is required 
on December 8, 2003.
    (2) [Reserved]

[[Page 527]]

    (g) Best available technologies (BATs) for radionuclides. The 
Administrator, pursuant to section 1412 of the Act, hereby identifies as 
indicated in the following table the best technology available for 
achieving compliance with the maximum contaminant levels for combined 
radium-226 and -228, uranium, gross alpha particle activity, and beta 
particle and photon radioactivity.

   Table B--BAT for Combined Radium-226 and Radium-228, Uranium, Gross
   Alpha Particle Activity, and Beta Particle and Photon Radioactivity
------------------------------------------------------------------------
              Contaminant                              BAT
------------------------------------------------------------------------
1. Combined radium-226 and radium-228..  Ion exchange, reverse osmosis,
                                          lime softening.
2. Uranium.............................  Ion exchange, reverse osmosis,
                                          lime softening, coagulation/
                                          filtration.
3. Gross alpha particle activity         Reverse osmosis.
 (excluding Radon and Uranium).
4. Beta particle and photon              Ion exchange, reverse osmosis.
 radioactivity.
------------------------------------------------------------------------

    (h) Small systems compliance technologies list for radionuclides.

         Table C--List of Small Systems Compliance Technologies for Radionuclides and Limitations to Use
----------------------------------------------------------------------------------------------------------------
                                           Limitations
            Unit technologies                 (see          Operator skill level     Raw water quality range and
                                           footnotes)           required \1\             considerations. \1\
----------------------------------------------------------------------------------------------------------------
1. Ion exchange (IE)....................        (\a\)   Intermediate...............  All ground waters.
2. Point of use (POU \2\) IE............        (\b\)   Basic......................  All ground waters.
3. Reverse osmosis (RO).................        (\c\)   Advanced...................  Surface waters usually
                                                                                      require pre-filtration.
4. POU \2\ RO...........................        (\b\)   Basic......................  Surface waters usually
                                                                                      require pre-filtration.
5. Lime softening.......................        (\d\)   Advanced...................  All waters.
6. Green sand filtration................        (\e\)   Basic.
7. Co-precipitation with Barium sulfate.        (\f\)   Intermediate to Advanced...  Ground waters with suitable
                                                                                      water quality.
8. Electrodialysis/electrodialysis        ............  Basic to Intermediate......  All ground waters.
 reversal.
9. Pre-formed hydrous Manganese oxide           (\g\)   Intermediate...............  All ground waters.
 filtration.
10. Activated alumina...................  (\a\), (\h\)  Advanced...................  All ground waters;
                                                                                      competing anion
                                                                                      concentrations may affect
                                                                                      regeneration frequency.
11. Enhanced coagulation/filtration.....        (\i\)   Advanced...................  Can treat a wide range of
                                                                                      water qualities.
----------------------------------------------------------------------------------------------------------------
\1\ National Research Council (NRC). Safe Water from Every Tap: Improving Water Service to Small Communities.
  National Academy Press. Washington, D.C. 1997.
\2\ A POU, or ``point-of-use'' technology is a treatment device installed at a single tap used for the purpose
  of reducing contaminants in drinking water at that one tap. POU devices are typically installed at the kitchen
  tap. See the April 21, 2000 NODA for more details.
 
 Limitations Footnotes: Technologies for Radionuclides:
\a\ The regeneration solution contains high concentrations of the contaminant ions. Disposal options should be
  carefully considered before choosing this technology.
\b\ When POU devices are used for compliance, programs for long-term operation, maintenance, and monitoring must
  be provided by water utility to ensure proper performance.
\c\ Reject water disposal options should be carefully considered before choosing this technology. See other RO
  limitations described in the SWTR Compliance Technologies Table.
\d\ The combination of variable source water quality and the complexity of the water chemistry involved may make
  this technology too complex for small surface water systems.
\e\ Removal efficiencies can vary depending on water quality.
\f\ This technology may be very limited in application to small systems. Since the process requires static
  mixing, detention basins, and filtration, it is most applicable to systems with sufficiently high sulfate
  levels that already have a suitable filtration treatment train in place.
\g\ This technology is most applicable to small systems that already have filtration in place.
\h\ Handling of chemicals required during regeneration and pH adjustment may be too difficult for small systems
  without an adequately trained operator.
\i\ Assumes modification to a coagulation/filtration process already in place.


                Table D--Compliance Technologies by System Size Category for Radionuclide NPDWR's
----------------------------------------------------------------------------------------------------------------
                                          Compliance technologies \1\ for system size
                                                categories (population served)
             Contaminant              --------------------------------------------------       3,300-10,000
                                                25-500                 501-3,300
----------------------------------------------------------------------------------------------------------------
1. Combined radium-226 and radium-228  1, 2, 3, 4, 5, 6, 7, 8,  1, 2, 3, 4, 5, 6, 7, 8,  1, 2, 3, 4, 5, 6, 7. 8,
                                        9.                       9.                       9.

[[Page 528]]

 
2. Gross alpha particle activity.....  3, 4...................  3, 4...................  3, 4.
3. Beta particle activity and photon   1, 2, 3, 4.............  1, 2, 3, 4.............  1, 2, 3, 4.
 activity.
4. Uranium...........................  1, 2, 4, 10, 11........  1, 2, 3, 4, 5, 10, 11..  1, 2, 3, 4, 5, 10, 11.
----------------------------------------------------------------------------------------------------------------
Note: \1\ Numbers correspond to those technologies found listed in the table C of 141.66(h).


[65 FR 76748, Dec. 7, 2000]



                  Subpart H_Filtration and Disinfection

    Source: 54 FR 27527, June 29, 1989, unless otherwise noted.



Sec.  141.70  General requirements.

    (a) The requirements of this subpart H constitute national primary 
drinking water regulations. These regulations establish criteria under 
which filtration is required as a treatment technique for public water 
systems supplied by a surface water source and public water systems 
supplied by a ground water source under the direct influence of surface 
water. In addition, these regulations establish treatment technique 
requirements in lieu of maximum contaminant levels for the following 
contaminants: Giardia lamblia, viruses, heterotrophic plate count 
bacteria, Legionella, and turbidity. Each public water system with a 
surface water source or a ground water source under the direct influence 
of surface water must provide treatment of that source water that 
complies with these treatment technique requirements. The treatment 
technique requirements consist of installing and properly operating 
water treatment processes which reliably achieve:
    (1) At least 99.9 percent (3-log) removal and/or inactivation of 
Giardia lamblia cysts between a point where the raw water is not subject 
to recontamination by surface water runoff and a point downstream before 
or at the first customer; and
    (2) At least 99.99 percent (4-log) removal and/or inactivation of 
viruses between a point where the raw water is not subject to 
recontamination by surface water runoff and a point downstream before or 
at the first customer.
    (b) A public water system using a surface water source or a ground 
water source under the direct influence of surface water is considered 
to be in compliance with the requirements of paragraph (a) of this 
section if:
    (1) It meets the requirements for avoiding filtration in Sec.  
141.71 and the disinfection requirements in Sec.  141.72(a); or
    (2) It meets the filtration requirements in Sec.  141.73 and the 
disinfection requirements in Sec.  141.72(b).
    (c) Each public water system using a surface water source or a 
ground water source under the direct influence of surface water must be 
operated by qualified personnel who meet the requirements specified by 
the State.
    (d) Additional requirements for systems serving at least 10,000 
people. In addition to complying with requirements in this subpart, 
systems serving at least 10,000 people must also comply with the 
requirements in subpart P of this part.
    (e) Additional requirements for systems serving fewer than 10,000 
people. In addition to complying with requirements in this subpart, 
systems serving fewer than 10,000 people must also comply with the 
requirements in subpart T of this part.

[54 FR 27527, June 29, 1989, as amended at 63 FR 69516, Dec. 16, 1998; 
67 FR 1836, Jan. 14, 2002]



Sec.  141.71  Criteria for avoiding filtration.

    A public water system that uses a surface water source must meet all 
of the conditions of paragraphs (a) and (b)

[[Page 529]]

of this section, and is subject to paragraph (c) of this section, 
beginning December 30, 1991, unless the State has determined, in writing 
pursuant to Sec.  1412(b)(7)(C)(iii), that filtration is required. A 
public water system that uses a ground water source under the direct 
influence of surface water must meet all of the conditions of paragraphs 
(a) and (b) of this section and is subject to paragraph (c) of this 
section, beginning 18 months after the State determines that it is under 
the direct influence of surface water, or December 30, 1991, whichever 
is later, unless the State has determined, in writing pursuant to Sec.  
1412(b)(7)(C)(iii), that filtration is required. If the State determines 
in writing pursuant to Sec.  1412(b)(7)(C)(iii) before December 30, 
1991, that filtration is required, the system must have installed 
filtration and meet the criteria for filtered systems specified in 
Sec. Sec.  141.72(b) and 141.73 by June 29, 1993. Within 18 months of 
the failure of a system using surface water or a ground water source 
under the direct influence of surface water to meet any one of the 
requirements of paragraphs (a) and (b) of this section or after June 29, 
1993, whichever is later, the system must have installed filtration and 
meet the criteria for filtered systems specified in Sec. Sec.  141.72(b) 
and 141.73.
    (a) Source water quality conditions. (1) The fecal coliform 
concentration must be equal to or less than 20/100 ml, or the total 
coliform concentration must be equal to or less than 100/100 ml 
(measured as specified in Sec.  141.74 (a) (1) and (2) and (b)(1)), in 
representative samples of the source water immediately prior to the 
first or only point of disinfectant application in at least 90 percent 
of the measurements made for the 6 previous months that the system 
served water to the public on an ongoing basis. If a system measures 
both fecal and total coliforms, the fecal coliform criterion, but not 
the total coliform criterion, in this paragraph must be met.
    (2) The turbidity level cannot exceed 5 NTU (measured as specified 
in Sec.  141.74 (a)(1) and (b)(2)) in representative samples of the 
source water immediately prior to the first or only point of 
disinfectant application unless: (i) the State determines that any such 
event was caused by circumstances that were unusual and unpredictable; 
and (ii) as a result of any such event, there have not been more than 
two events in the past 12 months the system served water to the public, 
or more than five events in the past 120 months the system served water 
to the public, in which the turbidity level exceeded 5 NTU. An ``event'' 
is a series of consecutive days during which at least one turbidity 
measurement each day exceeds 5 NTU.
    (b) Site-specific conditions. (1)(i) The public water system must 
meet the requirements of Sec.  141.72(a)(1) at least 11 of the 12 
previous months that the system served water to the public, on an 
ongoing basis, unless the system fails to meet the requirements during 2 
of the 12 previous months that the system served water to the public, 
and the State determines that at least one of these failures was caused 
by circumstances that were unusual and unpredictable.
    (ii) The public water system must meet the requirements of Sec.  
141.72(a)(2) at all times the system serves water to the public.
    (iii) The public water system must meet the requirements of Sec.  
141.72(a)(3) at all times the system serves water to the public unless 
the State determines that any such failure was caused by circumstances 
that were unusual and unpredictable.
    (iv) The public water system must meet the requirements of Sec.  
141.72(a)(4) on an ongoing basis unless the State determines that 
failure to meet these requirements was not caused by a deficiency in 
treatment of the source water.
    (2) The public water system must maintain a watershed control 
program which minimizes the potential for contamination by Giardia 
lamblia cysts and viruses in the source water. The State must determine 
whether the watershed control program is adequate to meet this goal. The 
adequacy of a program to limit potential contamination by Giardia 
lamblia cysts and viruses must be based on: the comprehensiveness of the 
watershed review; the effectiveness of the system's program to monitor

[[Page 530]]

and control detrimental activities occurring in the watershed; and the 
extent to which the water system has maximized land ownership and/or 
controlled land use within the watershed. At a minimum, the watershed 
control program must:
    (i) Characterize the watershed hydrology and land ownership;
    (ii) Identify watershed characteristics and activities which may 
have an adverse effect on source water quality; and
    (iii) Monitor the occurrence of activities which may have an adverse 
effect on source water quality.

The public water system must demonstrate through ownership and/or 
written agreements with landowners within the watershed that it can 
control all human activities which may have an adverse impact on the 
microbiological quality of the source water. The public water system 
must submit an annual report to the State that identifies any special 
concerns about the watershed and how they are being handled; describes 
activities in the watershed that affect water quality; and projects what 
adverse activities are expected to occur in the future and describes how 
the public water system expects to address them. For systems using a 
ground water source under the direct influence of surface water, an 
approved wellhead protection program developed under section 1428 of the 
Safe Drinking Water Act may be used, if the State deems it appropriate, 
to meet these requirements.
    (3) The public water system must be subject to an annual on-site 
inspection to assess the watershed control program and disinfection 
treatment process. Either the State or a party approved by the State 
must conduct the on-site inspection. The inspection must be conducted by 
competent individuals such as sanitary and civil engineers, sanitarians, 
or technicians who have experience and knowledge about the operation and 
maintenance of a public water system, and who have a sound understanding 
of public health principles and waterborne diseases. A report of the on-
site inspection summarizing all findings must be prepared every year. 
The on-site inspection must indicate to the State's satisfaction that 
the watershed control program and disinfection treatment process are 
adequately designed and maintained. The on-site inspection must include:
    (i) A review of the effectiveness of the watershed control program;
    (ii) A review of the physical condition of the source intake and how 
well it is protected;
    (iii) A review of the system's equipment maintenance program to 
ensure there is low probability for failure of the disinfection process;
    (iv) An inspection of the disinfection equipment for physical 
deterioration;
    (v) A review of operating procedures;
    (vi) A review of data records to ensure that all required tests are 
being conducted and recorded and disinfection is effectively practiced; 
and
    (vii) Identification of any improvements which are needed in the 
equipment, system maintenance and operation, or data collection.
    (4) The public water system must not have been identified as a 
source of a waterborne disease outbreak, or if it has been so 
identified, the system must have been modified sufficiently to prevent 
another such occurrence, as determined by the State.
    (5) The public water system must comply with the maximum contaminant 
level (MCL) for total coliforms in Sec.  141.63(a) and (b) and the MCL 
for E. coli in Sec.  141.63(c) at least 11 months of the 12 previous 
months that the system served water to the public, on an ongoing basis, 
unless the State determines that failure to meet this requirement was 
not caused by a deficiency in treatment of the source water.
    (6) The public water system must comply with the requirements for 
trihalomethanes in Sec. Sec.  141.12 and 141.30 until December 31, 2001. 
After December 31, 2001, the system must comply with the requirements 
for total trihalomethanes, haloacetic acids (five), bromate, chlorite, 
chlorine, chloramines, and chlorine dioxide in subpart L of this part.
    (c) Treatment technique violations. (1) A system that (i) fails to 
meet any one of the criteria in paragraphs (a) and (b) of this section 
and/or which the State has determined that filtration is required, in 
writing pursuant to

[[Page 531]]

Sec.  1412(b)(7)(C)(iii), and (ii) fails to install filtration by the 
date specified in the introductory paragraph of this section is in 
violation of a treatment technique requirement.
    (2) A system that has not installed filtration is in violation of a 
treatment technique requirement if:
    (i) The turbidity level (measured as specified in Sec.  141.74(a)(1) 
and (b)(2)) in a representative sample of the source water immediately 
prior to the first or only point of disinfection application exceeds 5 
NTU; or
    (ii) The system is identified as a source of a waterborne disease 
outbreak.

[54 FR 27527, June 29, 1989, as amended at 63 FR 69516, Dec. 16, 1998; 
66 FR 3776, Jan. 16, 2001; 69 FR 38855, June 29, 2004; 78 FR 10347, Feb. 
13, 2013]



Sec.  141.72  Disinfection.

    A public water system that uses a surface water source and does not 
provide filtration treatment must provide the disinfection treatment 
specified in paragraph (a) of this section beginning December 30, 1991, 
unless the State determines that filtration is required in writing 
pursuant to Sec.  1412 (b)(7)(C)(iii). A public water system that uses a 
ground water source under the direct influence of surface water and does 
not provide filtration treatment must provide disinfection treatment 
specified in paragraph (a) of this section beginning December 30, 1991, 
or 18 months after the State determines that the ground water source is 
under the influence of surface water, whichever is later, unless the 
State has determined that filtration is required in writing pursuant to 
Sec.  1412(b)(7)(C)(iii). If the State has determined that filtration is 
required, the system must comply with any interim disinfection 
requirements the State deems necessary before filtration is installed. A 
system that uses a surface water source that provides filtration 
treatment must provide the disinfection treatment specified in paragraph 
(b) of this section beginning June 29, 1993, or beginning when 
filtration is installed, whichever is later. A system that uses a ground 
water source under the direct influence of surface water and provides 
filtration treatment must provide disinfection treatment as specified in 
paragraph (b) of this section by June 29, 1993, or beginning when 
filtration is installed, whichever is later. Failure to meet any 
requirement of this section after the applicable date specified in this 
introductory paragraph is a treatment technique violation.
    (a) Disinfection requirements for public water systems that do not 
provide filtration. Each public water system that does not provide 
filtration treatment must provide disinfection treatment as follows:
    (1) The disinfection treatment must be sufficient to ensure at least 
99.9 percent (3-log) inactivation of Giardia lamblia cysts and 99.99 
percent (4-log) inactivation of viruses, every day the system serves 
water to the public, except any one day each month. Each day a system 
serves water to the public, the public water system must calculate the 
CT value(s) from the system's treatment parameters, using the procedure 
specified in Sec.  141.74(b)(3), and determine whether this value(s) is 
sufficient to achieve the specified inactivation rates for Giardia 
lamblia cysts and viruses. If a system uses a disinfectant other than 
chlorine, the system may demonstrate to the State, through the use of a 
State-approved protocol for on-site disinfection challenge studies or 
other information satisfactory to the State, that CT99.9 
values other than those specified in tables 2.1 and 3.1 in Sec.  
141.74(b)(3) or other operational parameters are adequate to demonstrate 
that the system is achieving minimum inactivation rates required by 
paragraph (a)(1) of this section.
    (2) The disinfection system must have either (i) redundant 
components, including an auxiliary power supply with automatic start-up 
and alarm to ensure that disinfectant application is maintained 
continuously while water is being delivered to the distribution system, 
or (ii) automatic shut-off of delivery of water to the distribution 
system whenever there is less than 0.2 mg/l of residual disinfectant 
concentration in the water. If the State determines that automatic shut-
off would cause unreasonable risk to health or interfere with fire 
protection, the system must comply with paragraph (a)(2)(i) of this 
section.

[[Page 532]]

    (3) The residual disinfectant concentration in the water entering 
the distribution system, measured as specified in Sec.  141.74 (a)(2) 
and (b)(5), cannot be less than 0.2 mg/l for more than 4 hours.
    (4)(i) The residual disinfectant concentration in the distribution 
system, measured as total chlorine, combined chlorine, or chlorine 
dioxide, as specified in Sec.  141.74 (a)(2) and (b)(6), cannot be 
undetectable in more than 5 percent of the samples each month, for any 
two consecutive months that the system serves water to the public. Water 
in the distribution system with a heterotrophic bacteria concentration 
less than or equal to 500/ml, measured as heterotrophic plate count 
(HPC) as specified in Sec.  141.74(a)(1), is deemed to have a detectable 
disinfectant residual for purposes of determining compliance with this 
requirement. Thus, the value ``V'' in the following formula cannot 
exceed 5 percent in one month, for any two consecutive months.
[GRAPHIC] [TIFF OMITTED] TC15NO91.131

where:

a = number of instances where the residual disinfectant concentration is 
          measured;
b = number of instances where the residual disinfectant concentration is 
          not measured but heterotrophic bacteria plate count (HPC) is 
          measured;
c = number of instances where the residual disinfectant concentration is 
          measured but not detected and no HPC is measured;
d = number of instances where the residual disinfectant concentration is 
          measured but not detected and where the HPC is 500/
          ml; and
e = number of instances where the residual disinfectant concentration is 
          not measured and HPC is 500/ml.

    (ii) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample transported and analyzed 
for HPC by a certified laboratory under the requisite time and 
temperature conditions specified by Sec.  141.74(a)(1) and that the 
system is providing adequate disinfection in the distribution system, 
the requirements of paragraph (a)(4)(i) of this section do not apply to 
that system.
    (b) Disinfection requirements for public water systems which provide 
filtration. Each public water system that provides filtration treatment 
must provide disinfection treatment as follows.
    (1) The disinfection treatment must be sufficient to ensure that the 
total treatment processes of that system achieve at least 99.9 percent 
(3-log) inactivation and/or removal of Giardia lamblia cysts and at 
least 99.99 percent (4-log) inactivation and/or removal of viruses, as 
determined by the State.
    (2) The residual disinfectant concentration in the water entering 
the distribution system, measured as specified in Sec.  141.74 (a)(2) 
and (c)(2), cannot be less than 0.2 mg/l for more than 4 hours.
    (3)(i) The residual disinfectant concentration in the distribution 
system, measured as total chlorine, combined chlorine, or chlorine 
dioxide, as specified in Sec.  141.74 (a)(2) and (c)(3), cannot be 
undetectable in more than 5 percent of the samples each month, for any 
two consecutive months that the system serves water to the public. Water 
in the distribution system with a heterotrophic bacteria concentration 
less than or equal to 500/ml, measured as heterotrophic plate count 
(HPC) as specified in Sec.  141.74(a)(1), is deemed to have a detectable 
disinfectant residual for purposes of determining compliance with this 
requirement. Thus, the value ``V'' in the following formula cannot 
exceed 5 percent in one month, for any two consecutive months.
[GRAPHIC] [TIFF OMITTED] TC15NO91.132

where:

a = number of instances where the residual disinfectant concentration is 
          measured;
b = number of instances where the residual disinfectant concentration is 
          not measured but heterotrophic bacteria plate count (HPC) is 
          measured;
c = number of instances where the residual disinfectant concentration is 
          measured but not detected and no HPC is measured;
d = number of instances where no residual disinfectant concentration is 
          detected and where the HPC is 500/ml; and
e = number of instances where the residual disinfectant concentration is 
          not measured and HPC is 500/ml.

    (ii) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample

[[Page 533]]

transported and analyzed for HPC by a certified laboratory under the 
requisite time and temperature conditions specified in Sec.  
141.74(a)(1) and that the system is providing adequate disinfection in 
the distribution system, the requirements of paragraph (b)(3)(i) of this 
section do not apply.

[54 FR 27527, June 29, 1989, as amended at 69 FR 38855, June 29, 2004]



Sec.  141.73  Filtration.

    A public water system that uses a surface water source or a ground 
water source under the direct influence of surface water, and does not 
meet all of the criteria in Sec.  141.71 (a) and (b) for avoiding 
filtration, must provide treatment consisting of both disinfection, as 
specified in Sec.  141.72(b), and filtration treatment which complies 
with the requirements of paragraph (a), (b), (c), (d), or (e) of this 
section by June 29, 1993, or within 18 months of the failure to meet any 
one of the criteria for avoiding filtration in Sec.  141.71 (a) and (b), 
whichever is later. Failure to meet any requirement of this section 
after the date specified in this introductory paragraph is a treatment 
technique violation.
    (a) Conventional filtration treatment or direct filtration. (1) For 
systems using conventional filtration or direct filtration, the 
turbidity level of representative samples of a system's filtered water 
must be less than or equal to 0.5 NTU in at least 95 percent of the 
measurements taken each month, measured as specified in Sec.  141.74 
(a)(1) and (c)(1), except that if the State determines that the system 
is capable of achieving at least 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts at some turbidity level higher 
than 0.5 NTU in at least 95 percent of the measurements taken each 
month, the State may substitute this higher turbidity limit for that 
system. However, in no case may the State approve a turbidity limit that 
allows more than 1 NTU in more than 5 percent of the samples taken each 
month, measured as specified in Sec.  141.74 (a)(1) and (c)(1).
    (2) The turbidity level of representative samples of a system's 
filtered water must at no time exceed 5 NTU, measured as specified in 
Sec.  141.74 (a)(1) and (c)(1).
    (3) Beginning January 1, 2002, systems serving at least 10,000 
people must meet the turbidity requirements in Sec.  141.173(a).
    (4) Beginning January 1, 2005, systems serving fewer than 10,000 
people must meet the turbidity requirements in Sec. Sec.  141.550 
through 141.553.
    (b) Slow sand filtration. (1) For systems using slow sand 
filtration, the turbidity level of representative samples of a system's 
filtered water must be less than or equal to 1 NTU in at least 95 
percent of the measurements taken each month, measured as specified in 
Sec.  141.74 (a)(1) and (c)(1), except that if the State determines 
there is no significant interference with disinfection at a higher 
turbidity level, the State may substitute this higher turbidity limit 
for that system.
    (2) The turbidity level of representative samples of a system's 
filtered water must at no time exceed 5 NTU, measured as specified in 
Sec.  141.74 (a)(1) and (c)(1).
    (c) Diatomaceous earth filtration. (1) For systems using 
diatomaceous earth filtration, the turbidity level of representative 
samples of a system's filtered water must be less than or equal to 1 NTU 
in at least 95 percent of the measurements taken each month, measured as 
specified in Sec.  141.74 (a)(1) and (c)(1).
    (2) The turbidity level of representative samples of a system's 
filtered water must at no time exceed 5 NTU, measured as specified in 
Sec.  141.74 (a)(1) and (c)(1).
    (d) Other filtration technologies. A public water system may use a 
filtration technology not listed in paragraphs (a) through (c) of this 
section if it demonstrates to the State, using pilot plant studies or 
other means, that the alternative filtration technology, in combination 
with disinfection treatment that meets the requirements of Sec.  
141.72(b), consistently achieves 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts and 99.99 percent removal and/or 
inactivation of viruses. For a system that makes this demonstration, the 
requirements of paragraph (b) of this section apply. Beginning January 
1, 2002, systems serving

[[Page 534]]

at least 10,000 people must meet the requirements for other filtration 
technologies in Sec.  141.173(b). Beginning January 14, 2005, systems 
serving fewer than 10,000 people must meet the requirements for other 
filtration technologies in Sec.  141.550 through 141.553.

[54 FR 27527, June 29, 1989, as amended at 63 FR 69516, Dec. 16, 1998; 
66 FR 3776, Jan. 16, 2001; 67 FR 1836, Jan. 14, 2002; 69 FR 38855, June 
29, 2004]



Sec.  141.74  Analytical and monitoring requirements.

    (a) Analytical requirements. Only the analytical method(s) specified 
in this paragraph, or otherwise approved by EPA, may be used to 
demonstrate compliance with Sec. Sec.  141.71, 141.72 and 141.73. 
Measurements for pH, turbidity, temperature and residual disinfectant 
concentrations must be conducted by a person approved by the State. 
Measurement for total coliforms, fecal coliforms and HPC must be 
conducted by a laboratory certified by the State or EPA to do such 
analysis. Until laboratory certification criteria are developed for the 
analysis of fecal coliforms and HPC, any laboratory certified for total 
coliforms analysis by the State or EPA is deemed certified for fecal 
coliforms and HPC analysis. The following procedures shall be conducted 
in accordance with the publications listed in the following section. 
This incorporation by reference was approved by the Director of the 
Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. 
Copies of the methods published in Standard Methods for the Examination 
of Water and Wastewater may be obtained from the American Public Health 
Association et al., 1015 Fifteenth Street, NW., Washington, DC 20005; 
copies of the Minimal Medium ONPG-MUG Method as set forth in the article 
``National Field Evaluation of a Defined Substrate Method for the 
Simultaneous Enumeration of Total Coliforms and Esherichia coli from 
Drinking Water: Comparison with the Standard Multiple Tube Fermentation 
Method'' (Edberg et al.), Applied and Environmental Microbiology, Volume 
54, pp. 1595-1601, June 1988 (as amended under Erratum, Applied and 
Environmental Microbiology, Volume 54, p. 3197, December, 1988), may be 
obtained from the American Water Works Association Research Foundation, 
6666 West Quincy Avenue, Denver, Colorado, 80235; and copies of the 
Indigo Method as set forth in the article ``Determination of Ozone in 
Water by the Indigo Method'' (Bader and Hoigne), may be obtained from 
Ozone Science & Engineering, Pergamon Press Ltd., Fairview Park, 
Elmsford, New York 10523. Copies may be inspected at the U.S. 
Environmental Protection Agency, Room EB15, 401 M St., SW., Washington, 
DC 20460 or at the National Archives and Records Administration (NARA). 
For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Public water systems must conduct analysis of pH and temperature 
in accordance with one of the methods listed at Sec.  141.23(k)(1). 
Public water systems must conduct analysis of total coliforms, fecal 
coliforms, heterotrophic bacteria, and turbidity in accordance with one 
of the following analytical methods or one of the alternative methods 
listed in appendix A to subpart C of this part and by using analytical 
test procedures contained in Technical Notes on Drinking Water Methods, 
EPA-600/R-94-173, October 1994. This document is available from the 
National Service Center for Environmental Publications (NSCEP), P.O. Box 
42419, Cincinnati, OH 45242-0419 or http://www.epa.gov/nscep/.

------------------------------------------------------------------------
            Organism                 Methodology         Citation \1\
------------------------------------------------------------------------
Total Coliform \2\.............  Total Coliform      9221 A, B, C
                                  Fermentation
                                  Technique \3 4 5\.
                                 Total Coliform      9222 A, B, C
                                  Membrane Filter
                                  Technique \6\.
                                 ONPG-MUG Test \7\.  9223
Fecal Coliforms \2\............  Fecal Coliform      9221 E
                                  Procedure \8\.
                                 Fecal Coliform      9222 D
                                  Filter Procedure.
Heterotrophic bacteria \2\.....  Pour Plate Method.  9215 B
                                 SimPlate \11\.....
Turbidity \13\.................  Nephelometric       2130 B
                                  Method.
                                 Nephelometric       180.1 \9\
                                  Method.
                                 Great Lakes         Method 2 \10\
                                  Instruments.

[[Page 535]]

 
                                 Hach FilterTrak...  10133 \12\
------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed
  below. The incorporation by reference of the following documents
  listed in footnotes 1, 6, 7 and 9-12 was approved by the Director of
  the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part
  51. Copies of the documents may be obtained from the sources listed
  below. Information regarding obtaining these documents can be obtained
  from the Safe Drinking Water Hotline at 800-426-4791. Documents may be
  inspected at EPA's Drinking Water Docket, 1301 Constitution Avenue,
  NW., EPA West, Room B102, Washington DC 20460 (Telephone: 202-566-
  2426); or at the National Archives and Records Administration (NARA).
  For information on the availability of this material at NARA, call 202-
  741-6030, or go to: http://www.archives.gov/federal_register/
  code_of_federal_regulations/ibr_locations.html.
\1\ Except where noted, all methods refer to Standard Methods for the
  Examination of Water and Wastewater, 18th edition (1992), 19th edition
  (1995), or 20th edition (1998), American Public Health Association,
  1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods
  published in any of these three editions may be used. In addition, the
  following online versions may also be used: 2130 B-01, 9215 B-00, 9221
  A, B, C, E-99, 9222 A, B, C, D-97, and 9223 B-97. Standard Methods
  Online are available at http://www.standardmethods.org. The year in
  which each method was approved by the Standard Methods Committee is
  designated by the last two digits in the method number. The methods
  listed are the only Online versions that may be used.
\2\ The time from sample collection to initiation of analysis may not
  exceed 8 hours. Systems must hold samples below 10 deg. C during
  transit.
\3\ Lactose broth, as commercially available, may be used in lieu of
  lauryl tryptose broth, if the system conducts at least 25 parallel
  tests between this medium and lauryl tryptose broth using the water
  normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform, using
  lactose broth, is less than 10 percent.
\4\ Media should cover inverted tubes at least one-half to two-thirds
  after the sample is added.
\5\ No requirement exists to run the completed phase on 10 percent of
  all total coliform-positive confirmed tubes.
\6\ MI agar also may be used. Preparation and use of MI agar is set
  forth in the article, ``New medium for the simultaneous detection of
  total coliform and Escherichia coli in water'' by Brenner, K.P., et.
  al., 1993, Appl. Environ. Microbiol. 59:3534-3544. Also available from
  the Office of Water Resource Center (RC-4100T), 1200 Pennsylvania
  Avenue, NW., Washington DC 20460, EPA/600/J-99/225. Verification of
  colonies is not required.
\7\ The ONPG-MUG Test is also known as the Autoanalysis Colilert System.
 
\8\ A-1 broth may be held up to 7 days in a tightly closed screw cap
  tube at 4 [deg]C.
\9\ ``Methods for the Determination of Inorganic Substances in
  Environmental Samples'', EPA/600/R-93/100, August 1993. Available at
  NTIS, PB94-121811.
\10\ GLI Method 2, ``Turbidity,'' November 2, 1992, Great Lakes
  Instruments, Inc., 8855 North 55th Street, Milwaukee, WI 53223.
\11\ A description of the SimPlate method, ``IDEXX SimPlate TM HPC Test
  Method for Heterotrophs in Water,'' November 2000, can be obtained
  from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092,
  telephone (800) 321-0207.
\12\ A description of the Hach FilterTrak Method 10133, ``Determination
  of Turbidity by Laser Nephelometry,'' January 2000, Revision 2.0, can
  be obtained from; Hach Co., P.O. Box 389, Loveland, CO 80539-0389,
  telephone: 800-227-4224.
\13\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and
  stabilized formazin (e.g., Hach StablCal \TM\ or equivalent) are
  acceptable substitutes for formazin.

    (2) Public water systems must measure residual disinfectant 
concentrations with one of the analytical methods in the following table 
or one of the alternative methods listed in appendix A to subpart C of 
this part. If approved by the State, residual disinfectant 
concentrations for free chlorine and combined chlorine also may be 
measured by using DPD colorimetric test kits. In addition States may 
approve the use of the ITS free chlorine test strip for the 
determination of free chlorine. Use of the test strips is described in 
Method D99-003, ``Free Chlorine Species (HOCl- and 
OCl-) by Test Strip,'' Revision 3.0, November 21, 2003, 
available from Industrial Test Systems, Inc., 1875 Langston St., Rock 
Hill, SC 29730. Free and total chlorine residuals may be measured 
continuously by adapting a specified chlorine residual method for use 
with a continuous monitoring instrument provided the chemistry, 
accuracy, and precision remain the same. Instruments used for continuous 
monitoring must be calibrated with a grab sample measurement at least 
every five days, or with a protocol approved by the State.

[[Page 536]]



----------------------------------------------------------------------------------------------------------------
          Residual                 Methodology           SM \1\       SM Online \2\              Other
----------------------------------------------------------------------------------------------------------------
Free Chlorine...............  Amperometric          4500-Cl D......  4500-Cl D-00...  D1253-03 \3\
                               Titration.
                              DPD Ferrous           4500-Cl F......  4500-Cl F-00...
                               Titrimetric.
                              DPD Colorimetric....  4500-Cl G......  4500-Cl G-00...
                              Syringaldazine        4500-Cl H......  4500-Cl H-00...
                               (FACTS).
Total Chlorine..............  Amperometric          4500-Cl D......  4500-Cl D-00...  D1253-03 \3\
                               Titration.
                              Amperometric          4500-Cl E......  4500-Cl E-00...
                               Titration (low
                               level measurement).
                              DPD Ferrous           4500-Cl F......  4500-Cl F-00...
                               Titrimetric.
                              DPD Colorimetric....  4500-Cl G......  4500-Cl G-00...
                              Iodometric Electrode  4500-Cl I......  4500-Cl I-00...
Chlorine Dioxide............  Amperometric          4500-ClO2 C....  4500-ClO2 C-00.
                               Titration.
                              DPD Method..........  4500-ClO2 D....
                              Amperometric          4500-ClO2 E....  4500-ClO2 E-00.
                               Titration.
                              Spectrophotometric..  ...............  ...............  327.0, Revision 1.1 \4\
Ozone.......................  Indigo Method.......  4500-O3 B......  4500-O3 B-97 ..
----------------------------------------------------------------------------------------------------------------
\1\ All the listed methods are contained in the 18th, 19th, and 20th editions of Standard Methods for the
  Examination of Water and Wastewater, 1992, 1995, and 1998; the cited methods published in any of these three
  editions may be used.
\2\ Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was
  approved by the Standard Methods Committee is designated by the last two digits in the method number. The
  methods listed are the only Online versions that may be used.
\3\ Annual Book of ASTM Standards, Vol. 11.01, 2004 ; ASTM International; any year containing the cited version
  of the method may be used. Copies of this method may be obtained from ASTM International, 100 Barr Harbor
  Drive, P.O. Box C700 West Conshohocken, PA 19428-2959.
\4\ EPA Method 327.0, Revision 1.1, ``Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using
  Lissamine Green B and Horseradish Peroxidase with Detection by Visible Spectrophotometry,'' USEPA, May 2005,
  EPA 815-R-05-008. Available online at http://www.epa.gov/safewater/methods/sourcalt.html.


[[Page 537]]

    (b) Monitoring requirements for systems that do not provide 
filtration. A public water system that uses a surface water source and 
does not provide filtration treatment must begin monitoring, as 
specified in this paragraph (b), beginning December 31, 1990, unless the 
State has determined that filtration is required in writing pursuant to 
Sec.  1412(b)(7)(C)(iii), in which case the State may specify 
alternative monitoring requirements, as appropriate, until filtration is 
in place. A public water system that uses a ground water source under 
the direct influence of surface water and does not provide filtration 
treatment must begin monitoring as specified in this paragraph (b) 
beginning December 31, 1990, or 6 months after the State determines that 
the ground water source is under the direct influence of surface water, 
whichever is later, unless the State has determined that filtration is 
required in writing pursuant to Sec.  1412(b)(7)(C)(iii), in which case 
the State may specify alternative monitoring requirements, as 
appropriate, until filtration is in place.
    (1) Fecal coliform or total coliform density measurements as 
required by Sec.  141.71(a)(1) must be performed on representative 
source water samples immediately prior to the first or only point of 
disinfectant application. The system must sample for fecal or total 
coliforms at the following minimum frequency each week the system serves 
water to the public:

------------------------------------------------------------------------
                                                                Samples/
                 System size (persons served)                   week \1\
------------------------------------------------------------------------
<=500........................................................          1
501 to 3,300.................................................          2
3,301 to 10,000..............................................          3
10,001 to 25,000.............................................          4
25,000............................................          5
------------------------------------------------------------------------
\1\ Must be taken on separate days.


Also, one fecal or total coliform density measurement must be made every 
day the system serves water to the public and the turbidity of the 
source water exceeds 1 NTU (these samples count towards the weekly 
coliform sampling requirement) unless the State determines that the 
system, for logistical reasons outside the system's control, cannot have 
the sample analyzed within 30 hours of collection.
    (2) Turbidity measurements as required by Sec.  141.71(a)(2) must be 
performed on representative grab samples of source water immediately 
prior to the first or only point of disinfectant application every four 
hours (or more frequently) that the system serves water to the public. A 
public water system may substitute continuous turbidity monitoring for 
grab sample monitoring if it validates the continuous measurement for 
accuracy on a regular basis using a protocol approved by the State.
    (3) The total inactivation ratio for each day that the system is in 
operation must be determined based on the CT99.9 values in 
tables 1.1-1.6, 2.1, and 3.1 of this section, as appropriate. The 
parameters necessary to determine the total inactivation ratio must be 
monitored as follows:
    (i) The temperature of the disinfected water must be measured at 
least once per day at each residual disinfectant concentration sampling 
point.
    (ii) If the system uses chlorine, the pH of the disinfected water 
must be measured at least once per day at each chlorine residual 
disinfectant concentration sampling point.
    (iii) The disinfectant contact time(s) (``T'') must be determined 
for each day during peak hourly flow.
    (iv) The residual disinfectant concentration(s) (``C'') of the water 
before or at the first customer must be measured each day during peak 
hourly flow.
    (v) If a system uses a disinfectant other than chlorine, the system 
may demonstrate to the State, through the use of a State-approved 
protocol for on-site disinfection challenge studies or other information 
satisfactory to the State, that CT99.9 values other than 
those specified in tables 2.1 and 3.1 in this section other operational 
parameters are adequate to demonstrate that the system is achieving the 
minimum inactivation rates required by Sec.  141.72(a)(1).

[[Page 538]]



  Table 1.1--CT Values (CT99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 0.5
                                               [deg]C or Lower \1\
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                       Residual (mg/l)                        --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................     137    163    195    237    277    329     390
0.6..........................................................     141    168    200    239    286    342     407
0.8..........................................................     145    172    205    246    295    354     422
1.0..........................................................     148    176    210    253    304    365     437
1.2..........................................................     152    180    215    259    313    376     451
1.4..........................................................     155    184    221    266    321    387     464
1.6..........................................................     157    189    226    273    329    397     477
1.8..........................................................     162    193    231    279    338    407     489
2.0..........................................................     165    197    236    286    346    417     500
2.2..........................................................     169    201    242    297    353    426     511
2.4..........................................................     172    205    247    298    361    435     522
2.6..........................................................     175    209    252    304    368    444     533
2.8..........................................................     178    213    257    310    375    452     543
3.0..........................................................     181    217    261    316    382    460     552
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature and at the higher pH.


  Table 1.2--CT Values (CT 99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 5.0
                                                   [deg]C \1\
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                     Free residual (mg/l)                     --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................      97    117    139    166    198    236     279
  0.6........................................................     100    120    143    171    204    244     291
  0.8........................................................     103    122    146    175    210    252     301
  1.0........................................................     105    125    149    179    216    260     312
  1.2........................................................     107    127    152    183    221    267     320
  1.4........................................................     109    130    155    187    227    274     329
  1.6........................................................     111    132    158    192    232    281     337
  1.8........................................................     114    135    162    196    238    287     345
  2.0........................................................     116    138    165    200    243    294     353
  2.2........................................................     118    140    169    204    248    300     361
  2.4........................................................     120    143    172    209    253    306     368
  2.6........................................................     122    146    175    213    258    312     375
  2.8........................................................     124    148    178    217    263    318     382
  3.0........................................................     126    151    182    221    268    324     389
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature, and at the higher pH.


 Table 1.3--CT Values (CT 99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 10.0
                                                   [deg]C \1\
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                     Free residual (mg/l)                     --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................      73     88    104    125    149    177     209
  0.6........................................................      75     90    107    128    153    183     218
  0.8........................................................      78     92    110    131    158    189     226
  1.0........................................................      79     94    112    134    162    195     234
  1.2........................................................      80     95    114    137    166    200     240
  1.4........................................................      82     98    116    140    170    206     247
  1.6........................................................      83     99    119    144    174    211     253
  1.8........................................................      86    101    122    147    179    215     259
  2.0........................................................      87    104    124    150    182    221     265
  2.2........................................................      89    105    127    153    186    225     271
  2.4........................................................      90    107    129    157    190    230     276
  2.6........................................................      92    110    131    160    194    234     281
  2.8........................................................      93    111    134    163    197    239     287
  3.0........................................................      95    113    137    166    201    243     292
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature, and at the higher pH.


 Table 1.4--CT Values (CT 99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 15.0
                                                   [deg]C \1\
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                     Free residual (mg/l)                     --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................      49     59     70     83     99    118     140
  0.6........................................................      50     60     72     86    102    122     146
  0.8........................................................      52     61     73     88    105    126     151
  1.0........................................................      53     63     75     90    108    130     156
  1.2........................................................      54     64     76     92    111    134     160
  1.4........................................................      55     65     78     94    114    137     165
  1.6........................................................      56     66     79     96    116    141     169
  1.8........................................................      57     68     81     98    119    144     173
  2.0........................................................      58     69     83    100    122    147     177
  2.2........................................................      59     70     85    102    124    150     181
  2.4........................................................      60     72     86    105    127    153     184
  2.6........................................................      61     73     88    107    129    156     188
  2.8........................................................      62     74     89    109    132    159     191
  3.0........................................................      63     76     91    111    134    162     195
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature, and at the higher pH.


   Table 1.5--CT Values (CT99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 20
                                                   [deg]C \1\
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                     Free residual (mg/l)                     --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................      36     44     52     62     74     89     105
0.6..........................................................      38     45     54     64     77     92     109
0.8..........................................................      39     46     55     66     79     95     113
1.0..........................................................      39     47     56     67     81     98     117
1.2..........................................................      40     48     57     69     83    100     120
1.4..........................................................      41     49     58     70     85    103     123
1.6..........................................................      42     50     59     72     87    105     126

[[Page 539]]

 
1.8..........................................................      43     51     61     74     89    108     129
2.0..........................................................      44     52     62     75     91    110     132
2.2..........................................................      44     53     63     77     93    113     135
2.4..........................................................      45     54     65     78     95    115     138
2.6..........................................................      46     55     66     80     97    117     141
2.8..........................................................      47     56     67     81     99    119     143
3.0..........................................................      47     57     68     83    101    122     146
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature, and at the higher pH.


   Table 1.6--CT Values (CT99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Free Chlorine at 25
                                              [deg]C \1\ and Higher
----------------------------------------------------------------------------------------------------------------
                                                                                       pH
                     Free residual (mg/l)                     --------------------------------------------------
                                                                <=6.0   6.5    7.0    7.5    8.0    8.5    <=9.0
----------------------------------------------------------------------------------------------------------------
<=0.4........................................................      24     29     35     42     50     59      70
0.6..........................................................      25     30     36     43     51     61      73
0.8..........................................................      26     31     37     44     53     63      75
1.0..........................................................      26     31     37     45     54     65      78
1.2..........................................................      27     32     38     46     55     67      80
1.4..........................................................      27     33     39     47     57     69      82
1.6..........................................................      28     33     40     48     58     70      84
1.8..........................................................      29     34     41     49     60     72      86
2.0..........................................................      29     35     41     50     61     74      88
2.2..........................................................      30     35     42     51     62     75      90
2.4..........................................................      30     36     43     52     63     77      92
2.6..........................................................      31     37     44     53     65     78      94
2.8..........................................................      31     37     45     54     66     80      96
3.0..........................................................      32     38     46     55     67     81     97
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than a 99.99 percent inactivation of viruses. CT values between the
  indicated pH values may be determined by linear interpolation. CT values between the indicated temperatures of
  different tables may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value
  at the lower temperature, and at the higher pH.


  Table 2.1--CT Values (CT99.9) for 99.9 Percent Inactivation of Giardia Lamblia Cysts by Chlorine Dioxide and
                                                    Ozone \1\
----------------------------------------------------------------------------------------------------------------
                                                                           Temperature
                                               -----------------------------------------------------------------
                                                   <1                  10        15        20     =25
                                                 [deg]C   5 [deg]C   [deg]C    [deg]C    [deg]C       [deg]C
----------------------------------------------------------------------------------------------------------------
Chlorine dioxide..............................      63        26        23       19        15           11
Ozone.........................................       2.9       1.9       1.4      0.95      0.72         0.48
----------------------------------------------------------------------------------------------------------------
\1\ These CT values achieve greater than 99.99 percent inactivation of viruses. CT values between the indicated
  temperatures may be determined by linear interpolation. If no interpolation is used, use the CT99.9 value at
  the lower temperature for determining CT99.9 values between indicated temperatures.


 Table 3.1--CT Values (CT 99.9) for 99.9 Percent Inactivation of Giardia
                    Lamblia Cysts By Chloramines \1\
------------------------------------------------------------------------
                               Temperature
-------------------------------------------------------------------------
 <1 [deg]C     5 [deg]C    10 [deg]C   15 [deg]C   20 [deg]C   25 [deg]C
------------------------------------------------------------------------
3,800            2,200       1,850       1,500       1,100         750
------------------------------------------------------------------------
\1\ These values are for pH values of 6 to 9. These CT values may be
  assumed to achieve greater than 99.99 percent inactivation of viruses
  only if chlorine is added and mixed in the water prior to the addition
  of ammonia. If this condition is not met, the system must demonstrate,
  based on on-site studies or other information, as approved by the
  State, that the system is achieving at least 99.99 percent
  inactivation of viruses. CT values between the indicated temperatures
  may be determined by linear interpolation. If no interpolation is
  used, use the CT99.9 value at the lower temperature for determining
  CT99.9 values between indicated temperatures.

    (4) The total inactivation ratio must be calculated as follows:
    (i) If the system uses only one point of disinfectant application, 
the system may determine the total inactivation ratio based on either of 
the following two methods:
    (A) One inactivation ratio (CTcalc/CT99.9) is determined 
before or at the first customer during peak hourly flow and if the 
CTcalc/CT99.9 =1.0, the 99.9 percent Giardia 
lamblia inactivation requirement has been achieved; or
    (B) Successive CTcalc/CT99.9 values, representing 
sequential inactivation ratios, are determined between the point of 
disinfectant application and a point before or at the first customer 
during peak hourly flow. Under this alternative, the following method 
must be used to calculate the total inactivation ratio:


[[Page 540]]


[GRAPHIC] [TIFF OMITTED] TC15NO91.133


lamblia inactivation requirement has been achieved.
    (ii) If the system uses more than one point of disinfectant 
application before or at the first customer, the system must determine 
the CT value of each disinfection sequence immediately prior to the next 
point of disinfectant application during peak hourly flow. The CTcalc/
CT99.9 value of each sequence and
[GRAPHIC] [TIFF OMITTED] TC15NO91.134


must be calculated using the method in paragraph (b)(4)(i)(B) of this 
section to determine if the system is in compliance with Sec.  
141.72(a).
    (iii) Although not required, the total percent inactivation for a 
system with one or more points of residual disinfectant concentration 
monitoring may be calculated by solving the following equation:
[GRAPHIC] [TIFF OMITTED] TC15NO91.135

    (5) The residual disinfectant concentration of the water entering 
the distribution system must be monitored continuously, and the lowest 
value must be recorded each day, except that if there is a failure in 
the continuous monitoring equipment, grab sampling every 4 hours may be 
conducted in lieu of continuous monitoring, but for no more than 5 
working days following the failure of the equipment, and systems serving 
3,300 or fewer persons may take grab samples in lieu of providing 
continuous monitoring on an ongoing basis at the frequencies prescribed 
below:

------------------------------------------------------------------------
                                                                Samples/
                  System size by population                     day \1\
------------------------------------------------------------------------
<500.........................................................          1
501 to 1,000.................................................          2
1,001 to 2,500...............................................          3
2,501 to 3,300...............................................          4
------------------------------------------------------------------------
\1\ The day's samples cannot be taken at the same time. The sampling
  intervals are subject to State review and approval.


If at any time the residual disinfectant concentration falls below 0.2 
mg/l in a system using grab sampling in lieu of continuous monitoring, 
the system must take a grab sample every 4 hours until the residual 
concentration is equal to or greater than 0.2 mg/l.
    (6)(i) Until March 31, 2016, the residual disinfectant concentration 
must be measured at least at the same points in the distribution system 
and at the same time as total coliforms are sampled, as specified in 
Sec.  141.21. Beginning April 1, 2016, the residual disinfectant 
concentration must be measured at least at the same points in the 
distribution system and at the same time as total coliforms are sampled, 
as specified in Sec. Sec.  141.854 through 141.858. The State may allow 
a public water system which uses both a surface water source or a ground 
water source under direct influence of surface water, and a ground water 
source, to take disinfectant residual samples at points other than the 
total coliform sampling points if the State determines that such points 
are more representative of treated (disinfected) water quality within 
the distribution system. Heterotrophic bacteria, measured as 
heterotrophic plate count (HPC) as

[[Page 541]]

specified in paragraph (a)(1) of this section, may be measured in lieu 
of residual disinfectant concentration.
    (ii) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample transported and analyzed 
for HPC by a certified laboratory under the requisite time and 
temperature conditions specified by paragraph (a)(1) of this section and 
that the system is providing adequate disinfection in the distribution 
system, the requirements of paragraph (b)(6)(i) of this section do not 
apply to that system.
    (c) Monitoring requirements for systems using filtration treatment. 
A public water system that uses a surface water source or a ground water 
source under the influence of surface water and provides filtration 
treatment must monitor in accordance with this paragraph (c) beginning 
June 29, 1993, or when filtration is installed, whichever is later.
    (1) Turbidity measurements as required by Sec.  141.73 must be 
performed on representative samples of the system's filtered water every 
four hours (or more frequently) that the system serves water to the 
public. A public water system may substitute continuous turbidity 
monitoring for grab sample monitoring if it validates the continuous 
measurement for accuracy on a regular basis using a protocol approved by 
the State. For any systems using slow sand filtration or filtration 
treatment other than conventional treatment, direct filtration, or 
diatomaceous earth filtration, the State may reduce the sampling 
frequency to once per day if it determines that less frequent monitoring 
is sufficient to indicate effective filtration performance. For systems 
serving 500 or fewer persons, the State may reduce the turbidity 
sampling frequency to once per day, regardless of the type of filtration 
treatment used, if the State determines that less frequent monitoring is 
sufficient to indicate effective filtration performance.
    (2) The residual disinfectant concentration of the water entering 
the distribution system must be monitored continuously, and the lowest 
value must be recorded each day, except that if there is a failure in 
the continuous monitoring equipment, grab sampling every 4 hours may be 
conducted in lieu of continuous monitoring, but for no more than 5 
working days following the failure of the equipment, and systems serving 
3,300 or fewer persons may take grab samples in lieu of providing 
continuous monitoring on an ongoing basis at the frequencies each day 
prescribed below:

------------------------------------------------------------------------
                                                                Samples/
                  System size by population                     day \1\
------------------------------------------------------------------------
500....................................          1
501 to 1,000.................................................          2
1,001 to 2,500...............................................          3
2,501 to 3,300...............................................         4
------------------------------------------------------------------------
\1\ The day's samples cannot be taken at the same time. The sampling
  intervals are subject to State review and approval.


If at any time the residual disinfectant concentration falls below 0.2 
mg/l in a system using grab sampling in lieu of continuous monitoring, 
the system must take a grab sample every 4 hours until the residual 
disinfectant concentration is equal to or greater than 0.2 mg/l.
    (3)(i) Until March 31, 2016, the residual disinfectant concentration 
must be measured at least at the same points in the distribution system 
and at the same time as total coliforms are sampled, as specified in 
Sec.  141.21. Beginning April 1, 2016, the residual disinfectant 
concentration must be measured at least at the same points in the 
distribution system and at the same time as total coliforms are sampled, 
as specified in Sec. Sec.  141.854 through 141.858. The State may allow 
a public water system which uses both a surface water source or a ground 
water source under direct influence of surface water, and a ground water 
source, to take disinfectant residual samples at points other than the 
total coliform sampling points if the State determines that such points 
are more representative of treated (disinfected) water quality within 
the distribution system. Heterotrophic bacteria, measured as 
heterotrophic plate count (HPC) as specified in paragraph (a)(1) of this 
section, may be measured in lieu of residual disinfectant concentration.
    (ii) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample transported and analyzed 
for HPC by a certified laboratory under the requisite

[[Page 542]]

time and temperature conditions specified by paragraph (a)(1) of this 
section and that the system is providing adequate disinfection in the 
distribution system, the requirements of paragraph (c)(3)(i) of this 
section do not apply to that system.

[54 FR 27527, June 29, 1989, as amended at 59 FR 62470, Dec. 5, 1994; 60 
FR 34086, June 29, 1995; 64 FR 67465, Dec. 1, 1999; 67 FR 65252, Oct. 
23, 2002; 67 FR 65901, Oct. 29, 2002; 69 FR 38856, June 29, 2004; 72 FR 
11247, Mar. 12, 2007; 74 FR 30958, June 29, 2009; 78 FR 10347, Feb. 13, 
2013]



Sec.  141.75  Reporting and recordkeeping requirements.

    (a) A public water system that uses a surface water source and does 
not provide filtration treatment must report monthly to the State the 
information specified in this paragraph (a) beginning December 31, 1990, 
unless the State has determined that filtration is required in writing 
pursuant to section 1412(b)(7)(C)(iii), in which case the State may 
specify alternative reporting requirements, as appropriate, until 
filtration is in place. A public water system that uses a ground water 
source under the direct influence of surface water and does not provide 
filtration treatment must report monthly to the State the information 
specified in this paragraph (a) beginning December 31, 1990, or 6 months 
after the State determines that the ground water source is under the 
direct influence of surface water, whichever is later, unless the State 
has determined that filtration is required in writing pursuant to Sec.  
1412(b)(7)(C)(iii), in which case the State may specify alternative 
reporting requirements, as appropriate, until filtration is in place.
    (1) Source water quality information must be reported to the State 
within 10 days after the end of each month the system serves water to 
the public. Information that must be reported includes:
    (i) The cumulative number of months for which results are reported.
    (ii) The number of fecal and/or total coliform samples, whichever 
are analyzed during the month (if a system monitors for both, only fecal 
coliforms must be reported), the dates of sample collection, and the 
dates when the turbidity level exceeded 1 NTU.
    (iii) The number of samples during the month that had equal to or 
less than 20/100 ml fecal coliforms and/or equal to or less than 100/100 
ml total coliforms, whichever are analyzed.
    (iv) The cumulative number of fecal or total coliform samples, 
whichever are analyzed, during the previous six months the system served 
water to the public.
    (v) The cumulative number of samples that had equal to or less than 
20/100 ml fecal coliforms or equal to or less than 100/100 ml total 
coliforms, whichever are analyzed, during the previous six months the 
system served water to the public.
    (vi) The percentage of samples that had equal to or less than 20/100 
ml fecal coliforms or equal to or less than 100/100 ml total coliforms, 
whichever are analyzed, during the previous six months the system served 
water to the public.
    (vii) The maximum turbidity level measured during the month, the 
date(s) of occurrence for any measurement(s) which exceeded 5 NTU, and 
the date(s) the occurrence(s) was reported to the State.
    (viii) For the first 12 months of recordkeeping, the dates and 
cumulative number of events during which the turbidity exceeded 5 NTU, 
and after one year of recordkeeping for turbidity measurements, the 
dates and cumulative number of events during which the turbidity 
exceeded 5 NTU in the previous 12 months the system served water to the 
public.
    (ix) For the first 120 months of recordkeeping, the dates and 
cumulative number of events during which the turbidity exceeded 5 NTU, 
and after 10 years of recordkeeping for turbidity measurements, the 
dates and cumulative number of events during which the turbidity 
exceeded 5 NTU in the previous 120 months the system served water to the 
public.
    (2) Disinfection information specified in Sec.  141.74(b) must be 
reported to the State within 10 days after the end of each month the 
system serves water to the public. Information that must be reported 
includes:

[[Page 543]]

    (i) For each day, the lowest measurement of residual disinfectant 
concentration in mg/l in water entering the distribution system.
    (ii) The date and duration of each period when the residual 
disinfectant concentration in water entering the distribution system 
fell below 0.2 mg/l and when the State was notified of the occurrence.
    (iii) The daily residual disinfectant concentration(s) (in mg/l) and 
disinfectant contact time(s) (in minutes) used for calculating the CT 
value(s).
    (iv) If chlorine is used, the daily measurement(s) of pH of 
disinfected water following each point of chlorine disinfection.
    (v) The daily measurement(s) of water temperature in [deg]C 
following each point of disinfection.
    (vi) The daily CTcalc and CTcalc/CT99.9 values for each 
disinfectant measurement or sequence and the sum of all CTcalc/
CT99.9 values ((CTcalc/CT99.9)) before or at the 
first customer.
    (vii) The daily determination of whether disinfection achieves 
adequate Giardia cyst and virus inactivation, i.e., whether (CTcalc/
CT99.9) is at least 1.0 or, where disinfectants other than 
chlorine are used, other indicator conditions that the State determines 
are appropriate, are met.
    (viii) The following information on the samples taken in the 
distribution system in conjunction with total coliform monitoring 
pursuant to Sec.  141.72:
    (A) Number of instances where the residual disinfectant 
concentration is measured;
    (B) Number of instances where the residual disinfectant 
concentration is not measured but heterotrophic bacteria plate count 
(HPC) is measured;
    (C) Number of instances where the residual disinfectant 
concentration is measured but not detected and no HPC is measured;
    (D) Number of instances where the residual disinfectant 
concentration is detected and where HPC is 500/ml;
    (E) Number of instances where the residual disinfectant 
concentration is not measured and HPC is 500/ml;
    (F) For the current and previous month the system served water to 
the public, the value of ``V'' in the following formula:
[GRAPHIC] [TIFF OMITTED] TC15NO91.136

where:

a = the value in paragraph (a)(2)(viii)(A) of this section,
b = the value in paragraph (a)(2)(viii)(B) of this section,
c = the value in paragraph (a)(2)(viii)(C) of this section,
d = the value in paragraph (a)(2)(viii)(D) of this section, and
e = the value in paragraph (a)(2)(viii)(E) of this section.

    (G) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample transported and analyzed 
for HPC by a certified laboratory under the requisite time and 
temperature conditions specified by Sec.  141.74(a)(1) and that the 
system is providing adequate disinfection in the distribution system, 
the requirements of paragraph (a)(2)(viii) (A)-(F) of this section do 
not apply to that system.
    (ix) A system need not report the data listed in paragraphs (a)(2) 
(i), and (iii)-(vi) of this section if all data listed in paragraphs 
(a)(2) (i)-(viii) of this section remain on file at the system, and the 
State determines that:
    (A) The system has submitted to the State all the information 
required by paragraphs (a)(2) (i)-(viii) of this section for at least 12 
months; and
    (B) The State has determined that the system is not required to 
provide filtration treatment.
    (3) No later than ten days after the end of each Federal fiscal year 
(September 30), each system must provide to the State a report which 
summarizes its compliance with all watershed control program 
requirements specified in Sec.  141.71(b)(2).
    (4) No later than ten days after the end of each Federal fiscal year 
(September 30), each system must provide to the State a report on the 
on-site inspection conducted during that year pursuant to Sec.  
141.71(b)(3), unless the on-site inspection was conducted by the State. 
If the inspection was conducted by the State, the State must provide a 
copy of its report to the public water system.

[[Page 544]]

    (5)(i) Each system, upon discovering that a waterborne disease 
outbreak potentially attributable to that water system has occurred, 
must report that occurrence to the State as soon as possible, but no 
later than by the end of the next business day.
    (ii) If at any time the turbidity exceeds 5 NTU, the system must 
consult with the primacy agency as soon as practical, but no later than 
24 hours after the exceedance is known, in accordance with the public 
notification requirements under Sec.  141.203(b)(3).
    (iii) If at any time the residual falls below 0.2 mg/l in the water 
entering the distribution system, the system must notify the State as 
soon as possible, but no later than by the end of the next business day. 
The system also must notify the State by the end of the next business 
day whether or not the residual was restored to at least 0.2 mg/l within 
4 hours.
    (b) A public water system that uses a surface water source or a 
ground water source under the direct influence of surface water and 
provides filtration treatment must report monthly to the State the 
information specified in this paragraph (b) beginning June 29, 1993, or 
when filtration is installed, whichever is later.
    (1) Turbidity measurements as required by Sec.  141.74(c)(1) must be 
reported within 10 days after the end of each month the system serves 
water to the public. Information that must be reported includes:
    (i) The total number of filtered water turbidity measurements taken 
during the month.
    (ii) The number and percentage of filtered water turbidity 
measurements taken during the month which are less than or equal to the 
turbidity limits specified in Sec.  141.73 for the filtration technology 
being used.
    (iii) The date and value of any turbidity measurements taken during 
the month which exceed 5 NTU.
    (2) Disinfection information specified in Sec.  141.74(c) must be 
reported to the State within 10 days after the end of each month the 
system serves water to the public. Information that must be reported 
includes:
    (i) For each day, the lowest measurement of residual disinfectant 
concentration in mg/l in water entering the distribution system.
    (ii) The date and duration of each period when the residual 
disinfectant concentration in water entering the distribution system 
fell below 0.2 mg/l and when the State was notified of the occurrence.
    (iii) The following information on the samples taken in the 
distribution system in conjunction with total coliform monitoring 
pursuant to Sec.  141.72:
    (A) Number of instances where the residual disinfectant 
concentration is measured;
    (B) Number of instances where the residual disinfectant 
concentration is not measured but heterotrophic bacteria plate count 
(HPC) is measured;
    (C) Number of instances where the residual disinfectant 
concentration is measured but not detected and no HPC is measured;
    (D) Number of instances where no residual disinfectant concentration 
is detected and where HPC is 500/ml;
    (E) Number of instances where the residual disinfectant 
concentration is not measured and HPC is 500/ml;
    (F) For the current and previous month the system serves water to 
the public, the value of ``V'' in the following formula:
[GRAPHIC] [TIFF OMITTED] TC15NO91.137

where:

a = the value in paragraph (b)(2)(iii)(A) of this section,
b = the value in paragraph (b)(2)(iii)(B) of this section,
c = the value in paragraph (b)(2)(iii)(C) of this section,
d = the value in paragraph (b)(2)(iii)(D) of this section, and
e = the value in paragraph (b)(2)(iii)(E) of this section.

    (G) If the State determines, based on site-specific considerations, 
that a system has no means for having a sample transported and analyzed 
for HPC by a certified laboratory within the requisite time and 
temperature conditions specified by Sec.  141.74(a)(1) and that the 
system is providing adequate disinfection in the distribution system, 
the requirements of paragraph (b)(2)(iii) (A)-(F) of this section do not 
apply.

[[Page 545]]

    (iv) A system need not report the data listed in paragraph (b)(2)(i) 
of this section if all data listed in paragraphs (b)(2) (i)-(iii) of 
this section remain on file at the system and the State determines that 
the system has submitted all the information required by paragraphs 
(b)(2) (i)-(iii) of this section for at least 12 months.
    (3)(i) Each system, upon discovering that a waterborne disease 
outbreak potentially attributable to that water system has occurred, 
must report that occurrence to the State as soon as possible, but no 
later than by the end of the next business day.
    (ii) If at any time the turbidity exceeds 5 NTU, the system must 
consult with the primacy agency as soon as practical, but no later than 
24 hours after the exceedance is known, in accordance with the public 
notification requirements under Sec.  141.203(b)(3).
    (iii) If at any time the residual falls below 0.2 mg/l in the water 
entering the distribution system, the system must notify the State as 
soon as possible, but no later than by the end of the next business day. 
The system also must notify the State by the end of the next business 
day whether or not the residual was restored to at least 0.2 mg/l within 
4 hours.

[54 FR 27527, June 29, 1989, as amended at 65 FR 26022, May 4, 2000; 69 
FR 38856, June 29, 2004]



Sec.  141.76  Recycle provisions.

    (a) Applicability. All subpart H systems that employ conventional 
filtration or direct filtration treatment and that recycle spent filter 
backwash water, thickener supernatant, or liquids from dewatering 
processes must meet the requirements in paragraphs (b) through (d) of 
this section.
    (b) Reporting. A system must notify the State in writing by 
Decemeber 8, 2003, if the system recycles spent filter backwash water, 
thickener supernatant, or liquids from dewatering processes. This 
notification must include, at a minimum, the information specified in 
paragraphs (b)(1) and (2) of this section.
    (1) A plant schematic showing the origin of all flows which are 
recycled (including, but not limited to, spent filter backwash water, 
thickener supernatant, and liquids from dewatering processes), the 
hydraulic conveyance used to transport them, and the location where they 
are re-introduced back into the treatment plant.
    (2) Typical recycle flow in gallons per minute (gpm), the highest 
observed plant flow experienced in the previous year (gpm), design flow 
for the treatment plant (gpm), and State-approved operating capacity for 
the plant where the State has made such determinations.
    (c) Treatment technique requirement. Any system that recycles spent 
filter backwash water, thickener supernatant, or liquids from dewatering 
processes must return these flows through the processes of a system's 
existing conventional or direct filtration system as defined in Sec.  
141.2 or at an alternate location approved by the State by June 8, 2004. 
If capital improvements are required to modify the recycle location to 
meet this requirement, all capital improvements must be completed no 
later than June 8, 2006.
    (d) Recordkeeping. The system must collect and retain on file 
recycle flow information specified in paragraphs (d)(1) through (6) of 
this section for review and evaluation by the State beginning June 8, 
2004.
    (1) Copy of the recycle notification and information submitted to 
the State under paragraph (b) of this section.
    (2) List of all recycle flows and the frequency with which they are 
returned.
    (3) Average and maximum backwash flow rate through the filters and 
the average and maximum duration of the filter backwash process in 
minutes.
    (4) Typical filter run length and a written summary of how filter 
run length is determined.
    (5) The type of treatment provided for the recycle flow.
    (6) Data on the physical dimensions of the equalization and/or 
treatment units, typical and maximum hydraulic loading rates, type of 
treatment chemicals used and average dose and frequency of use, and 
frequency at which solids are removed, if applicable.

[66 FR 31103, June 8, 2001]

[[Page 546]]



                  Subpart I_Control of Lead and Copper

    Source: 56 FR 26548, June 7, 1991, unless otherwise noted.



Sec.  141.80  General requirements.

    (a) Applicability and effective dates. (1) The requirements of this 
subpart I constitute the national primary drinking water regulations for 
lead and copper. Unless otherwise indicated, each of the provisions of 
this subpart applies to community water systems and non-transient, non-
community water systems (hereinafter referred to as ``water systems'' or 
``systems'').
    (2) [Reserved]
    (b) Scope. These regulations establish a treatment technique that 
includes requirements for corrosion control treatment, source water 
treatment, lead service line replacement, and public education. These 
requirements are triggered, in some cases, by lead and copper action 
levels measured in samples collected at consumers' taps.
    (c) Lead and copper action levels. (1) The lead action level is 
exceeded if the concentration of lead in more than 10 percent of tap 
water samples collected during any monitoring period conducted in 
accordance with Sec.  141.86 is greater than 0.015 mg/L (i.e., if the 
``90th percentile'' lead level is greater than 0.015 mg/L).
    (2) The copper action level is exceeded if the concentration of 
copper in more than 10 percent of tap water samples collected during any 
monitoring period conducted in accordance with Sec.  141.86 is greater 
than 1.3 mg/L (i.e., if the ``90th percentile'' copper level is greater 
than 1.3 mg/L).
    (3) The 90th percentile lead and copper levels shall be computed as 
follows:
    (i) The results of all lead or copper samples taken during a 
monitoring period shall be placed in ascending order from the sample 
with the lowest concentration to the sample with the highest 
concentration. Each sampling result shall be assigned a number, 
ascending by single integers beginning with the number 1 for the sample 
with the lowest contaminant level. The number assigned to the sample 
with the highest contaminant level shall be equal to the total number of 
samples taken.
    (ii) The number of samples taken during the monitoring period shall 
be multiplied by 0.9.
    (iii) The contaminant concentration in the numbered sample yielded 
by the calculation in paragraph (c)(3)(ii) is the 90th percentile 
contaminant level.
    (iv) For water systems serving fewer than 100 people that collect 5 
samples per monitoring period, the 90th percentile is computed by taking 
the average of the highest and second highest concentrations.
    (v) For a public water system that has been allowed by the State to 
collect fewer than five samples in accordance with Sec.  141.86(c), the 
sample result with the highest concentration is considered the 90th 
percentile value.
    (d) Corrosion control treatment requirements. (1) All water systems 
shall install and operate optimal corrosion control treatment as defined 
in Sec.  141.2.
    (2) Any water system that complies with the applicable corrosion 
control treatment requirements specified by the State under Sec. Sec.  
141.81 and 141.82 shall be deemed in compliance with the treatment 
requirement contained in paragraph (d)(1) of this section.
    (e) Source water treatment requirements. Any system exceeding the 
lead or copper action level shall implement all applicable source water 
treatment requirements specified by the State under Sec.  141.83.
    (f) Lead service line replacement requirements. Any system exceeding 
the lead action level after implementation of applicable corrosion 
control and source water treatment requirements shall complete the lead 
service line replacement requirements contained in Sec.  141.84.
    (g) Public education requirements. Pursuant to Sec.  141.85, all 
water systems must provide a consumer notice of lead tap water 
monitoring results to persons served at the sites (taps) that are 
tested. Any system exceeding the lead action level shall implement the 
public education requirements.
    (h) Monitoring and analytical requirements. Tap water monitoring for 
lead

[[Page 547]]

and copper, monitoring for water quality parameters, source water 
monitoring for lead and copper, and analyses of the monitoring results 
under this subpart shall be completed in compliance with Sec. Sec.  
141.86, 141.87, 141.88, and 141.89.
    (i) Reporting requirements. Systems shall report to the State any 
information required by the treatment provisions of this subpart and 
Sec.  141.90.
    (j) Recordkeeping requirements. Systems shall maintain records in 
accordance with Sec.  141.91.
    (k) Violation of national primary drinking water regulations. 
Failure to comply with the applicable requirements of Sec. Sec.  141.80-
141.91, including requirements established by the State pursuant to 
these provisions, shall constitute a violation of the national primary 
drinking water regulations for lead and/or copper.

[56 FR 26548, June 7, 1991; 57 FR 28788, June 29, 1992, as amended at 72 
FR 57814, Oct. 10, 2007]



Sec.  141.81  Applicability of corrosion control treatment steps to small, 
medium-size and large water systems.

    (a) Systems shall complete the applicable corrosion control 
treatment requirements described in Sec.  141.82 by the deadlines 
established in this section.
    (1) A large system (serving 50,000 persons) shall 
complete the corrosion control treatment steps specified in paragraph 
(d) of this section, unless it is deemed to have optimized corrosion 
control under paragraph (b)(2) or (b)(3) of this section.
    (2) A small system (serving <=3300 persons) and a medium-size system 
(serving 3,300 and <=50,000 persons) shall complete the 
corrosion control treatment steps specified in paragraph (e) of this 
section, unless it is deemed to have optimized corrosion control under 
paragraph (b)(1), (b)(2), or (b)(3) of this section.
    (b) A system is deemed to have optimized corrosion control and is 
not required to complete the applicable corrosion control treatment 
steps identified in this section if the system satisfies one of the 
criteria specified in paragraphs (b)(1) through (b)(3) of this section. 
Any such system deemed to have optimized corrosion control under this 
paragraph, and which has treatment in place, shall continue to operate 
and maintain optimal corrosion control treatment and meet any 
requirements that the State determines appropriate to ensure optimal 
corrosion control treatment is maintained.
    (1) A small or medium-size water system is deemed to have optimized 
corrosion control if the system meets the lead and copper action levels 
during each of two consecutive six-month monitoring periods conducted in 
accordance with Sec.  141.86.
    (2) Any water system may be deemed by the State to have optimized 
corrosion control treatment if the system demonstrates to the 
satisfaction of the State that it has conducted activities equivalent to 
the corrosion control steps applicable to such system under this 
section. If the State makes this determination, it shall provide the 
system with written notice explaining the basis for its decision and 
shall specify the water quality control parameters representing optimal 
corrosion control in accordance with Sec.  141.82(f). Water systems 
deemed to have optimized corrosion control under this paragraph shall 
operate in compliance with the State-designated optimal water quality 
control parameters in accordance with Sec.  141.82(g) and continue to 
conduct lead and copper tap and water quality parameter sampling in 
accordance with Sec.  141.86(d)(3) and Sec.  141.87(d), respectively. A 
system shall provide the State with the following information in order 
to support a determination under this paragraph:
    (i) The results of all test samples collected for each of the water 
quality parameters in Sec.  141.82(c)(3).
    (ii) A report explaining the test methods used by the water system 
to evaluate the corrosion control treatments listed in Sec.  
141.82(c)(1), the results of all tests conducted, and the basis for the 
system's selection of optimal corrosion control treatment;
    (iii) A report explaining how corrosion control has been installed 
and how it is being maintained to insure minimal lead and copper 
concentrations at consumers' taps; and
    (iv) The results of tap water samples collected in accordance with 
Sec.  141.86 at least once every six months for one

[[Page 548]]

year after corrosion control has been installed.
    (3) Any water system is deemed to have optimized corrosion control 
if it submits results of tap water monitoring conducted in accordance 
with Sec.  141.86 and source water monitoring conducted in accordance 
with Sec.  141.88 that demonstrates for two consecutive 6-month 
monitoring periods that the difference between the 90th percentile tap 
water lead level computed under Sec.  141.80(c)(3), and the highest 
source water lead concentration is less than the Practical Quantitation 
Level for lead specified in Sec.  141.89(a)(1)(ii).
    (i) Those systems whose highest source water lead level is below the 
Method Detection Limit may also be deemed to have optimized corrosion 
control under this paragraph if the 90th percentile tap water lead level 
is less than or equal to the Practical Quantitation Level for lead for 
two consecutive 6-month monitoring periods.
    (ii) Any water system deemed to have optimized corrosion control in 
accordance with this paragraph shall continue monitoring for lead and 
copper at the tap no less frequently than once every three calendar 
years using the reduced number of sites specified in Sec.  141.86(c) and 
collecting the samples at times and locations specified in Sec.  
141.86(d)(4)(iv). Any such system that has not conducted a round of 
monitoring pursuant to Sec.  141.86(d) since September 30, 1997, shall 
complete a round of monitoring pursuant to this paragraph no later than 
September 30, 2000.
    (iii) Any water system deemed to have optimized corrosion control 
pursuant to this paragraph shall notify the State in writing pursuant to 
Sec.  141.90(a)(3) of any upcoming long-term change in treatment or 
addition of a new source as described in that section. The State must 
review and approve the addition of a new source or long-term change in 
water treatment before it is implemented by the water system. The State 
may require any such system to conduct additional monitoring or to take 
other action the State deems appropriate to ensure that such systems 
maintain minimal levels of corrosion in the distribution system.
    (iv) As of July 12, 2001, a system is not deemed to have optimized 
corrosion control under this paragraph, and shall implement corrosion 
control treatment pursuant to paragraph (b)(3)(v) of this section unless 
it meets the copper action level.
    (v) Any system triggered into corrosion control because it is no 
longer deemed to have optimized corrosion control under this paragraph 
shall implement corrosion control treatment in accordance with the 
deadlines in paragraph (e) of this section. Any such large system shall 
adhere to the schedule specified in that paragraph for medium-size 
systems, with the time periods for completing each step being triggered 
by the date the system is no longer deemed to have optimized corrosion 
control under this paragraph.
    (c) Any small or medium-size water system that is required to 
complete the corrosion control steps due to its exceedance of the lead 
or copper action level may cease completing the treatment steps whenever 
the system meets both action levels during each of two consecutive 
monitoring periods conducted pursuant to Sec.  141.86 and submits the 
results to the State. If any such water system thereafter exceeds the 
lead or copper action level during any monitoring period, the system (or 
the State, as the case may be) shall recommence completion of the 
applicable treatment steps, beginning with the first treatment step 
which was not previously completed in its entirety. The State may 
require a system to repeat treatment steps previously completed by the 
system where the State determines that this is necessary to implement 
properly the treatment requirements of this section. The State shall 
notify the system in writing of such a determination and explain the 
basis for its decision. The requirement for any small- or medium-size 
system to implement corrosion control treatment steps in accordance with 
paragraph (e) of this section (including systems deemed to have 
optimized corrosion control under paragraph (b)(1) of this section) is 
triggered whenever any small- or medium-size system exceeds the lead or 
copper action level.
    (d) Treatment steps and deadlines for large systems. Except as 
provided in paragraph (b) (2) and (3) of this section,

[[Page 549]]

large systems shall complete the following corrosion control treatment 
steps (described in the referenced portions of Sec. Sec.  141.82, 
141.86, and 141.87) by the indicated dates.
    (1) Step 1: The system shall conduct initial monitoring (Sec.  
141.86(d)(1) and Sec.  141.87(b)) during two consecutive six-month 
monitoring periods by January 1, 1993.
    (2) Step 2: The system shall complete corrosion control studies 
(Sec.  141.82(c)) by July 1, 1994.
    (3) Step 3: The State shall designate optimal corrosion control 
treatment (Sec.  141.82(d)) by January 1, 1995.
    (4) Step 4: The system shall install optimal corrosion control 
treatment (Sec.  141.82(e)) by January 1, 1997.
    (5) Step 5: The system shall complete follow-up sampling (Sec.  
141.86(d)(2) and Sec.  141.87(c)) by January 1, 1998.
    (6) Step 6: The State shall review installation of treatment and 
designate optimal water quality control parameters (Sec.  141.82(f)) by 
July 1, 1998.
    (7) Step 7: The system shall operate in compliance with the State-
specified optimal water quality control parameters (Sec.  141.82(g)) and 
continue to conduct tap sampling (Sec.  141.86(d)(3) and Sec.  
141.87(d)).
    (e) Treatment Steps and deadlines for small and medium-size systems. 
Except as provided in paragraph (b) of this section, small and medium-
size systems shall complete the following corrosion control treatment 
steps (described in the referenced portions of Sec. Sec.  141.82, 141.86 
and 141.87) by the indicated time periods.
    (1) Step 1: The system shall conduct initial tap sampling (Sec.  
141.86(d)(1) and Sec.  141.87(b)) until the system either exceeds the 
lead or copper action level or becomes eligible for reduced monitoring 
under Sec.  141.86(d)(4). A system exceeding the lead or copper action 
level shall recommend optimal corrosion control treatment (Sec.  
141.82(a)) within six months after the end of the monitoring period 
during which it exceeds one of the action levels.
    (2) Step 2: Within 12 months after the end of the monitoring period 
during which a system exceeds the lead or copper action level, the State 
may require the system to perform corrosion control studies (Sec.  
141.82(b)). If the State does not require the system to perform such 
studies, the State shall specify optimal corrosion control treatment 
(Sec.  141.82(d)) within the following timeframes:
    (i) For medium-size systems, within 18 months after the end of the 
monitoring period during which such system exceeds the lead or copper 
action level.
    (ii) For small systems, within 24 months after the end of the 
monitoring period during which such system exceeds the lead or copper 
action level.
    (3) Step 3: If the State requires a system to perform corrosion 
control studies under step 2, the system shall complete the studies 
(Sec.  141.82(c)) within 18 months after the State requires that such 
studies be conducted.
    (4) Step 4: If the system has performed corrosion control studies 
under step 2, the State shall designate optimal corrosion control 
treatment (Sec.  141.82(d)) within 6 months after completion of step 3.
    (5) Step 5: The system shall install optimal corrosion control 
treatment (Sec.  141.82(e)) within 24 months after the State designates 
such treatment.
    (6) Step 6: The system shall complete follow-up sampling (Sec.  
141.86(d)(2) and Sec.  141.87(c)) within 36 months after the State 
designates optimal corrosion control treatment.
    (7) Step 7: The State shall review the system's installation of 
treatment and designate optimal water quality control parameters (Sec.  
141.82(f)) within 6 months after completion of step 6.
    (8) Step 8: The system shall operate in compliance with the State-
designated optimal water quality control parameters (Sec.  141.82(g)) 
and continue to conduct tap sampling (Sec.  141.86(d)(3) and Sec.  
141.87(d)).

[56 FR 26548, June 7, 1991, as amended at 59 FR 33862, June 30, 1994; 65 
FR 2004, Jan. 12, 2000; 72 FR 57814, Oct. 10, 2007]



Sec.  141.82  Description of corrosion control treatment requirements.

    Each system shall complete the corrosion control treatment 
requirements described below which are applicable to such system under 
Sec.  141.81.
    (a) System recommendation regarding corrosion control treatment. 
Based upon the results of lead and copper tap monitoring and water 
quality parameter monitoring, small and medium-size

[[Page 550]]

water systems exceeding the lead or copper action level shall recommend 
installation of one or more of the corrosion control treatments listed 
in paragraph (c)(1) of this section which the system believes 
constitutes optimal corrosion control for that system. The State may 
require the system to conduct additional water quality parameter 
monitoring in accordance with Sec.  141.87(b) to assist the State in 
reviewing the system's recommendation.
    (b) State decision to require studies of corrosion control treatment 
(applicable to small and medium-size systems). The State may require any 
small or medium-size system that exceeds the lead or copper action level 
to perform corrosion control studies under paragraph (c) of this section 
to identify optimal corrosion control treatment for the system.
    (c) Performance of corrosion control studies. (1) Any public water 
system performing corrosion control studies shall evaluate the 
effectiveness of each of the following treatments, and, if appropriate, 
combinations of the following treatments to identify the optimal 
corrosion control treatment for that system:
    (i) Alkalinity and pH adjustment;
    (ii) Calcium hardness adjustment; and
    (iii) The addition of a phosphate or silicate based corrosion 
inhibitor at a concentration sufficient to maintain an effective 
residual concentration in all test tap samples.
    (2) The water system shall evaluate each of the corrosion control 
treatments using either pipe rig/loop tests, metal coupon tests, 
partial-system tests, or analyses based on documented analogous 
treatments with other systems of similar size, water chemistry and 
distribution system configuration.
    (3) The water system shall measure the following water quality 
parameters in any tests conducted under this paragraph before and after 
evaluating the corrosion control treatments listed above:
    (i) Lead;
    (ii) Copper;
    (iii) pH;
    (iv) Alkalinity;
    (v) Calcium;
    (vi) Conductivity;
    (vii) Orthophosphate (when an inhibitor containing a phosphate 
compound is used);
    (viii) Silicate (when an inhibitor containing a silicate compound is 
used);
    (ix) Water temperature.
    (4) The water system shall identify all chemical or physical 
constraints that limit or prohibit the use of a particular corrosion 
control treatment and document such constraints with at least one of the 
following:
    (i) Data and documentation showing that a particular corrosion 
control treatment has adversely affected other water treatment processes 
when used by another water system with comparable water quality 
characteristics; and/or
    (ii) Data and documentation demonstrating that the water system has 
previously attempted to evaluate a particular corrosion control 
treatment and has found that the treatment is ineffective or adversely 
affects other water quality treatment processes.
    (5) The water system shall evaluate the effect of the chemicals used 
for corrosion control treatment on other water quality treatment 
processes.
    (6) On the basis of an analysis of the data generated during each 
evaluation, the water system shall recommend to the State in writing the 
treatment option that the corrosion control studies indicate constitutes 
optimal corrosion control treatment for that system. The water system 
shall provide a rationale for its recommendation along with all 
supporting documentation specified in paragraphs (c) (1) through (5) of 
this section.
    (d) State designation of optimal corrosion control treatment. (1) 
Based upon consideration of available information including, where 
applicable, studies performed under paragraph (c) of this section and a 
system's recommended treatment alternative, the State shall either 
approve the corrosion control treatment option recommended by the 
system, or designate alternative corrosion control treatment(s) from 
among those listed in paragraph (c)(1) of this section. When designating 
optimal treatment the State shall consider the

[[Page 551]]

effects that additional corrosion control treatment will have on water 
quality parameters and on other water quality treatment processes.
    (2) The State shall notify the system of its decision on optimal 
corrosion control treatment in writing and explain the basis for this 
determination. If the State requests additional information to aid its 
review, the water system shall provide the information.
    (e) Installation of optimal corrosion control. Each system shall 
properly install and operate throughout its distribution system the 
optimal corrosion control treatment designated by the State under 
paragraph (d) of this section.
    (f) State review of treatment and specification of optimal water 
quality control parameters. The State shall evaluate the results of all 
lead and copper tap samples and water quality parameter samples 
submitted by the water system and determine whether the system has 
properly installed and operated the optimal corrosion control treatment 
designated by the State in paragraph (d) of this section. Upon reviewing 
the results of tap water and water quality parameter monitoring by the 
system, both before and after the system installs optimal corrosion 
control treatment, the State shall designate:
    (1) A minimum value or a range of values for pH measured at each 
entry point to the distribution system;
    (2) A minimum pH value, measured in all tap samples. Such value 
shall be equal to or greater than 7.0, unless the State determines that 
meeting a pH level of 7.0 is not technologically feasible or is not 
necessary for the system to optimize corrosion control;
    (3) If a corrosion inhibitor is used, a minimum concentration or a 
range of concentrations for the inhibitor, measured at each entry point 
to the distribution system and in all tap samples, that the State 
determines is necessary to form a passivating film on the interior walls 
of the pipes of the distribution system;
    (4) If alkalinity is adjusted as part of optimal corrosion control 
treatment, a minimum concentration or a range of concentrations for 
alkalinity, measured at each entry point to the distribution system and 
in all tap samples;
    (5) If calcium carbonate stabilization is used as part of corrosion 
control, a minimum concentration or a range of concentrations for 
calcium, measured in all tap samples.

The values for the applicable water quality control parameters listed 
above shall be those that the State determines to reflect optimal 
corrosion control treatment for the system. The State may designate 
values for additional water quality control parameters determined by the 
State to reflect optimal corrosion control for the system. The State 
shall notify the system in writing of these determinations and explain 
the basis for its decisions.
    (g) Continued operation and monitoring. All systems optimizing 
corrosion control shall continue to operate and maintain optimal 
corrosion control treatment, including maintaining water quality 
parameters at or above minimum values or within ranges designated by the 
State under paragraph (f) of this section, in accordance with this 
paragraph for all samples collected under Sec.  141.87(d) through (f). 
Compliance with the requirements of this paragraph shall be determined 
every six months, as specified under Sec.  141.87(d). A water system is 
out of compliance with the requirements of this paragraph for a six-
month period if it has excursions for any State-specified parameter on 
more than nine days during the period. An excursion occurs whenever the 
daily value for one or more of the water quality parameters measured at 
a sampling location is below the minimum value or outside the range 
designated by the State. Daily values are calculated as follows. States 
have discretion to delete results of obvious sampling errors from this 
calculation.
    (1) On days when more than one measurement for the water quality 
parameter is collected at the sampling location, the daily value shall 
be the average of all results collected during the day regardless of 
whether they are collected through continuous monitoring, grab sampling, 
or a combination of both. If EPA has approved an alternative formula 
under Sec.  142.16 of this chapter in the State's application for a

[[Page 552]]

program revision submitted pursuant to Sec.  142.12 of this chapter, the 
State's formula shall be used to aggregate multiple measurements taken 
at a sampling point for the water quality parameter in lieu of the 
formula in this paragraph.
    (2) On days when only one measurement for the water quality 
parameter is collected at the sampling location, the daily value shall 
be the result of that measurement.
    (3) On days when no measurement is collected for the water quality 
parameter at the sampling location, the daily value shall be the daily 
value calculated on the most recent day on which the water quality 
parameter was measured at the sample site.
    (h) Modification of State treatment decisions. Upon its own 
initiative or in response to a request by a water system or other 
interested party, a State may modify its determination of the optimal 
corrosion control treatment under paragraph (d) of this section or 
optimal water quality control parameters under paragraph (f) of this 
section. A request for modification by a system or other interested 
party shall be in writing, explain why the modification is appropriate, 
and provide supporting documentation. The State may modify its 
determination where it concludes that such change is necessary to ensure 
that the system continues to optimize corrosion control treatment. A 
revised determination shall be made in writing, set forth the new 
treatment requirements, explain the basis for the State's decision, and 
provide an implementation schedule for completing the treatment 
modifications.
    (i) Treatment decisions by EPA in lieu of the State. Pursuant to the 
procedures in Sec.  142.19, the EPA Regional Administrator may review 
treatment determinations made by a State under paragraphs (d), (f), or 
(h) of this section and issue federal treatment determinations 
consistent with the requirements of those paragraphs where the Regional 
Administrator finds that:
    (1) A State has failed to issue a treatment determination by the 
applicable deadlines contained in Sec.  141.81,
    (2) A State has abused its discretion in a substantial number of 
cases or in cases affecting a substantial population, or
    (3) The technical aspects of a State's determination would be 
indefensible in an expected Federal enforcement action taken against a 
system.

[56 FR 26548, June 7, 1991, as amended at 65 FR 2004, Jan. 12, 2000]



Sec.  141.83  Source water treatment requirements.

    Systems shall complete the applicable source water monitoring and 
treatment requirements (described in the referenced portions of 
paragraph (b) of this section, and in Sec. Sec.  141.86, and 141.88) by 
the following deadlines.
    (a) Deadlines for completing source water treatment steps--(1) Step 
1: A system exceeding the lead or copper action level shall complete 
lead and copper source water monitoring (Sec.  141.88(b)) and make a 
treatment recommendation to the State (Sec.  141.83(b)(1)) no later than 
180 days after the end of the monitoring period during which the lead or 
copper action level was exceeded.
    (2) Step 2: The State shall make a determination regarding source 
water treatment (Sec.  141.83(b)(2)) within 6 months after submission of 
monitoring results under step 1.
    (3) Step 3: If the State requires installation of source water 
treatment, the system shall install the treatment (Sec.  141.83(b)(3)) 
within 24 months after completion of step 2.
    (4) Step 4: The system shall complete follow-up tap water monitoring 
(Sec.  141.86(d)(2) and source water monitoring (Sec.  141.88(c)) within 
36 months after completion of step 2.
    (5) Step 5: The State shall review the system's installation and 
operation of source water treatment and specify maximum permissible 
source water levels (Sec.  141.83(b)(4)) within 6 months after 
completion of step 4.
    (6) Step 6: The system shall operate in compliance with the State-
specified maximum permissible lead and copper source water levels (Sec.  
141.83(b)(4)) and continue source water monitoring (Sec.  141.88(d)).
    (b) Description of source water treatment requirements--(1) System 
treatment recommendation. Any system which exceeds the lead or copper 
action level

[[Page 553]]

shall recommend in writing to the State the installation and operation 
of one of the source water treatments listed in paragraph (b)(2) of this 
section. A system may recommend that no treatment be installed based 
upon a demonstration that source water treatment is not necessary to 
minimize lead and copper levels at users' taps.
    (2) State determination regarding source water treatment. The State 
shall complete an evaluation of the results of all source water samples 
submitted by the water system to determine whether source water 
treatment is necessary to minimize lead or copper levels in water 
delivered to users' taps. If the State determines that treatment is 
needed, the State shall either require installation and operation of the 
source water treatment recommended by the system (if any) or require the 
installation and operation of another source water treatment from among 
the following: Ion exchange, reverse osmosis, lime softening or 
coagulation/filtration. If the State requests additional information to 
aid in its review, the water system shall provide the information by the 
date specified by the State in its request. The State shall notify the 
system in writing of its determination and set forth the basis for its 
decision.
    (3) Installation of source water treatment. Each system shall 
properly install and operate the source water treatment designated by 
the State under paragraph (b)(2) of this section.
    (4) State review of source water treatment and specification of 
maximum permissible source water levels. The State shall review the 
source water samples taken by the water system both before and after the 
system installs source water treatment, and determine whether the system 
has properly installed and operated the source water treatment 
designated by the State. Based upon its review, the State shall 
designate the maximum permissible lead and copper concentrations for 
finished water entering the distribution system. Such levels shall 
reflect the contaminant removal capability of the treatment properly 
operated and maintained. The State shall notify the system in writing 
and explain the basis for its decision.
    (5) Continued operation and maintenance. Each water system shall 
maintain lead and copper levels below the maximum permissible 
concentrations designated by the State at each sampling point monitored 
in accordance with Sec.  141.88. The system is out of compliance with 
this paragraph if the level of lead or copper at any sampling point is 
greater than the maximum permissible concentration designated by the 
State.
    (6) Modification of State treatment decisions. Upon its own 
initiative or in response to a request by a water system or other 
interested party, a State may modify its determination of the source 
water treatment under paragraph (b)(2) of this section, or maximum 
permissible lead and copper concentrations for finished water entering 
the distribution system under paragraph (b)(4) of this section. A 
request for modification by a system or other interested party shall be 
in writing, explain why the modification is appropriate, and provide 
supporting documentation. The State may modify its determination where 
it concludes that such change is necessary to ensure that the system 
continues to minimize lead and copper concentrations in source water. A 
revised determination shall be made in writing, set forth the new 
treatment requirements, explain the basis for the State's decision, and 
provide an implementation schedule for completing the treatment 
modifications.
    (7) Treatment decisions by EPA in lieu of the State. Pursuant to the 
procedures in Sec.  142.19, the EPA Regional Administrator may review 
treatment determinations made by a State under paragraphs (b) (2), (4), 
or (6) of this section and issue Federal treatment determinations 
consistent with the requirements of those paragraphs where the 
Administrator finds that:
    (i) A State has failed to issue a treatment determination by the 
applicable deadlines contained in Sec.  141.83(a),
    (ii) A state has abused its discretion in a substantial number of 
cases or in cases affecting a substantial population, or

[[Page 554]]

    (iii) The technical aspects of a State's determination would be 
indefensible in an expected Federal enforcement action taken against a 
system.

[56 FR 26548, June 7, 1991, as amended at 72 FR 57815, Oct. 10, 2007]



Sec.  141.84  Lead service line replacement requirements.

    (a) Systems that fail to meet the lead action level in tap samples 
taken pursuant to Sec.  141.86(d)(2), after installing corrosion control 
and/or source water treatment (whichever sampling occurs later), shall 
replace lead service lines in accordance with the requirements of this 
section. If a system is in violation of Sec.  141.81 or Sec.  141.83 for 
failure to install source water or corrosion control treatment, the 
State may require the system to commence lead service line replacement 
under this section after the date by which the system was required to 
conduct monitoring under Sec.  141.86(d)(2) has passed.
    (b)(1) A water system shall replace annually at least 7 percent of 
the initial number of lead service lines in its distribution system. The 
initial number of lead service lines is the number of lead lines in 
place at the time the replacement program begins. The system shall 
identify the initial number of lead service lines in its distribution 
system, including an identification of the portion(s) owned by the 
system, based on a materials evaluation, including the evaluation 
required under Sec.  141.86(a) and relevant legal authorities (e.g., 
contracts, local ordinances) regarding the portion owned by the system. 
The first year of lead service line replacement shall begin on the first 
day following the end of the monitoring period in which the action level 
was exceeded under paragraph (a) of this section. If monitoring is 
required annually or less frequently, the end of the monitoring period 
is September 30 of the calendar year in which the sampling occurs. If 
the State has established an alternate monitoring period, then the end 
of the monitoring period will be the last day of that period.
    (2) Any water system resuming a lead service line replacement 
program after the cessation of its lead service line replacement program 
as allowed by paragraph (f) of this section shall update its inventory 
of lead service lines to include those sites that were previously 
determined not to require replacement through the sampling provision 
under paragraph (c) of this section. The system will then divide the 
updated number of remaining lead service lines by the number of 
remaining years in the program to determine the number of lines that 
must be replaced per year (7 percent lead service line replacement is 
based on a 15-year replacement program, so, for example, systems 
resuming lead service line replacement after previously conducting two 
years of replacement would divide the updated inventory by 13). For 
those systems that have completed a 15-year lead service line 
replacement program, the State will determine a schedule for replacing 
or retesting lines that were previously tested out under the replacement 
program when the system re-exceeds the action level.
    (c) A system is not required to replace an individual lead service 
line if the lead concentration in all service line samples from that 
line, taken pursuant to Sec.  141.86(b)(3), is less than or equal to 
0.015 mg/L.
    (d) A water system shall replace that portion of the lead service 
line that it owns. In cases where the system does not own the entire 
lead service line, the system shall notify the owner of the line, or the 
owner's authorized agent, that the system will replace the portion of 
the service line that it owns and shall offer to replace the owner's 
portion of the line. A system is not required to bear the cost of 
replacing the privately-owned portion of the line, nor is it required to 
replace the privately-owned portion where the owner chooses not to pay 
the cost of replacing the privately-owned portion of the line, or where 
replacing the privately-owned portion would be precluded by State, local 
or common law. A water system that does not replace the entire length of 
the service line also shall complete the following tasks.
    (1) At least 45 days prior to commencing with the partial 
replacement of a lead service line, the water system shall provide 
notice to the resident(s) of all buildings served by the line explaining 
that they may experience a temporary increase of lead levels in

[[Page 555]]

their drinking water, along with guidance on measures consumers can take 
to minimize their exposure to lead. The State may allow the water system 
to provide notice under the previous sentence less than 45 days prior to 
commencing partial lead service line replacement where such replacement 
is in conjunction with emergency repairs. In addition, the water system 
shall inform the resident(s) served by the line that the system will, at 
the system's expense, collect a sample from each partially-replaced lead 
service line that is representative of the water in the service line for 
analysis of lead content, as prescribed under Sec.  141.86(b)(3), within 
72 hours after the completion of the partial replacement of the service 
line. The system shall collect the sample and report the results of the 
analysis to the owner and the resident(s) served by the line within 
three business days of receiving the results. Mailed notices post-marked 
within three business days of receiving the results shall be considered 
``on time.''
    (2) The water system shall provide the information required by 
paragraph (d)(1) of this section to the residents of individual 
dwellings by mail or by other methods approved by the State. In 
instances where multi-family dwellings are served by the line, the water 
system shall have the option to post the information at a conspicuous 
location.
    (e) The State shall require a system to replace lead service lines 
on a shorter schedule than that required by this section, taking into 
account the number of lead service lines in the system, where such a 
shorter replacement schedule is feasible. The State shall make this 
determination in writing and notify the system of its finding within 6 
months after the system is triggered into lead service line replacement 
based on monitoring referenced in paragraph (a) of this section.
    (f) Any system may cease replacing lead service lines whenever first 
draw samples collected pursuant to Sec.  141.86(b)(2) meet the lead 
action level during each of two consecutive monitoring periods and the 
system submits the results to the State. If first draw tap samples 
collected in any such system thereafter exceeds the lead action level, 
the system shall recommence replacing lead service lines pursuant to 
paragraph (b)(2) of this section.
    (g) To demonstrate compliance with paragraphs (a) through (d) of 
this section, a system shall report to the State the information 
specified in Sec.  141.90(e).

[56 FR 26548, June 7, 1991; 57 FR 28788, June 29, 1992, as amended at 65 
FR 2005, Jan. 12, 2000; 72 FR 57815, Oct. 10, 2007]



Sec.  141.85  Public education and supplemental monitoring requirements.

    All water systems must deliver a consumer notice of lead tap water 
monitoring results to persons served by the water system at sites that 
are tested, as specified in paragraph (d) of this section. A water 
system that exceeds the lead action level based on tap water samples 
collected in accordance with Sec.  141.86 shall deliver the public 
education materials contained in paragraph (a) of this section in 
accordance with the requirements in paragraph (b) of this section. Water 
systems that exceed the lead action level must sample the tap water of 
any customer who requests it in accordance with paragraph (c) of this 
section.
    (a) Content of written public education materials--(1) Community 
water systems and non-transient non-community water systems. Water 
systems must include the following elements in printed materials (e.g., 
brochures and pamphlets) in the same order as listed below. In addition, 
language in paragraphs (a)(1)(i) through (ii) and (a)(1)(vi) of this 
section must be included in the materials, exactly as written, except 
for the text in brackets in these paragraphs for which the water system 
must include system-specific information. Any additional information 
presented by a water system must be consistent with the information 
below and be in plain language that can be understood by the general 
public. Water systems must submit all written public education materials 
to the State prior to delivery. The State may require the system to 
obtain approval of the content of written public materials prior to 
delivery.
    (i) IMPORTANT INFORMATION ABOUT LEAD IN YOUR DRINKING WATER. [INSERT 
NAME OF WATER

[[Page 556]]

SYSTEM] found elevated levels of lead in drinking water in some homes/
buildings. Lead can cause serious health problems, especially for 
pregnant women and young children. Please read this information closely 
to see what you can do to reduce lead in your drinking water.
    (ii) Health effects of lead. Lead can cause serious health problems 
if too much enters your body from drinking water or other sources. It 
can cause damage to the brain and kidneys, and can interfere with the 
production of red blood cells that carry oxygen to all parts of your 
body. The greatest risk of lead exposure is to infants, young children, 
and pregnant women. Scientists have linked the effects of lead on the 
brain with lowered IQ in children. Adults with kidney problems and high 
blood pressure can be affected by low levels of lead more than healthy 
adults. Lead is stored in the bones, and it can be released later in 
life. During pregnancy, the child receives lead from the mother's bones, 
which may affect brain development.
    (iii) Sources of lead. (A) Explain what lead is.
    (B) Explain possible sources of lead in drinking water and how lead 
enters drinking water. Include information on home/building plumbing 
materials and service lines that may contain lead.
    (C) Discuss other important sources of lead exposure in addition to 
drinking water (e.g., paint).
    (iv) Discuss the steps the consumer can take to reduce their 
exposure to lead in drinking water.
    (A) Encourage running the water to flush out the lead.
    (B) Explain concerns with using hot water from the tap and 
specifically caution against the use of hot water for preparing baby 
formula.
    (C) Explain that boiling water does not reduce lead levels.
    (D) Discuss other options consumers can take to reduce exposure to 
lead in drinking water, such as alternative sources or treatment of 
water.
    (E) Suggest that parents have their child's blood tested for lead.
    (v) Explain why there are elevated levels of lead in the system's 
drinking water (if known) and what the water system is doing to reduce 
the lead levels in homes/buildings in this area.
    (vi) For more information, call us at [INSERT YOUR NUMBER] [(IF 
APPLICABLE), or visit our Web site at [INSERT YOUR WEB SITE HERE]]. For 
more information on reducing lead exposure around your home/building and 
the health effects of lead, visit EPA's Web site at http://www.epa.gov/
lead or contact your health care provider.
    (2) Community water systems. In addition to including the elements 
specified in paragraph (a)(1) of this section, community water systems 
must:
    (i) Tell consumers how to get their water tested.
    (ii) Discuss lead in plumbing components and the difference between 
low lead and lead free.
    (b) Delivery of public education materials. (1) For public water 
systems serving a large proportion of non-English speaking consumers, as 
determined by the State, the public education materials must contain 
information in the appropriate language(s) regarding the importance of 
the notice or contain a telephone number or address where persons served 
may contact the water system to obtain a translated copy of the public 
education materials or to request assistance in the appropriate 
language.
    (2) A community water system that exceeds the lead action level on 
the basis of tap water samples collected in accordance with Sec.  
141.86, and that is not already conducting public education tasks under 
this section, must conduct the public education tasks under this section 
within 60 days after the end of the monitoring period in which the 
exceedance occurred:
    (i) Deliver printed materials meeting the content requirements of 
paragraph (a) of this section to all bill paying customers.
    (ii)(A) Contact customers who are most at risk by delivering 
education materials that meet the content requirements of paragraph (a) 
of this section to local public health agencies even if they are not 
located within the water system's service area, along with an 
informational notice that encourages distribution to all the 
organization's potentially affected customers or community water 
system's users.

[[Page 557]]

The water system must contact the local public health agencies directly 
by phone or in person. The local public health agencies may provide a 
specific list of additional community based organizations serving target 
populations, which may include organizations outside the service area of 
the water system. If such lists are provided, systems must deliver 
education materials that meet the content requirements of paragraph (a) 
of this section to all organizations on the provided lists.
    (B) Contact customers who are most at risk by delivering materials 
that meet the content requirements of paragraph (a) of this section to 
the following organizations listed in 1 through 6 that are located 
within the water system's service area, along with an informational 
notice that encourages distribution to all the organization's 
potentially affected customers or community water system's users:
    (1) Public and private schools or school boards.
    (2) Women, Infants and Children (WIC) and Head Start programs.
    (3) Public and private hospitals and medical clinics.
    (4) Pediatricians.
    (5) Family planning clinics.
    (6) Local welfare agencies.
    (C) Make a good faith effort to locate the following organizations 
within the service area and deliver materials that meet the content 
requirements of paragraph (a) of this section to them, along with an 
informational notice that encourages distribution to all potentially 
affected customers or users. The good faith effort to contact at-risk 
customers may include requesting a specific contact list of these 
organizations from the local public health agencies, even if the 
agencies are not located within the water system's service area:
    (1) Licensed childcare centers
    (2) Public and private preschools.
    (3) Obstetricians-Gynecologists and Midwives.
    (iii) No less often than quarterly, provide information on or in 
each water bill as long as the system exceeds the action level for lead. 
The message on the water bill must include the following statement 
exactly as written except for the text in brackets for which the water 
system must include system-specific information: [INSERT NAME OF WATER 
SYSTEM] found high levels of lead in drinking water in some homes. Lead 
can cause serious health problems. For more information please call 
[INSERT NAME OF WATER SYSTEM] [or visit (INSERT YOUR WEB SITE HERE)]. 
The message or delivery mechanism can be modified in consultation with 
the State; specifically, the State may allow a separate mailing of 
public education materials to customers if the water system cannot place 
the information on water bills.
    (iv) Post material meeting the content requirements of paragraph (a) 
of this section on the water system's Web site if the system serves a 
population greater than 100,000.
    (v) Submit a press release to newspaper, television and radio 
stations.
    (vi) In addition to paragraphs (b)(2)(i) through (v) of this 
section, systems must implement at least three activities from one or 
more categories listed below. The educational content and selection of 
these activities must be determined in consultation with the State.
    (A) Public Service Announcements.
    (B) Paid advertisements.
    (C) Public Area Information Displays.
    (D) E-mails to customers.
    (E) Public Meetings.
    (F) Household Deliveries.
    (G) Targeted Individual Customer Contact.
    (H) Direct material distribution to all multi-family homes and 
institutions.
    (I) Other methods approved by the State.
    (vii) For systems that are required to conduct monitoring annually 
or less frequently, the end of the monitoring period is September 30 of 
the calendar year in which the sampling occurs, or, if the State has 
established an alternate monitoring period, the last day of that period.
    (3) As long as a community water system exceeds the action level, it 
must repeat the activities pursuant to paragraph (b)(2) of this section 
as described in paragraphs (b)(3)(i) through (iv) of this section.

[[Page 558]]

    (i) A community water system shall repeat the tasks contained in 
paragraphs (b)(2)(i), (ii) and (vi) of this section every 12 months.
    (ii) A community water system shall repeat tasks contained in 
paragraph (b)(2)(iii) of this section with each billing cycle.
    (iii) A community water system serving a population greater than 
100,000 shall post and retain material on a publicly accessible Web site 
pursuant to paragraph (b)(2)(iv) of this section.
    (iv) The community water system shall repeat the task in paragraph 
(b)(2)(v) of this section twice every 12 months on a schedule agreed 
upon with the State. The State can allow activities in paragraph (b)(2) 
of this section to extend beyond the 60-day requirement if needed for 
implementation purposes on a case-by-case basis; however, this extension 
must be approved in writing by the State in advance of the 60-day 
deadline.
    (4) Within 60 days after the end of the monitoring period in which 
the exceedance occurred (unless it already is repeating public education 
tasks pursuant to paragraph (b)(5) of this section), a non-transient 
non-community water system shall deliver the public education materials 
specified by paragraph (a) of this section as follows:
    (i) Post informational posters on lead in drinking water in a public 
place or common area in each of the buildings served by the system; and
    (ii) Distribute informational pamphlets and/or brochures on lead in 
drinking water to each person served by the non-transient non-community 
water system. The State may allow the system to utilize electronic 
transmission in lieu of or combined with printed materials as long as it 
achieves at least the same coverage.
    (iii) For systems that are required to conduct monitoring annually 
or less frequently, the end of the monitoring period is September 30 of 
the calendar year in which the sampling occurs, or, if the State has 
established an alternate monitoring period, the last day of that period.
    (5) A non-transient non-community water system shall repeat the 
tasks contained in paragraph (b)(4) of this section at least once during 
each calendar year in which the system exceeds the lead action level. 
The State can allow activities in (b)(4) of this section to extend 
beyond the 60-day requirement if needed for implementation purposes on a 
case-by-case basis; however, this extension must be approved in writing 
by the State in advance of the 60-day deadline.
    (6) A water system may discontinue delivery of public education 
materials if the system has met the lead action level during the most 
recent six-month monitoring period conducted pursuant to Sec.  141.86. 
Such a system shall recommence public education in accordance with this 
section if it subsequently exceeds the lead action level during any 
monitoring period.
    (7) A community water system may apply to the State, in writing 
(unless the State has waived the requirement for prior State approval), 
to use only the text specified in paragraph (a)(1) of this section in 
lieu of the text in paragraphs (a)(1) and (a)(2) of this section and to 
perform the tasks listed in paragraphs (b)(4) and (b)(5) of this section 
in lieu of the tasks in paragraphs (b)(2) and (b)(3) of this section if:
    (i) The system is a facility, such as a prison or a hospital, where 
the population served is not capable of or is prevented from making 
improvements to plumbing or installing point of use treatment devices; 
and
    (ii) The system provides water as part of the cost of services 
provided and does not separately charge for water consumption.
    (8) A community water system serving 3,300 or fewer people may limit 
certain aspects of their public education programs as follows:
    (i) With respect to the requirements of paragraph (b)(2)(vi) of this 
section, a system serving 3,300 or fewer must implement at least one of 
the activities listed in that paragraph.
    (ii) With respect to the requirements of paragraph (b)(2)(ii) of 
this section, a system serving 3,300 or fewer people may limit the 
distribution of the public education materials required under that 
paragraph to facilities and organizations served by the system that are 
most likely to be visited regularly by pregnant women and children.

[[Page 559]]

    (iii) With respect to the requirements of paragraph (b)(2)(v) of 
this section, the State may waive this requirement for systems serving 
3,300 or fewer persons as long as system distributes notices to every 
household served by the system.
    (c) Supplemental monitoring and notification of results. A water 
system that fails to meet the lead action level on the basis of tap 
samples collected in accordance with Sec.  141.86 shall offer to sample 
the tap water of any customer who requests it. The system is not 
required to pay for collecting or analyzing the sample, nor is the 
system required to collect and analyze the sample itself.
    (d) Notification of results--(1) Reporting requirement. All water 
systems must provide a notice of the individual tap results from lead 
tap water monitoring carried out under the requirements of Sec.  141.86 
to the persons served by the water system at the specific sampling site 
from which the sample was taken (e.g., the occupants of the residence 
where the tap was tested).
    (2) Timing of notification. A water system must provide the consumer 
notice as soon as practical, but no later than 30 days after the system 
learns of the tap monitoring results.
    (3) Content. The consumer notice must include the results of lead 
tap water monitoring for the tap that was tested, an explanation of the 
health effects of lead, list steps consumers can take to reduce exposure 
to lead in drinking water and contact information for the water utility. 
The notice must also provide the maximum contaminant level goal and the 
action level for lead and the definitions for these two terms from Sec.  
141.153(c).
    (4) Delivery. The consumer notice must be provided to persons served 
at the tap that was tested, either by mail or by another method approved 
by the State. For example, upon approval by the State, a non-transient 
non-community water system could post the results on a bulletin board in 
the facility to allow users to review the information. The system must 
provide the notice to customers at sample taps tested, including 
consumers who do not receive water bills.

[72 FR 57815, Oct. 10, 2007]



Sec.  141.86  Monitoring requirements for lead and copper in tap water.

    (a) Sample site location. (1) By the applicable date for 
commencement of monitoring under paragraph (d)(1) of this section, each 
water system shall complete a materials evaluation of its distribution 
system in order to identify a pool of targeted sampling sites that meets 
the requirements of this section, and which is sufficiently large to 
ensure that the water system can collect the number of lead and copper 
tap samples required in paragraph (c) of this section. All sites from 
which first draw samples are collected shall be selected from this pool 
of targeted sampling sites. Sampling sites may not include faucets that 
have point-of-use or point-of-entry treatment devices designed to remove 
inorganic contaminants.
    (2) A water system shall use the information on lead, copper, and 
galvanized steel that it is required to collect under Sec.  141.42(d) of 
this part [special monitoring for corrosivity characteristics] when 
conducting a materials evaluation. When an evaluation of the information 
collected pursuant to Sec.  141.42(d) is insufficient to locate the 
requisite number of lead and copper sampling sites that meet the 
targeting criteria in paragraph (a) of this section, the water system 
shall review the sources of information listed below in order to 
identify a sufficient number of sampling sites. In addition, the system 
shall seek to collect such information where possible in the course of 
its normal operations (e.g., checking service line materials when 
reading water meters or performing maintenance activities):
    (i) All plumbing codes, permits, and records in the files of the 
building department(s) which indicate the plumbing materials that are 
installed within publicly and privately owned structures connected to 
the distribution system;
    (ii) All inspections and records of the distribution system that 
indicate the material composition of the service connections that 
connect a structure to the distribution system; and
    (iii) All existing water quality information, which includes the 
results of

[[Page 560]]

all prior analyses of the system or individual structures connected to 
the system, indicating locations that may be particularly susceptible to 
high lead or copper concentrations.
    (3) The sampling sites selected for a community water system's 
sampling pool (``tier l sampling sites'') shall consist of single family 
structures that:
    (i) Contain copper pipes with lead solder installed after 1982 or 
contain lead pipes; and/or
    (ii) Are served by a lead service line. When multiple-family 
residences comprise at least 20 percent of the structures served by a 
water system, the system may include these types of structures in its 
sampling pool.
    (4) Any community water system with insufficient tier 1 sampling 
sites shall complete its sampling pool with ``tier 2 sampling sites'', 
consisting of buildings, including multiple-family residences that:
    (i) Contain copper pipes with lead solder installed after 1982 or 
contain lead pipes; and/or
    (ii) Are served by a lead service line.
    (5) Any community water system with insufficient tier 1 and tier 2 
sampling sites shall complete its sampling pool with ``tier 3 sampling 
sites'', consisting of single family structures that contain copper 
pipes with lead solder installed before 1983. A community water system 
with insufficient tier 1, tier 2, and tier 3 sampling sites shall 
complete its sampling pool with representative sites throughout the 
distribution system. For the purpose of this paragraph, a representative 
site is a site in which the plumbing materials used at that site would 
be commonly found at other sites served by the water system.
    (6) The sampling sites selected for a non-transient noncommunity 
water system (``tier l sampling sites'') shall consist of buildings 
that:
    (i) Contain copper pipes with lead solder installed after 1982 or 
contain lead pipes; and/or
    (ii) Are served by a lead service line.
    (7) A non-transient non-community water system with insufficient 
tier 1 sites that meet the targeting criteria in paragraph (a)(6) of 
this section shall complete its sampling pool with sampling sites that 
contain copper pipes with lead solder installed before 1983. If 
additional sites are needed to complete the sampling pool, the non-
transient non-community water system shall use representative sites 
throughout the distribution system. For the purpose of this paragraph, a 
representative site is a site in which the plumbing materials used at 
that site would be commonly found at other sites served by the water 
system.
    (8) Any water system whose distribution system contains lead service 
lines shall draw 50 percent of the samples it collects during each 
monitoring period from sites that contain lead pipes, or copper pipes 
with lead solder, and 50 percent of the samples from sites served by a 
lead service line. A water system that cannot identify a sufficient 
number of sampling sites served by a lead service line shall collect 
first-draw samples from all of the sites identified as being served by 
such lines.
    (b) Sample collection methods. (1) All tap samples for lead and 
copper collected in accordance with this subpart, with the exception of 
lead service line samples collected under Sec.  141.84(c) and samples 
collected under paragraph (b)(5) of this section, shall be first-draw 
samples.
    (2) Each first-draw tap sample for lead and copper shall be one 
liter in volume and have stood motionless in the plumbing system of each 
sampling site for at least six hours. First-draw samples from 
residential housing shall be collected from the cold water kitchen tap 
or bathroom sink tap. First-draw samples from a nonresidential building 
shall be one liter in volume and shall be collected at an interior tap 
from which water is typically drawn for consumption. Non-first-draw 
samples collected in lieu of first-draw samples pursuant to paragraph 
(b)(5) of this section shall be one liter in volume and shall be 
collected at an interior tap from which water is typically drawn for 
consumption. First-draw samples may be collected by the system or the 
system may allow residents to collect first-draw samples after 
instructing the residents of the sampling procedures specified in this 
paragraph. To avoid problems of residents handling nitric acid, 
acidification of first-draw samples may be done up to 14

[[Page 561]]

days after the sample is collected. After acidification to resolubilize 
the metals, the sample must stand in the original container for the time 
specified in the approved EPA method before the sample can be analyzed. 
If a system allows residents to perform sampling, the system may not 
challenge, based on alleged errors in sample collection, the accuracy of 
sampling results.
    (3) Each service line sample shall be one liter in volume and have 
stood motionless in the lead service line for at least six hours. Lead 
service line samples shall be collected in one of the following three 
ways:
    (i) At the tap after flushing the volume of water between the tap 
and the lead service line. The volume of water shall be calculated based 
on the interior diameter and length of the pipe between the tap and the 
lead service line;
    (ii) Tapping directly into the lead service line; or
    (iii) If the sampling site is a building constructed as a single-
family residence, allowing the water to run until there is a significant 
change in temperature which would be indicative of water that has been 
standing in the lead service line.
    (4) A water system shall collect each first draw tap sample from the 
same sampling site from which it collected a previous sample. If, for 
any reason, the water system cannot gain entry to a sampling site in 
order to collect a follow-up tap sample, the system may collect the 
follow-up tap sample from another sampling site in its sampling pool as 
long as the new site meets the same targeting criteria, and is within 
reasonable proximity of the original site.
    (5) A non-transient non-community water system, or a community water 
system that meets the criteria of Sec.  141.85(b)(7), that does not have 
enough taps that can supply first-draw samples, as defined in Sec.  
141.2, may apply to the State in writing to substitute non-first-draw 
samples. Such systems must collect as many first-draw samples from 
appropriate taps as possible and identify sampling times and locations 
that would likely result in the longest standing time for the remaining 
sites. The State has the discretion to waive the requirement for prior 
State approval of non-first-draw sample sites selected by the system, 
either through State regulation or written notification to the system.
    (c) Number of samples. Water systems shall collect at least one 
sample during each monitoring period specified in paragraph (d) of this 
section from the number of sites listed in the first column (``standard 
monitoring'') of the table in this paragraph. A system conducting 
reduced monitoring under paragraph (d)(4) of this section shall collect 
at least one sample from the number of sites specified in the second 
column (``reduced monitoring'') of the table in this paragraph during 
each monitoring period specified in paragraph (d)(4) of this section. 
Such reduced monitoring sites shall be representative of the sites 
required for standard monitoring. A public water system that has fewer 
than five drinking water taps, that can be used for human consumption 
meeting the sample site criteria of paragraph (a) of this section to 
reach the required number of sample sites listed in paragraph (c) of 
this section, must collect at least one sample from each tap and then 
must collect additional samples from those taps on different days during 
the monitoring period to meet the required number of sites. 
Alternatively the State may allow these public water systems to collect 
a number of samples less than the number of sites specified in paragraph 
(c) of this section, provided that 100 percent of all taps that can be 
used for human consumption are sampled. The State must approve this 
reduction of the minimum number of samples in writing based on a request 
from the system or onsite verification by the State. States may specify 
sampling locations when a system is conducting reduced monitoring. The 
table is as follows:

------------------------------------------------------------------------
                                                 Number of    Number of
                                                   sites        sites
     System size (number of people served)       (standard     (reduced
                                                monitoring)  monitoring)
------------------------------------------------------------------------
100,000............................        100           50
10,001 to 100,000.............................         60           30
3,301 to 10,000...............................         40           20
501 to 3,300..................................         20           10
101 to 500....................................         10            5

[[Page 562]]

 
<=100.........................................          5            5
------------------------------------------------------------------------

    (d) Timing of monitoring--(1) Initial tap sampling. The first six-
month monitoring period for small, medium-size and large systems shall 
begin on the following dates:

------------------------------------------------------------------------
                                           First six-month monitoring
    System size (No. people served)             period begins on
------------------------------------------------------------------------
50,000.....................  January 1, 1992.
3,301 to 50,000.......................  July 1, 1992.
<=3,300...............................  July 1, 1993.
------------------------------------------------------------------------

    (i) All large systems shall monitor during two consecutive six-month 
periods.
    (ii) All small and medium-size systems shall monitor during each 
six-month monitoring period until:
    (A) The system exceeds the lead or copper action level and is 
therefore required to implement the corrosion control treatment 
requirements under Sec.  141.81, in which case the system shall continue 
monitoring in accordance with paragraph (d)(2) of this section, or
    (B) The system meets the lead and copper action levels during two 
consecutive six-month monitoring periods, in which case the system may 
reduce monitoring in accordance with paragraph (d)(4) of this section.
    (2) Monitoring after installation of corrosion control and source 
water treatment. (i) Any large system which installs optimal corrosion 
control treatment pursuant to Sec.  141.81(d)(4) shall monitor during 
two consecutive six-month monitoring periods by the date specified in 
Sec.  141.81(d)(5).
    (ii) Any small or medium-size system which installs optimal 
corrosion control treatment pursuant to Sec.  141.81(e)(5) shall monitor 
during two consecutive six-month monitoring periods by the date 
specified in Sec.  141.81(e)(6).
    (iii) Any system which installs source water treatment pursuant to 
Sec.  141.83(a)(3) shall monitor during two consecutive six-month 
monitoring periods by the date specified in Sec.  141.83(a)(4).
    (3) Monitoring after State specifies water quality parameter values 
for optimal corrosion control. After the State specifies the values for 
water quality control parameters under Sec.  141.82(f), the system shall 
monitor during each subsequent six-month monitoring period, with the 
first monitoring period to begin on the date the State specifies the 
optimal values under Sec.  141.82(f).
    (4) Reduced monitoring. (i) A small or medium-size water system that 
meets the lead and copper action levels during each of two consecutive 
six-month monitoring periods may reduce the number of samples in 
accordance with paragraph (c) of this section, and reduce the frequency 
of sampling to once per year. A small or medium water system collecting 
fewer than five samples as specified in paragraph (c) of this section, 
that meets the lead and copper action levels during each of two 
consecutive six-month monitoring periods may reduce the frequency of 
sampling to once per year. In no case can the system reduce the number 
of samples required below the minimum of one sample per available tap. 
This sampling shall begin during the calendar year immediately following 
the end of the second consecutive six-month monitoring period.
    (ii) Any water system that meets the lead action level and maintains 
the range of values for the water quality control parameters reflecting 
optimal corrosion control treatment specified by the State under Sec.  
141.82(f) during each of two consecutive six-month monitoring periods 
may reduce the frequency of monitoring to once per year and reduce the 
number of lead and copper samples in accordance with paragraph (c) of 
this section if it receives written approval from the State. This 
sampling shall begin during the calendar year immediately following the 
end of the second consecutive six-month monitoring period. The State 
shall review monitoring, treatment, and other relevant information 
submitted by the water system in accordance with Sec.  141.90, and shall 
notify the system in writing when it determines the system is eligible 
to commence reduced monitoring pursuant to this paragraph. The State 
shall review, and where appropriate, revise its determination when the 
system submits new monitoring or treatment data, or when

[[Page 563]]

other data relevant to the number and frequency of tap sampling becomes 
available.
    (iii) A small or medium-size water system that meets the lead and 
copper action levels during three consecutive years of monitoring may 
reduce the frequency of monitoring for lead and copper from annually to 
once every three years. Any water system that meets the lead action 
level and maintains the range of values for the water quality control 
parameters reflecting optimal corrosion control treatment specified by 
the State under Sec.  141.82(f) during three consecutive years of 
monitoring may reduce the frequency of monitoring from annually to once 
every three years if it receives written approval from the State. 
Samples collected once every three years shall be collected no later 
than every third calendar year. The State shall review monitoring, 
treatment, and other relevant information submitted by the water system 
in accordance with Sec.  141.90, and shall notify the system in writing 
when it determines the system is eligible to reduce the frequency of 
monitoring to once every three years. The State shall review, and where 
appropriate, revise its determination when the system submits new 
monitoring or treatment data, or when other data relevant to the number 
and frequency of tap sampling becomes available.
    (iv) A water system that reduces the number and frequency of 
sampling shall collect these samples from representative sites included 
in the pool of targeted sampling sites identified in paragraph (a) of 
this section. Systems sampling annually or less frequently shall conduct 
the lead and copper tap sampling during the months of June, July, 
August, or September unless the State has approved a different sampling 
period in accordance with paragraph (d)(4)(iv)(A) of this section.
    (A) The State, at its discretion, may approve a different period for 
conducting the lead and copper tap sampling for systems collecting a 
reduced number of samples. Such a period shall be no longer than four 
consecutive months and must represent a time of normal operation where 
the highest levels of lead are most likely to occur. For a non-transient 
non-community water system that does not operate during the months of 
June through September, and for which the period of normal operation 
where the highest levels of lead are most likely to occur is not known, 
the State shall designate a period that represents a time of normal 
operation for the system. This sampling shall begin during the period 
approved or designated by the State in the calendar year immediately 
following the end of the second consecutive six-month monitoring period 
for systems initiating annual monitoring and during the three-year 
period following the end of the third consecutive calendar year of 
annual monitoring for systems initiating triennial monitoring.
    (B) Systems monitoring annually, that have been collecting samples 
during the months of June through September and that receive State 
approval to alter their sample collection period under paragraph 
(d)(4)(iv)(A) of this section, must collect their next round of samples 
during a time period that ends no later than 21 months after the 
previous round of sampling. Systems monitoring triennially that have 
been collecting samples during the months of June through September, and 
receive State approval to alter the sampling collection period as per 
paragraph (d)(4)(iv)(A) of this section, must collect their next round 
of samples during a time period that ends no later than 45 months after 
the previous round of sampling. Subsequent rounds of sampling must be 
collected annually or triennially, as required by this section. Small 
systems with waivers, granted pursuant to paragraph (g) of this section, 
that have been collecting samples during the months of June through 
September and receive State approval to alter their sample collection 
period under paragraph (d)(4)(iv)(A) of this section must collect their 
next round of samples before the end of the 9-year period.
    (v) Any water system that demonstrates for two consecutive 6-month 
monitoring periods that the tap water lead level computed under Sec.  
141.80(c)(3) is less than or equal to 0.005 mg/L and the tap water 
copper level computed under Sec.  141.80(c)(3) is less than or equal

[[Page 564]]

to 0.65 mg/L may reduce the number of samples in accordance with 
paragraph (c) of this section and reduce the frequency of sampling to 
once every three calendar years.
    (vi)(A) A small or medium-size water system subject to reduced 
monitoring that exceeds the lead or copper action level shall resume 
sampling in accordance with paragraph (d)(3) of this section and collect 
the number of samples specified for standard monitoring under paragraph 
(c) of this section. Such a system shall also conduct water quality 
parameter monitoring in accordance with Sec.  141.87(b), (c) or (d) (as 
appropriate) during the monitoring period in which it exceeded the 
action level. Any such system may resume annual monitoring for lead and 
copper at the tap at the reduced number of sites specified in paragraph 
(c) of this section after it has completed two subsequent consecutive 
six-month rounds of monitoring that meet the criteria of paragraph 
(d)(4)(i) of this section and/or may resume triennial monitoring for 
lead and copper at the reduced number of sites after it demonstrates 
through subsequent rounds of monitoring that it meets the criteria of 
either paragraph (d)(4)(iii) or (d)(4)(v) of this section.
    (B) Any water system subject to the reduced monitoring frequency 
that fails to meet the lead action level during any four-month 
monitoring period or that fails to operate at or above the minimum value 
or within the range of values for the water quality parameters specified 
by the State under Sec.  141.82(f) for more than nine days in any six-
month period specified in Sec.  141.87(d) shall conduct tap water 
sampling for lead and copper at the frequency specified in paragraph 
(d)(3) of this section, collect the number of samples specified for 
standard monitoring under paragraph (c) of this section, and shall 
resume monitoring for water quality parameters within the distribution 
system in accordance with Sec.  141.87(d). This standard tap water 
sampling shall begin no later than the six-month period beginning 
January 1 of the calendar year following the lead action level 
exceedance or water quality parameter excursion. Such a system may 
resume reduced monitoring for lead and copper at the tap and for water 
quality parameters within the distribution system under the following 
conditions:
    (1) The system may resume annual monitoring for lead and copper at 
the tap at the reduced number of sites specified in paragraph (c) of 
this section after it has completed two subsequent six-month rounds of 
monitoring that meet the criteria of paragraph (d)(4)(ii) of this 
section and the system has received written approval from the State that 
it is appropriate to resume reduced monitoring on an annual frequency. 
This sampling shall begin during the calendar year immediately following 
the end of the second consecutive six-month monitoring period.
    (2) The system may resume triennial monitoring for lead and copper 
at the tap at the reduced number of sites after it demonstrates through 
subsequent rounds of monitoring that it meets the criteria of either 
paragraph (d)(4)(iii) or (d)(4)(v) of this section and the system has 
received written approval from the State that it is appropriate to 
resume triennial monitoring.
    (3) The system may reduce the number of water quality parameter tap 
water samples required in accordance with Sec.  141.87(e)(1) and the 
frequency with which it collects such samples in accordance with Sec.  
141.87(e)(2). Such a system may not resume triennial monitoring for 
water quality parameters at the tap until it demonstrates, in accordance 
with the requirements of Sec.  141.87(e)(2), that it has re-qualified 
for triennial monitoring.
    (vii) Any water system subject to a reduced monitoring frequency 
under paragraph (d)(4) of this section shall notify the State in writing 
in accordance with Sec.  141.90(a)(3) of any upcoming long-term change 
in treatment or addition of a new source as described in that section. 
The State must review and approve the addition of a new source or long-
term change in water treatment before it is implemented by the water 
system. The State may require the system to resume sampling in 
accordance with paragraph (d)(3) of this section and collect the number 
of samples specified for standard monitoring under paragraph (c) of this 
section or take other appropriate steps

[[Page 565]]

such as increased water quality parameter monitoring or re-evaluation of 
its corrosion control treatment given the potentially different water 
quality considerations.
    (e) Additional monitoring by systems. The results of any monitoring 
conducted in addition to the minimum requirements of this section shall 
be considered by the system and the State in making any determinations 
(i.e., calculating the 90th percentile lead or copper level) under this 
subpart.
    (f) Invalidation of lead or copper tap water samples. A sample 
invalidated under this paragraph does not count toward determining lead 
or copper 90th percentile levels under Sec.  141.80(c)(3) or toward 
meeting the minimum monitoring requirements of paragraph (c) of this 
section.
    (1) The State may invalidate a lead or copper tap water sample at 
least if one of the following conditions is met.
    (i) The laboratory establishes that improper sample analysis caused 
erroneous results.
    (ii) The State determines that the sample was taken from a site that 
did not meet the site selection criteria of this section.
    (iii) The sample container was damaged in transit.
    (iv) There is substantial reason to believe that the sample was 
subject to tampering.
    (2) The system must report the results of all samples to the State 
and all supporting documentation for samples the system believes should 
be invalidated.
    (3) To invalidate a sample under paragraph (f)(1) of this section, 
the decision and the rationale for the decision must be documented in 
writing. States may not invalidate a sample solely on the grounds that a 
follow-up sample result is higher or lower than that of the original 
sample.
    (4) The water system must collect replacement samples for any 
samples invalidated under this section if, after the invalidation of one 
or more samples, the system has too few samples to meet the minimum 
requirements of paragraph (c) of this section. Any such replacement 
samples must be taken as soon as possible, but no later than 20 days 
after the date the State invalidates the sample or by the end of the 
applicable monitoring period, whichever occurs later. Replacement 
samples taken after the end of the applicable monitoring period shall 
not also be used to meet the monitoring requirements of a subsequent 
monitoring period. The replacement samples shall be taken at the same 
locations as the invalidated samples or, if that is not possible, at 
locations other than those already used for sampling during the 
monitoring period.
    (g) Monitoring waivers for small systems. Any small system that 
meets the criteria of this paragraph may apply to the State to reduce 
the frequency of monitoring for lead and copper under this section to 
once every nine years (i.e., a ``full waiver'') if it meets all of the 
materials criteria specified in paragraph (g)(1) of this section and all 
of the monitoring criteria specified in paragraph (g)(2) of this 
section. If State regulations permit, any small system that meets the 
criteria in paragraphs (g)(1) and (2) of this section only for lead, or 
only for copper, may apply to the State for a waiver to reduce the 
frequency of tap water monitoring to once every nine years for that 
contaminant only (i.e., a ``partial waiver'').
    (1) Materials criteria. The system must demonstrate that its 
distribution system and service lines and all drinking water supply 
plumbing, including plumbing conveying drinking water within all 
residences and buildings connected to the system, are free of lead-
containing materials and/or copper-containing materials, as those terms 
are defined in this paragraph, as follows:
    (i) Lead. To qualify for a full waiver, or a waiver of the tap water 
monitoring requirements for lead (i.e., a ``lead waiver''), the water 
system must provide certification and supporting documentation to the 
State that the system is free of all lead-containing materials, as 
follows:
    (A) It contains no plastic pipes which contain lead plasticizers, or 
plastic service lines which contain lead plasticizers; and
    (B) It is free of lead service lines, lead pipes, lead soldered pipe 
joints, and leaded brass or bronze alloy fittings and fixtures, unless 
such fittings

[[Page 566]]

and fixtures meet the specifications of any standard established 
pursuant to 42 U.S.C. 300g-6(e) (SDWA section 1417(e)).
    (ii) Copper. To qualify for a full waiver, or a waiver of the tap 
water monitoring requirements for copper (i.e., a ``copper waiver''), 
the water system must provide certification and supporting documentation 
to the State that the system contains no copper pipes or copper service 
lines.
    (2) Monitoring criteria for waiver issuance. The system must have 
completed at least one 6-month round of standard tap water monitoring 
for lead and copper at sites approved by the State and from the number 
of sites required by paragraph (c) of this section and demonstrate that 
the 90th percentile levels for any and all rounds of monitoring 
conducted since the system became free of all lead-containing and/or 
copper-containing materials, as appropriate, meet the following 
criteria.
    (i) Lead levels. To qualify for a full waiver, or a lead waiver, the 
system must demonstrate that the 90th percentile lead level does not 
exceed 0.005 mg/L.
    (ii) Copper levels. To qualify for a full waiver, or a copper 
waiver, the system must demonstrate that the 90th percentile copper 
level does not exceed 0.65 mg/L.
    (3) State approval of waiver application. The State shall notify the 
system of its waiver determination, in writing, setting forth the basis 
of its decision and any condition of the waiver. As a condition of the 
waiver, the State may require the system to perform specific activities 
(e.g., limited monitoring, periodic outreach to customers to remind them 
to avoid installation of materials that might void the waiver) to avoid 
the risk of lead or copper concentration of concern in tap water. The 
small system must continue monitoring for lead and copper at the tap as 
required by paragraphs (d)(1) through (d)(4) of this section, as 
appropriate, until it receives written notification from the State that 
the waiver has been approved.
    (4) Monitoring frequency for systems with waivers. (i) A system with 
a full waiver must conduct tap water monitoring for lead and copper in 
accordance with paragraph (d)(4)(iv) of this section at the reduced 
number of sampling sites identified in paragraph (c) of this section at 
least once every nine years and provide the materials certification 
specified in paragraph (g)(1) of this section for both lead and copper 
to the State along with the monitoring results. Samples collected every 
nine years shall be collected no later than every ninth calendar year.
    (ii) A system with a partial waiver must conduct tap water 
monitoring for the waived contaminant in accordance with paragraph 
(d)(4)(iv) of this section at the reduced number of sampling sites 
specified in paragraph (c) of this section at least once every nine 
years and provide the materials certification specified in paragraph 
(g)(1) of this section pertaining to the waived contaminant along with 
the monitoring results. Such a system also must continue to monitor for 
the non-waived contaminant in accordance with requirements of paragraph 
(d)(1) through (d)(4) of this section, as appropriate.
    (iii) Any water system with a full or partial waiver shall notify 
the State in writing in accordance with Sec.  141.90(a)(3) of any 
upcoming long-term change in treatment or addition of a new source, as 
described in that section. The State must review and approve the 
addition of a new source or long-term change in water treatment before 
it is implemented by the water system. The State has the authority to 
require the system to add or modify waiver conditions (e.g., require 
recertification that the system is free of lead-containing and/or 
copper-containing materials, require additional round(s) of monitoring), 
if it deems such modifications are necessary to address treatment or 
source water changes at the system.
    (iv) If a system with a full or partial waiver becomes aware that it 
is no longer free of lead-containing or copper-containing materials, as 
appropriate, (e.g., as a result of new construction or repairs), the 
system shall notify the State in writing no later than 60 days after 
becoming aware of such a change.
    (5) Continued eligibility. If the system continues to satisfy the 
requirements of paragraph (g)(4) of this section, the waiver will be 
renewed automatically, unless any of the conditions listed in

[[Page 567]]

paragraph (g)(5)(i) through (g)(5)(iii) of this section occurs. A system 
whose waiver has been revoked may re-apply for a waiver at such time as 
it again meets the appropriate materials and monitoring criteria of 
paragraphs (g)(1) and (g)(2) of this section.
    (i) A system with a full waiver or a lead waiver no longer satisfies 
the materials criteria of paragraph (g)(1)(i) of this section or has a 
90th percentile lead level greater than 0.005 mg/L.
    (ii) A system with a full waiver or a copper waiver no longer 
satisfies the materials criteria of paragraph (g)(1)(ii) of this section 
or has a 90th percentile copper level greater than 0.65 mg/L.
    (iii) The State notifies the system, in writing, that the waiver has 
been revoked, setting forth the basis of its decision.
    (6) Requirements following waiver revocation. A system whose full or 
partial waiver has been revoked by the State is subject to the corrosion 
control treatment and lead and copper tap water monitoring requirements, 
as follows:
    (i) If the system exceeds the lead and/or copper action level, the 
system must implement corrosion control treatment in accordance with the 
deadlines specified in Sec.  141.81(e), and any other applicable 
requirements of this subpart.
    (ii) If the system meets both the lead and the copper action level, 
the system must monitor for lead and copper at the tap no less 
frequently than once every three years using the reduced number of 
sample sites specified in paragraph (c) of this section.
    (7) Pre-existing waivers. Small system waivers approved by the State 
in writing prior to April 11, 2000 shall remain in effect under the 
following conditions:
    (i) If the system has demonstrated that it is both free of lead-
containing and copper-containing materials, as required by paragraph 
(g)(1) of this section and that its 90th percentile lead levels and 90th 
percentile copper levels meet the criteria of paragraph (g)(2) of this 
section, the waiver remains in effect so long as the system continues to 
meet the waiver eligibility criteria of paragraph (g)(5) of this 
section. The first round of tap water monitoring conducted pursuant to 
paragraph (g)(4) of this section shall be completed no later than nine 
years after the last time the system has monitored for lead and copper 
at the tap.
    (ii) If the system has met the materials criteria of paragraph 
(g)(1) of this section but has not met the monitoring criteria of 
paragraph (g)(2) of this section, the system shall conduct a round of 
monitoring for lead and copper at the tap demonstrating that it meets 
the criteria of paragraph (g)(2) of this section no later than September 
30, 2000. Thereafter, the waiver shall remain in effect as long as the 
system meets the continued eligibility criteria of paragraph (g)(5) of 
this section. The first round of tap water monitoring conducted pursuant 
to paragraph (g)(4) of this section shall be completed no later than 
nine years after the round of monitoring conducted pursuant to paragraph 
(g)(2) of this section.

[56 FR 26548, June 7, 1991; 56 FR 32113, July 15, 1991; 57 FR 28788, 
June 29, 1992, as amended at 65 FR 2007, Jan. 12, 2000; 72 FR 57817, 
Oct. 10, 2007]



Sec.  141.87  Monitoring requirements for water quality parameters.

    All large water systems, and all small- and medium-size systems that 
exceed the lead or copper action level shall monitor water quality 
parameters in addition to lead and copper in accordance with this 
section. The requirements of this section are summarized in the table at 
the end of this section.
    (a) General requirements--(1) Sample collection methods. (i) Tap 
samples shall be representative of water quality throughout the 
distribution system taking into account the number of persons served, 
the different sources of water, the different treatment methods employed 
by the system, and seasonal variability. Tap sampling under this section 
is not required to be conducted at taps targeted for lead and copper 
sampling under Sec.  141.86(a). [Note: Systems may find it convenient to 
conduct tap sampling for water quality parameters at sites used for 
coliform sampling under 40 CFR 141.21.]
    (ii) Samples collected at the entry point(s) to the distribution 
system shall be from locations representative

[[Page 568]]

of each source after treatment. If a system draws water from more than 
one source and the sources are combined before distribution, the system 
must sample at an entry point to the distribution system during periods 
of normal operating conditions (i.e., when water is representative of 
all sources being used).
    (2) Number of samples. (i) Systems shall collect two tap samples for 
applicable water quality parameters during each monitoring period 
specified under paragraphs (b) through (e) of this section from the 
following number of sites.

------------------------------------------------------------------------
                                                           No. of sites
                                                             for water
             System size (No. people served)                  quality
                                                            parameters
------------------------------------------------------------------------
100,000......................................              25
10,001-100,000..........................................              10
3,301 to 10,000.........................................               3
501 to 3,300............................................               2
101 to 500..............................................               1
<=100...................................................               1
------------------------------------------------------------------------

    (ii) Except as provided in paragraph (c)(3) of this section, systems 
shall collect two samples for each applicable water quality parameter at 
each entry point to the distribution system during each monitoring 
period specified in paragraph (b) of this section. During each 
monitoring period specified in paragraphs (c)-(e) of this section, 
systems shall collect one sample for each applicable water quality 
parameter at each entry point to the distribution system.
    (b) Initial sampling All large water systems shall measure the 
applicable water quality parameters as specified below at taps and at 
each entry point to the distribution system during each six-month 
monitoring period specified in Sec.  141.86(d)(1). All small and medium-
size systems shall measure the applicable water quality parameters at 
the locations specified below during each six-month monitoring period 
specified in Sec.  141.86(d)(1) during which the system exceeds the lead 
or copper action level.
    (1) At taps:
    (i) pH;
    (ii) Alkalinity;
    (iii) Orthophosphate, when an inhibitor containing a phosphate 
compound is used;
    (iv) Silica, when an inhibitor containing a silicate compound is 
used;
    (v) Calcium;
    (vi) Conductivity; and
    (vii) Water temperature.
    (2) At each entry point to the distribution system: all of the 
applicable parameters listed in paragraph (b)(1) of this section.
    (c) Monitoring after installation of corrosion control. Any large 
system which installs optimal corrosion control treatment pursuant to 
Sec.  141.81(d)(4) shall measure the water quality parameters at the 
locations and frequencies specified below during each six-month 
monitoring period specified in Sec.  141.86(d)(2)(i). Any small or 
medium-size system which installs optimal corrosion control treatment 
shall conduct such monitoring during each six-month monitoring period 
specified in Sec.  141.86(d)(2)(ii) in which the system exceeds the lead 
or copper action level.
    (1) At taps, two samples for:
    (i) pH;
    (ii) Alkalinity;
    (iii) Orthophosphate, when an inhibitor containing a phosphate 
compound is used;
    (iv) Silica, when an inhibitor containing a silicate compound is 
used;
    (v) Calcium, when calcium carbonate stabilization is used as part of 
corrosion control.
    (2) Except as provided in paragraph (c)(3) of this section, at each 
entry point to the distribution system, at least one sample no less 
frequently than every two weeks (biweekly) for:
    (i) pH;
    (ii) When alkalinity is adjusted as part of optimal corrosion 
control, a reading of the dosage rate of the chemical used to adjust 
alkalinity, and the alkalinity concentration; and
    (iii) When a corrosion inhibitor is used as part of optimal 
corrosion control, a reading of the dosage rate of the inhibitor used, 
and the concentration of orthophosphate or silica (whichever is 
applicable).
    (3) Any ground water system can limit entry point sampling described 
in paragraph (c)(2) of this section to those entry points that are 
representative of water quality and treatment conditions throughout the 
system. If water from untreated ground water sources mixes with water 
from treated ground

[[Page 569]]

water sources, the system must monitor for water quality parameters both 
at representative entry points receiving treatment and representative 
entry points receiving no treatment. Prior to the start of any 
monitoring under this paragraph, the system shall provide to the State 
written information identifying the selected entry points and 
documentation, including information on seasonal variability, sufficient 
to demonstrate that the sites are representative of water quality and 
treatment conditions throughout the system.
    (d) Monitoring after State specifies water quality parameter values 
for optimal corrosion control. After the State specifies the values for 
applicable water quality control parameters reflecting optimal corrosion 
control treatment under Sec.  141.82(f), all large systems shall measure 
the applicable water quality parameters in accordance with paragraph (c) 
of this section and determine compliance with the requirements of Sec.  
141.82(g) every six months with the first six-month period to begin on 
either January 1 or July 1, whichever comes first, after the State 
specifies the optimal values under Sec.  141.82(f). Any small or medium-
size system shall conduct such monitoring during each six-month period 
specified in this paragraph in which the system exceeds the lead or 
copper action level. For any such small and medium-size system that is 
subject to a reduced monitoring frequency pursuant to Sec.  141.86(d)(4) 
at the time of the action level exceedance, the start of the applicable 
six-month monitoring period under this paragraph shall coincide with the 
start of the applicable monitoring period under Sec.  141.86(d)(4). 
Compliance with State-designated optimal water quality parameter values 
shall be determined as specified under Sec.  141.82(g).
    (e) Reduced monitoring. (1) Any water system that maintains the 
range of values for the water quality parameters reflecting optimal 
corrosion control treatment during each of two consecutive six-month 
monitoring periods under paragraph (d) of this section shall continue 
monitoring at the entry point(s) to the distribution system as specified 
in paragraph (c)(2) of this section. Such system may collect two tap 
samples for applicable water quality parameters from the following 
reduced number of sites during each six-month monitoring period.

------------------------------------------------------------------------
                                                          Reduced No. of
                                                             sites for
           System size (No. of people served)              water quality
                                                            parameters
------------------------------------------------------------------------
100,000......................................              10
10,001 to 100,000.......................................               7
3,301 to 10,000.........................................               3
501 to 3,300............................................               2
101 to 500..............................................               1
<=100...................................................               1
------------------------------------------------------------------------

    (2)(i) Any water system that maintains the range of values for the 
water quality parameters reflecting optimal corrosion control treatment 
specified by the State under Sec.  141.82(f) during three consecutive 
years of monitoring may reduce the frequency with which it collects the 
number of tap samples for applicable water quality parameters specified 
in this paragraph (e)(1) of this section from every six months to 
annually. This sampling begins during the calendar year immediately 
following the end of the monitoring period in which the third 
consecutive year of six-month monitoring occurs. Any water system that 
maintains the range of values for the water quality parameters 
reflecting optimal corrosion control treatment specified by the State 
under Sec.  141.82(f), during three consecutive years of annual 
monitoring under this paragraph may reduce the frequency with which it 
collects the number of tap samples for applicable water quality 
parameters specified in paragraph (e)(1) of this section from annually 
to every three years. This sampling begins no later than the third 
calendar year following the end of the monitoring period in which the 
third consecutive year of monitoring occurs.
    (ii) A water system may reduce the frequency with which it collects 
tap samples for applicable water quality parameters specified in 
paragraph (e)(1) of this section to every three years if it demonstrates 
during two consecutive monitoring periods that its tap water lead level 
at the 90th percentile is less than or equal to the PQL for lead 
specified in Sec.  141.89 (a)(1)(ii), that its tap water copper level at 
the 90th percentile is less than or equal to 0.65 mg/L for copper in 
Sec.  141.80(c)(2), and that it

[[Page 570]]

also has maintained the range of values for the water quality parameters 
reflecting optimal corrosion control treatment specified by the State 
under Sec.  141.82(f). Monitoring conducted every three years shall be 
done no later than every third calendar year.
    (3) A water system that conducts sampling annually shall collect 
these samples evenly throughout the year so as to reflect seasonal 
variability.
    (4) Any water system subject to the reduced monitoring frequency 
that fails to operate at or above the minimum value or within the range 
of values for the water quality parameters specified by the State in 
Sec.  141.82(f) for more than nine days in any six-month period 
specified in Sec.  141.82(g) shall resume distribution system tap water 
sampling in accordance with the number and frequency requirements in 
paragraph (d) of this section. Such a system may resume annual 
monitoring for water quality parameters at the tap at the reduced number 
of sites specified in paragraph (e)(1) of this section after it has 
completed two subsequent consecutive six-month rounds of monitoring that 
meet the criteria of that paragraph and/or may resume triennial 
monitoring for water quality parameters at the tap at the reduced number 
of sites after it demonstrates through subsequent rounds of monitoring 
that it meets the criteria of either paragraph (e)(2)(i) or (e)(2)(ii) 
of this section.
    (f) Additional monitoring by systems. The results of any monitoring 
conducted in addition to the minimum requirements of this section shall 
be considered by the system and the State in making any determinations 
(i.e., determining concentrations of water quality parameters) under 
this section or Sec.  141.82.

                       Summary of Monitoring Requirements for Water Quality Parameters \1\
----------------------------------------------------------------------------------------------------------------
          Monitoring period                 Parameters \2\              Location                Frequency
----------------------------------------------------------------------------------------------------------------
Initial monitoring...................  pH, alkalinity,          Taps and at entry        Every 6 months.
                                        orthophosphate or        point(s) to
                                        silica \3\, calcium,     distribution system.
                                        conductivity,
                                        temperature.
After installation of corrosion        pH, alkalinity,          Taps...................  Every 6 months.
 control.                               orthophosphate or
                                        silica \3\, calcium
                                        \4\.
                                       pH, alkalinity, dosage   Entry point(s) to        No less frequently than
                                        rate and concentration   distribution system      every two weeks.
                                        (if alkalinity           \6\.
                                        adjusted as part of
                                        corrosion control),
                                        inhibitor dosage rate
                                        and inhibitor residual
                                        \5\.
After State specifies parameter        pH, alkalinity,          Taps...................  Every 6 months.
 values for optimal corrosion control.  orthophosphate or
                                        silica \3\, calcium
                                        \4\.
                                       pH, alkalinity dosage    Entry point(s) to        No less frequently than
                                        rate and concentration   distribution system      every two weeks.
                                        (if alkalinity           \6\.
                                        adjusted as part of
                                        corrosion control),
                                        inhibitor dosage rate
                                        and inhibitor residual
                                        \5\.
Reduced monitoring...................  pH, alkalinity,          Taps...................  Every 6 months,
                                        orthophosphate or                                 annually \7\ or every
                                        silica \3\, calcium                               3 years \8\; reduced
                                        \4\.                                              number of sites.
                                       pH, alkalinity dosage    Entry point(s) to        No less frequently than
                                        rate and concentration   distribution system      every two weeks.
                                        (if alkalinity           \6\.
                                        adjusted as part of
                                        corrosion control),
                                        inhibitor dosage rate
                                        and inhibitor residual
                                        \5\.
----------------------------------------------------------------------------------------------------------------
\1\ Table is for illustrative purposes; consult the text of this section for precise regulatory requirements.
\2\ Small and medium-size systems have to monitor for water quality parameters only during monitoring periods in
  which the system exceeds the lead or copper action level.
\3\ Orthophosphate must be measured only when an inhibitor containing a phosphate compound is used. Silica must
  be measured only when an inhibitor containing silicate compound is used.
\4\ Calcium must be measured only when calcium carbonate stabilization is used as part of corrosion control.
\5\ Inhibitor dosage rates and inhibitor residual concentrations (orthophosphate or silica) must be measured
  only when an inhibitor is used.
\6\ Ground water systems may limit monitoring to representative locations throughout the system.
\7\ Water systems may reduce frequency of monitoring for water quality parameters at the tap from every six
  months to annually if they have maintained the range of values for water quality parameters reflecting optimal
  corrosion control during 3 consecutive years of monitoring.
\8\ Water systems may further reduce the frequency of monitoring for water quality parameters at the tap from
  annually to once every 3 years if they have maintained the range of values for water quality parameters
  reflecting optimal corrosion control during 3 consecutive years of annual monitoring. Water systems may
  accelerate to triennial monitoring for water quality parameters at the tap if they have maintained 90th
  percentile lead levels less than or equal to 0.005 mg/L, 90th percentile copper levels less than or equal to
  0.65 mg/L, and the range of water quality parameters designated by the State under Sec.   141.82(f) as
  representing optimal corrosion control during two consecutive six-month monitoring periods.


[[Page 571]]


[56 FR 26548, June 7, 1991; 57 FR 28788, June 29, 1992, as amended at 59 
FR 33862, June 30, 1994; 65 FR 2010, Jan. 12, 2000; 72 FR 57818, Oct. 
10, 2007]



Sec.  141.88  Monitoring requirements for lead and copper in source water.

    (a) Sample location, collection methods, and number of samples. (1) 
A water system that fails to meet the lead or copper action level on the 
basis of tap samples collected in accordance with Sec.  141.86 shall 
collect lead and copper source water samples in accordance with the 
following requirements regarding sample location, number of samples, and 
collection methods:
    (i) Groundwater systems shall take a minimum of one sample at every 
entry point to the distribution system which is representative of each 
well after treatment (hereafter called a sampling point). The system 
shall take one sample at the same sampling point unless conditions make 
another sampling point more representative of each source or treatment 
plant.
    (ii) Surface water systems shall take a minimum of one sample at 
every entry point to the distribution system after any application of 
treatment or in the distribution system at a point which is 
representative of each source after treatment (hereafter called a 
sampling point). The system shall take each sample at the same sampling 
point unless conditions make another sampling point more representative 
of each source or treatment plant.

    Note to paragraph (a)(1)(ii): For the purposes of this paragraph, 
surface water systems include systems with a combination of surface and 
ground sources.

    (iii) If a system draws water from more than one source and the 
sources are combined before distribution, the system must sample at an 
entry point to the distribution system during periods of normal 
operating conditions (i.e., when water is representative of all sources 
being used).
    (iv) The State may reduce the total number of samples which must be 
analyzed by allowing the use of compositing. Compositing of samples must 
be done by certified laboratory personnel. Composite samples from a 
maximum of five samples are allowed, provided that if the lead 
concentration in the composite sample is greater than or equal to 0.001 
mg/L or the copper concentration is greater than or equal to 0.160 mg/L, 
then either:
    (A) A follow-up sample shall be taken and analyzed within 14 days at 
each sampling point included in the composite; or
    (B) If duplicates of or sufficient quantities from the original 
samples from each sampling point used in the composite are available, 
the system may use these instead of resampling.
    (2) Where the results of sampling indicate an exceedance of maximum 
permissible source water levels established under Sec.  141.83(b)(4), 
the State may require that one additional sample be collected as soon as 
possible after the initial sample was taken (but not to exceed two 
weeks) at the same sampling point. If a State-required confirmation 
sample is taken for lead or copper, then the results of the initial and 
confirmation sample shall be averaged in determining compliance with the 
State-specified maximum permissible levels. Any sample value below the 
detection limit shall be considered to be zero. Any value above the 
detection limit but below the PQL shall either be considered as the 
measured value or be considered one-half the PQL.
    (b) Monitoring frequency after system exceeds tap water action 
level. Any system which exceeds the lead or copper action level at the 
tap shall collect one source water sample from each entry point to the 
distribution system no later than six months after the end of the 
monitoring period during which the lead or copper action level was 
exceeded. For monitoring periods that are annual or less frequent, the 
end of the monitoring period is September 30 of the calendar year in 
which the sampling occurs, or if the State has established an alternate 
monitoring period, the last day of that period.
    (c) Monitoring frequency after installation of source water 
treatment. Any system which installs source water treatment pursuant to 
Sec.  141.83(a)(3) shall collect an additional source water sample from 
each entry point to the distribution system during two consecutive

[[Page 572]]

six-month monitoring periods by the deadline specified in Sec.  
141.83(a)(4).
    (d) Monitoring frequency after State specifies maximum permissible 
source water levels or determines that source water treatment is not 
needed. (1) A system shall monitor at the frequency specified below in 
cases where the State specifies maximum permissible source water levels 
under Sec.  141.83(b)(4) or determines that the system is not required 
to install source water treatment under Sec.  141.83(b)(2).
    (i) A water system using only groundwater shall collect samples once 
during the three-year compliance period (as that term is defined in 
Sec.  141.2) in effect when the applicable State determination under 
paragraph (d)(1) of this section is made. Such systems shall collect 
samples once during each subsequent compliance period. Triennial samples 
shall be collected every third calendar year.
    (ii) A water system using surface water (or a combination of surface 
and ground water) shall collect samples once during each calendar year, 
the first annual monitoring period to begin during the year in which the 
applicable State determination is made under paragraph (d)(1) of this 
section.
    (2) A system is not required to conduct source water sampling for 
lead and/or copper if the system meets the action level for the specific 
contaminant in tap water samples during the entire source water sampling 
period applicable to the system under paragraph (d)(1) (i) or (ii) of 
this section.
    (e) Reduced monitoring frequency. (1) A water system using only 
ground water may reduce the monitoring frequency for lead and copper in 
source water to once during each nine-year compliance cycle (as that 
term is defined in Sec.  141.2) provided that the samples are collected 
no later than every ninth calendar year and if the system meets one of 
the following criteria:
    (i) The system demonstrates that finished drinking water entering 
the distribution system has been maintained below the maximum 
permissible lead and copper concentrations specified by the State in 
Sec.  141.83(b)(4) during at least three consecutive compliance periods 
under paragraph (d)(1) of this section; or
    (ii) The State has determined that source water treatment is not 
needed and the system demonstrates that, during at least three 
consecutive compliance periods in which sampling was conducted under 
paragraph (d)(1) of this section, the concentration of lead in source 
water was less than or equal to 0.005 mg/L and the concentration of 
copper in source water was less than or equal to 0.65 mg/L.
    (2) A water system using surface water (or a combination of surface 
water and ground water) may reduce the monitoring frequency in paragraph 
(d)(1) of this section to once during each nine-year compliance cycle 
(as that term is defined in Sec.  141.2) provided that the samples are 
collected no later than every ninth calendar year and if the system 
meets one of the following criteria:
    (i) The system demonstrates that finished drinking water entering 
the distribution system has been maintained below the maximum 
permissible lead and copper concentrations specified by the State in 
Sec.  141.83(b)(4) for at least three consecutive years; or
    (ii) The State has determined that source water treatment is not 
needed and the system demonstrates that, during at least three 
consecutive years, the concentration of lead in source water was less 
than or equal to 0.005 mg/L and the concentration of copper in source 
water was less than or equal to 0.65 mg/L.
    (3) A water system that uses a new source of water is not eligible 
for reduced monitoring for lead and/or copper until concentrations in 
samples collected from the new source during three consecutive 
monitoring periods are below the maximum permissible lead and copper 
concentrations specified by the State in Sec.  141.83(a)(5).

[56 FR 26548, June 7, 1991; 57 FR 28788 and 28789, June 29, 1992, as 
amended at 65 FR 2012, Jan. 12, 2000; 72 FR 57819, Oct. 10, 2007]



Sec.  141.89  Analytical methods.

    (a) Analyses for lead, copper, pH, conductivity, calcium, 
alkalinity, orthophosphate, silica, and temperature shall be conducted 
with the methods in Sec.  141.23(k)(1).

[[Page 573]]

    (1) Analyses for alkalinity, calcium, conductivity, orthophosphate, 
pH, silica, and temperature may be performed by any person acceptable to 
the State. Analyses under this section for lead and copper shall only be 
conducted by laboratories that have been certified by EPA or the State. 
To obtain certification to conduct analyses for lead and copper, 
laboratories must:
    (i) Analyze Performance Evaluation samples, which include lead and 
copper, provided by or acceptable to EPA or the State at least once a 
year by each method for which the laboratory desires certification; and
    (ii) Achieve quantitative acceptance limits as follows:
    (A) For lead: 30 percent of the actual amount 
in the Performance Evaluation sample when the actual amount is greater 
than or equal to 0.005 mg/L. The Practical Quantitation Level, or PQL 
for lead is 0.005 mg/L.
    (B) For Copper: 10 percent of the actual 
amount in the Performance Evaluation sample when the actual amount is 
greater than or equal to 0.050 mg/L. The Practical Quantitation Level, 
or PQL for copper is 0.050 mg/L.
    (iii) Achieve the method detection limit for lead of 0.001 mg/L 
according to the procedures in appendix B of part 136 of this title. 
This need only be accomplished if the laboratory will be processing 
source water composite samples under Sec.  141.88(a)(1)(iv).
    (iv) Be currently certified by EPA or the State to perform analyses 
to the specifications described in paragraph (a)(1) of this section.
    (2) States have the authority to allow the use of previously 
collected monitoring data for purposes of monitoring, if the data were 
collected and analyzed in accordance with the requirements of this 
subpart.
    (3) All lead and copper levels measured between the PQL and MDL must 
be either reported as measured or they can be reported as one-half the 
PQL specified for lead and copper in paragraph (a)(1)(ii) of this 
section. All levels below the lead and copper MDLs must be reported as 
zero.
    (4) All copper levels measured between the PQL and the MDL must be 
either reported as measured or they can be reported as one-half the PQL 
(0.025 mg/L). All levels below the copper MDL must be reported as zero.
    (b) [Reserved]

[56 FR 26548, June 7, 1991, as amended at 57 FR 28789, June 29, 1992; 57 
FR 31847, July 17, 1992; 59 FR 33863, June 30, 1994; 59 FR 62470, Dec. 
5, 1994; 64 FR 67466, Dec. 1, 1999; 65 FR 2012, Jan. 12, 2000; 72 FR 
57819, Oct. 10, 2007]



Sec.  141.90  Reporting requirements.

    All water systems shall report all of the following information to 
the State in accordance with this section.
    (a) Reporting requirements for tap water monitoring for lead and 
copper and for water quality parameter monitoring. (1) Except as 
provided in paragraph (a)(1)(viii) of this section, a water system shall 
report the information specified below for all tap water samples 
specified in Sec.  141.86 and for all water quality parameter samples 
specified in Sec.  141.87 within the first 10 days following the end of 
each applicable monitoring period specified in Sec.  141.86 and Sec.  
141.87 (i.e., every six months, annually, every 3 years, or every 9 
years). For monitoring periods with a duration less than six months, the 
end of the monitoring period is the last date samples can be collected 
during that period as specified in Sec. Sec.  141.86 and 141.87.
    (i) The results of all tap samples for lead and copper including the 
location of each site and the criteria under Sec.  141.86(a) (3), (4), 
(5), (6), and/or (7) under which the site was selected for the system's 
sampling pool;
    (ii) Documentation for each tap water lead or copper sample for 
which the water system requests invalidation pursuant to Sec.  
141.86(f)(2);
    (iii) [Reserved]
    (iv) The 90th percentile lead and copper concentrations measured 
from among all lead and copper tap water samples collected during each 
monitoring period (calculated in accordance with Sec.  141.80(c)(3)), 
unless the State calculates the system's 90th percentile lead and copper 
levels under paragraph (h) of this section;
    (v) With the exception of initial tap sampling conducted pursuant to 
Sec.  141.86(d)(1), the system shall designate any site which was not 
sampled during previous monitoring periods, and include an explanation 
of why sampling sites have changed;

[[Page 574]]

    (vi) The results of all tap samples for pH, and where applicable, 
alkalinity, calcium, conductivity, temperature, and orthophosphate or 
silica collected under Sec.  141.87 (b)-(e);
    (vii) The results of all samples collected at the entry point(s) to 
the distribution system for applicable water quality parameters under 
Sec.  141.87 (b)-(e);
    (viii) A water system shall report the results of all water quality 
parameter samples collected under Sec.  141.87(c) through (f) during 
each six-month monitoring period specified in Sec.  141.87(d) within the 
first 10 days following the end of the monitoring period unless the 
State has specified a more frequent reporting requirement.
    (2) For a non-transient non-community water system, or a community 
water system meeting the criteria of Sec.  141.85(b)(7), that does not 
have enough taps that can provide first-draw samples, the system must 
either:
    (i) Provide written documentation to the State identifying standing 
times and locations for enough non-first-draw samples to make up its 
sampling pool under Sec.  141.86(b)(5) by the start of the first 
applicable monitoring period under Sec.  141.86(d) that commences after 
April 11, 2000, unless the State has waived prior State approval of non-
first-draw sample sites selected by the system pursuant to Sec.  
141.86(b)(5); or
    (ii) If the State has waived prior approval of non-first-draw sample 
sites selected by the system, identify, in writing, each site that did 
not meet the six-hour minimum standing time and the length of standing 
time for that particular substitute sample collected pursuant to Sec.  
141.86(b)(5) and include this information with the lead and copper tap 
sample results required to be submitted pursuant to paragraph (a)(1)(i) 
of this section.
    (3) At a time specified by the State, or if no specific time is 
designated by the State, then as early as possible prior to the addition 
of a new source or any long-term change in water treatment, a water 
system deemed to have optimized corrosion control under Sec.  
141.81(b)(3), a water system subject to reduced monitoring pursuant to 
Sec.  141.86(d)(4), or a water system subject to a monitoring waiver 
pursuant to Sec.  141.86(g), shall submit written documentation to the 
State describing the change or addition. The State must review and 
approve the addition of a new source or long-term change in treatment 
before it is implemented by the water system. Examples of long-term 
treatment changes include the addition of a new treatment process or 
modification of an existing treatment process. Examples of modifications 
include switching secondary disinfectants, switching coagulants (e.g., 
alum to ferric chloride), and switching corrosion inhibitor products 
(e.g., orthophosphate to blended phosphate). Long-term changes can 
include dose changes to existing chemicals if the system is planning 
long-term changes to its finished water pH or residual inhibitor 
concentration. Long-term treatment changes would not include chemical 
dose fluctuations associated with daily raw water quality changes.
    (4) Any small system applying for a monitoring waiver under Sec.  
141.86(g), or subject to a waiver granted pursuant to Sec.  
141.86(g)(3), shall provide the following information to the State in 
writing by the specified deadline:
    (i) By the start of the first applicable monitoring period in Sec.  
141.86(d), any small water system applying for a monitoring waiver shall 
provide the documentation required to demonstrate that it meets the 
waiver criteria of Sec. Sec.  141.86(g)(1) and (2).
    (ii) No later than nine years after the monitoring previously 
conducted pursuant to Sec.  141.86(g)(2) or Sec.  141.86(g)(4)(i), each 
small system desiring to maintain its monitoring waiver shall provide 
the information required by Sec. Sec.  141.86(g)(4)(i) and (ii).
    (iii) No later than 60 days after it becomes aware that it is no 
longer free of lead-containing and/or copper-containing material, as 
appropriate, each small system with a monitoring waiver shall provide 
written notification to the State, setting forth the circumstances 
resulting in the lead-containing and/or copper-containing materials 
being introduced into the system and what corrective action, if any, the 
system plans to remove these materials.
    (iv) By October 10, 2000, any small system with a waiver granted 
prior to

[[Page 575]]

April 11, 2000 and that has not previously met the requirements of Sec.  
141.86(g)(2) shall provide the information required by that paragraph.
    (5) Each ground water system that limits water quality parameter 
monitoring to a subset of entry points under Sec.  141.87(c)(3) shall 
provide, by the commencement of such monitoring, written correspondence 
to the State that identifies the selected entry points and includes 
information sufficient to demonstrate that the sites are representative 
of water quality and treatment conditions throughout the system.
    (b) Source water monitoring reporting requirements. (1) A water 
system shall report the sampling results for all source water samples 
collected in accordance with Sec.  141.88 within the first 10 days 
following the end of each source water monitoring period (i.e., 
annually, per compliance period, per compliance cycle) specified in 
Sec.  141.88.
    (2) With the exception of the first round of source water sampling 
conducted pursuant to Sec.  141.88(b), the system shall specify any site 
which was not sampled during previous monitoring periods, and include an 
explanation of why the sampling point has changed.
    (c) Corrosion control treatment reporting requirements. By the 
applicable dates under Sec.  141.81, systems shall report the following 
information:
    (1) For systems demonstrating that they have already optimized 
corrosion control, information required in Sec.  141.81(b) (2) or (3).
    (2) For systems required to optimize corrosion control, their 
recommendation regarding optimal corrosion control treatment under Sec.  
141.82(a).
    (3) For systems required to evaluate the effectiveness of corrosion 
control treatments under Sec.  141.82(c), the information required by 
that paragraph.
    (4) For systems required to install optimal corrosion control 
designated by the State under Sec.  141.82(d), a letter certifying that 
the system has completed installing that treatment.
    (d) Source water treatment reporting requirements. By the applicable 
dates in Sec.  141.83, systems shall provide the following information 
to the State:
    (1) If required under Sec.  141.83(b)(1), their recommendation 
regarding source water treatment;
    (2) For systems required to install source water treatment under 
Sec.  141.83(b)(2), a letter certifying that the system has completed 
installing the treatment designated by the State within 24 months after 
the State designated the treatment.
    (e) Lead service line replacement reporting requirements. Systems 
shall report the following information to the State to demonstrate 
compliance with the requirements of Sec.  141.84:
    (1) No later than 12 months after the end of a monitoring period in 
which a system exceeds the lead action level in sampling referred to in 
Sec.  141.84(a), the system must submit written documentation to the 
State of the material evaluation conducted as required in Sec.  
141.86(a), identify the initial number of lead service lines in its 
distribution system at the time the system exceeds the lead action 
level, and provide the system's schedule for annually replacing at least 
7 percent of the initial number of lead service lines in its 
distribution system.
    (2) No later than 12 months after the end of a monitoring period in 
which a system exceeds the lead action level in sampling referred to in 
Sec.  141.84(a), and every 12 months thereafter, the system shall 
demonstrate to the State in writing that the system has either:
    (i) Replaced in the previous 12 months at least 7 percent of the 
initial lead service lines (or a greater number of lines specified by 
the State under Sec.  141.84(e)) in its distribution system, or
    (ii) Conducted sampling which demonstrates that the lead 
concentration in all service line samples from an individual line(s), 
taken pursuant to Sec.  141.86(b)(3), is less than or equal to 0.015 mg/
L. In such cases, the total number of lines replaced and/or which meet 
the criteria in Sec.  141.84(c) shall equal at least 7 percent of the 
initial number of lead lines identified under paragraph (e)(1) of this 
section (or the percentage specified by the State under Sec.  
141.84(e)).
    (3) The annual letter submitted to the State under paragraph (e)(2) 
of this section shall contain the following information:

[[Page 576]]

    (i) The number of lead service lines scheduled to be replaced during 
the previous year of the system's replacement schedule;
    (ii) The number and location of each lead service line replaced 
during the previous year of the system's replacement schedule;
    (iii) If measured, the water lead concentration and location of each 
lead service line sampled, the sampling method, and the date of 
sampling.
    (4) Any system which collects lead service line samples following 
partial lead service line replacement required by Sec.  141.84 shall 
report the results to the State within the first ten days of the month 
following the month in which the system receives the laboratory results, 
or as specified by the State. States, at their discretion may eliminate 
this requirement to report these monitoring results. Systems shall also 
report any additional information as specified by the State, and in a 
time and manner prescribed by the State, to verify that all partial lead 
service line replacement activities have taken place.
    (f) Public education program reporting requirements. (1) Any water 
system that is subject to the public education requirements in Sec.  
141.85 shall, within ten days after the end of each period in which the 
system is required to perform public education in accordance with Sec.  
141.85(b), send written documentation to the State that contains:
    (i) A demonstration that the system has delivered the public 
education materials that meet the content requirements in Sec.  
141.85(a) and the delivery requirements in Sec.  141.85(b); and
    (ii) A list of all the newspapers, radio stations, television 
stations, and facilities and organizations to which the system delivered 
public education materials during the period in which the system was 
required to perform public education tasks.
    (2) Unless required by the State, a system that previously has 
submitted the information required by paragraph (f)(1)(ii) of this 
section need not resubmit the information required by paragraph 
(f)(1)(ii) of this section, as long as there have been no changes in the 
distribution list and the system certifies that the public education 
materials were distributed to the same list submitted previously.
    (3) No later than 3 months following the end of the monitoring 
period, each system must mail a sample copy of the consumer notification 
of tap results to the State along with a certification that the 
notification has been distributed in a manner consistent with the 
requirements of Sec.  141.85(d).
    (g) Reporting of additional monitoring data. Any system which 
collects sampling data in addition to that required by this subpart 
shall report the results to the State within the first ten days 
following the end of the applicable monitoring period under Sec. Sec.  
141.86, 141.87 and 141.88 during which the samples are collected.
    (h) Reporting of 90th percentile lead and copper concentrations 
where the State calculates a system's 90th percentile concentrations. A 
water system is not required to report the 90th percentile lead and 
copper concentrations measured from among all lead and copper tap water 
samples collected during each monitoring period, as required by 
paragraph (a)(1)(iv) of this section if:
    (1) The State has previously notified the water system that it will 
calculate the water system's 90th percentile lead and copper 
concentrations, based on the lead and copper tap results submitted 
pursuant to paragraph (h)(2)(i) of this section, and has specified a 
date before the end of the applicable monitoring period by which the 
system must provide the results of lead and copper tap water samples;
    (2) The system has provided the following information to the State 
by the date specified in paragraph (h)(1) of this section:
    (i) The results of all tap samples for lead and copper including the 
location of each site and the criteria under Sec.  141.86(a)(3), (4), 
(5), (6), and/or (7) under which the site was selected for the system's 
sampling pool, pursuant to paragraph (a)(1)(i) of this section; and
    (ii) An identification of sampling sites utilized during the current 
monitoring period that were not sampled during previous monitoring 
periods, and an explanation why sampling sites have changed; and
    (3) The State has provided the results of the 90th percentile lead 
and copper

[[Page 577]]

calculations, in writing, to the water system before the end of the 
monitoring period.

[56 FR 26548, June 7, 1991; 57 FR 28789, June 29, 1992, as amended at 59 
FR 33864, June 30, 1994; 65 FR 2012, Jan. 12, 2000; 72 FR 57819, Oct. 
10, 2007]



Sec.  141.91  Recordkeeping requirements.

    Any system subject to the requirements of this subpart shall retain 
on its premises original records of all sampling data and analyses, 
reports, surveys, letters, evaluations, schedules, State determinations, 
and any other information required by Sec. Sec.  141.81 through 141.88. 
Each water system shall retain the records required by this section for 
no fewer than 12 years.



           Subpart J_Use of Non-Centralized Treatment Devices

    Source: 52 FR 25716, July 8, 1987, unless otherwise noted.



Sec.  141.100  Criteria and procedures for public water systems 
using point-of-entry devices.

    (a) Public water systems may use point-of-entry devices to comply 
with maximum contaminant levels only if they meet the requirements of 
this section.
    (b) It is the responsibility of the public water system to operate 
and maintain the point-of-entry treatment system.
    (c) The public water system must develop and obtain State approval 
for a monitoring plan before point-of-entry devices are installed for 
compliance. Under the plan approved by the State, point-of-entry devices 
must provide health protection equivalent to central water treatment. 
``Equivalent'' means that the water would meet all national primary 
drinking water regulations and would be of acceptable quality similar to 
water distributed by a well-operated central treatment plant. In 
addition to the VOCs, monitoring must include physical measurements and 
observations such as total flow treated and mechanical condition of the 
treatment equipment.
    (d) Effective technology must be properly applied under a plan 
approved by the State and the microbiological safety of the water must 
be maintained.
    (1) The State must require adequate certification of performance, 
field testing, and, if not included in the certification process, a 
rigorous engineering design review of the point-of-entry devices.
    (2) The design and application of the point-of-entry devices must 
consider the tendency for increase in heterotrophic bacteria 
concentrations in water treated with activated carbon. It may be 
necessary to use frequent backwashing, post-contactor disinfection, and 
Heterotrophic Plate Count monitoring to ensure that the microbiological 
safety of the water is not compromised.
    (e) All consumers shall be protected. Every building connected to 
the system must have a point-of-entry device installed, maintained, and 
adequately monitored. The State must be assured that every building is 
subject to treatment and monitoring, and that the rights and 
responsibilities of the public water system customer convey with title 
upon sale of property.

[52 FR 25716, July 8, 1987; 53 FR 25111, July 1, 1988]



Sec.  141.101  Use of bottled water.

    Public water systems shall not use bottled water to achieve 
compliance with an MCL. Bottled water may be used on a temporary basis 
to avoid unreasonable risk to health.

[63 FR 31934, June 11, 1998]



                     Subpart K_Treatment Techniques

    Source: 56 FR 3594, Jan. 30, 1991, unless otherwise noted.



Sec.  141.110  General requirements.

    The requirements of subpart K of this part constitute national 
primary drinking water regulations. These regulations establish 
treatment techniques in lieu of maximum contaminant levels for specified 
contaminants.



Sec.  141.111  Treatment techniques for acrylamide and epichlorohydrin.

    Each public water system must certify annually in writing to the 
State (using third party or manufacturer's

[[Page 578]]

certification) that when acrylamide and epichlorohydrin are used in 
drinking water systems, the combination (or product) of dose and monomer 
level does not exceed the levels specified as follows:

Acrylamide = 0.05% dosed at 1 ppm (or equivalent)
Epichlorohydrin = 0.01% dosed at 20 ppm (or equivalent)


Certifications can rely on manufacturers or third parties, as approved 
by the State.



     Subpart L_Disinfectant Residuals, Disinfection Byproducts, and 
                    Disinfection Byproduct Precursors



Sec.  141.130  General requirements.

    (a) The requirements of this subpart L constitute national primary 
drinking water regulations.
    (1) The regulations in this subpart establish criteria under which 
community water systems (CWSs) and nontransient, noncommunity water 
systems (NTNCWSs) which add a chemical disinfectant to the water in any 
part of the drinking water treatment process must modify their practices 
to meet MCLs and MRDLs in Sec. Sec.  141.64 and 141.65, respectively, 
and must meet the treatment technique requirements for disinfection 
byproduct precursors in Sec.  141.135.
    (2) The regulations in this subpart establish criteria under which 
transient NCWSs that use chlorine dioxide as a disinfectant or oxidant 
must modify their practices to meet the MRDL for chlorine dioxide in 
Sec.  141.65.
    (3) EPA has established MCLs for TTHM and HAA5 and treatment 
technique requirements for disinfection byproduct precursors to limit 
the levels of known and unknown disinfection byproducts which may have 
adverse health effects. These disinfection byproducts may include 
chloroform; bromodichloromethane; dibromochloromethane; bromoform; 
dichloroacetic acid; and trichloroacetic acid.
    (b) Compliance dates--(1) CWSs and NTNCWSs. Unless otherwise noted, 
systems must comply with the requirements of this subpart as follows. 
Subpart H systems serving 10,000 or more persons must comply with this 
subpart beginning January 1, 2002. Subpart H systems serving fewer than 
10,000 persons and systems using only ground water not under the direct 
influence of surface water must comply with this subpart beginning 
January 1, 2004.
    (2) Transient NCWSs. Subpart H systems serving 10,000 or more 
persons and using chlorine dioxide as a disinfectant or oxidant must 
comply with any requirements for chlorine dioxide in this subpart 
beginning January 1, 2002. Subpart H systems serving fewer than 10,000 
persons and using chlorine dioxide as a disinfectant or oxidant and 
systems using only ground water not under the direct influence of 
surface water and using chlorine dioxide as a disinfectant or oxidant 
must comply with any requirements for chlorine dioxide in this subpart 
beginning January 1, 2004.
    (c) Each CWS and NTNCWS regulated under paragraph (a) of this 
section must be operated by qualified personnel who meet the 
requirements specified by the State and are included in a State register 
of qualified operators.
    (d) Control of disinfectant residuals. Notwithstanding the MRDLs in 
Sec.  141.65, systems may increase residual disinfectant levels in the 
distribution system of chlorine or chloramines (but not chlorine 
dioxide) to a level and for a time necessary to protect public health, 
to address specific microbiological contamination problems caused by 
circumstances such as, but not limited to, distribution line breaks, 
storm run-off events, source water contamination events, or cross-
connection events.

[63 FR 69466, Dec. 16, 1998, as amended at 66 FR 3776, Jan. 16, 2001]



Sec.  141.131  Analytical requirements.

    (a) General. (1) Systems must use only the analytical methods 
specified in this section, or their equivalent as approved by EPA, to 
demonstrate compliance with the requirements of this subpart and with 
the requirements of subparts U and V of this part. These methods are 
effective for compliance monitoring February 16, 1999, unless a

[[Page 579]]

different effective date is specified in this section or by the State.
    (2) The following documents are incorporated by reference. The 
Director of the Federal Register approves this incorporation by 
reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies 
may be inspected at EPA's Drinking Water Docket, 1301 Constitution 
Avenue, NW., EPA West, Room B102, Washington, DC 20460, or at the 
National Archives and Records Administration (NARA). For information on 
the availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html. EPA Method 552.1 is in Methods for the Determination 
of Organic Compounds in Drinking Water-Supplement II, USEPA, August 
1992, EPA/600/R-92/129 (available through National Information Technical 
Service (NTIS), PB92-207703). EPA Methods 502.2, 524.2, 551.1, and 552.2 
are in Methods for the Determination of Organic Compounds in Drinking 
Water-Supplement III, USEPA, August 1995, EPA/600/R-95/131 (available 
through NTIS, PB95-261616). EPA Method 300.0 is in Methods for the 
Determination of Inorganic Substances in Environmental Samples, USEPA, 
August 1993, EPA/600/R-93/100 (available through NTIS, PB94-121811). EPA 
Methods 300.1 and 321.8 are in Methods for the Determination of Organic 
and Inorganic Compounds in Drinking Water, Volume 1, USEPA, August 2000, 
EPA 815-R-00-014 (available through NTIS, PB2000-106981). EPA Method 
317.0, Revision 2.0, ``Determination of Inorganic Oxyhalide Disinfection 
By-Products in Drinking Water Using Ion Chromatography with the Addition 
of a Postcolumn Reagent for Trace Bromate Analysis,'' USEPA, July 2001, 
EPA 815-B-01-001, EPA Method 326.0, Revision 1.0, ``Determination of 
Inorganic Oxyhalide Disinfection By-Products in Drinking Water Using Ion 
Chromatography Incorporating the Addition of a Suppressor Acidified 
Postcolumn Reagent for Trace Bromate Analysis,'' USEPA, June 2002, EPA 
815-R-03-007, EPA Method 327.0, Revision 1.1, ``Determination of 
Chlorine Dioxide and Chlorite Ion in Drinking Water Using Lissamine 
Green B and Horseradish Peroxidase with Detection by Visible 
Spectrophotometry,'' USEPA, May 2005, EPA 815-R-05-008 and EPA Method 
552.3, Revision 1.0, ``Determination of Haloacetic Acids and Dalapon in 
Drinking Water by Liquid-liquid Microextraction, Derivatization, and Gas 
Chromatography with Electron Capture Detection,'' USEPA, July 2003, EPA-
815-B-03-002 can be accessed and downloaded directly on-line at http://
www.epa.gov/safewater/methods/sourcalt.html. EPA Method 415.3, Revision 
1.1, ``Determination of Total Organic Carbon and Specific UV Absorbance 
at 254 nm in Source Water and Drinking Water,'' USEPA, February 2005, 
EPA/600/R-05/055 can be accessed and downloaded directly on-line at 
www.epa.gov/nerlcwww/ordmeth.htm. Standard Methods 4500-Cl D, 4500-Cl E, 
4500-Cl F, 4500-Cl G, 4500-Cl H, 500-Cl I, 4500-ClO2 D, 4500-
ClO2 E, 6251 B, and 5910 B shall be followed in accordance 
with Standard Methods for the Examination of Water and Wastewater, 19th 
or 20th Editions, American Public Health Association, 1995 and 1998, 
respectively. The cited methods published in either edition may be used. 
Standard Methods 5310 B, 5310 C, and 5310 D shall be followed in 
accordance with the Supplement to the 19th Edition of Standard Methods 
for the Examination of Water and Wastewater, or the Standard Methods for 
the Examination of Water and Wastewater, 20th Edition, American Public 
Health Association, 1996 and 1998, respectively. The cited methods 
published in either edition may be used. Copies may be obtained from the 
American Public Health Association, 1015 Fifteenth Street, NW., 
Washington, DC 20005. Standard Methods 4500-Cl D-00, 4500-Cl E-00, 4500-
Cl F-00, 4500-Cl G-00, 4500-Cl H-00, 4500-Cl I-00, 4500-ClO2 
E-00, 6251 B-94, 5310 B-00, 5310 C-00, 5310 D-00 and 5910 B-00 are 
available at http://www.standardmethods.org or at EPA's Water Docket. 
The year in which each method was approved by the Standard Methods 
Committee is designated by the last two digits in the method number. The 
methods listed are the only Online versions that are IBR-approved. ASTM 
Methods D 1253-86 and D 1253-86 (Reapproved 1996) shall be followed in 
accordance with the Annual Book of

[[Page 580]]

ASTM Standards, Volume 11.01, American Society for Testing and Materials 
International, 1996 or any ASTM edition containing the IBR-approved 
version of the method may be used. ASTM Method D1253-03 shall be 
followed in accordance with the Annual Book of ASTM Standards, Volume 
11.01, American Society for Testing and Materials International, 2004 or 
any ASTM edition containing the IBR-approved version of the method may 
be used. ASTM Method D 6581-00 shall be followed in accordance with the 
Annual Book of ASTM Standards, Volume 11.01, American Society for 
Testing and Materials International, 2001 or any ASTM edition containing 
the IBR-approved version of the method may be used; copies may be 
obtained from the American Society for Testing and Materials 
International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959.
    (b) Disinfection byproducts. (1) Systems must measure disinfection 
byproducts by the methods (as modified by the footnotes) listed in the 
following table or one of the alternative methods listed in appendix A 
to subpart C of this part:

                        Approved Methods for Disinfection Byproduct Compliance Monitoring
----------------------------------------------------------------------------------------------------------------
                                                     Standard method
Contaminant and methodology \1\      EPA method            \2\           SM online \9\        ASTM method \3\
----------------------------------------------------------------------------------------------------------------
TTHM
    P&T/GC/ElCD & PID..........  502.2 \4\........
    P&T/GC/MS..................  524.2............
    LLE/GC/ECD.................  551.1............
HAA5
    LLE (diazomethane)/GC/ECD..  .................  6251 B \5\.......  6251 B-94........
    SPE (acidic methanol)/GC/    552.1 \5\........
     ECD.
    LLE (acidic methanol)/GC/    552.2, 552.3.....
     ECD.
Bromate
    Ion chromatography.........  300.1............  .................  .................  D 6581-00
    Ion chromatography & post    317.0 Rev 2.0
     column reaction.             \6\, 326.0 \6\.
    IC/ICP-MS..................  321.8 \6 7\......
Chlorite
    Amperometric titration.....  .................  4500-ClO2 E \8\..  4500-ClO2 E-00
                                                                        \8\.
    Spectrophotometry..........  327.0 Rev 1.1 \8\
    Ion chromatography.........  300.0, 300.1,      .................  .................  D 6581-00
                                  317.0 Rev 2.0,
                                  326.0.
----------------------------------------------------------------------------------------------------------------
\1\ P&T = purge and trap; GC = gas chromatography; ElCD = electrolytic conductivity detector; PID =
  photoionization detector; MS = mass spectrometer; LLE = liquid/liquid extraction; ECD = electron capture
  detector; SPE = solid phase extraction; IC = ion chromatography; ICP-MS = inductively coupled plasma/mass
  spectrometer.
\2\ 19th and 20th editions of Standard Methods for the Examination of Water and Wastewater, 1995 and 1998,
  respectively, American Public Health Association; either of these editions may be used.
\3\ Annual Book of ASTM Standards, 2001 or any year containing the cited version of the method, Vol 11.01.
\4\ If TTHMs are the only analytes being measured in the sample, then a PID is not required.
\5\ The samples must be extracted within 14 days of sample collection.
\6\ Ion chromatography & post column reaction or IC/ICP-MS must be used for monitoring of bromate for purposes
  of demonstrating eligibility of reduced monitoring, as prescribed in Sec.   141.132(b)(3)(ii).
\7\ Samples must be preserved at the time of sampling with 50 mg ethylenediamine (EDA)/L of sample and must be
  analyzed within 28 days.
\8\ Amperometric titration or spectrophotometry may be used for routine daily monitoring of chlorite at the
  entrance to the distribution system, as prescribed in Sec.   141.132(b)(2)(i)(A). Ion chromatography must be
  used for routine monthly monitoring of chlorite and additional monitoring of chlorite in the distribution
  system, as prescribed in Sec.   141.132(b)(2)(i)(B) and (b)(2)(ii).
\9\ The Standard Methods Online version that is approved is indicated by the last two digits in the method
  number which is the year of approval by the Standard Method Committee. Standard Methods Online are available
  at http://www.standardmethods.org.

    (2) Analyses under this section for disinfection byproducts must be 
conducted by laboratories that have received certification by EPA or the 
State, except as specified under paragraph (b)(3) of this section. To 
receive certification to conduct analyses for the DBP contaminants in 
Sec. Sec.  141.64, 141.135, and subparts U and V of this part, the 
laboratory must:
    (i) Analyze Performance Evaluation (PE) samples that are acceptable 
to EPA or the State at least once during each consecutive 12 month 
period by each method for which the laboratory desires certification.
    (ii) Until March 31, 2007, in these analyses of PE samples, the 
laboratory must achieve quantitative results

[[Page 581]]

within the acceptance limit on a minimum of 80% of the analytes included 
in each PE sample. The acceptance limit is defined as the 95% confidence 
interval calculated around the mean of the PE study between a maximum 
and minimum acceptance limit of 50% and 15% of the study mean.
    (iii) Beginning April 1, 2007, the laboratory must achieve 
quantitative results on the PE sample analyses that are within the 
following acceptance limits:

------------------------------------------------------------------------
                                      Acceptance
                                        limits
                DBP                   (percent of         Comments
                                      true value)
------------------------------------------------------------------------
TTHM
    Chloroform....................  20   all 4 individual
                                                     THM acceptance
                                                     limits in order to
                                                     successfully pass a
                                                     PE sample for TTHM
    Bromodichloromethane..........  20
    Dibromochloromethane..........  20
    Bromoform.....................  20
HAA5
    Monochloroacetic Acid.........  40   the acceptance
                                                     limits for 4 out of
                                                     5 of the HAA5
                                                     compounds in order
                                                     to successfully
                                                     pass a PE sample
                                                     for HAA5
    Dichloroacetic Acid...........  40
    Trichloroacetic Acid..........  40
    Monobromoacetic Acid..........  40
    Dibromoacetic Acid............  40
Chlorite..........................  30
Bromate...........................  30
------------------------------------------------------------------------

    (iv) Beginning April 1, 2007, report quantitative data for 
concentrations at least as low as the ones listed in the following table 
for all DBP samples analyzed for compliance with Sec. Sec.  141.64, 
141.135, and subparts U and V of this part:

------------------------------------------------------------------------
                                       Minimum
                                      reporting
                DBP                   level (mg/         Comments
                                        L) \1\
------------------------------------------------------------------------
TTHM \2\
    Chloroform.....................       0.0010
    Bromodichloromethane...........       0.0010
    Dibromochloromethane...........       0.0010
    Bromoform......................       0.0010
HAA5 \2\
    Monochloroacetic Acid..........       0.0020
    Dichloroacetic Acid............       0.0010
    Trichloroacetic Acid...........       0.0010
    Monobromoacetic Acid...........       0.0010
    Dibromoacetic Acid.............       0.0010
Chlorite...........................        0.020  Applicable to
                                                   monitoring as
                                                   prescribed in Sec.
                                                   141.132(b)(2)(1)(B)
                                                   and (b)(2)(ii).
Bromate............................    0.0050 or  Laboratories that use
                                          0.0010   EPA Methods 317.0
                                                   Revision 2.0, 326.0
                                                   or 321.8 must meet a
                                                   0.0010 mg/L MRL for
                                                   bromate.
------------------------------------------------------------------------
\1\ The calibration curve must encompass the regulatory minimum
  reporting level (MRL) concentration. Data may be reported for
  concentrations lower than the regulatory MRL as long as the precision
  and accuracy criteria are met by analyzing an MRL check standard at
  the lowest reporting limit chosen by the laboratory. The laboratory
  must verify the accuracy of the calibration curve at the MRL
  concentration by analyzing an MRL check standard with a concentration
  less than or equal to 110% of the MRL with each batch of samples. The
  measured concentration for the MRL check standard must be 50% of the expected value, if any field sample in the
  batch has a concentration less than 5 times the regulatory MRL. Method
  requirements to analyze higher concentration check standards and meet
  tighter acceptance criteria for them must be met in addition to the
  MRL check standard requirement.
\2\ When adding the individual trihalomethane or haloacetic acid
  concentrations to calculate the TTHM or HAA5 concentrations,
  respectively, a zero is used for any analytical result that is less
  than the MRL concentration for that DBP, unless otherwise specified by
  the State.

    (3) A party approved by EPA or the State must measure daily chlorite 
samples at the entrance to the distribution system.
    (c) Disinfectant residuals. (1) Systems must measure residual 
disinfectant concentration for free chlorine, combined chlorine 
(chloramines), and chlorine dioxide by the methods listed in the 
following table or one of the alternative methods listed in appendix A 
to subpart C of this part:

[[Page 582]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                         Residual measured \1\
           Methodology             SM (19th or 20th    SM Online \2\       ASTM method         EPA method    -------------------------------------------
                                         ed)                                                                  Free Cl2  Combined Cl2  Total Cl2    ClO2
--------------------------------------------------------------------------------------------------------------------------------------------------------
Amperometric Titration..........  4500-Cl D          4500-Cl D-00       D 1253-86 (96),    .................  X         X             X          .......
                                                                         03
Low Level Amperometric Titration  4500-Cl E          4500-Cl E-00       .................  .................  ........  ............  X
DPD Ferrous Titrimetric.........  4500-Cl F          4500-Cl F-00       .................  .................  X         X             X          .......
DPD Colorimetric................  4500-Cl G          4500-Cl G-00       .................  .................  X         X             X          .......
Syringaldazine (FACTS)..........  4500-Cl H          4500-Cl H-00       .................  .................  X         ............  .........  .......
Iodometric Electrode............  4500-Cl I          4500-Cl I-00       .................  .................  ........  ............  X          .......
DPD.............................  4500-ClO2 D        .................  .................  .................  ........  ............  .........  X
Amperometric Method II..........  4500-ClO2 E        4500-ClO2 E-00     .................  .................  ........  ............  .........  X
Lissamine Green                   .................  .................  .................  327.0 Rev 1.1      ........  ............  .........  X
 Spectrophotometric.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ X indicates method is approved for measuring specified disinfectant residual. Free chlorine or total chlorine may be measured for demonstrating
  compliance with the chlorine MRDL and combined chlorine, or total chlorine may be measured for demonstrating compliance with the chloramine MRDL.
\2\ The Standard Methods Online version that is approved is indicated by the last two digits in the method number which is the year of approval by the
  Standard Method Committee. Standard Methods Online are available at http://www.standardmethods.org.

    (2) If approved by the State, systems may also measure residual 
disinfectant concentrations for chlorine, chloramines, and chlorine 
dioxide by using DPD colorimetric test kits.
    (3) A party approved by EPA or the State must measure residual 
disinfectant concentration.
    (d) Additional analytical methods. Systems required to analyze 
parameters not included in paragraphs (b) and (c) of this section must 
use the following methods or one of the alternative methods listed in 
appendix A to subpart C of this part. A party approved by EPA or the 
State must measure these parameters.
    (1) Alkalinity. All methods allowed in Sec.  141.89(a) for measuring 
alkalinity.
    (2) Bromide. EPA Methods 300.0, 300.1, 317.0 Revision 2.0, 326.0, or 
ASTM D 6581-00.
    (3) Total Organic Carbon (TOC). Standard Method 5310 B or 5310 B-00 
(High-Temperature Combustion Method) or Standard Method 5310 C or 5310 
C-00 (Persulfate-Ultraviolet or Heated-Persulfate Oxidation Method) or 
Standard Method 5310 D or 5310 D-00 (Wet-Oxidation Method) or EPA Method 
415.3 Revision 1.1. Inorganic carbon must be removed from the samples 
prior to analysis. TOC samples may not be filtered prior to analysis. 
TOC samples must be acidified at the time of sample collection to 
achieve pH less than or equal to 2 with minimal addition of the acid 
specified in the method or by the instrument manufacturer. Acidified TOC 
samples must be analyzed within 28 days.
    (4) Specific Ultraviolet Absorbance (SUVA). SUVA is equal to the UV 
absorption at 254nm (UV254) (measured in m-\1\ divided by the 
dissolved organic carbon (DOC) concentration (measured as mg/L). In 
order to determine SUVA, it is necessary to separately measure 
UV254 and DOC. When determining SUVA, systems must use the 
methods stipulated in paragraph (d)(4)(i) of this section to measure DOC 
and the method stipulated in paragraph (d)(4)(ii) of this section to 
measure UV254. SUVA must be determined on water prior to the 
addition of disinfectants/oxidants by the system. DOC and 
UV254 samples used to determine a SUVA value must be taken at 
the same time and at the same location.
    (i) Dissolved Organic Carbon (DOC). Standard Method 5310 B or 5310 
B-00 (High-Temperature Combustion Method) or Standard Method 5310 C or 
5310 C-00 (Persulfate-Ultraviolet or Heated-Persulfate Oxidation Method) 
or Standard Method 5310 D or 5310 D-00 (Wet-Oxidation Method) or EPA 
Method 415.3 Revision 1.1. DOC samples must be filtered through the 0.45 
[mu]m pore-diameter filter as soon as practical after sampling, not to 
exceed 48 hours. After filtration, DOC samples must be acidified to 
achieve pH less than or equal to 2 with minimal addition of the acid 
specified in the method or by the instrument manufacturer. Acidified DOC 
samples must be analyzed within 28

[[Page 583]]

days of sample collection. Inorganic carbon must be removed from the 
samples prior to analysis. Water passed through the filter prior to 
filtration of the sample must serve as the filtered blank. This filtered 
blank must be analyzed using procedures identical to those used for 
analysis of the samples and must meet the following criteria: DOC <0.5 
mg/L.
    (ii) Ultraviolet Absorption at 254 nm (UV254). Standard 
Method 5910 B or 5910 B-00 (Ultraviolet Absorption Method) or EPA Method 
415.3 Revision 1.1. UV absorption must be measured at 253.7 nm (may be 
rounded off to 254 nm). Prior to analysis, UV254 samples must 
be filtered through a 0.45 [mu]m pore-diameter filter. The pH of 
UV254 samples may not be adjusted. Samples must be analyzed 
as soon as practical after sampling, not to exceed 48 hours.
    (5) pH. All methods allowed in Sec.  141.23(k)(1) for measuring pH.
    (6) Magnesium. All methods allowed in Sec.  141.23(k)(1) for 
measuring magnesium.

[63 FR 69466, Dec. 16, 1998, as amended at 66 FR 3776, Jan. 16, 2001; 71 
FR 479, Jan. 4, 2006; 71 FR 37168, June 29, 2006; 74 FR 30958, June 29, 
2009]



Sec.  141.132  Monitoring requirements.

    (a) General requirements. (1) Systems must take all samples during 
normal operating conditions.
    (2) Systems may consider multiple wells drawing water from a single 
aquifer as one treatment plant for determining the minimum number of 
TTHM and HAA5 samples required, with State approval in accordance with 
criteria developed under Sec.  142.16(h)(5) of this chapter.
    (3) Failure to monitor in accordance with the monitoring plan 
required under paragraph (f) of this section is a monitoring violation.
    (4) Failure to monitor will be treated as a violation for the entire 
period covered by the annual average where compliance is based on a 
running annual average of monthly or quarterly samples or averages and 
the system's failure to monitor makes it impossible to determine 
compliance with MCLs or MRDLs.
    (5) Systems may use only data collected under the provisions of this 
subpart to qualify for reduced monitoring.
    (b) Monitoring requirements for disinfection byproducts--(1) TTHMs 
and HAA5--(i) Routine monitoring. Systems must monitor at the frequency 
indicated in the following table:

                                 Routine Monitoring Frequency for TTHM and HAA5
----------------------------------------------------------------------------------------------------------------
                                               Minimum monitoring         Sample location in the distribution
             Type of system                        frequency                             system
----------------------------------------------------------------------------------------------------------------
Subpart H system serving at least 10,000  Four water samples per       At least 25 percent of all samples
 persons.                                  quarter per treatment        collected each quarter at locations
                                           plant.                       representing maximum residence time.
                                                                        Remaining samples taken at locations
                                                                        representative of at least average
                                                                        residence time in the distribution
                                                                        system and representing the entire
                                                                        distribution system, taking into account
                                                                        number of persons served, different
                                                                        sources of water, and different
                                                                        treatment methods. \1\
Subpart H system serving from 500 to      One water sample per         Locations representing maximum residence
 9,999 persons.                            quarter per treatment        time. \1\
                                           plant.
Subpart H system serving fewer than 500   One sample per year per      Locations representing maximum residence
 persons.                                  treatment plant during       time. \1\ If the sample (or average of
                                           month of warmest water       annual samples, if more than one sample
                                           temperature.                 is taken) exceeds the MCL, the system
                                                                        must increase monitoring to one sample
                                                                        per treatment plant per quarter, taken
                                                                        at a point reflecting the maximum
                                                                        residence time in the distribution
                                                                        system, until the system meets criteria
                                                                        in paragraph (b)(1)(iv) of this section.
System using only ground water not under  One water sample per         Locations representing maximum residence
 direct influence of surface water using   quarter per treatment        time. \1\
 chemical disinfectant and serving at      plant \2\.
 least 10,000 persons.

[[Page 584]]

 
System using only ground water not under  One sample per year per      Locations representing maximum residence
 direct influence of surface water using   treatment plant \2\ during   time. \1\ If the sample (or average of
 chemical disinfectant and serving fewer   month of warmest water       annual samples, if more than one sample
 than 10,000 persons.                      temperature.                 is taken) exceeds the MCL, the system
                                                                        must increase monitoring to one sample
                                                                        per treatment plant per quarter, taken
                                                                        at a point reflecting the maximum
                                                                        residence time in the distribution
                                                                        system, until the system meets criteria
                                                                        in paragraph (b)(1)(iv) of this section.
 
----------------------------------------------------------------------------------------------------------------
\1\ If a system elects to sample more frequently than the minimum required, at least 25 percent of all samples
  collected each quarter (including those taken in excess of the required frequency) must be taken at locations
  that represent the maximum residence time of the water in the distribution system. The remaining samples must
  be taken at locations representative of at least average residence time in the distribution system.
\2\ Multiple wells drawing water from a single aquifer may be considered one treatment plant for determining the
  minimum number of samples required, with State approval in accordance with criteria developed under Sec.
  142.16(h)(5) of this chapter.

    (ii) Systems may reduce monitoring, except as otherwise provided, in 
accordance with the following table:

                                 Reduced Monitoring Frequency for TTHM and HAA5
----------------------------------------------------------------------------------------------------------------
                                           You may reduce monitoring
                                            if you have monitored at
           If you are a . . .             least one year and your . .                To this level
                                                       .
----------------------------------------------------------------------------------------------------------------
Subpart H system serving at least 10,000  TTHM annual average <=0.040  One sample per treatment plant per
 persons which has a source water annual   mg/L and HAA5 annual         quarter at distribution system location
 average TOC level, before any             average <=0.030 mg/L.        reflecting maximum residence time.
 treatment, <=4.0 mg/L.
Subpart H system serving from 500 to      TTHM annual average <=0.040  One sample per treatment plant per year
 9,999 persons which has a source water    mg/L and HAA5 annual         at distribution system location
 annual average TOC level, before any      average <=0.030 mg/L.        reflecting maximum residence time during
 treatment, <=4.0 mg/L.                                                 month of warmest water temperature.
                                                                        NOTE: Any Subpart H system serving fewer
                                                                        than 500 persons may not reduce its
                                                                        monitoring to less than one sample per
                                                                        treatment plant per year.
System using only ground water not under  TTHM annual average <=0.040  One sample per treatment plant per year
 direct influence of surface water using   mg/L and HAA5 annual         at distribution system location
 chemical disinfectant and serving at      average <=0.030 mg/L.        reflecting maximum residence time during
 least 10,000 persons.                                                  month of warmest water temperature
System using only ground water not under  TTHM annual average <=0.040  One sample per treatment plant per three
 direct influence of surface water using   mg/L and HAA5 annual         year monitoring cycle at distribution
 chemical disinfectant and serving fewer   average <=0.030 mg/L for     system location reflecting maximum
 than 10,000 persons.                      two consecutive years OR     residence time during month of warmest
                                           TTHM annual average          water temperature, with the three-year
                                           <=0.020 mg/L and HAA5        cycle beginning on January 1 following
                                           annual average <=0.015 mg/   quarter in which system qualifies for
                                           L for one year.              reduced monitoring.
----------------------------------------------------------------------------------------------------------------

    (iii) Monitoring requirements for source water TOC. In order to 
qualify for reduced monitoring for TTHM and HAA5 under paragraph 
(b)(1)(ii) of this section, subpart H systems not monitoring under the 
provisions of paragraph (d) of this section must take monthly TOC 
samples every 30 days at a location prior to any treatment, beginning 
April 1, 2008 or earlier, if specified by the State. In addition to 
meeting other criteria for reduced monitoring in paragraph (b)(1)(ii) of 
this section, the source water TOC running annual average must be <=4.0 
mg/L (based on the most recent four quarters of monitoring) on a 
continuing basis at each treatment plant to reduce or remain on reduced 
monitoring for TTHM and HAA5. Once qualified for reduced monitoring for 
TTHM and HAA5 under paragraph (b)(1)(ii) of this section, a system may 
reduce source water TOC monitoring to quarterly TOC samples taken every 
90 days at a location prior to any treatment.
    (iv) Systems on a reduced monitoring schedule may remain on that 
reduced schedule as long as the average of all samples taken in the year 
(for systems which must monitor quarterly) or the result of the sample 
(for systems which

[[Page 585]]

must monitor no more frequently than annually) is no more than 0.060 mg/
L and 0.045 mg/L for TTHMs and HAA5, respectively. Systems that do not 
meet these levels must resume monitoring at the frequency identified in 
paragraph (b)(1)(i) of this section (minimum monitoring frequency 
column) in the quarter immediately following the monitoring period in 
which the system exceeds 0.060 mg/L or 0.045 mg/L for TTHMs and HAA5, 
respectively. For systems using only ground water not under the direct 
influence of surface water and serving fewer than 10,000 persons, if 
either the TTHM annual average is 0.080 mg/L or the HAA5 
annual average is 0.060 mg/L, the system must go to the 
increased monitoring identified in paragraph (b)(1)(i) of this section 
(sample location column) in the quarter immediately following the 
monitoring period in which the system exceeds 0.080 mg/L or 0.060 mg/L 
for TTHMs or HAA5 respectively.
    (v) Systems on increased monitoring may return to routine monitoring 
if, after at least one year of monitoring their TTHM annual average is 
<=0.060 mg/L and their HAA5 annual average is <=0.045 mg/L.
    (vi) The State may return a system to routine monitoring at the 
State's discretion.
    (2) Chlorite. Community and nontransient noncommunity water systems 
using chlorine dioxide, for disinfection or oxidation, must conduct 
monitoring for chlorite.
    (i) Routine monitoring. (A) Daily monitoring. Systems must take 
daily samples at the entrance to the distribution system. For any daily 
sample that exceeds the chlorite MCL, the system must take additional 
samples in the distribution system the following day at the locations 
required by paragraph (b)(2)(ii) of this section, in addition to the 
sample required at the entrance to the distribution system.
    (B) Monthly monitoring. Systems must take a three-sample set each 
month in the distribution system. The system must take one sample at 
each of the following locations: near the first customer, at a location 
representative of average residence time, and at a location reflecting 
maximum residence time in the distribution system. Any additional 
routine sampling must be conducted in the same manner (as three-sample 
sets, at the specified locations). The system may use the results of 
additional monitoring conducted under paragraph (b)(2)(ii) of this 
section to meet the requirement for monitoring in this paragraph.
    (ii) Additional monitoring. On each day following a routine sample 
monitoring result that exceeds the chlorite MCL at the entrance to the 
distribution system, the system is required to take three chlorite 
distribution system samples at the following locations: as close to the 
first customer as possible, in a location representative of average 
residence time, and as close to the end of the distribution system as 
possible (reflecting maximum residence time in the distribution system).
    (iii) Reduced monitoring. (A) Chlorite monitoring at the entrance to 
the distribution system required by paragraph (b)(2)(i)(A) of this 
section may not be reduced.
    (B) Chlorite monitoring in the distribution system required by 
paragraph (b)(2)(i)(B) of this section may be reduced to one three-
sample set per quarter after one year of monitoring where no individual 
chlorite sample taken in the distribution system under paragraph 
(b)(2)(i)(B) of this section has exceeded the chlorite MCL and the 
system has not been required to conduct monitoring under paragraph 
(b)(2)(ii) of this section. The system may remain on the reduced 
monitoring schedule until either any of the three individual chlorite 
samples taken quarterly in the distribution system under paragraph 
(b)(2)(i)(B) of this section exceeds the chlorite MCL or the system is 
required to conduct monitoring under paragraph (b)(2)(ii) of this 
section, at which time the system must revert to routine monitoring.
    (3) Bromate--(i) Routine monitoring. Community and nontransient 
noncommunity systems using ozone, for disinfection or oxidation, must 
take one sample per month for each treatment plant in the system using 
ozone. Systems must take samples monthly at the entrance to the 
distribution system while the ozonation system is operating under normal 
conditions.

[[Page 586]]

    (ii) Reduced monitoring. (A) Until March 31, 2009, systems required 
to analyze for bromate may reduce monitoring from monthly to quarterly, 
if the system's average source water bromide concentration is less than 
0.05 mg/L based on representative monthly bromide measurements for one 
year. The system may remain on reduced bromate monitoring until the 
running annual average source water bromide concentration, computed 
quarterly, is equal to or greater than 0.05 mg/L based on representative 
monthly measurements. If the running annual average source water bromide 
concentration is =0.05 mg/L, the system must resume routine 
monitoring required by paragraph (b)(3)(i) of this section in the 
following month.
    (B) Beginning April 1, 2009, systems may no longer use the 
provisions of paragraph (b)(3)(ii)(A) of this section to qualify for 
reduced monitoring. A system required to analyze for bromate may reduce 
monitoring from monthly to quarterly, if the system's running annual 
average bromate concentration is <=0.0025 mg/L based on monthly bromate 
measurements under paragraph (b)(3)(i) of this section for the most 
recent four quarters, with samples analyzed using Method 317.0 Revision 
2.0, 326.0 or 321.8. If a system has qualified for reduced bromate 
monitoring under paragraph (b)(3)(ii)(A) of this section, that system 
may remain on reduced monitoring as long as the running annual average 
of quarterly bromate samples <=0.0025 mg/L based on samples analyzed 
using Method 317.0 Revision 2.0, 326.0, or 321.8. If the running annual 
average bromate concentration is 0.0025 mg/L, the system must 
resume routine monitoring required by paragraph (b)(3)(i) of this 
section.
    (c) Monitoring requirements for disinfectant residuals--(1) Chlorine 
and chloramines--(i) Routine monitoring. Until March 31, 2016, community 
and non-transient non-community water systems that use chlorine or 
chloramines must measure the residual disinfectant level in the 
distribution system at the same point in the distribution system and at 
the same time as total coliforms are sampled, as specified in Sec.  
141.21. Beginning April 1, 2016, community and non-transient non-
community water systems that use chlorine or chloramines must measure 
the residual disinfectant level in the distribution system at the same 
point in the distribution system and at the same time as total coliforms 
are sampled, as specified in Sec. Sec.  141.854 through 141.858. Subpart 
H systems of this part may use the results of residual disinfectant 
concentration sampling conducted under Sec.  141.74(b)(6)(i) for 
unfiltered systems or Sec.  141.74(c)(3)(i) for systems which filter, in 
lieu of taking separate samples.
    (ii) Reduced monitoring. Monitoring may not be reduced.
    (2) Chlorine dioxide--(i) Routine monitoring. Community, 
nontransient noncommunity, and transient noncommunity water systems that 
use chlorine dioxide for disinfection or oxidation must take daily 
samples at the entrance to the distribution system. For any daily sample 
that exceeds the MRDL, the system must take samples in the distribution 
system the following day at the locations required by paragraph 
(c)(2)(ii) of this section, in addition to the sample required at the 
entrance to the distribution system.
    (ii) Additional monitoring. On each day following a routine sample 
monitoring result that exceeds the MRDL, the system is required to take 
three chlorine dioxide distribution system samples. If chlorine dioxide 
or chloramines are used to maintain a disinfectant residual in the 
distribution system, or if chlorine is used to maintain a disinfectant 
residual in the distribution system and there are no disinfection 
addition points after the entrance to the distribution system (i.e., no 
booster chlorination), the system must take three samples as close to 
the first customer as possible, at intervals of at least six hours. If 
chlorine is used to maintain a disinfectant residual in the distribution 
system and there are one or more disinfection addition points after the 
entrance to the distribution system (i.e., booster chlorination), the 
system must take one sample at each of the following locations: as close 
to the first customer as possible, in a location representative of 
average residence time, and as close to the end of

[[Page 587]]

the distribution system as possible (reflecting maximum residence time 
in the distribution system).
    (iii) Reduced monitoring. Chlorine dioxide monitoring may not be 
reduced.
    (d) Monitoring requirements for disinfection byproduct precursors 
(DBPP)--(1) Routine monitoring. Subpart H systems which use conventional 
filtration treatment (as defined in Sec.  141.2) must monitor each 
treatment plant for TOC no later than the point of combined filter 
effluent turbidity monitoring and representative of the treated water. 
All systems required to monitor under this paragraph (d)(1) must also 
monitor for TOC in the source water prior to any treatment at the same 
time as monitoring for TOC in the treated water. These samples (source 
water and treated water) are referred to as paired samples. At the same 
time as the source water sample is taken, all systems must monitor for 
alkalinity in the source water prior to any treatment. Systems must take 
one paired sample and one source water alkalinity sample per month per 
plant at a time representative of normal operating conditions and 
influent water quality.
    (2) Reduced monitoring. Subpart H systems with an average treated 
water TOC of less than 2.0 mg/L for two consecutive years, or less than 
1.0 mg/L for one year, may reduce monitoring for both TOC and alkalinity 
to one paired sample and one source water alkalinity sample per plant 
per quarter. The system must revert to routine monitoring in the month 
following the quarter when the annual average treated water TOC 
=2.0 mg/L.
    (e) Bromide. Systems required to analyze for bromate may reduce 
bromate monitoring from monthly to once per quarter, if the system 
demonstrates that the average source water bromide concentration is less 
than 0.05 mg/L based upon representative monthly measurements for one 
year. The system must continue bromide monitoring to remain on reduced 
bromate monitoring.
    (f) Monitoring plans. Each system required to monitor under this 
subpart must develop and implement a monitoring plan. The system must 
maintain the plan and make it available for inspection by the State and 
the general public no later than 30 days following the applicable 
compliance dates in Sec.  141.130(b). All Subpart H systems serving more 
than 3300 people must submit a copy of the monitoring plan to the State 
no later than the date of the first report required under Sec.  141.134. 
The State may also require the plan to be submitted by any other system. 
After review, the State may require changes in any plan elements. The 
plan must include at least the following elements.
    (1) Specific locations and schedules for collecting samples for any 
parameters included in this subpart.
    (2) How the system will calculate compliance with MCLs, MRDLs, and 
treatment techniques.
    (3) If approved for monitoring as a consecutive system, or if 
providing water to a consecutive system, under the provisions of Sec.  
141.29, the sampling plan must reflect the entire distribution system.

[63 FR 69466, Dec. 16, 1998, as amended at 66 FR 3776, Jan. 16, 2001; 69 
FR 38856, June 29, 2004; 71 FR 482, Jan. 4, 2006; 78 FR 10348, Feb. 13, 
2013]



Sec.  141.133  Compliance requirements.

    (a) General requirements. (1) Where compliance is based on a running 
annual average of monthly or quarterly samples or averages and the 
system fails to monitor for TTHM, HAA5, or bromate, this failure to 
monitor will be treated as a monitoring violation for the entire period 
covered by the annual average. Where compliance is based on a running 
annual average of monthly or quarterly samples or averages and the 
system failure to monitor makes it impossible to determine compliance 
with MRDLs for chlorine and chloramines, this failure to monitor will be 
treated as a monitoring violation for the entire period covered by the 
annual average.
    (2) All samples taken and analyzed under the provisions of this 
subpart must be included in determining compliance, even if that number 
is greater than the minimum required.
    (3) If, during the first year of monitoring under Sec.  141.132, any 
individual quarter's average will cause the running annual average of 
that system to exceed the MCL for total trihalomethanes, haloacetic 
acids

[[Page 588]]

(five), or bromate; or the MRDL for chlorine or chloramine, the system 
is out of compliance at the end of that quarter.
    (b) Disinfection byproducts--(1) TTHMs and HAA5. (i) For systems 
monitoring quarterly, compliance with MCLs in Sec.  141.64 must be based 
on a running annual arithmetic average, computed quarterly, of quarterly 
arithmetic averages of all samples collected by the system as prescribed 
by Sec.  141.132(b)(1).
    (ii) For systems monitoring less frequently than quarterly, systems 
demonstrate MCL compliance if the average of samples taken that year 
under the provisions of Sec.  141.132(b)(1) does not exceed the MCLs in 
Sec.  141.64. If the average of these samples exceeds the MCL, the 
system must increase monitoring to once per quarter per treatment plant 
and such a system is not in violation of the MCL until it has completed 
one year of quarterly monitoring, unless the result of fewer than four 
quarters of monitoring will cause the running annual average to exceed 
the MCL, in which case the system is in violation at the end of that 
quarter. Systems required to increase monitoring frequency to quarterly 
monitoring must calculate compliance by including the sample which 
triggered the increased monitoring plus the following three quarters of 
monitoring.
    (iii) If the running annual arithmetic average of quarterly averages 
covering any consecutive four-quarter period exceeds the MCL, the system 
is in violation of the MCL and must notify the public pursuant to Sec.  
141.32 or Sec.  141.202, whichever is effective for your system, in 
addition to reporting to the State pursuant to Sec.  141.134.
    (iv) If a PWS fails to complete four consecutive quarters of 
monitoring, compliance with the MCL for the last four-quarter compliance 
period must be based on an average of the available data.
    (2) Bromate. Compliance must be based on a running annual arithmetic 
average, computed quarterly, of monthly samples (or, for months in which 
the system takes more than one sample, the average f all samples taken 
during the month) collected by the system as prescribed by Sec.  
141.132(b)(3). If the average of samples covering any consecutive four-
quarter period exceeds the MCL, the system is in violation of the MCL 
and must notify the public pursuant to subpart Q, in addition to 
reporting to the State pursuant to Sec.  141.134. If a PWS fails to 
complete 12 consecutive months' monitoring, compliance with the MCL for 
the last four-quarter compliance period must be based on an average of 
the available data.
    (3) Chlorite. Compliance must be based on an arithmetic average of 
each three sample set taken in the distribution system as prescribed by 
Sec.  141.132(b)(2)(i)(B) and Sec.  141.132(b)(2)(ii). If the arithmetic 
average of any three sample set exceeds the MCL, the system is in 
violation of the MCL and must notify the public pursuant to subpart Q, 
in addition to reporting to the State pursuant to Sec.  141.134.
    (c) Disinfectant residuals--(1) Chlorine and chloramines. (i) 
Compliance must be based on a running annual arithmetic average, 
computed quarterly, of monthly averages of all samples collected by the 
system under Sec.  141.132(c)(1). If the average covering any 
consecutive four-quarter period exceeds the MRDL, the system is in 
violation of the MRDL and must notify the public pursuant to subpart Q, 
in addition to reporting to the State pursuant to Sec.  141.134.
    (ii) In cases where systems switch between the use of chlorine and 
chloramines for residual disinfection during the year, compliance must 
be determined by including together all monitoring results of both 
chlorine and chloramines in calculating compliance. Reports submitted 
pursuant to Sec.  141.134 must clearly indicate which residual 
disinfectant was analyzed for each sample.
    (2) Chlorine dioxide. (i) Acute violations. Compliance must be based 
on consecutive daily samples collected by the system under Sec.  
141.132(c)(2). If any daily sample taken at the entrance to the 
distribution system exceeds the MRDL, and on the following day one (or 
more) of the three samples taken in the distribution system exceed the 
MRDL, the system is in violation of the MRDL and must take immediate 
corrective action to lower the level of chlorine dioxide below the MRDL 
and

[[Page 589]]

must notify the public pursuant to the procedures for acute health risks 
in subpart Q in addition to reporting to the State pursuant to Sec.  
141.134. Failure to take samples in the distribution system the day 
following an exceedance of the chlorine dioxide MRDL at the entrance to 
the distribution system will also be considered an MRDL violation and 
the system must notify the public of the violation in accordance with 
the provisions for acute violations under subpart Q in addition to 
reporting to the State pursuant to Sec.  141.134.
    (ii) Nonacute violations. Compliance must be based on consecutive 
daily samples collected by the system under Sec.  141.132(c)(2). If any 
two consecutive daily samples taken at the entrance to the distribution 
system exceed the MRDL and all distribution system samples taken are 
below the MRDL, the system is in violation of the MRDL and must take 
corrective action to lower the level of chlorine dioxide below the MRDL 
at the point of sampling and will notify the public pursuant to the 
procedures for nonacute health risks in subpart Q in addition to 
reporting to the State pursuant to Sec.  141.134. Failure to monitor at 
the entrance to the distribution system the day following an exceedance 
of the chlorine dioxide MRDL at the entrance to the distribution system 
is also an MRDL violation and the system must notify the public of the 
violation in accordance with the provisions for nonacute violations 
under Sec.  141.32(e)(78) in addition to reporting to the State pursuant 
to Sec.  141.134.
    (d) Disinfection byproduct precursors (DBPP). Compliance must be 
determined as specified by Sec.  141.135(c). Systems may begin 
monitoring to determine whether Step 1 TOC removals can be met 12 months 
prior to the compliance date for the system. This monitoring is not 
required and failure to monitor during this period is not a violation. 
However, any system that does not monitor during this period, and then 
determines in the first 12 months after the compliance date that it is 
not able to meet the Step 1 requirements in Sec.  141.135(b)(2) and must 
therefore apply for alternate minimum TOC removal (Step 2) requirements, 
is not eligible for retroactive approval of alternate minimum TOC 
removal (Step 2) requirements as allowed pursuant to Sec.  141.135(b)(3) 
and is in violation. Systems may apply for alternate minimum TOC removal 
(Step 2) requirements any time after the compliance date. For systems 
required to meet Step 1 TOC removals, if the value calculated under 
Sec.  141.135(c)(1)(iv) is less than 1.00, the system is in violation of 
the treatment technique requirements and must notify the public pursuant 
to subpart Q of this part, in addition to reporting to the State 
pursuant to Sec.  141.134.

[63 FR 69466, Dec. 16, 1998, as amended at 65 FR 26022, May 4, 2000; 65 
FR 40521, June 30, 2000; 66 FR 3777, Jan. 16, 2001; 69 FR 38856, June 
29, 2004; 71 FR 482, Jan. 4, 2006]



Sec.  141.134  Reporting and recordkeeping requirements.

    (a) Systems required to sample quarterly or more frequently must 
report to the State within 10 days after the end of each quarter in 
which samples were collected, notwithstanding the provisions of Sec.  
141.31. Systems required to sample less frequently than quarterly must 
report to the State within 10 days after the end of each monitoring 
period in which samples were collected.
    (b) Disinfection byproducts. Systems must report the information 
specified in the following table:

------------------------------------------------------------------------
           If you are a * * *                 You must report * * *
------------------------------------------------------------------------
(1) System monitoring for TTHMs and      (i) The number of samples taken
 HAA5 under the requirements of Sec.      during the last quarter.
 141.132(b) on a quarterly or more       (ii) The location, date, and
 frequent basis.                          result of each sample taken
                                          during the last quarter.
                                         (iii) The arithmetic average of
                                          all samples taken in the last
                                          quarter.
                                         (iv) The annual arithmetic
                                          average of the quarterly
                                          arithmetic averages of this
                                          section for the last four
                                          quarters.
                                         (v) Whether, based on Sec.
                                          141.133(b)(1), the MCL was
                                          violated.

[[Page 590]]

 
(2) System monitoring for TTHMs and      (i) The number of samples taken
 HAA5 under the requirements of Sec.      during the last year.
 141.132(b) less frequently than         (ii) The location, date, and
 quarterly (but as least annually).       result of each sample taken
                                          during the last monitoring
                                          period.
                                         (iii) The arithmetic average of
                                          all samples taken over the
                                          last year.
                                         (iv) Whether, based on Sec.
                                          141.133(b)(1), the MCL was
                                          violated.
(3) System monitoring for TTHMs and      (i) The location, date, and
 HAA5 under the requriements of Sec.      result of each sample taken
 141.132(b) less frequently than         (ii) Whether, based on Sec.
 annually.                                141.133(b)(1), the MCL was
                                          violated.
(4) System monitoring for chlorite       (i) The number of entry point
 under the requirements of Sec.           samples taken each month for
 141.132(b).                              the last 3 months.
                                         (ii) The location, date, and
                                          result of each sample (both
                                          entry point and distribution
                                          system) taken during the last
                                          quarter.
                                         (iii) For each month in the
                                          reporting period, the
                                          arithmetic average of all
                                          samples taken in each three
                                          samples set taken in the
                                          distribution system.
                                         (iv) Whether, based on Sec.
                                          141.133(b)(3), the MCL was
                                          violated, in which month, and
                                          how many times it was violated
                                          each month.
(5) System monitoring for bromate under  (i)The number of samples taken
 the requirements of Sec.   141.132(b).   during the last quarter.
                                         (ii)The location, date, and
                                          result of each sample taken
                                          during the last quarter.
                                         (iii) The arithmetic average of
                                          the monthly arithmetic
                                          averages of all samples taken
                                          in the last year.
                                         (iv) Whether, based on Sec.
                                          141.133(b)(2), the MCL was
                                          violated.
------------------------------------------------------------------------
\1\ The State may choose to perform calculations and determine whether
  the MCL was exceeded, in lieu of having the system report that
  information

    (c) Disinfectants. Systems must report the information specified in 
the following table:

------------------------------------------------------------------------
           If you are a * * *                 You must report * * *
------------------------------------------------------------------------
(1) System monitoring for chlorine or    (i) The number of samples taken
 chloramines under the requirements of    during each month of the last
 Sec.   141.132(c).                       quarter.
                                         (ii) The month arithmetic
                                          average of all samples taken
                                          in each month for the last 12
                                          months.
                                         (iii) The arithmetic average of
                                          the monthly averages for the
                                          last 12 months.
                                         (iv) Whether, based on Sec.
                                          141.133(c)(1), the MRD was
                                          violated.
(2) System monitoring for chlorine       (i) The dates, result, and
 dioxide under the requirements of Sec.   locations of samples taken
   141.132(c).                            during the last quarter.
                                         (ii) Whether, based on Sec.
                                          141.133(c)(2), the MRDL was
                                          violated.
                                         (iii) Whether the MRDL was
                                          exceeded in any two
                                          consecutive daily samples and
                                          whether the resulting
                                          violation was acuate or
                                          nonacute.
------------------------------------------------------------------------
\1\ The State may choose to perform calculations and determine whether
  the MRDL was exceeded, in lieu of having the system report that
  information.

    (d) Disinfection byproduct precursors and enhanced coagulation or 
enhanced softening. Systems must report the information specified in the 
following table:

------------------------------------------------------------------------
           If you are a. . .                 You must report. . . \1\
------------------------------------------------------------------------
(1) System monitoring monthly or         (i) The number of paired
 quarterly for TOC under the              (source water and treated
 requirements of Sec.   141.132(d) and    water) samples taken during
 required to meet the enhanced            the last quarter.
 coagulation or enhanced softening       (ii) The location, date, and
 requirements in Sec.   141.135(b)(2)     results of each paired sample
 or (3).                                  and associated alkalinity
                                          taken during the last quarter.
                                         (iii) For each month in the
                                          reporting period that paired
                                          samples were taken, the
                                          arithmetic average of the
                                          percent reduction of TOC for
                                          each paired sample and the
                                          required TOC percent removal.
                                         (iv) Calculations for
                                          determining compliance with
                                          the TOC percent removal
                                          requirements, as provided in
                                          Sec.   141.135(c)(1).
                                         (v) Whether the system is in
                                          compliance with the enhanced
                                          coagulation or enhanced
                                          softening percent removal
                                          requirements in Sec.
                                          141.135(b) for the last four
                                          quarters.
(2) System monitoring monthly or         (i) The alternative compliance
 quarterly for TOC under the              criterion that the system is
 requirements of Sec.   141.132(d) and    using.
 meeting one or more of the alternative
 compliance criteria in Sec.
 141.135(a)(2) or (3).
                                         (ii) The number of paired
                                          samples taken during the last
                                          quarter.

[[Page 591]]

 
                                         (iii) The location, date, and
                                          result of each paired sample
                                          and associated alkalinity
                                          taken during the last quarter.
                                         (iv) The running annual
                                          arithmetic average based on
                                          monthly averages (or quarterly
                                          samples) of source water TOC
                                          for systems meeting a
                                          criterion in Sec.  Sec.
                                          141.135(a)(2)(i) or (iii) or
                                          of treated water TOC for
                                          systems meeting the criterion
                                          in Sec.   141.135(a)(2)(ii).
                                         (v) The running annual
                                          arithmetic average based on
                                          monthly averages (or quarterly
                                          samples) of source water SUVA
                                          for systems meeting the
                                          criterion in Sec.
                                          141.135(a)(2)(v) or of treated
                                          water SUVA for systems meeting
                                          the criterion in Sec.
                                          141.135(a)(2)(vi).
                                         (vi) The running annual average
                                          of source water alkalinity for
                                          systems meeting the criterion
                                          in Sec.   141.135(a)(2)(iii)
                                          and of treated water
                                          alkalinity for systems meeting
                                          the criterion in Sec.
                                          141.135(a)(3)(i).
                                         (vii) The running annual
                                          average for both TTHM and HAA5
                                          for systems meeting the
                                          criterion in Sec.
                                          141.135(a)(2)(iii) or (iv).
                                         (viii) The running annual
                                          average of the amount of
                                          magnesium hardness removal (as
                                          CaCO3, in mg/L) for systems
                                          meeting the criterion in Sec.
                                           141.135(a)(3)(ii).
                                         (ix) Whether the system is in
                                          compliance with the particular
                                          alternative compliance
                                          criterion in Sec.
                                          141.135(a)(2) or (3).
------------------------------------------------------------------------
\1\ The State may choose to perform calculations and determine whether
  the treatment technique was met, in lieu of having the system report
  that information.


[63 FR 69466, Dec. 16, 1998, as amended at 66 FR 3778, Jan. 16, 2001; 66 
FR 9903, Feb. 12, 2001]



Sec.  141.135  Treatment technique for control of disinfection byproduct 
(DBP) precursors.

    (a) Applicability. (1) Subpart H systems using conventional 
filtration treatment (as defined in Sec.  141.2) must operate with 
enhanced coagulation or enhanced softening to achieve the TOC percent 
removal levels specified in paragraph (b) of this section unless the 
system meets at least one of the alternative compliance criteria listed 
in paragraph (a)(2) or (a)(3) of this section.
    (2) Alternative compliance criteria for enhanced coagulation and 
enhanced softening systems. Subpart H systems using conventional 
filtration treatment may use the alternative compliance criteria in 
paragraphs (a)(2)(i) through (vi) of this section to comply with this 
section in lieu of complying with paragraph (b) of this section. Systems 
must still comply with monitoring requirements in Sec.  141.132(d).
    (i) The system's source water TOC level, measured according to Sec.  
141.131(d)(3), is less than 2.0 mg/L, calculated quarterly as a running 
annual average.
    (ii) The system's treated water TOC level, measured according to 
Sec.  141.131(d)(3), is less than 2.0 mg/L, calculated quarterly as a 
running annual average.
    (iii) The system's source water TOC level, measured according to 
Sec.  141.131(d)(3), is less than 4.0 mg/L, calculated quarterly as a 
running annual average; the source water alkalinity, measured according 
to Sec.  141.131(d)(1), is greater than 60 mg/L (as CaCO3), 
calculated quarterly as a running annual average; and either the TTHM 
and HAA5 running annual averages are no greater than 0.040 mg/L and 
0.030 mg/L, respectively; or prior to the effective date for compliance 
in Sec.  141.130(b), the system has made a clear and irrevocable 
financial commitment not later than the effective date for compliance in 
Sec.  141.130(b) to use of technologies that will limit the levels of 
TTHMs and HAA5 to no more than 0.040 mg/L and 0.030 mg/L, respectively. 
Systems must submit evidence of a clear and irrevocable financial 
commitment, in addition to a schedule containing milestones and periodic 
progress reports for installation and operation of appropriate 
technologies, to the State for approval not later than the effective 
date for compliance in Sec.  141.130(b). These technologies must be 
installed and operating not later than June 30, 2005. Failure to install 
and operate these technologies by the date in the

[[Page 592]]

approved schedule will constitute a violation of National Primary 
Drinking Water Regulations.
    (iv) The TTHM and HAA5 running annual averages are no greater than 
0.040 mg/L and 0.030 mg/L, respectively, and the system uses only 
chlorine for primary disinfection and maintenance of a residual in the 
distribution system.
    (v) The system's source water SUVA, prior to any treatment and 
measured monthly according to Sec.  141.131(d)(4), is less than or equal 
to 2.0 L/mg-m, calculated quarterly as a running annual average.
    (vi) The system's finished water SUVA, measured monthly according to 
Sec.  141.131(d)(4), is less than or equal to 2.0 L/mg-m, calculated 
quarterly as a running annual average.
    (3) Additional alternative compliance criteria for softening 
systems. Systems practicing enhanced softening that cannot achieve the 
TOC removals required by paragraph (b)(2) of this section may use the 
alternative compliance criteria in paragraphs (a)(3)(i) and (ii) of this 
section in lieu of complying with paragraph (b) of this section. Systems 
must still comply with monitoring requirements in Sec.  141.132(d).
    (i) Softening that results in lowering the treated water alkalinity 
to less than 60 mg/L (as CaCO3), measured monthly according 
to Sec.  141.131(d)(1) and calculated quarterly as a running annual 
average.
    (ii) Softening that results in removing at least 10 mg/L of 
magnesium hardness (as CaCO3), measured monthly according to 
Sec.  141.131(d)(6) and calculated quarterly as a running annual 
average.
    (b) Enhanced coagulation and enhanced softening performance 
requirements. (1) Systems must achieve the percent reduction of TOC 
specified in paragraph (b)(2) of this section between the source water 
and the combined filter effluent, unless the State approves a system's 
request for alternate minimum TOC removal (Step 2) requirements under 
paragraph (b)(3) of this section.
    (2) Required Step 1 TOC reductions, indicated in the following 
table, are based upon specified source water parameters measured in 
accordance with Sec.  141.131(d). Systems practicing softening are 
required to meet the Step 1 TOC reductions in the far-right column 
(Source water alkalinity 120 mg/L) for the specified source 
water TOC:

    Step 1 Required Removal of TOC by Enhanced Coagulation and Enhanced Softening for Subpart H Systems Using
                                          Conventional Treatment \1 2\
----------------------------------------------------------------------------------------------------------------
                                                                   Source-water alkalinity, mg/L as CaCO 3 (in
                                                                                   precentages)
                     Source-water TOC, mg/L                     ------------------------------------------------
                                                                                                  120
                                                                     0-60      60-120        \3\
----------------------------------------------------------------------------------------------------------------
2.0-4.0.............................................         35.0             25.0             15.0
4.0-8.0.............................................         45.0             35.0             25.0
8.0.................................................         50.0             40.0            30.0
----------------------------------------------------------------------------------------------------------------
\1\ Systems meeting at least one of the conditions in paragraph (a)(2)(i)-(vi) of this section are not required
  to operate with enhanced coagulation.
\2\ Softening system meeting one of the alternative compliance criteria in paragraph (a)(3) of this section are
  not required to operate with enhanced softening.
\3\ System practicing softening must meet the TOC removal requirements in this column.

    (3) Subpart H conventional treatment systems that cannot achieve the 
Step 1 TOC removals required by paragraph (b)(2) of this section due to 
water quality parameters or operational constraints must apply to the 
State, within three months of failure to achieve the TOC removals 
required by paragraph (b)(2) of this section, for approval of 
alternative minimum TOC (Step 2) removal requirements submitted by the 
system. If the State approves the alternative minimum TOC removal (Step 
2) requirements, the State may make those requirements retroactive for 
the purposes of determining compliance. Until the State approves the 
alternate minimum TOC removal (Step 2) requirements, the system must 
meet the Step 1 TOC removals contained in paragraph (b)(2) of this 
section.
    (4) Alternate minimum TOC removal (Step 2) requirements. 
Applications made to the State by enhanced coagulation

[[Page 593]]

systems for approval of alternate minimum TOC removal (Step 2) 
requirements under paragraph (b)(3) of this section must include, at a 
minimum, results of bench- or pilot-scale testing conducted under 
paragraph (b)(4)(i) of this section. The submitted bench- or pilot-scale 
testing must be used to determine the alternate enhanced coagulation 
level.
    (i) Alternate enhanced coagulation level is defined as coagulation 
at a coagulant dose and pH as determined by the method described in 
paragraphs (b)(4)(i) through (v) of this section such that an 
incremental addition of 10 mg/L of alum (or equivalent amount of ferric 
salt) results in a TOC removal of <=0.3 mg/L. The percent removal of TOC 
at this point on the ``TOC removal versus coagulant dose'' curve is then 
defined as the minimum TOC removal required for the system. Once 
approved by the State, this minimum requirement supersedes the minimum 
TOC removal required by the table in paragraph (b)(2) of this section. 
This requirement will be effective until such time as the State approves 
a new value based on the results of a new bench- and pilot-scale test. 
Failure to achieve State-set alternative minimum TOC removal levels is a 
violation of National Primary Drinking Water Regulations.
    (ii) Bench- or pilot-scale testing of enhanced coagulation must be 
conducted by using representative water samples and adding 10 mg/L 
increments of alum (or equivalent amounts of ferric salt) until the pH 
is reduced to a level less than or equal to the enhanced coagulation 
Step 2 target pH shown in the following table:

                  Enhanced Coagulation Step 2 target pH
------------------------------------------------------------------------
                 Alkalinity (mg/L as CaCO3)                   Target pH
------------------------------------------------------------------------
0-60.......................................................          5.5
60-120..........................................          6.3
120-240.........................................          7.0
240.............................................          7.5
------------------------------------------------------------------------

    (iii) For waters with alkalinities of less than 60 mg/L for which 
addition of small amounts of alum or equivalent addition of iron 
coagulant drives the pH below 5.5 before significant TOC removal occurs, 
the system must add necessary chemicals to maintain the pH between 5.3 
and 5.7 in samples until the TOC removal of 0.3 mg/L per 10 mg/L alum 
added (or equivalant addition of iron coagulant) is reached.
    (iv) The system may operate at any coagulant dose or pH necessary 
(consistent with other NPDWRs) to achieve the minimum TOC percent 
removal approved under paragraph (b)(3) of this section.
    (v) If the TOC removal is consistently less than 0.3 mg/L of TOC per 
10 mg/L of incremental alum dose at all dosages of alum (or equivalant 
addition of iron coagulant), the water is deemed to contain TOC not 
amenable to enhanced coagulation. The system may then apply to the State 
for a waiver of enhanced coagulation requirements.
    (c) Compliance calculations. (1) Subpart H systems other than those 
identified in paragraph (a)(2) or (a)(3) of this section must comply 
with requirements contained in paragraph (b)(2) or (b)(3) of this 
section. Systems must calculate compliance quarterly, beginning after 
the system has collected 12 months of data, by determining an annual 
average using the following method:
    (i) Determine actual monthly TOC percent removal, equal to:

(1-(treated water TOC/source water TOC)) x 100

    (ii) Determine the required monthly TOC percent removal (from either 
the table in paragraph (b)(2) of this section or from paragraph (b)(3) 
of this section).
    (iii) Divide the value in paragraph (c)(1)(i) of this section by the 
value in paragraph (c)(1)(ii) of this section.
    (iv) Add together the results of paragraph (c)(1)(iii) of this 
section for the last 12 months and divide by 12.
    (v) If the value calculated in paragraph (c)(1)(iv) of this section 
is less than 1.00, the system is not in compliance with the TOC percent 
removal requirements.
    (2) Systems may use the provisions in paragraphs (c)(2)(i) through 
(v) of this section in lieu of the calculations in paragraph (c)(1)(i) 
through (v) of this section to determine compliance with TOC percent 
removal requirements.
    (i) In any month that the system's treated or source water TOC 
level,

[[Page 594]]

measured according to Sec.  141.131(d)(3), is less than 2.0 mg/L, the 
system may assign a monthly value of 1.0 (in lieu of the value 
calculated in paragraph (c)(1)(iii) of this section) when calculating 
compliance under the provisions of paragraph (c)(1) of this section.
    (ii) In any month that a system practicing softening removes at 
least 10 mg/L of magnesium hardness (as CaCO3), the system 
may assign a monthly value of 1.0 (in lieu of the value calculated in 
paragraph (c)(1)(iii) of this section) when calculating compliance under 
the provisions of paragraph (c)(1) of this section.
    (iii) In any month that the system's source water SUVA, prior to any 
treatment and measured according to Sec.  141.131(d)(4), is <=2.0 L/mg-
m, the system may assign a monthly value of 1.0 (in lieu of the value 
calculated in paragraph (c)(1)(iii) of this section) when calculating 
compliance under the provisions of paragraph (c)(1) of this section.
    (iv) In any month that the system's finished water SUVA, measured 
according to Sec.  141.131(d)(4), is <=2.0 L/mg-m, the system may assign 
a monthly value of 1.0 (in lieu of the value calculated in paragraph 
(c)(1)(iii) of this section) when calculating compliance under the 
provisions of paragraph (c)(1) of this section.
    (v) In any month that a system practicing enhanced softening lowers 
alkalinity below 60 mg/L (as CaCO3), the system may assign a 
monthly value of 1.0 (in lieu of the value calculated in paragraph 
(c)(1)(iii) of this section) when calculating compliance under the 
provisions of paragraph (c)(1) of this section.
    (3) Subpart H systems using conventional treatment may also comply 
with the requirements of this section by meeting the criteria in 
paragraph (a)(2) or (3) of this section.
    (d) Treatment technique requirements for DBP precursors. The 
Administrator identifies the following as treatment techniques to 
control the level of disinfection byproduct precursors in drinking water 
treatment and distribution systems: For Subpart H systems using 
conventional treatment, enhanced coagulation or enhanced softening.

[63 FR 69466, Dec. 16, 1998, as amended at 66 FR 3779, Jan. 16, 2001; 71 
FR 482, Jan. 4, 2006]

Subparts M-N [Reserved]



                  Subpart O_Consumer Confidence Reports

    Source: 63 FR 44526, Aug. 19, 1998, unless otherwise noted.



Sec.  141.151  Purpose and applicability of this subpart.

    (a) This subpart establishes the minimum requirements for the 
content of annual reports that community water systems must deliver to 
their customers. These reports must contain information on the quality 
of the water delivered by the systems and characterize the risks (if 
any) from exposure to contaminants detected in the drinking water in an 
accurate and understandable manner.
    (b) Notwithstanding the provisions of Sec.  141.3, this subpart 
applies only to community water systems.
    (c) For the purpose of this subpart, customers are defined as 
billing units or service connections to which water is delivered by a 
community water system.
    (d) For the purpose of this subpart, detected means: at or above the 
levels prescribed by Sec.  141.23(a)(4) for inorganic contaminants, at 
or above the levels prescribed by Sec.  141.24(f)(7) for the 
contaminants listed in Sec.  141.61(a), at or above the levels 
prescribed by Sec.  141.24(h)(18) for the contaminants listed in Sec.  
141.61(c), at or above the levels prescribed by Sec.  141.131(b)(2)(iv) 
for the contaminants or contaminant groups listed in Sec.  141.64, and 
at or above the levels prescribed by Sec.  141.25(c) for radioactive 
contaminants.
    (e) A State that has primary enforcement responsibility may adopt by 
rule, after notice and comment, alternative requirements for the form 
and content of the reports. The alternative requirements must provide 
the same type and amount of information as required by Sec. Sec.  
141.153 and 141.154, and must be designed to achieve an equivalent level 
of

[[Page 595]]

public information and education as would be achieved under this 
subpart.
    (f) For purpose of Sec. Sec.  141.154 and 141.155 of this subpart, 
the term ``primacy agency'' refers to the State or tribal government 
entity that has jurisdiction over, and primary enforcement 
responsibility for, public water systems, even if that government does 
not have interim or final primary enforcement responsibility for this 
rule. Where the State or tribe does not have primary enforcement 
responsibility for public water systems, the term ``primacy agency'' 
refers to the appropriate EPA regional office.

[63 FR 44526, Aug. 19, 1998, as amended at 71 FR 483, Jan. 4, 2006]



Sec.  141.152  Effective dates.

    (a) The regulations in this subpart shall take effect on September 
18, 1998.
    (b) Each existing community water system must deliver its first 
report by October 19, 1999, its second report by July 1, 2000, and 
subsequent reports by July 1 annually thereafter. The first report must 
contain data collected during, or prior to, calendar year 1998 as 
prescribed in Sec.  141.153(d)(3). Each report thereafter must contain 
data collected during, or prior to, the previous calendar year.
    (c) A new community water system must deliver its first report by 
July 1 of the year after its first full calendar year in operation and 
annually thereafter.
    (d) A community water system that sells water to another community 
water system must deliver the applicable information required in Sec.  
141.153 to the buyer system:
    (1) No later than April 19, 1999, by April 1, 2000, and by April 1 
annually thereafter or
    (2) On a date mutually agreed upon by the seller and the purchaser, 
and specifically included in a contract between the parties.



Sec.  141.153  Content of the reports.

    (a) Each community water system must provide to its customers an 
annual report that contains the information specified in this section 
and Sec.  141.154.
    (b) Information on the source of the water delivered:
    (1) Each report must identify the source(s) of the water delivered 
by the community water system by providing information on:
    (i) The type of the water: e.g., surface water, ground water; and
    (ii) The commonly used name (if any) and location of the body (or 
bodies) of water.
    (2) If a source water assessment has been completed, the report must 
notify consumers of the availability of this information and the means 
to obtain it. In addition, systems are encouraged to highlight in the 
report significant sources of contamination in the source water area if 
they have readily available information. Where a system has received a 
source water assessment from the primacy agency, the report must include 
a brief summary of the system's susceptibility to potential sources of 
contamination, using language provided by the primacy agency or written 
by the operator.
    (c) Definitions. (1) Each report must include the following 
definitions:
    (i) Maximum Contaminant Level Goal or MCLG: The level of a 
contaminant in drinking water below which there is no known or expected 
risk to health. MCLGs allow for a margin of safety.
    (ii) Maximum Contaminant Level or MCL: The highest level of a 
contaminant that is allowed in drinking water. MCLs are set as close to 
the MCLGs as feasible using the best available treatment technology.
    (2) A report for a community water system operating under a variance 
or an exemption issued under Sec.  1415 or 1416 of SDWA must include the 
following definition: Variances and Exemptions: State or EPA permission 
not to meet an MCL or a treatment technique under certain conditions.
    (3) A report that contains data on contaminants that EPA regulates 
using any of the following terms must include the applicable 
definitions:
    (i) Treatment Technique: A required process intended to reduce the 
level of a contaminant in drinking water.
    (ii) Action Level: The concentration of a contaminant which, if 
exceeded, triggers treatment or other requirements which a water system 
must follow.
    (iii) Maximum residual disinfectant level goal or MRDLG: The level 
of a

[[Page 596]]

drinking water disinfectant below which there is no known or expected 
risk to health. MRDLGs do not reflect the benefits of the use of 
disinfectants to control microbial contaminants.
    (iv) Maximum residual disinfectant level or MRDL: The highest level 
of a disinfectant allowed in drinking water. There is convincing 
evidence that addition of a disinfectant is necessary for control of 
microbial contaminants.
    (4) A report that contains information regarding a Level 1 or Level 
2 Assessment required under Subpart Y of this part must include the 
applicable definitions:
    (i) Level 1 Assessment: A Level 1 assessment is a study of the water 
system to identify potential problems and determine (if possible) why 
total coliform bacteria have been found in our water system.
    (ii) Level 2 Assessment: A Level 2 assessment is a very detailed 
study of the water system to identify potential problems and determine 
(if possible) why an E. coli MCL violation has occurred and/or why total 
coliform bacteria have been found in our water system on multiple 
occasions.
    (d) Information on detected contaminants.
    (1) This sub-section specifies the requirements for information to 
be included in each report for contaminants subject to mandatory 
monitoring (except Cryptosporidium). It applies to:
    (i) Contaminants subject to a MCL, action level, maximum residual 
disinfectant level, or treatment technique (regulated contaminants).
    (ii) Contaminants for which monitoring is required by Sec.  141.40 
(unregulated contaminants); and
    (iii) Disinfection by-products or microbial contaminants for which 
monitoring is required by Sec. Sec.  141.142 and 141.143, except as 
provided under paragraph (e)(1) of this section, and which are detected 
in the finished water.
    (2) The data relating to these contaminants must be displayed in one 
table or in several adjacent tables. Any additional monitoring results 
which a community water system chooses to include in its report must be 
displayed separately.
    (3) The data must be derived from data collected to comply with EPA 
and State monitoring and analytical requirements during calendar year 
1998 for the first report and subsequent calendar years thereafter 
except that:
    (i) Where a system is allowed to monitor for regulated contaminants 
less often than once a year, the table(s) must include the date and 
results of the most recent sampling and the report must include a brief 
statement indicating that the data presented in the report are from the 
most recent testing done in accordance with the regulations. No data 
older than 5 years need be included.
    (ii) Results of monitoring in compliance with Sec. Sec.  141.142 and 
141.143 need only be included for 5 years from the date of last sample 
or until any of the detected contaminants becomes regulated and subject 
to routine monitoring requirements, whichever comes first.
    (4) For detected regulated contaminants (listed in appendix A to 
this subpart), the table(s) must contain:
    (i) The MCL for that contaminant expressed as a number equal to or 
greater than 1.0 (as provided in appendix A to this subpart);
    (ii) The MCLG for that contaminant expressed in the same units as 
the MCL;
    (iii) If there is no MCL for a detected contaminant, the table must 
indicate that there is a treatment technique, or specify the action 
level, applicable to that contaminant, and the report must include the 
definitions for treatment technique and/or action level, as appropriate, 
specified in paragraph (c)(3) of this section;
    (iv) For contaminants subject to an MCL, except turbidity, total 
coliform, fecal coliform and E. coli, the highest contaminant level used 
to determine compliance with an NPDWR and the range of detected levels, 
as follows:
    (A) When compliance with the MCL is determined annually or less 
frequently: The highest detected level at any sampling point and the 
range of detected levels expressed in the same units as the MCL.
    (B) When compliance with the MCL is determined by calculating a 
running annual average of all samples taken at

[[Page 597]]

a monitoring location: the highest average of any of the monitoring 
locations and the range of all monitoring locations expressed in the 
same units as the MCL. For the MCLs for TTHM and HAA5 in Sec.  
141.64(b)(2), systems must include the highest locational running annual 
average for TTHM and HAA5 and the range of individual sample results for 
all monitoring locations expressed in the same units as the MCL. If more 
than one location exceeds the TTHM or HAA5 MCL, the system must include 
the locational running annual averages for all locations that exceed the 
MCL.
    (C) When compliance with the MCL is determined on a system-wide 
basis by calculating a running annual average of all samples at all 
monitoring locations: the average and range of detection expressed in 
the same units as the MCL. The system is required to include individual 
sample results for the IDSE conducted under subpart U of this part when 
determining the range of TTHM and HAA5 results to be reported in the 
annual consumer confidence report for the calendar year that the IDSE 
samples were taken.

    Note to paragraph (d)(4)(iv): When rounding of results to determine 
compliance with the MCL is allowed by the regulations, rounding should 
be done prior to multiplying the results by the factor listed in 
appendix A of this subpart.

    (v) For turbidity.
    (A) When it is reported pursuant to Sec.  141.13: The highest 
average monthly value.
    (B) When it is reported pursuant to the requirements of Sec.  
141.71: the highest monthly value. The report should include an 
explanation of the reasons for measuring turbidity.
    (C) When it is reported pursuant to Sec.  141.73 or Sec.  141.173 or 
Sec.  141.551: the highest single measurement and the lowest monthly 
percentage of samples meeting the turbidity limits specified in Sec.  
141.73 or Sec.  141.173, or Sec.  141.551 for the filtration technology 
being used. The report should include an explanation of the reasons for 
measuring turbidity;
    (vi) For lead and copper: the 90th percentile value of the most 
recent round of sampling and the number of sampling sites exceeding the 
action level;
    (vii) For total coliform analytical results until March 31, 2016:
    (A) The highest monthly number of positive samples for systems 
collecting fewer than 40 samples per month; or
    (B) The highest monthly percentage of positive samples for systems 
collecting at least 40 samples per month;
    (viii) For fecal coliform and E. coli until March 31, 2016: The 
total number of positive samples;
    (ix) The likely source(s) of detected contaminants to the best of 
the operator's knowledge. Specific information regarding contaminants 
may be available in sanitary surveys and source water assessments, and 
should be used when available to the operator. If the operator lacks 
specific information on the likely source, the report must include one 
or more of the typical sources for that contaminant listed in appendix A 
to this subpart that is most applicable to the system.
    (x) For E. coli analytical results under subpart Y: The total number 
of positive samples.
    (5) If a community water system distributes water to its customers 
from multiple hydraulically independent distribution systems that are 
fed by different raw water sources, the table should contain a separate 
column for each service area and the report should identify each 
separate distribution system. Alternatively, systems could produce 
separate reports tailored to include data for each service area.
    (6) The table(s) must clearly identify any data indicating 
violations of MCLs, MRDLs, or treatment techniques, and the report must 
contain a clear and readily understandable explanation of the violation 
including: the length of the violation, the potential adverse health 
effects, and actions taken by the system to address the violation. To 
describe the potential health effects, the system must use the relevant 
language of appendix A to this subpart.
    (7) For detected unregulated contaminants for which monitoring is 
required (except Cryptosporidium), the table(s) must contain the average 
and range at which the contaminant was detected. The report may include 
a brief explanation of the reasons for

[[Page 598]]

monitoring for unregulated contaminants.
    (e) Information on Cryptosporidium, radon, and other contaminants:
    (1) If the system has performed any monitoring for Cryptosporidium, 
including monitoring performed to satisfy the requirements of Sec.  
141.143, which indicates that Cryptosporidium may be present in the 
source water or the finished water, the report must include:
    (i) A summary of the results of the monitoring; and
    (ii) An explanation of the significance of the results.
    (2) If the system has performed any monitoring for radon which 
indicates that radon may be present in the finished water, the report 
must include:
    (i) The results of the monitoring; and
    (ii) An explanation of the significance of the results.
    (3) If the system has performed additional monitoring which 
indicates the presence of other contaminants in the finished water, EPA 
strongly encourages systems to report any results which may indicate a 
health concern. To determine if results may indicate a health concern, 
EPA recommends that systems find out if EPA has proposed an NPDWR or 
issued a health advisory for that contaminant by calling the Safe 
Drinking Water Hotline (800-426-4791). EPA considers detects above a 
proposed MCL or health advisory level to indicate possible health 
concerns. For such contaminants, EPA recommends that the report include:
    (i) The results of the monitoring; and
    (ii) An explanation of the significance of the results noting the 
existence of a health advisory or a proposed regulation.
    (f) Compliance with NPDWR. In addition to the requirements of Sec.  
141.153(d)(6), the report must note any violation that occurred during 
the year covered by the report of a requirement listed below, and 
include a clear and readily understandable explanation of the violation, 
any potential adverse health effects, and the steps the system has taken 
to correct the violation.
    (1) Monitoring and reporting of compliance data;
    (2) Filtration and disinfection prescribed by subpart H of this 
part. For systems which have failed to install adequate filtration or 
disinfection equipment or processes, or have had a failure of such 
equipment or processes which constitutes a violation, the report must 
include the following language as part of the explanation of potential 
adverse health effects: Inadequately treated water may contain disease-
causing organisms. These organisms include bacteria, viruses, and 
parasites which can cause symptoms such as nausea, cramps, diarrhea, and 
associated headaches.
    (3) Lead and copper control requirements prescribed by subpart I of 
this part. For systems that fail to take one or more actions prescribed 
by Sec. Sec.  141.80(d), 141.81, 141.82, 141.83 or 141.84, the report 
must include the applicable language of appendix A to this subpart for 
lead, copper, or both.
    (4) Treatment techniques for Acrylamide and Epichlorohydrin 
prescribed by subpart K of this part. For systems that violate the 
requirements of subpart K of this part, the report must include the 
relevant language from appendix A to this subpart.
    (5) Recordkeeping of compliance data.
    (6) Special monitoring requirements prescribed by Sec. Sec.  141.40 
and 141.41; and
    (7) Violation of the terms of a variance, an exemption, or an 
administrative or judicial order.
    (g) Variances and Exemptions. If a system is operating under the 
terms of a variance or an exemption issued under Sec.  1415 or 1416 of 
SDWA, the report must contain:
    (1) An explanation of the reasons for the variance or exemption;
    (2) The date on which the variance or exemption was issued;
    (3) A brief status report on the steps the system is taking to 
install treatment, find alternative sources of water, or otherwise 
comply with the terms and schedules of the variance or exemption; and
    (4) A notice of any opportunity for public input in the review, or 
renewal, of the variance or exemption.
    (h) Additional information:
    (1) The report must contain a brief explanation regarding 
contaminants which may reasonably be expected to be found in drinking 
water including bottled water. This explanation may

[[Page 599]]

include the language of paragraphs (h)(1) (i) through (iii) or systems 
may use their own comparable language. The report also must include the 
language of paragraph (h)(1)(iv) of this section.
    (i) The sources of drinking water (both tap water and bottled water) 
include rivers, lakes, streams, ponds, reservoirs, springs, and wells. 
As water travels over the surface of the land or through the ground, it 
dissolves naturally-occurring minerals and, in some cases, radioactive 
material, and can pick up substances resulting from the presence of 
animals or from human activity.
    (ii) Contaminants that may be present in source water include:
    (A) Microbial contaminants, such as viruses and bacteria, which may 
come from sewage treatment plants, septic systems, agricultural 
livestock operations, and wildlife.
    (B) Inorganic contaminants, such as salts and metals, which can be 
naturally-occurring or result from urban stormwater runoff, industrial 
or domestic wastewater discharges, oil and gas production, mining, or 
farming.
    (C) Pesticides and herbicides, which may come from a variety of 
sources such as agriculture, urban stormwater runoff, and residential 
uses.
    (D) Organic chemical contaminants, including synthetic and volatile 
organic chemicals, which are by-products of industrial processes and 
petroleum production, and can also come from gas stations, urban 
stormwater runoff, and septic systems.
    (E) Radioactive contaminants, which can be naturally-occurring or be 
the result of oil and gas production and mining activities.
    (iii) In order to ensure that tap water is safe to drink, EPA 
prescribes regulations which limit the amount of certain contaminants in 
water provided by public water systems. FDA regulations establish limits 
for contaminants in bottled water which must provide the same protection 
for public health.
    (iv) Drinking water, including bottled water, may reasonably be 
expected to contain at least small amounts of some contaminants. The 
presence of contaminants does not necessarily indicate that water poses 
a health risk. More information about contaminants and potential health 
effects can be obtained by calling the Environmental Protection Agency's 
Safe Drinking Water Hotline (800-426-4791).
    (2) The report must include the telephone number of the owner, 
operator, or designee of the community water system as a source of 
additional information concerning the report.
    (3) In communities with a large proportion of non-English speaking 
residents, as determined by the Primacy Agency, the report must contain 
information in the appropriate language(s) regarding the importance of 
the report or contain a telephone number or address where such residents 
may contact the system to obtain a translated copy of the report or 
assistance in the appropriate language.
    (4) The report must include information (e.g., time and place of 
regularly scheduled board meetings) about opportunities for public 
participation in decisions that may affect the quality of the water.
    (5) The systems may include such additional information as they deem 
necessary for public education consistent with, and not detracting from, 
the purpose of the report.
    (6) Systems required to comply with subpart S. (i) Any ground water 
system that receives notice from the State of a significant deficiency 
or notice from a laboratory of a fecal indicator-positive ground water 
source sample that is not invalidated by the State under Sec.  
141.402(d) must inform its customers of any significant deficiency that 
is uncorrected at the time of the next report or of any fecal indicator-
positive ground water source sample in the next report. The system must 
continue to inform the public annually until the State determines that 
particular significant deficiency is corrected or the fecal 
contamination in the ground water source is addressed under Sec.  
141.403(a). Each report must include the following elements.
    (A) The nature of the particular significant deficiency or the 
source of the fecal contamination (if the source is known) and the date 
the significant deficiency was identified by the State or the dates of 
the fecal indicator-positive ground water source samples;

[[Page 600]]

    (B) If the fecal contamination in the ground water source has been 
addressed under Sec.  141.403(a) and the date of such action;
    (C) For each significant deficiency or fecal contamination in the 
ground water source that has not been addressed under Sec.  141.403(a), 
the State-approved plan and schedule for correction, including interim 
measures, progress to date, and any interim measures completed; and
    (D) If the system receives notice of a fecal indicator-positive 
ground water source sample that is not invalidated by the State under 
Sec.  141.402(d), the potential health effects using the health effects 
language of Appendix A of subpart O.
    (ii) If directed by the State, a system with significant 
deficiencies that have been corrected before the next report is issued 
must inform its customers of the significant deficiency, how the 
deficiency was corrected, and the date of correction under paragraph 
(h)(6)(i) of this section.
    (7) Systems required to comply with subpart Y. (i) Any system 
required to comply with the Level 1 assessment requirement or a Level 2 
assessment requirement that is not due to an E. coli MCL violation must 
include in the report the text found in paragraph (h)(7)(i)(A) and 
paragraphs (h)(7)(i)(B) and (C) of this section as appropriate, filling 
in the blanks accordingly and the text found in paragraphs 
(h)(7)(i)(D)(1) and (2) of this section if appropriate.
    (A) Coliforms are bacteria that are naturally present in the 
environment and are used as an indicator that other, potentially 
harmful, waterborne pathogens may be present or that a potential pathway 
exists through which contamination may enter the drinking water 
distribution system. We found coliforms indicating the need to look for 
potential problems in water treatment or distribution. When this occurs, 
we are required to conduct assessment(s) to identify problems and to 
correct any problems that were found during these assessments.
    (B) During the past year we were required to conduct [INSERT NUMBER 
OF LEVEL 1ASSESSMENTS] Level 1 assessment(s). [INSERT NUMBER OF LEVEL 1 
ASSESSMENTS] Level 1 assessment(s) were completed. In addition, we were 
required to take [INSERT NUMBER OF CORRECTIVE ACTIONS] corrective 
actions and we completed [INSERT NUMBER OF CORRECTIVE ACTIONS] of these 
actions.
    (C) During the past year [INSERT NUMBER OF LEVEL 2 ASSESSMENTS] 
Level 2 assessments were required to be completed for our water system. 
[INSERT NUMBER OF LEVEL 2 ASSESSMENTS] Level 2 assessments were 
completed. In addition, we were required to take [INSERT NUMBER OF 
CORRECTIVE ACTIONS] corrective actions and we completed [INSERT NUMBER 
OF CORRECTIVE ACTIONS] of these actions.
    (D) Any system that has failed to complete all the required 
assessments or correct all identified sanitary defects, is in violation 
of the treatment technique requirement and must also include one or both 
of the following statements, as appropriate:
    (1) During the past year we failed to conduct all of the required 
assessment(s).
    (2) During the past year we failed to correct all identified defects 
that were found during the assessment.
    (ii) Any system required to conduct a Level 2 assessment due to an 
E. coli MCL violation must include in the report the text found in 
paragraphs (h)(7)(ii)(A) and (B) of this section, filling in the blanks 
accordingly and the text found in paragraphs (h)(7)(ii)(C)(1) and (2) of 
this section, if appropriate.
    (A) E. coli are bacteria whose presence indicates that the water may 
be contaminated with human or animal wastes. Human pathogens in these 
wastes can cause short-term effects, such as diarrhea, cramps, nausea, 
headaches, or other symptoms. They may pose a greater health risk for 
infants, young children, the elderly, and people with severely 
compromised immune systems. We found E. coli bacteria, indicating the 
need to look for potential problems in water treatment or distribution. 
When this occurs, we are required to conduct assessment(s) to identify 
problems and to correct any problems that were found during these 
assessments.

[[Page 601]]

    (B) We were required to complete a Level 2 assessment because we 
found E. coli in our water system. In addition, we were required to take 
[INSERT NUMBER OF CORRECTIVE ACTIONS] corrective actions and we 
completed [INSERT NUMBER OF CORRECTIVE ACTIONS] of these actions.
    (C) Any system that has failed to complete the required assessment 
or correct all identified sanitary defects, is in violation of the 
treatment technique requirement and must also include one or both of the 
following statements, as appropriate:
    (1) We failed to conduct the required assessment.
    (2) We failed to correct all sanitary defects that were identified 
during the assessment that we conducted.
    (iii) If a system detects E. coli and has violated the E. coli MCL, 
in addition to completing the table as required in paragraph (d)(4) of 
this section, the system must include one or more of the following 
statements to describe any noncompliance, as applicable:
    (A) We had an E. coli-positive repeat sample following a total 
coliform-positive routine sample.
    (B) We had a total coliform-positive repeat sample following an E. 
coli-positive routine sample.
    (C) We failed to take all required repeat samples following an E. 
coli-positive routine sample.
    (D) We failed to test for E. coli when any repeat sample tests 
positive for total coliform.
    (iv) If a system detects E. coli and has not violated the E. coli 
MCL, in addition to completing the table as required in paragraph (d)(4) 
of this section, the system may include a statement that explains that 
although they have detected E. coli, they are not in violation of the E. 
coli MCL.

[63 FR 44526, Aug. 19, 1998, as amended at 63 FR 69516, Dec. 16, 1998; 
64 FR 34733, June 29, 1999; 65 FR 26022, May 4, 2000; 67 FR 1836, Jan. 
14, 2002; 71 FR 483, Jan. 4, 2006; 71 FR 65651, Nov. 8, 2006; 78 FR 
10348, Feb. 13, 2013]



Sec.  141.154  Required additional health information.

    (a) All reports must prominently display the following language: 
Some people may be more vulnerable to contaminants in drinking water 
than the general population. Immuno-compromised persons such as persons 
with cancer undergoing chemotherapy, persons who have undergone organ 
transplants, people with HIV/AIDS or other immune system disorders, some 
elderly, and infants can be particularly at risk from infections. These 
people should seek advice about drinking water from their health care 
providers. EPA/CDC guidelines on appropriate means to lessen the risk of 
infection by Cryptosporidium and other microbial contaminants are 
available from the Safe Drinking Water Hotline (800-426-4791).
    (b) Ending in the report due by July 1, 2001, a system which detects 
arsenic at levels above 0.025 mg/L, but below the 0.05 mg/L, and 
beginning in the report due by July 1, 2002, a system that detects 
arsenic above 0.005 mg/L and up to and including 0.010 mg/L:
    (1) Must include in its report a short informational statement about 
arsenic, using language such as: While your drinking water meets EPA's 
standard for arsenic, it does contain low levels of arsenic. EPA's 
standard balances the current understanding of arsenic's possible health 
effects against the costs of removing arsenic from drinking water. EPA 
continues to research the health effects of low levels of arsenic, which 
is a mineral known to cause cancer in humans at high concentrations and 
is linked to other health effects such as skin damage and circulatory 
problems.
    (2) May write its own educational statement, but only in 
consultation with the Primacy Agency.
    (c) A system which detects nitrate at levels above 5 mg/l, but below 
the MCL:
    (1) Must include a short informational statement about the impacts 
of nitrate on children using language such as: Nitrate in drinking water 
at levels above 10 ppm is a health risk for infants of less than six 
months of age. High nitrate levels in drinking water can cause blue baby 
syndrome. Nitrate levels may rise quickly for short periods of time 
because of rainfall or agricultural activity. If you are caring for an 
infant you should ask advice from your health care provider.

[[Page 602]]

    (2) May write its own educational statement, but only in 
consultation with the Primacy Agency.
    (d) Every report must include the following lead-specific 
information:
    (1) A short informational statement about lead in drinking water and 
its effects on children. The statement must include the following 
information:

If present, elevated levels of lead can cause serious health problems, 
especially for pregnant women and young children. Lead in drinking water 
is primarily from materials and components associated with service lines 
and home plumbing. [NAME OF UTILITY] is responsible for providing high 
quality drinking water, but cannot control the variety of materials used 
in plumbing components. When your water has been sitting for several 
hours, you can minimize the potential for lead exposure by flushing your 
tap for 30 seconds to 2 minutes before using water for drinking or 
cooking. If you are concerned about lead in your water, you may wish to 
have your water tested. Information on lead in drinking water, testing 
methods, and steps you can take to minimize exposure is available from 
the Safe Drinking Water Hotline or at http://www.epa.gov/safewater/lead.

    (2) A system may write its own educational statement, but only in 
consultation with the State.
    (e) Community water systems that detect TTHM above 0.080 mg/l, but 
below the MCL in Sec.  141.12, as an annual average, monitored and 
calculated under the provisions of Sec.  141.30, must include health 
effects language for TTHMs prescribed by appendix A.
    (f) Beginning in the report due by July 1, 2002, and ending January 
22, 2006, a community water system that detects arsenic above 0.010 mg/L 
and up to and including 0.05 mg/L must include the arsenic health 
effects language prescribed by appendix A to subpart O of this part.

[63 FR 44526, Aug. 19, 1998, as amended at 63 FR 69475, Dec. 16, 1998; 
64 FR 34733, June 29, 1999; 65 FR 26023, May 4, 2000; 66 FR 7064, Jan. 
22, 2001; 68 FR 14506, Mar. 25, 2003; 72 FR 57820, Oct. 10, 2007]



Sec.  141.155  Report delivery and recordkeeping.

    (a) Except as provided in paragraph (g) of this section, each 
community water system must mail or otherwise directly deliver one copy 
of the report to each customer.
    (b) The system must make a good faith effort to reach consumers who 
do not get water bills, using means recommended by the primacy agency. 
EPA expects that an adequate good faith effort will be tailored to the 
consumers who are served by the system but are not bill-paying 
customers, such as renters or workers. A good faith effort to reach 
consumers would include a mix of methods appropriate to the particular 
system such as: Posting the reports on the Internet; mailing to postal 
patrons in metropolitan areas; advertising the availability of the 
report in the news media; publication in a local newspaper; posting in 
public places such as cafeterias or lunch rooms of public buildings; 
delivery of multiple copies for distribution by single-biller customers 
such as apartment buildings or large private employers; delivery to 
community organizations.
    (c) No later than the date the system is required to distribute the 
report to its customers, each community water system must mail a copy of 
the report to the primacy agency, followed within 3 months by a 
certification that the report has been distributed to customers, and 
that the information is correct and consistent with the compliance 
monitoring data previously submitted to the primacy agency.
    (d) No later than the date the system is required to distribute the 
report to its customers, each community water system must deliver the 
report to any other agency or clearinghouse identified by the primacy 
agency.
    (e) Each community water system must make its reports available to 
the public upon request.
    (f) Each community water system serving 100,000 or more persons must 
post its current year's report to a publicly-accessible site on the 
Internet.
    (g) The Governor of a State or his designee, or the Tribal Leader 
where the tribe has met the eligibility requirements contained in Sec.  
142.72 for the purposes of waiving the mailing requirement, can waive 
the requirement of paragraph (a) of this section for community water 
systems serving fewer than 10,000 persons. In consultation with the 
tribal government, the Regional Administrator may waive the requirement 
of Sec.  141.155(a) in areas in

[[Page 603]]

Indian country where no tribe has been deemed eligible.
    (1) Such systems must:
    (i) Publish the reports in one or more local newspapers serving the 
area in which the system is located;
    (ii) Inform the customers that the reports will not be mailed, 
either in the newspapers in which the reports are published or by other 
means approved by the State; and
    (iii) Make the reports available to the public upon request.
    (2) Systems serving 500 or fewer persons may forego the requirements 
of paragraphs (g)(1)(i) and (ii) of this section if they provide notice 
at least once per year to their customers by mail, door-to-door delivery 
or by posting in an appropriate location that the report is available 
upon request.
    (h) Any system subject to this subpart must retain copies of its 
Consumer Confidence Report for no less than 3 years.

[63 FR 44526, Aug. 19, 1998, as amended at 65 FR 26023, May 4, 2000]

[[Page 604]]

       Appendix A to Subpart O of Part 141--Regulated Contaminants

--------------------------------------------------------------------------------------------------------------------------------------------------------
                                  Traditional MCL     To convert for                                            Major sources in       Health effects
      Contaminant (units)             in mg/L        CCR, multiply by   MCL in CCR units         MCLG            drinking water           language
--------------------------------------------------------------------------------------------------------------------------------------------------------
Microbiological contaminants:
    Total Coliform Bacteria      MCL (systems that  .................  MCL (systems that  0.................  Naturally present in  Coliforms are
     [dagger].                    collect =40 samples/                       eq>=40 samples/                                              naturally present
                                  month) 5% of                          month) 5% of                                                 in the environment
                                  monthly samples                       monthly samples                                              and are used as an
                                  are positive;                         are positive;                                                indicator that
                                  (systems that                         (systems that                                                other, potentially-
                                  collect <40                           collect <40                                                  harmful, bacteria
                                  samples/month) 1                      samples/month) 1                                             may be present.
                                  positive monthly                      positive monthly                                             Coliforms were
                                  sample.                               sample..                                                     found in more
                                                                                                                                     samples than
                                                                                                                                     allowed and this
                                                                                                                                     was a warning of
                                                                                                                                     potential problems.
    Total Coliform Bacteria      TT...............  .................  TT...............  N/A...............  Naturally present in  Use language found
     [Dagger].                                                                                                 the environment.      in Sec.
                                                                                                                                     141.153(h)(7)(i)(A)
Fecal coliform and E. coli       0................  .................  0................  0.................  Human and animal      Fecal coliforms and
 [dagger].                                                                                                     fecal waste.          E. coli are
                                                                                                                                     bacteria whose
                                                                                                                                     presence indicates
                                                                                                                                     that the water may
                                                                                                                                     be contaminated
                                                                                                                                     with human or
                                                                                                                                     animal wastes.
                                                                                                                                     Microbes in these
                                                                                                                                     wastes can cause
                                                                                                                                     short-term effects,
                                                                                                                                     such as diarrhea,
                                                                                                                                     cramps, nausea,
                                                                                                                                     headaches, or other
                                                                                                                                     symptoms. They may
                                                                                                                                     pose a special
                                                                                                                                     health risk for
                                                                                                                                     infants, young
                                                                                                                                     children, some of
                                                                                                                                     the elderly, and
                                                                                                                                     people with
                                                                                                                                     severely
                                                                                                                                     compromised immune
                                                                                                                                     systems.

[[Page 605]]

 
E. coli [Dagger]...............  Routine and        .................  Routine and        0.................  Human and animal      E. coli are bacteria
                                  repeat samples                        repeat samples                         fecal waste.          whose presence
                                  are total                             are total                                                    indicates that the
                                  coliform-                             coliform-                                                    water may be
                                  positive and                          positive and                                                 contaminated with
                                  either is E.                          either is E.                                                 human or animal
                                  coli-positive or                      coli-positive or                                             wastes. Human
                                  system fails to                       system fails to                                              pathogens in these
                                  take repeat                           take repeat                                                  wastes can cause
                                  samples                               samples                                                      short-term effects,
                                  following E.                          following E.                                                 such as diarrhea,
                                  coli-positive                         coli-positive                                                cramps, nausea,
                                  routine sample                        routine sample                                               headaches, or other
                                  or system fails                       or system fails                                              symptoms. They may
                                  to analyze total                      to analyze total                                             pose a greater
                                  coliform-                             coliform-                                                    health risk for
                                  positive repeat                       positive repeat                                              infants, young
                                  sample for E.                         sample for E.                                                children, the
                                  coli.                                 coli.                                                        elderly, and people
                                                                                                                                     with severely-
                                                                                                                                     compromised immune
                                                                                                                                     systems.
    Fecal Indicators             TT...............  .................  TT...............  N/A...............  Human and animal      Fecal indicators are
     (enterococci or coliphage).                                                                               fecal waste.          microbes whose
                                                                                                                                     presence indicates
                                                                                                                                     that the water may
                                                                                                                                     be contaminated
                                                                                                                                     with human or
                                                                                                                                     animal wastes.
                                                                                                                                     Microbes in these
                                                                                                                                     wastes can cause
                                                                                                                                     short-term health
                                                                                                                                     effects, such as
                                                                                                                                     diarrhea, cramps,
                                                                                                                                     nausea, headaches,
                                                                                                                                     or other symptoms.
                                                                                                                                     They may pose a
                                                                                                                                     special health risk
                                                                                                                                     for infants, young
                                                                                                                                     children, some of
                                                                                                                                     the elderly, and
                                                                                                                                     people with
                                                                                                                                     severely
                                                                                                                                     compromised immune
                                                                                                                                     systems.
    Total organic carbon (ppm).  TT...............  .................  TT...............  N/A...............  Naturally present in  Total organic carbon
                                                                                                               the environment.      (TOC) has no health
                                                                                                                                     effects. However,
                                                                                                                                     total organic
                                                                                                                                     carbon provides a
                                                                                                                                     medium for the
                                                                                                                                     formation of
                                                                                                                                     disinfection by
                                                                                                                                     products. These
                                                                                                                                     byproducts include
                                                                                                                                     trihalomethanes
                                                                                                                                     (THMs) and
                                                                                                                                     haloacetic acids
                                                                                                                                     (HAAs). Drinking
                                                                                                                                     water containing
                                                                                                                                     these byproducts in
                                                                                                                                     excess of the MCL
                                                                                                                                     may lead to adverse
                                                                                                                                     health effects,
                                                                                                                                     liver or kidney
                                                                                                                                     problems, or
                                                                                                                                     nervous system
                                                                                                                                     effects, and may
                                                                                                                                     lead to an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.

[[Page 606]]

 
    Turbidity (NTU)............  TT...............  .................  TT...............  N/A...............  Soil runoff.........  Turbidity has no
                                                                                                                                     health effects.
                                                                                                                                     However, turbidity
                                                                                                                                     can interfere with
                                                                                                                                     disinfection and
                                                                                                                                     provide a medium
                                                                                                                                     for microbial
                                                                                                                                     growth. Turbidity
                                                                                                                                     may indicate the
                                                                                                                                     presence of disease-
                                                                                                                                     causing organisms.
                                                                                                                                     These organisms
                                                                                                                                     include bacteria,
                                                                                                                                     viruses, and
                                                                                                                                     parasites that can
                                                                                                                                     cause symptoms such
                                                                                                                                     as nausea, cramps,
                                                                                                                                     diarrhea and
                                                                                                                                     associated
                                                                                                                                     headaches.
Radioactive contaminants:
    Beta/photon emitters (mrem/  4 mrem/yr........  -................  4................  0.................  Decay of natural and  Certain minerals are
     yr).                                                                                                      man-made deposits.    radioactive and may
                                                                                                                                     emit forms of
                                                                                                                                     radiation known as
                                                                                                                                     photons and beta
                                                                                                                                     radiation. Some
                                                                                                                                     people who drink
                                                                                                                                     water containing
                                                                                                                                     beta particle and
                                                                                                                                     photon
                                                                                                                                     radioactivity in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Alpha emitters (pCi/L).....  15 pCi/L.........  -................  15...............  0.................  Erosion of natural    Certain minerals are
                                                                                                               deposits.             radioactive and may
                                                                                                                                     emit a form of
                                                                                                                                     radiation known as
                                                                                                                                     alpha radiation.
                                                                                                                                     Some people who
                                                                                                                                     drink water
                                                                                                                                     containing alpha
                                                                                                                                     emitters in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years may have
                                                                                                                                     an increased risk
                                                                                                                                     of getting cancer.
    Combined radium (pCi/L)....  5 pCi/L..........  -................  5................  0.................  Erosion of natural    Some people who
                                                                                                               deposits.             drink water
                                                                                                                                     containing radium-
                                                                                                                                     226 or -228 in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Uranium (pCi/L)............  30 [micro]g/L....  -................  30...............  0.................  Erosion of natural    Some people who
                                                                                                               deposits.             drink water
                                                                                                                                     containing uranium
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer and
                                                                                                                                     kidney toxicity.

[[Page 607]]

 
Inorganic contaminants:
    Antimony (ppb).............  .006.............  1000.............  6................  6.................  Discharge from        Some people who
                                                                                                               petroleum             drink water
                                                                                                               refineries; fire      containing antimony
                                                                                                               retardants;           well in excess of
                                                                                                               ceramics;             the MCL over many
                                                                                                               electronics; solder.  years could
                                                                                                                                     experience
                                                                                                                                     increases in blood
                                                                                                                                     cholesterol and
                                                                                                                                     decreases in blood
                                                                                                                                     sugar.
    Arsenic (ppb)..............  \1\ 0.010........  1000.............  \1\ 10...........  \1\ 0.............  Erosion of natural    Some people who
                                                                                                               deposits; Runoff      drink water
                                                                                                               from orchards;        containing arsenic
                                                                                                               Runoff from glass     in excess of the
                                                                                                               and electronics       MCL over many years
                                                                                                               production wastes.    could experience
                                                                                                                                     skin damage or
                                                                                                                                     problems with their
                                                                                                                                     circulatory system,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Asbestos (MFL).............  7 MFL............  .................  7................  7.................  Decay of asbestos     Some people who
                                                                                                               cement water mains;   drink water
                                                                                                               Erosion of natural    containing asbestos
                                                                                                               deposits.             in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     developing benign
                                                                                                                                     intestinal polyps.
    Barium (ppm)...............  2................  .................  2................  2.................  Discharge of          Some people who
                                                                                                               drilling wastes;      drink water
                                                                                                               Discharge from        containing barium
                                                                                                               metal refineries;     in excess of the
                                                                                                               Erosion of natural    MCL over many years
                                                                                                               deposits.             could experience an
                                                                                                                                     increase in their
                                                                                                                                     blood pressure.
    Beryllium (ppb)............  .004.............  1000.............  4................  4.................  Discharge from metal  Some people who
                                                                                                               refineries and coal-  drink water
                                                                                                               burning factories;    containing
                                                                                                               Discharge from        beryllium well in
                                                                                                               electrical,           excess of the MCL
                                                                                                               aerospace, and        over many years
                                                                                                               defense industries.   could develop
                                                                                                                                     intestinal lesions
    Bromate (ppb)..............  .010.............  1000.............  10...............  0.................  By-product of         Some people who
                                                                                                               drinkig water         drink water of
                                                                                                               disinfection.         containing bromate
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Cadmium (ppb)..............  .005.............  1000.............  5................  5.................  Corrosion of          Some people who
                                                                                                               galvanized pipes;     drink water
                                                                                                               Erosion of natural    containing cadmium
                                                                                                               deposits; Discharge   in excess of the
                                                                                                               from metal            MCL over many years
                                                                                                               refineries; Runoff    could experience
                                                                                                               from waste            kidney damage.
                                                                                                               batteries and
                                                                                                               paints.

[[Page 608]]

 
    Chloramines (ppm)..........  MRDL = 4.........  .................  MRDL = 4.........  MRDLG = 4.........  Water additive used   Some people who use
                                                                                                               to control microbes.  water containing
                                                                                                                                     chloramines well in
                                                                                                                                     excess of the MRDL
                                                                                                                                     could experience
                                                                                                                                     irritating effects
                                                                                                                                     to their eyes and
                                                                                                                                     nose. Some people
                                                                                                                                     who drink water
                                                                                                                                     containing
                                                                                                                                     chloramines well in
                                                                                                                                     excess of the MRDL
                                                                                                                                     could experience
                                                                                                                                     stomach discomfort
                                                                                                                                     or anemia.
    Chlorine (ppm).............  MRDL = 4.........  .................  MRDL = 4.........  MRDLG = 4.........  Water additive used   Some people who use
                                                                                                               to control microbes.  water containing
                                                                                                                                     chlorine well in
                                                                                                                                     excess of the MRDL
                                                                                                                                     could experience
                                                                                                                                     irritating effects
                                                                                                                                     to their eyes and
                                                                                                                                     nose. Some people
                                                                                                                                     who drink water
                                                                                                                                     containing chlorine
                                                                                                                                     well in excess of
                                                                                                                                     the MRDL could
                                                                                                                                     experience stomach
                                                                                                                                     discomfort.
    Chlorine dioxide (ppb).....  MRDL = .8........  1000.............  MRDL = 800.......  MRDLG = 800.......  Water additive used   Some infants and
                                                                                                               to control micorbes.  young children who
                                                                                                                                     drink water
                                                                                                                                     chlorine dioxide in
                                                                                                                                     excess of the MRDL
                                                                                                                                     could experience
                                                                                                                                     nervous system
                                                                                                                                     effects. Similar
                                                                                                                                     effects may occur
                                                                                                                                     in fetuses of
                                                                                                                                     pregnant women who
                                                                                                                                     drink water
                                                                                                                                     containing chlorine
                                                                                                                                     dioxide in excess
                                                                                                                                     of the MRDL. Some
                                                                                                                                     people may
                                                                                                                                     experience anemia.
    Chlorite (ppm).............  1................  .................  1................  0.8...............  By-product of         Some infants and
                                                                                                               drinking water        young children who
                                                                                                               disinfection.         drink water
                                                                                                                                     containing chlorite
                                                                                                                                     in excess of the
                                                                                                                                     MCL could
                                                                                                                                     experience nervous
                                                                                                                                     system effects.
                                                                                                                                     Similar effects may
                                                                                                                                     occur in fetuses of
                                                                                                                                     pregnant women who
                                                                                                                                     drink water
                                                                                                                                     containing chlorite
                                                                                                                                     in excess of the
                                                                                                                                     MCL. Some people
                                                                                                                                     may experience
                                                                                                                                     anemia.
    Chromium (ppb).............  .1...............  1000.............  100..............  100...............  Discharge from steel  Some people who use
                                                                                                               and pulp mills;       water containing
                                                                                                               Erosion of natural    chromium well in
                                                                                                               deposits.             excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     allergic
                                                                                                                                     dermatitis.

[[Page 609]]

 
    Copper (ppm)...............  AL = 1.3.........  .................  AL = 1.3.........  1.3...............  Corrosion of          Copper is an
                                                                                                               household plumbing    essential nutrient,
                                                                                                               systems; Erosion of   but some people who
                                                                                                               natural deposits.     drink water
                                                                                                                                     containing copper
                                                                                                                                     in excess of the
                                                                                                                                     action level over a
                                                                                                                                     relatively short
                                                                                                                                     amount of time
                                                                                                                                     could experience
                                                                                                                                     gastrointestinal
                                                                                                                                     distress. Some
                                                                                                                                     people who drink
                                                                                                                                     water containing
                                                                                                                                     copper in excess of
                                                                                                                                     the action level
                                                                                                                                     over many years
                                                                                                                                     could suffer liver
                                                                                                                                     or kidney damage.
                                                                                                                                     People with
                                                                                                                                     Wilson's disease
                                                                                                                                     should consult
                                                                                                                                     their personal
                                                                                                                                     doctor.
    Cyanide (ppb)..............  .2...............  1000.............  200..............  200...............  Discharge from steel/ Some people who
                                                                                                               metal factories;      drink water
                                                                                                               Discharge from        containing cyanide
                                                                                                               plastic and           well in excess of
                                                                                                               fertilizer            the MCL over many
                                                                                                               factories.            years could
                                                                                                                                     experience nerve
                                                                                                                                     damage or problems
                                                                                                                                     with their thyroid.
    Fluoride (ppm).............  4................  .................  4................  4.................  Erosion of natural    Some people who
                                                                                                               deposits; Water       drink water
                                                                                                               additive which        containing fluoride
                                                                                                               promotes strong       in excess of the
                                                                                                               teeth; Discharge      MCL over many years
                                                                                                               from fertilizer and   could get bone
                                                                                                               aluminum factories.   disease, including
                                                                                                                                     pain and tenderness
                                                                                                                                     of the bones.
                                                                                                                                     Fluoride in
                                                                                                                                     drinking water at
                                                                                                                                     half the MCL or
                                                                                                                                     more may cause
                                                                                                                                     mottling of
                                                                                                                                     children's teeth,
                                                                                                                                     usually in children
                                                                                                                                     less than nine
                                                                                                                                     years old.
                                                                                                                                     Mottling, also
                                                                                                                                     known as dental
                                                                                                                                     fluorosis, may
                                                                                                                                     include brown
                                                                                                                                     staining and/or
                                                                                                                                     pitting of the
                                                                                                                                     teeth, and occurs
                                                                                                                                     only in developing
                                                                                                                                     teeth before they
                                                                                                                                     erupt from the
                                                                                                                                     gums.
    Lead (ppb).................  AL = .015........  1000.............  AL = 15..........  0.................  Corrosion of          Infants and children
                                                                                                               household plumbing    who drink water
                                                                                                               systems; Erosion of   containing lead in
                                                                                                               natural deposits.     excess of the
                                                                                                                                     action level could
                                                                                                                                     experience delays
                                                                                                                                     in their physical
                                                                                                                                     or mental
                                                                                                                                     development.
                                                                                                                                     Children could show
                                                                                                                                     slight deficits in
                                                                                                                                     attention span and
                                                                                                                                     learning abilities.
                                                                                                                                     Adults who drink
                                                                                                                                     this water over
                                                                                                                                     many years could
                                                                                                                                     develop kidney
                                                                                                                                     problems or high
                                                                                                                                     blood pressure.

[[Page 610]]

 
    Mercury [inorganic] (ppb)..  .002.............  1000.............  2................  2.................  Erosion of natural    Some people who
                                                                                                               deposits; Dis         drink water
                                                                                                               charge from           containing
                                                                                                               refineries and        inorganic mercury
                                                                                                               factories; Runoff     well in excess of
                                                                                                               from landfills;       the MCL over many
                                                                                                               Runoff from           years could
                                                                                                               cropland.             experience kidney
                                                                                                                                     damage.
    Nitrate (ppm)..............  10...............  .................  10...............  10................  Runoff from           Infants below the
                                                                                                               fertilizer use;       age of six months
                                                                                                               Leaching from         who drink water
                                                                                                               septic tanks, sew     containing nitrate
                                                                                                               age; Erosion of       in excess of the
                                                                                                               natural deposits.     MCL could become
                                                                                                                                     seriously ill and,
                                                                                                                                     if untreated, may
                                                                                                                                     die. Symptoms
                                                                                                                                     include shortness
                                                                                                                                     of breath and blue
                                                                                                                                     baby syndrome.
    Nitrite (ppm)..............  1................  .................  1................  1.................  Runoff from           Infants below the
                                                                                                               fertilizer use;       age of six months
                                                                                                               Leaching from         who drink water
                                                                                                               septic tanks, sew     containing nitrite
                                                                                                               age; Erosion of       in excess of the
                                                                                                               natural deposits.     MCL could become
                                                                                                                                     seriously ill and,
                                                                                                                                     if untreated, may
                                                                                                                                     die. Symptoms
                                                                                                                                     include shortness
                                                                                                                                     of breath and blue
                                                                                                                                     baby syndrome.
    Selenium (ppb).............  .05..............  1000.............  50...............  50................  Discharge from        Selenium is an
                                                                                                               petroleum and metal   essential nutrient.
                                                                                                               refineries; Erosion   However, some
                                                                                                               of natural            people who drink
                                                                                                               deposits; Discharge   water containing
                                                                                                               from mines.           selenium in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years could
                                                                                                                                     experience hair or
                                                                                                                                     fingernail losses,
                                                                                                                                     numbness in fingers
                                                                                                                                     or toes, or
                                                                                                                                     problems with their
                                                                                                                                     circulation.
    Thallium (ppb).............  .002.............  1000.............  2................  0.5...............  Leaching from ore-    Some people who
                                                                                                               processing sites;     drink water
                                                                                                               Discharge from        containing thallium
                                                                                                               electronics, glass,   in excess of the
                                                                                                               and drug factories.   MCL over many years
                                                                                                                                     could experience
                                                                                                                                     hair loss, changes
                                                                                                                                     in their blood, or
                                                                                                                                     problems with their
                                                                                                                                     kidneys,
                                                                                                                                     intestines, or
                                                                                                                                     liver.
Synthetic organic contaminants
 including pesticides and
 herbicides:
    2,4-D (ppb)................  .07..............  1000.............  70...............  70................  Runoff from           Some people who
                                                                                                               herbicide used on     drink water
                                                                                                               row crops.            containing the weed
                                                                                                                                     killer 2,4-D well
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     kidneys, liver, or
                                                                                                                                     adrenal glands.

[[Page 611]]

 
    2,4,5-TP [Silvex](ppb).....  .05..............  1000.............  50...............  50................  Residue of banned     Some people who
                                                                                                               herbicide.            drink water
                                                                                                                                     containing silvex
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     liver problems.
    Acrylamide.................  TT...............  .................  TT...............  0.................  Added to water        Some people who
                                                                                                               during sewage/        drink water
                                                                                                               wastewater            containing high
                                                                                                               treatment.            levels of
                                                                                                                                     acrylamide over a
                                                                                                                                     long period of time
                                                                                                                                     could have problems
                                                                                                                                     with their nervous
                                                                                                                                     system or blood,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Alachlor (ppb).............  .002.............  1000.............  2................  0.................  Runoff from           Some people who
                                                                                                               herbicide used on     drink water
                                                                                                               row crops.            containing alachlor
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could have problems
                                                                                                                                     with their eyes,
                                                                                                                                     liver, kidneys, or
                                                                                                                                     spleen, or
                                                                                                                                     experience anemia,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Atrazine (ppb).............  .003.............  1000.............  3................  3.................  Runoff from           Some people who
                                                                                                               herbicide used on     drink water
                                                                                                               row crops.            containing atrazine
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience problems
                                                                                                                                     with their
                                                                                                                                     cardiovascular
                                                                                                                                     system or
                                                                                                                                     reproductive
                                                                                                                                     difficulties.
    Benzo(a)pyrene [PAH]         .0002............  1,000,000........  200..............  0.................  Leaching from         Some people who
     (nanograms/l).                                                                                            linings of water      drink water
                                                                                                               storage tanks and     containing
                                                                                                               distribution lines.   benzo(a)pyrene in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     experience
                                                                                                                                     reproductive
                                                                                                                                     difficulties and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Carbofuran (ppb)...........  .04..............  1000.............  40...............  40................  Leaching of soil      Some people who
                                                                                                               fumigant used on      drink water
                                                                                                               rice and alfalfa.     containing
                                                                                                                                     carbofuran in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     blood, or nervous
                                                                                                                                     or reproductive
                                                                                                                                     systems.
    Chlordane (ppb)............  .002.............  1000.............  2................  0.................  Residue of banned     Some people who
                                                                                                               termiticide.          drink water
                                                                                                                                     containing
                                                                                                                                     chlordane in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years could
                                                                                                                                     experience problems
                                                                                                                                     with their liver or
                                                                                                                                     nervous system, and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.

[[Page 612]]

 
    Dalapon (ppb)..............  .2...............  1000.............  200..............  200...............  Runoff from           Some people who
                                                                                                               herbicide used on     drink water
                                                                                                               rights of way.        containing dalapon
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience minor
                                                                                                                                     kidney changes.
    Di(2-ethylhexyl) adipate     .4...............  1000.............  400..............  400...............  Discharge from        Some people who
     (ppb).                                                                                                    chemical factories.   drink water
                                                                                                                                     containing di(2-
                                                                                                                                     ethylhexyl) adipate
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience toxic
                                                                                                                                     effects such as
                                                                                                                                     weight loss, liver
                                                                                                                                     enlargement or
                                                                                                                                     possible
                                                                                                                                     reproductive
                                                                                                                                     difficulties.
    Di(2-ethylhexyl) phthalate   .006.............  1000.............  6................  0.................  Discharge from        Some people who
     (ppb).                                                                                                    rubber and chemical   drink water
                                                                                                               factories.            containing di(2-
                                                                                                                                     ethylhexyl)
                                                                                                                                     phthalate well in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have problems with
                                                                                                                                     their liver, or
                                                                                                                                     experience
                                                                                                                                     reproductive
                                                                                                                                     difficulties, and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Dibromochloropropane (ppt).  .0002............  1,000,000........  200..............  0.................  Runoff/leaching from  Some people who
                                                                                                               soil fumigant used    drink water
                                                                                                               on soybeans,          containing DBCP in
                                                                                                               cotton, pineapples,   excess of the MCL
                                                                                                               and orchards.         over many years
                                                                                                                                     could experience
                                                                                                                                     reproductive
                                                                                                                                     problems and may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Dinoseb (ppb)..............  .007.............  1000.............  7................  7.................  Runoff from           Some people who
                                                                                                               herbicide used on     drink water
                                                                                                               soybeans and          containing dinoseb
                                                                                                               vegetables.           well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience
                                                                                                                                     reproductive
                                                                                                                                     difficulties.
    Diquat (ppb)...............  .02..............  1000.............  20...............  20................  Runoff from           Some people who
                                                                                                               herbicide use.        drink water
                                                                                                                                     containing diquat
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could get
                                                                                                                                     cataracts.
    Dioxin [2,3,7,8-TCDD] (ppq)  .00000003........  1,000,000, 000...  30...............  0.................  Emissions from waste  Some people who
                                                                                                               incineration and      drink water
                                                                                                               other combustion;     containing dioxin
                                                                                                               Discharge from        in excess of the
                                                                                                               chemical factories.   MCL over many years
                                                                                                                                     could experience
                                                                                                                                     reproductive
                                                                                                                                     difficulties and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.

[[Page 613]]

 
    Endothall (ppb)............  .1...............  1000.............  100..............  100...............  Runoff from           Some people who
                                                                                                               herbicide use.        drink water
                                                                                                                                     containing
                                                                                                                                     endothall in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years could
                                                                                                                                     experience problems
                                                                                                                                     with their stomach
                                                                                                                                     or intestines.
    Endrin (ppb)...............  .002.............  1000.............  2................  2.................  Residue of banned     Some people who
                                                                                                               insecticide.          drink water
                                                                                                                                     containing endrin
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     liver problems.
    Epichlorohydrin............  TT...............  .................  TT...............  0.................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories; An         containing high
                                                                                                               impurity of some      levels of
                                                                                                               water treatment       epichlorohydrin
                                                                                                               chemicals.            over a long period
                                                                                                                                     of time could
                                                                                                                                     experience stomach
                                                                                                                                     problems, and may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Ethylene dibromide (ppt)...  .00005...........  1,000,000........  50...............  0.................  Discharge from        Some people who
                                                                                                               petroleum             drink water
                                                                                                               refineries.           containing ethylene
                                                                                                                                     dibromide in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years could
                                                                                                                                     experience problems
                                                                                                                                     with their liver,
                                                                                                                                     stomach,
                                                                                                                                     reproductive
                                                                                                                                     system, or kidneys,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Glyphosate (ppb)...........  .7...............  1000.............  700..............  700...............  Runoff from           Some people who
                                                                                                               herbicide use.        drink water
                                                                                                                                     containing
                                                                                                                                     glyphosate in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     kidneys or
                                                                                                                                     reproductive
                                                                                                                                     difficulties.
    Heptachlor (ppt)...........  .0004............  1,000,000........  400..............  0.................  Residue of banned     Some people who
                                                                                                               pesticide.            drink water
                                                                                                                                     containing
                                                                                                                                     heptachlor in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     liver damage and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Heptachlor epoxide (ppt)...  .0002............  1,000,000........  200..............  0.................  Breakdown of          Some people who
                                                                                                               heptachlor.           drink water
                                                                                                                                     containing
                                                                                                                                     heptachlor epoxide
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     liver damage, and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.

[[Page 614]]

 
    Hexachlorobenzene (ppb)....  .001.............  1000.............  1................  0.................  Discharge from metal  Some people who
                                                                                                               refineries and        drink water
                                                                                                               agricultural          containing
                                                                                                               chemical factories.   hexachlorobenzene
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver or kidneys,
                                                                                                                                     or adverse
                                                                                                                                     reproductive
                                                                                                                                     effects, and may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Hexachlorocyclopentadiene    .05..............  1000.............  50...............  50................  Discharge from        Some people who
     (ppb).                                                                                                    chemical factories.   drink water
                                                                                                                                     containing
                                                                                                                                     hexachlorocyclopent
                                                                                                                                     adiene well in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     kidneys or stomach.
    Lindane (ppt)..............  .0002............  1,000,000........  200..............  200...............  Runoff/leaching from  Some people who
                                                                                                               insecticide used on   drink water
                                                                                                               cattle, lumber,       containing lindane
                                                                                                               gardens.              in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     kidneys or liver.
    Methoxychlor (ppb).........  .04..............  1000.............  40...............  40................  Runoff/leaching from  Some people who
                                                                                                               insecticide used on   drink water
                                                                                                               fruits, vegetables,   containing
                                                                                                               alfalfa, livestock.   methoxychlor in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     reproductive
                                                                                                                                     difficulties.
    Oxamyl [Vydate] (ppb)......  .2...............  1000.............  200..............  200...............  Runoff/leaching from  Some people who
                                                                                                               insecticide used on   drink water
                                                                                                               apples, potatoes      containing oxamyl
                                                                                                               and tomatoes.         in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     slight nervous
                                                                                                                                     system effects.
    PCBs [Polychlorinated        .0005............  1,000,000........  500..............  0.................  Runoff from           Some people who
     biphenyls] (ppt).                                                                                         landfills;            drink water
                                                                                                               Discharge of waste    containing PCBs in
                                                                                                               chemicals.            excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     changes in their
                                                                                                                                     skin, problems with
                                                                                                                                     their thymus gland,
                                                                                                                                     immune
                                                                                                                                     deficiencies, or
                                                                                                                                     reproductive or
                                                                                                                                     nervous system
                                                                                                                                     difficulties, and
                                                                                                                                     may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.

[[Page 615]]

 
    Pentachlorophenol (ppb)....  .001.............  1000.............  1................  0.................  Discharge from wood   Some people who
                                                                                                               preserving            drink water
                                                                                                               factories.            containing
                                                                                                                                     pentachlorophenol
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver or kidneys,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Picloram (ppb).............  .5...............  1000.............  500..............  500...............  Herbicide runoff....  Some people who
                                                                                                                                     drink water
                                                                                                                                     containing picloram
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver.
    Simazine (ppb).............  .004.............  1000.............  4................  4.................  Herbicide runoff....  Some people who
                                                                                                                                     drink water
                                                                                                                                     containing simazine
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     blood.
    Toxaphene (ppb)............  .003.............  1000.............  3................  0.................  Runoff/leaching from  Some people who
                                                                                                               insecticide used on   drink water
                                                                                                               cotton and cattle.    containing
                                                                                                                                     toxaphene in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years could
                                                                                                                                     have problems with
                                                                                                                                     their kidneys,
                                                                                                                                     liver, or thyroid,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
Volatile organic contaminants:
    Benzene (ppb)..............  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               factories; Leaching   drink water
                                                                                                               from gas storage      containing benzene
                                                                                                               tanks and landfills.  in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     anemia or a
                                                                                                                                     decrease in blood
                                                                                                                                     platelets, and may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Carbon tetrachloride (ppb).  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               chemical plants and   drink water
                                                                                                               other industrial      containing carbon
                                                                                                               activities.           tetrachloride in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver and may have
                                                                                                                                     an increased risk
                                                                                                                                     of getting cancer.
    Chlorobenzene (ppb)........  .1...............  1000.............  100..............  100...............  Discharge from        Some people who
                                                                                                               chemical and          drink water
                                                                                                               agricultural          containing
                                                                                                               chemical factories.   chlorobenzene in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver or kidneys.
    o-Dichlorobenzene (ppb)....  .6...............  1000.............  600..............  600...............  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing o-
                                                                                                                                     dichlorobenzene
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience problems
                                                                                                                                     with their liver,
                                                                                                                                     kidneys, or
                                                                                                                                     circulatory
                                                                                                                                     systems.

[[Page 616]]

 
    p-Dichlorobenzene (ppb)....  .075.............  1000.............  75...............  75................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing p-
                                                                                                                                     dichlorobenzene in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     anemia, damage to
                                                                                                                                     their liver,
                                                                                                                                     kidneys, or spleen,
                                                                                                                                     or changes in their
                                                                                                                                     blood.
    1,2-Dichloroethane (ppb)...  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing 1,2-
                                                                                                                                     dichloroethane in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    1,1-Dichloroethylene (ppb).  .007.............  1000.............  7................  7.................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing 1,1-
                                                                                                                                     dichloroethylene in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver.
    cis-1,2-Dichloroethylene     .07..............  1000.............  70...............  70................  Discharge from        Some people who
     (ppb).                                                                                                    industrial chemical   drink water
                                                                                                               factories.            containing cis-1,2-
                                                                                                                                     dichloroethylene in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver.
    trans-1,2-Dichloroethylene   .1...............  1000.............  100..............  100...............  Discharge from        Some people who
     (ppb).                                                                                                    industrial chemical   drink water
                                                                                                               factories.            containing trans-
                                                                                                                                     1,2-
                                                                                                                                     dichloroethylene
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience problems
                                                                                                                                     with their liver.
    Dichloromethane (ppb)......  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               pharmaceutical and    drink water
                                                                                                               chemical factories.   containing
                                                                                                                                     dichloromethane in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could have liver
                                                                                                                                     problems and may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    1,2-Dichloropropane (ppb)..  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing 1,2-
                                                                                                                                     dichloropropane in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Ethylbenzene (ppb).........  .7...............  1000.............  700..............  700...............  Discharge from        Some people who
                                                                                                               petroleum             drink water
                                                                                                               refineries.           containing
                                                                                                                                     ethylbenzene well
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver or kidneys.

[[Page 617]]

 
    Haloacetic Acids (HAA)       .060.............  1000.............  60...............  N/A...............  By-product of         Some people who
     (ppb).                                                                                                    drinking water        drink water
                                                                                                               disinfection.         containing
                                                                                                                                     haloacetic acids in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     have an increased
                                                                                                                                     risk of getting
                                                                                                                                     cancer.
    Styrene (ppb)..............  .1...............  1000.............  100..............  100...............  Discharge from        Some people who
                                                                                                               rubber and plastic    drink water
                                                                                                               factories; Leaching   containing styrene
                                                                                                               from landfills.       well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could have
                                                                                                                                     problems with their
                                                                                                                                     liver, kidneys, or
                                                                                                                                     circulatory system.
    Tetrachloroethylene (ppb)..  .005.............  1000.............  5................  0.................  Discharge from        Some people who
                                                                                                               factories and dry     drink water
                                                                                                               cleaners.             containing
                                                                                                                                     tetrachloroethylene
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could have problems
                                                                                                                                     with their liver,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    1,2,4-Trichlorobenzene       .07..............  1000.............  70...............  70................  Discharge from        Some people who
     (ppb).                                                                                                    textile-finishing     drink water
                                                                                                               factories.            containing 1,2,4-
                                                                                                                                     trichlorobenzene
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could
                                                                                                                                     experience changes
                                                                                                                                     in their adrenal
                                                                                                                                     glands.
    1,1,1-Trichloroethane (ppb)  .2...............  1000.............  200..............  200...............  Discharge from metal  Some people who
                                                                                                               degreasing sites      drink water
                                                                                                               and other factories.  containing 1,1,1-
                                                                                                                                     trichloroethane in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver, nervous
                                                                                                                                     system, or
                                                                                                                                     circulatory system.
    1,1,2-Trichloroethane (ppb)  .005.............  1000.............  5................  3.................  Discharge from        Some people who
                                                                                                               industrial chemical   drink water
                                                                                                               factories.            containing 1,1,2-
                                                                                                                                     trichloroethane
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could have
                                                                                                                                     problems with their
                                                                                                                                     liver, kidneys, or
                                                                                                                                     immune systems.
    Trichloroethylene (ppb)....  .005.............  1000.............  5................  0.................  Discharge from metal  Some people who
                                                                                                               degreasing sites      drink water
                                                                                                               and other factories.  containing
                                                                                                                                     trichloroethylene
                                                                                                                                     in excess of the
                                                                                                                                     MCL over many years
                                                                                                                                     could experience
                                                                                                                                     problems with their
                                                                                                                                     liver and may have
                                                                                                                                     an increased risk
                                                                                                                                     of getting cancer.

[[Page 618]]

 
    TTHMs [Total                 0.10/.080........  1000.............  100/80...........  N/A...............  By-product of         Some people who
     trihalomethanes] (ppb).                                                                                   drinking water        drink water
                                                                                                               disinfection.         containing
                                                                                                                                     trihalomethanes in
                                                                                                                                     excess of the MCL
                                                                                                                                     over many years may
                                                                                                                                     experience problems
                                                                                                                                     with their liver,
                                                                                                                                     kidneys, or central
                                                                                                                                     nervous systems,
                                                                                                                                     and may have an
                                                                                                                                     increased risk of
                                                                                                                                     getting cancer.
    Toluene (ppm)..............  1................  .................  1................  1.................  Discharge from        Some people who
                                                                                                               petroleum factories.  drink water
                                                                                                                                     containing toluene
                                                                                                                                     well in excess of
                                                                                                                                     the MCL over many
                                                                                                                                     years could have
                                                                                                                                     problems with their
                                                                                                                                     nervous system,
                                                                                                                                     kidneys, or liver.
    Vinyl Chloride (ppb).......  .002.............  1000.............  2................  0.................  Leaching from PVC     Some people who
                                                                                                               piping; Discharge     drink water
                                                                                                               from plastics         containing vinyl
                                                                                                               factories.            chloride in excess
                                                                                                                                     of the MCL over
                                                                                                                                     many years may have
                                                                                                                                     an increased risk
                                                                                                                                     of getting cancer.
    Xylenes (ppm)..............  10...............  .................  10...............  10................  Discharge from        Some people who
                                                                                                               petroleum             drink water
                                                                                                               factories;            containing xylenes
                                                                                                               Discharge from        in excess of the
                                                                                                               chemical factories.   MCL over many years
                                                                                                                                     could experience
                                                                                                                                     damage to their
                                                                                                                                     nervous system.
--------------------------------------------------------------------------------------------------------------------------------------------------------
[dagger] Until March 31, 2016.
[Dagger] Beginning April 1, 2016.
\1\ These arsenic values are effective January 23, 2006. Until then, the MCL is 0.05 mg/L and there is no MCLG.
Key:
AL = Action Level
MCL = Maximum Contaminant Level
MCLG = Maximum Contaminant Level Goal
MFL = million fibers per liter
MRDL = Maximum Residual Disinfectant Level
MRDLG = Maximum Residual Disinfectant Level Goal
mrem/year = millirems per year (a measure of radiation absorbed by the body)
N/A = Not Applicable
NTU = Nephelometric Turbidity Units (a measure of water clarity)
pCi/l = picocuries per liter (a measure of radioactivity)
ppm = parts per million, or milligrams per liter (mg/l)
ppb = parts per billion, or micrograms per liter ([micro]g/l)
ppt = parts per trillion, or nanograms per liter
ppq = parts per quadrillion, or picograms per liter
TT = Treatment Technique


[65 FR 26024, May 4, 2000, as amended at 65 FR 76749, Dec. 7, 2000; 66 
FR 7064, Jan. 22, 2001; 67 FR 70855, Nov. 27, 2002; 67 FR 73011, Dec. 9, 
2002; 68 FR 14506, Mar. 25, 2003; 71 FR 65652, Nov. 8, 2006; 78 FR 
10349, Feb. 13, 2013]

[[Page 619]]



Subpart P_Enhanced Filtration and Disinfection_Systems Serving 10,000 or 
                               More People

    Source: 63 FR 69516, Dec. 16, 1998, unless otherwise noted.



Sec.  141.170  General requirements.

    (a) The requirements of this subpart P constitute national primary 
drinking water regulations. These regulations establish requirements for 
filtration and disinfection that are in addition to criteria under which 
filtration and disinfection are required under subpart H of this part. 
The requirements of this subpart are applicable to subpart H systems 
serving at least 10,000 people, beginning January 1, 2002 unless 
otherwise specified in this subpart. The regulations in this subpart 
establish or extend treatment technique requirements in lieu of maximum 
contaminant levels for the following contaminants: Giardia lamblia, 
viruses, heterotrophic plate count bacteria, Legionella, 
Cryptosporidium, and turbidity. Each subpart H system serving at least 
10,000 people must provide treatment of its source water that complies 
with these treatment technique requirements and are in addition to those 
identified in Sec.  141.70. The treatment technique requirements consist 
of installing and properly operating water treatment processes which 
reliably achieve:
    (1) At least 99 percent (2-log) removal of Cryptosporidium between a 
point where the raw water is not subject to recontamination by surface 
water runoff and a point downstream before or at the first customer for 
filtered systems, or Cryptosporidium control under the watershed control 
plan for unfiltered systems.
    (2) Compliance with the profiling and benchmark requirements under 
the provisions of Sec.  141.172.
    (b) A public water system subject to the requirements of this 
subpart is considered to be in compliance with the requirements of 
paragraph (a) of this section if:
    (1) It meets the requirements for avoiding filtration in Sec. Sec.  
141.71 and 141.171 and the disinfection requirements in Sec. Sec.  
141.72 and 141.172; or
    (2) It meets the applicable filtration requirements in either Sec.  
141.73 or Sec.  141.173 and the disinfection requirements in Sec. Sec.  
141.72 and 141.172.
    (c) Systems are not permitted to begin construction of uncovered 
finished water storage facilities beginning February 16, 1999.
    (d) Subpart H systems that did not conduct optional monitoring under 
Sec.  141.172 because they served fewer than 10,000 persons when such 
monitoring was required, but serve more than 10,000 persons prior to 
January 1, 2005 must comply with Sec. Sec.  141.170, 141.171, 141.173, 
141.174, and 141.175. These systems must also consult with the State to 
establish a disinfection benchmark. A system that decides to make a 
significant change to its disinfection practice, as described in Sec.  
141.172(c)(1)(i) through (iv) must consult with the State prior to 
making such change.

[63 FR 69516, Dec. 16, 1998, as amended at 66 FR 3779, Jan. 16, 2001; 67 
FR 1836, Jan. 14, 2002; 69 FR 38856, June 29, 2004]



Sec.  141.171  Criteria for avoiding filtration.

    In addition to the requirements of Sec.  141.71, a public water 
system subject to the requirements of this subpart that does not provide 
filtration must meet all of the conditions of paragraphs (a) and (b) of 
this section.
    (a) Site-specific conditions. In addition to site-specific 
conditions in Sec.  141.71(b), systems must maintain the watershed 
control program under Sec.  141.71(b)(2) to minimize the potential for 
contamination by Cryptosporidium oocysts in the source water. The 
watershed control program must, for Cryptosporidium:
    (1) Identify watershed characteristics and activities which may have 
an adverse effect on source water quality; and
    (2) Monitor the occurrence of activities which may have an adverse 
effect on source water quality.
    (b) During the onsite inspection conducted under the provisions of 
Sec.  141.71(b)(3), the State must determine whether the watershed 
control program established under Sec.  141.71(b)(2) is adequate to 
limit potential contamination by Cryptosporidium oocysts. The adequacy 
of the program must be based

[[Page 620]]

on the comprehensiveness of the watershed review; the effectiveness of 
the system's program to monitor and control detrimental activities 
occurring in the watershed; and the extent to which the water system has 
maximized land ownership and/or controlled land use within the 
watershed.



Sec.  141.172  Disinfection profiling and benchmarking.

    (a) Determination of systems required to profile. A public water 
system subject to the requirements of this subpart must determine its 
TTHM annual average using the procedure in paragraph (a)(1) of this 
section and its HAA5 annual average using the procedure in paragraph 
(a)(2) of this section. The annual average is the arithmetic average of 
the quarterly averages of four consecutive quarters of monitoring.
    (1) The TTHM annual average must be the annual average during the 
same period as is used for the HAA5 annual average.
    (i) Those systems that collected data under the provisions of 
subpart M (Information Collection Rule) must use the results of the 
samples collected during the last four quarters of required monitoring 
under Sec.  141.142.
    (ii) Those systems that use ``grandfathered'' HAA5 occurrence data 
that meet the provisions of paragraph (a)(2)(ii) of this section must 
use TTHM data collected at the same time under the provisions of 
Sec. Sec.  141.12 and 141.30.
    (iii) Those systems that use HAA5 occurrence data that meet the 
provisions of paragraph (a)(2)(iii)(A) of this section must use TTHM 
data collected at the same time under the provisions of Sec. Sec.  
141.12 and 141.30.
    (2) The HAA5 annual average must be the annual average during the 
same period as is used for the TTHM annual average.
    (i) Those systems that collected data under the provisions of 
subpart M (Information Collection Rule) must use the results of the 
samples collected during the last four quarters of required monitoring 
under Sec.  141.142.
    (ii) Those systems that have collected four quarters of HAA5 
occurrence data that meets the routine monitoring sample number and 
location requirements for TTHM in Sec. Sec.  141.12 and 141.30 and 
handling and analytical method requirements of Sec.  141.142(b)(1) may 
use those data to determine whether the requirements of this section 
apply.
    (iii) Those systems that have not collected four quarters of HAA5 
occurrence data that meets the provisions of either paragraph (a)(2)(i) 
or (ii) of this section by March 16, 1999 must either:
    (A) Conduct monitoring for HAA5 that meets the routine monitoring 
sample number and location requirements for TTHM in Sec. Sec.  141.12 
and 141.30 and handling and analytical method requirements of Sec.  
141.142(b)(1) to determine the HAA5 annual average and whether the 
requirements of paragraph (b) of this section apply. This monitoring 
must be completed so that the applicability determination can be made no 
later than March 31, 2000, or
    (B) Comply with all other provisions of this section as if the HAA5 
monitoring had been conducted and the results required compliance with 
paragraph (b) of this section.
    (3) The system may request that the State approve a more 
representative annual data set than the data set determined under 
paragraph (a)(1) or (2) of this section for the purpose of determining 
applicability of the requirements of this section.
    (4) The State may require that a system use a more representative 
annual data set than the data set determined under paragraph (a)(1) or 
(2) of this section for the purpose of determining applicability of the 
requirements of this section.
    (5) The system must submit data to the State on the schedule in 
paragraphs (a)(5)(i) through (v) of this section.
    (i) Those systems that collected TTHM and HAA5 data under the 
provisions of subpart M (Information Collection Rule), as required by 
paragraphs (a)(1)(i) and (a)(2)(i) of this section, must submit the 
results of the samples collected during the last 12 months of required 
monitoring under Sec.  141.142 not later than December 31, 1999.
    (ii) Those systems that have collected four consecutive quarters of 
HAA5 occurrence data that meets the routine monitoring sample number and 
location for TTHM in Sec. Sec.  141.12 and 141.30

[[Page 621]]

and handling and analytical method requirements of Sec.  141.142(b)(1), 
as allowed by paragraphs (a)(1)(ii) and (a)(2)(ii) of this section, must 
submit those data to the State not later than April 16, 1999. Until the 
State has approved the data, the system must conduct monitoring for HAA5 
using the monitoring requirements specified under paragraph (a)(2)(iii) 
of this section.
    (iii) Those systems that conduct monitoring for HAA5 using the 
monitoring requirements specified by paragraphs (a)(1)(iii) and 
(a)(2)(iii)(A) of this section, must submit TTHM and HAA5 data not later 
than March 31, 2000.
    (iv) Those systems that elect to comply with all other provisions of 
this section as if the HAA5 monitoring had been conducted and the 
results required compliance with this section, as allowed under 
paragraphs (a)(2)(iii)(B) of this section, must notify the State in 
writing of their election not later than December 31, 1999.
    (v) If the system elects to request that the State approve a more 
representative annual data set than the data set determined under 
paragraph (a)(2)(i) of this section, the system must submit this request 
in writing not later than December 31, 1999.
    (6) Any system having either a TTHM annual average =0.064 
mg/L or an HAA5 annual average =0.048 mg/L during the period 
identified in paragraphs (a)(1) and (2) of this section must comply with 
paragraph (b) of this section.
    (b) Disinfection profiling. (1) Any system that meets the criteria 
in paragraph (a)(6) of this section must develop a disinfection profile 
of its disinfection practice for a period of up to three years.
    (2) The system must monitor daily for a period of 12 consecutive 
calendar months to determine the total logs of inactivation for each day 
of operation, based on the CT99.9 values in Tables 1.1-1.6, 2.1, and 3.1 
of Sec.  141.74(b), as appropriate, through the entire treatment plant. 
This system must begin this monitoring not later than April 1, 2000. As 
a minimum, the system with a single point of disinfectant application 
prior to entrance to the distribution system must conduct the monitoring 
in paragraphs (b)(2)(i) through (iv) of this section. A system with more 
than one point of disinfectant application must conduct the monitoring 
in paragraphs (b)(2)(i) through (iv) of this section for each 
disinfection segment. The system must monitor the parameters necessary 
to determine the total inactivation ratio, using analytical methods in 
Sec.  141.74(a), as follows:
    (i) The temperature of the disinfected water must be measured once 
per day at each residual disinfectant concentration sampling point 
during peak hourly flow.
    (ii) If the system uses chlorine, the pH of the disinfected water 
must be measured once per day at each chlorine residual disinfectant 
concentration sampling point during peak hourly flow.
    (iii) The disinfectant contact time(s) (``T'') must be determined 
for each day during peak hourly flow.
    (iv) The residual disinfectant concentration(s) (``C'') of the water 
before or at the first customer and prior to each additional point of 
disinfection must be measured each day during peak hourly flow.
    (3) In lieu of the monitoring conducted under the provisions of 
paragraph (b)(2) of this section to develop the disinfection profile, 
the system may elect to meet the requirements of paragraph (b)(3)(i) of 
this section. In addition to the monitoring conducted under the 
provisions of paragraph (b)(2) of this section to develop the 
disinfection profile, the system may elect to meet the requirements of 
paragraph (b)(3)(ii) of this section.
    (i) A PWS that has three years of existing operational data may 
submit those data, a profile generated using those data, and a request 
that the State approve use of those data in lieu of monitoring under the 
provisions of paragraph (b)(2) of this section not later than March 31, 
2000. The State must determine whether these operational data are 
substantially equivalent to data collected under the provisions of 
paragraph (b)(2) of this section. These data must also be representative 
of Giardia lamblia inactivation through the entire treatment plant and 
not just of certain treatment segments. Until the State approves this 
request, the

[[Page 622]]

system is required to conduct monitoring under the provisions of 
paragraph (b)(2) of this section.
    (ii) In addition to the disinfection profile generated under 
paragraph (b)(2) of this section, a PWS that has existing operational 
data may use those data to develop a disinfection profile for additional 
years. Such systems may use these additional yearly disinfection 
profiles to develop a benchmark under the provisions of paragraph (c) of 
this section. The State must determine whether these operational data 
are substantially equivalent to data collected under the provisions of 
paragraph (b)(2) of this section. These data must also be representative 
of inactivation through the entire treatment plant and not just of 
certain treatment segments.
    (4) The system must calculate the total inactivation ratio as 
follows:
    (i) If the system uses only one point of disinfectant application, 
the system may determine the total inactivation ratio for the 
disinfection segment based on either of the methods in paragraph 
(b)(4)(i)(A) or (b)(4)(i)(B) of this section.
    (A) Determine one inactivation ratio (CTcalc/CT99.9) 
before or at the first customer during peak hourly flow.
    (B) Determine successive CTcalc/CT99.9 values, 
representing sequential inactivation ratios, between the point of 
disinfectant application and a point before or at the first customer 
during peak hourly flow. Under this alternative, the system must 
calculate the total inactivation ratio by determining (CTcalc/
CT99.9) for each sequence and then adding the (CTcalc/
CT99.9) values together to determine ([Sigma] (CTcalc/
CT99.9)).
    (ii) If the system uses more than one point of disinfectant 
application before the first customer, the system must determine the CT 
value of each disinfection segment immediately prior to the next point 
of disinfectant application, or for the final segment, before or at the 
first customer, during peak hourly flow. The (CTcalc/CT99.9) 
value of each segment and ([Sigma](CTcalc/CT99.9)) must be 
calculated using the method in paragraph (b)(4)(i) of this section.
    (iii) The system must determine the total logs of inactivation by 
multiplying the value calculated in paragraph (b)(4)(i) or (ii) of this 
section by 3.0.
    (5) A system that uses either chloramines or ozone for primary 
disinfection must also calculate the logs of inactivation for viruses 
using a method approved by the State.
    (6) The system must retain disinfection profile data in graphic 
form, as a spreadsheet, or in some other format acceptable to the State 
for review as part of sanitary surveys conducted by the State.
    (c) Disinfection benchmarking. (1) Any system required to develop a 
disinfection profile under the provisions of paragraphs (a) and (b) of 
this section and that decides to make a significant change to its 
disinfection practice must consult with the State prior to making such 
change. Significant changes to disinfection practice are:
    (i) Changes to the point of disinfection;
    (ii) Changes to the disinfectant(s) used in the treatment plant;
    (iii) Changes to the disinfection process; and
    (iv) Any other modification identified by the State.
    (2) Any system that is modifying its disinfection practice must 
calculate its disinfection benchmark using the procedure specified in 
paragraphs (c)(2)(i) through (ii) of this section.
    (i) For each year of profiling data collected and calculated under 
paragraph (b) of this section, the system must determine the lowest 
average monthly Giardia lamblia inactivation in each year of profiling 
data. The system must determine the average Giardia lamblia inactivation 
for each calendar month for each year of profiling data by dividing the 
sum of daily Giardia lamblia of inactivation by the number of values 
calculated for that month.
    (ii) The disinfection benchmark is the lowest monthly average value 
(for systems with one year of profiling data) or average of lowest 
monthly average values (for systems with more than one year of profiling 
data) of the monthly logs of Giardia lamblia inactivation in each year 
of profiling data.

[[Page 623]]

    (3) A system that uses either chloramines or ozone for primary 
disinfection must also calculate the disinfection benchmark for viruses 
using a method approved by the State.
    (4) The system must submit information in paragraphs (c)(4)(i) 
through (iii) of this section to the State as part of its consultation 
process.
    (i) A description of the proposed change;
    (ii) The disinfection profile for Giardia lamblia (and, if 
necessary, viruses) under paragraph (b) of this section and benchmark as 
required by paragraph (c)(2) of this section; and
    (iii) An analysis of how the proposed change will affect the current 
levels of disinfection.

[63 FR 69516, Dec. 16, 1998, as amended at 66 FR 3779, Jan. 16, 2001]



Sec.  141.173  Filtration.

    A public water system subject to the requirements of this subpart 
that does not meet all of the criteria in this subpart and subpart H of 
this part for avoiding filtration must provide treatment consisting of 
both disinfection, as specified in Sec.  141.72(b), and filtration 
treatment which complies with the requirements of paragraph (a) or (b) 
of this section or Sec.  141.73 (b) or (c) by December 31, 2001.
    (a) Conventional filtration treatment or direct filtration. (1) For 
systems using conventional filtration or direct filtration, the 
turbidity level of representative samples of a system's filtered water 
must be less than or equal to 0.3 NTU in at least 95 percent of the 
measurements taken each month, measured as specified in Sec.  141.74(a) 
and (c).
    (2) The turbidity level of representative samples of a system's 
filtered water must at no time exceed 1 NTU, measured as specified in 
Sec.  141.74(a) and (c).
    (3) A system that uses lime softening may acidify representative 
samples prior to analysis using a protocol approved by the State.
    (b) Filtration technologies other than conventional filtration 
treatment, direct filtration, slow sand filtration, or diatomaceous 
earth filtration. A public water system may use a filtration technology 
not listed in paragraph (a) of this section or in Sec.  141.73(b) or (c) 
if it demonstrates to the State, using pilot plant studies or other 
means, that the alternative filtration technology, in combination with 
disinfection treatment that meets the requirements of Sec.  141.72(b), 
consistently achieves 99.9 percent removal and/or inactivation of 
Giardia lamblia cysts and 99.99 percent removal and/or inactivation of 
viruses, and 99 percent removal of Cryptosporidium oocysts, and the 
State approves the use of the filtration technology. For each approval, 
the State will set turbidity performance requirements that the system 
must meet at least 95 percent of the time and that the system may not 
exceed at any time at a level that consistently achieves 99.9 percent 
removal and/or inactivation of Giardia lamblia cysts, 99.99 percent 
removal and/or inactivation of viruses, and 99 percent removal of 
Cryptosporidium oocysts.

[63 FR 69516, Dec. 16, 1998, as amended at 65 FR 20313, Apr. 14, 2000; 
66 FR 3779, Jan. 16, 2001]



Sec.  141.174  Filtration sampling requirements.

    (a) Monitoring requirements for systems using filtration treatment. 
In addition to monitoring required by Sec.  141.74, a public water 
system subject to the requirements of this subpart that provides 
conventional filtration treatment or direct filtration must conduct 
continuous monitoring of turbidity for each individual filter using an 
approved method in Sec.  141.74(a) and must calibrate turbidimeters 
using the procedure specified by the manufacturer. Systems must record 
the results of individual filter monitoring every 15 minutes.
    (b) If there is a failure in the continuous turbidity monitoring 
equipment, the system must conduct grab sampling every four hours in 
lieu of continuous monitoring, but for no more than five working days 
following the failure of the equipment.



Sec.  141.175  Reporting and recordkeeping requirements.

    In addition to the reporting and recordkeeping requirements in Sec.  
141.75, a public water system subject to the requirements of this 
subpart that provides conventional filtration treatment

[[Page 624]]

or direct filtration must report monthly to the State the information 
specified in paragraphs (a) and (b) of this section beginning January 1, 
2002. In addition to the reporting and recordkeeping requirements in 
Sec.  141.75, a public water system subject to the requirements of this 
subpart that provides filtration approved under Sec.  141.173(b) must 
report monthly to the State the information specified in paragraph (a) 
of this section beginning January 1, 2002. The reporting in paragraph 
(a) of this section is in lieu of the reporting specified in Sec.  
141.75(b)(1).
    (a) Turbidity measurements as required by Sec.  141.173 must be 
reported within 10 days after the end of each month the system serves 
water to the public. Information that must be reported includes:
    (1) The total number of filtered water turbidity measurements taken 
during the month.
    (2) The number and percentage of filtered water turbidity 
measurements taken during the month which are less than or equal to the 
turbidity limits specified in Sec.  141.173(a) or (b).
    (3) The date and value of any turbidity measurements taken during 
the month which exceed 1 NTU for systems using conventional filtration 
treatment or direct filtration, or which exceed the maximum level set by 
the State under Sec.  141.173(b).
    (b) Systems must maintain the results of individual filter 
monitoring taken under Sec.  141.174 for at least three years. Systems 
must report that they have conducted individual filter turbidity 
monitoring under Sec.  141.174 within 10 days after the end of each 
month the system serves water to the public. Systems must report 
individual filter turbidity measurement results taken under Sec.  
141.174 within 10 days after the end of each month the system serves 
water to the public only if measurements demonstrate one or more of the 
conditions in paragraphs (b)(1) through (4) of this section. Systems 
that use lime softening may apply to the State for alternative 
exceedance levels for the levels specified in paragraphs (b)(1) through 
(4) of this section if they can demonstrate that higher turbidity levels 
in individual filters are due to lime carryover only and not due to 
degraded filter performance.
    (1) For any individual filter that has a measured turbidity level of 
greater than 1.0 NTU in two consecutive measurements taken 15 minutes 
apart, the system must report the filter number, the turbidity 
measurement, and the date(s) on which the exceedance occurred. In 
addition, the system must either produce a filter profile for the filter 
within 7 days of the exceedance (if the system is not able to identify 
an obvious reason for the abnormal filter performance) and report that 
the profile has been produced or report the obvious reason for the 
exceedance.
    (2) For any individual filter that has a measured turbidity level of 
greater than 0.5 NTU in two consecutive measurements taken 15 minutes 
apart at the end of the first four hours of continuous filter operation 
after the filter has been backwashed or otherwise taken offline, the 
system must report the filter number, the turbidity, and the date(s) on 
which the exceedance occurred. In addition, the system must either 
produce a filter profile for the filter within 7 days of the exceedance 
(if the system is not able to identify an obvious reason for the 
abnormal filter performance) and report that the profile has been 
produced or report the obvious reason for the exceedance.
    (3) For any individual filter that has a measured turbidity level of 
greater than 1.0 NTU in two consecutive measurements taken 15 minutes 
apart at any time in each of three consecutive months, the system must 
report the filter number, the turbidity measurement, and the date(s) on 
which the exceedance occurred. In addition, the system must conduct a 
self-assessment of the filter within 14 days of the exceedance and 
report that the self-assessment was conducted. The self assessment must 
consist of at least the following components: assessment of filter 
performance; development of a filter profile; identification and 
prioritization of factors limiting filter performance; assessment of the 
applicability of corrections; and preparation of a filter self-
assessment report.
    (4) For any individual filter that has a measured turbidity level of 
greater

[[Page 625]]

than 2.0 NTU in two consecutive measurements taken 15 minutes apart at 
any time in each of two consecutive months, the system must report the 
filter number, the turbidity measurement, and the date(s) on which the 
exceedance occurred. In addition, the system must arrange for the 
conduct of a comprehensive performance evaluation by the State or a 
third party approved by the State no later than 30 days following the 
exceedance and have the evaluation completed and submitted to the State 
no later than 90 days following the exceedance.
    (c) Additional reporting requirements. (1) If at any time the 
turbidity exceeds 1 NTU in representative samples of filtered water in a 
system using conventional filtration treatment or direct filtration, the 
system must inform the State as soon as possible, but no later than the 
end of the next business day.
    (2) If at any time the turbidity in representative samples of 
filtered water exceeds the maximum level set by the State under Sec.  
141.173(b) for filtration technologies other than conventional 
filtration treatment, direct filtration, slow sand filtration, or 
diatomaceous earth filtration, the system must inform the State as soon 
as possible, but no later than the end of the next business day.

[63 FR 69516, Dec. 16, 1998, as amended at 66 FR 3779, Jan. 16, 2001]



       Subpart Q_Public Notification of Drinking Water Violations

    Source: 65 FR 26035, May 4, 2000, unless otherwise noted.



Sec.  141.201  General public notification requirements.

    Public water systems in States with primacy for the public water 
system supervision (PWSS) program must comply with the requirements in 
this subpart no later than May 6, 2002 or on the date the State-adopted 
rule becomes effective, whichever comes first. Public water systems in 
jurisdictions where EPA directly implements the PWSS program must comply 
with the requirements in this subpart on October 31, 2000. Prior to 
these dates, public water systems must continue to comply with the 
public notice requirements in Sec.  141.32 of this part. The term 
``primacy agency'' is used in this subpart to refer to either EPA or the 
State or the Tribe in cases where EPA, the State, or the Tribe exercises 
primary enforcement responsibility for this subpart.
    (a) Who must give public notice? Each owner or operator of a public 
water system (community water systems, non-transient non-community water 
systems, and transient non-community water systems) must give notice for 
all violations of national primary drinking water regulations (NPDWR) 
and for other situations, as listed in Table 1. The term ``NPDWR 
violations'' is used in this subpart to include violations of the 
maximum contaminant level (MCL), maximum residual disinfection level 
(MRDL), treatment technique (TT), monitoring requirements, and testing 
procedures in this part 141. Appendix A to this subpart identifies the 
tier assignment for each specific violation or situation requiring a 
public notice.

  Table 1 to Sec.   141.201--Violation Categories and Other Situations
                        Requiring a Public Notice
------------------------------------------------------------------------
 
-------------------------------------------------------------------------
(1) NPDWR violations:
  (i) Failure to comply with an applicable maximum contaminant level
   (MCL) or maximum residual disinfectant level (MRDL).
  (ii) Failure to comply with a prescribed treatment technique (TT).
  (iii) Failure to perform water quality monitoring, as required by the
   drinking water regulations.
  (iv) Failure to comply with testing procedures as prescribed by a
   drinking water regulation.
(2) Variance and exemptions under sections 1415 and 1416 of SDWA:
  (i) Operation under a variance or an exemption.
  (ii) Failure to comply with the requirements of any schedule that has
   been set under a variance or exemption.
(3) Special public notices:
  (i) Occurrence of a waterborne disease outbreak or other waterborne
   emergency.

[[Page 626]]

 
  (ii) Exceedance of the nitrate MCL by non-community water systems
   (NCWS), where granted permission by the primacy agency under
   141.11(d) of this part.
  (iii) Exceedance of the secondary maximum contaminant level (SMCL) for
   fluoride.
  (iv) Availability of unregulated contaminant monitoring data.
  (v) Other violations and situations determined by the primacy agency
   to require a public notice under this subpart, not already listed in
   Appendix A.
------------------------------------------------------------------------

    (b) What type of public notice is required for each violation or 
situation? Public notice requirements are divided into three tiers, to 
take into account the seriousness of the violation or situation and of 
any potential adverse health effects that may be involved. The public 
notice requirements for each violation or situation listed in Table 1 of 
this section are determined by the tier to which it is assigned. Table 2 
of this section provides the definition of each tier. Appendix A of this 
part identifies the tier assignment for each specific violation or 
situation.

      Table 2 to Sec.   141.201--Definition of Public Notice Tiers
------------------------------------------------------------------------
 
-------------------------------------------------------------------------
(1) Tier 1 public notice--required for NPDWR violations and situations
 with significant potential to have serious adverse effects on human
 health as a result of short-term exposure.
(2) Tier 2 public notice--required for all other NPDWR violations and
 situations with potential to have serious adverse effects on human
 health.
(3) Tier 3 public notice--required for all other NPDWR violations and
 situations not included in Tier 1 and Tier 2.
------------------------------------------------------------------------

    (c) Who must be notified? (1) Each public water system must provide 
public notice to persons served by the water system, in accordance with 
this subpart. Public water systems that sell or otherwise provide 
drinking water to other public water systems (i.e., to consecutive 
systems) are required to give public notice to the owner or operator of 
the consecutive system; the consecutive system is responsible for 
providing public notice to the persons it serves.
    (2) If a public water system has a violation in a portion of the 
distribution system that is physically or hydraulically isolated from 
other parts of the distribution system, the primacy agency may allow the 
system to limit distribution of the public notice to only persons served 
by that portion of the system which is out of compliance. Permission by 
the primacy agency for limiting distribution of the notice must be 
granted in writing.
    (3) A copy of the notice must also be sent to the primacy agency, in 
accordance with the requirements under Sec.  141.31(d).



Sec.  141.202  Tier 1 Public Notice--Form, manner, and frequency of notice.

    (a) Which violations or situations require a Tier 1 public notice? 
Table 1 of this section lists the violation categories and other 
situations requiring a Tier 1 public notice. Appendix A to this subpart 
identifies the tier assignment for each specific violation or situation.

  Table 1 to Sec.   141.202--Violation Categories and Other Situations
                    Requiring a Tier 1 Public Notice
------------------------------------------------------------------------
 
-------------------------------------------------------------------------
(1) Violation of the MCL for total coliforms when fecal coliform or E.
 coli are present in the water distribution system (as specified in Sec.
   141.63(b)), or when the water system fails to test for fecal
 coliforms or E. coli when any repeat sample tests positive for coliform
 (as specified in Sec.   141.21(e)); Violation of the MCL for E. coli
 (as specified in Sec.   141.63(c));
(2) Violation of the MCL for nitrate, nitrite, or total nitrate and
 nitrite, as defined in Sec.   141.62, or when the water system fails to
 take a confirmation sample within 24 hours of the system's receipt of
 the first sample showing an exceedance of the nitrate or nitrite MCL,
 as specified in Sec.   141.23(f)(2);
(3) Exceedance of the nitrate MCL by non-community water systems, where
 permitted to exceed the MCL by the primacy agency under Sec.
 141.11(d), as required under Sec.   141.209;

[[Page 627]]

 
(4) Violation of the MRDL for chlorine dioxide, as defined in Sec.
 141.65(a), when one or more samples taken in the distribution system
 the day following an exceedance of the MRDL at the entrance of the
 distribution system exceed the MRDL, or when the water system does not
 take the required samples in the distribution system, as specified in
 Sec.   141.133(c)(2)(i);
(5) Violation of the turbidity MCL under Sec.   141.13(b), where the
 primacy agency determines after consultation that a Tier 1 notice is
 required or where consultation does not take place within 24 hours
 after the system learns of the violation;
(6) Violation of the Surface Water Treatment Rule (SWTR), Interim
 Enhanced Surface Water Treatment Rule (IESWTR) or Long Term 1 Enhanced
 Surface Water Treatment Rule (LT1ESWTR) treatment technique requirement
 resulting from a single exceedance of the maximum allowable turbidity
 limit (as identified in appendix A), where the primacy agency
 determines after consultation that a Tier 1 notice is required or where
 consultation does not take place within 24 hours after the system
 learns of the violation;
(7) Occurrence of a waterborne disease outbreak, as defined in Sec.
 141.2, or other waterborne emergency (such as a failure or significant
 interruption in key water treatment processes, a natural disaster that
 disrupts the water supply or distribution system, or a chemical spill
 or unexpected loading of possible pathogens into the source water that
 significantly increases the potential for drinking water
 contamination);
(8) Detection of E. coli, enterococci, or coliphage in source water
 samples as specified in Sec.   141.402(a) and Sec.   141.402(b);
(9) Other violations or situations with significant potential to have
 serious adverse effects on human health as a result of short-term
 exposure, as determined by the primacy agency either in its regulations
 or on a case-by-case basis.
------------------------------------------------------------------------

    (b) When is the Tier 1 public notice to be provided? What additional 
steps are required? Public water systems must:
    (1) Provide a public notice as soon as practical but no later than 
24 hours after the system learns of the violation;
    (2) Initiate consultation with the primacy agency as soon as 
practical, but no later than 24 hours after the public water system 
learns of the violation or situation, to determine additional public 
notice requirements; and
    (3) Comply with any additional public notification requirements 
(including any repeat notices or direction on the duration of the posted 
notices) that are established as a result of the consultation with the 
primacy agency. Such requirements may include the timing, form, manner, 
frequency, and content of repeat notices (if any) and other actions 
designed to reach all persons served.
    (c) What is the form and manner of the public notice? Public water 
systems must provide the notice within 24 hours in a form and manner 
reasonably calculated to reach all persons served. The form and manner 
used by the public water system are to fit the specific situation, but 
must be designed to reach residential, transient, and non-transient 
users of the water system. In order to reach all persons served, water 
systems are to use, at a minimum, one or more of the following forms of 
delivery:
    (1) Appropriate broadcast media (such as radio and television);
    (2) Posting of the notice in conspicuous locations throughout the 
area served by the water system;
    (3) Hand delivery of the notice to persons served by the water 
system; or
    (4) Another delivery method approved in writing by the primacy 
agency.

[65 FR 26035, May 4, 2000, as amended at 67 FR 1836, Jan. 14, 2002; 71 
FR 65652, Nov. 8, 2006; 78 FR 10350, Feb. 13, 2013]



Sec.  141.203  Tier 2 Public Notice--Form, manner, and frequency of notice.

    (a) Which violations or situations require a Tier 2 public notice? 
Table 1 of this section lists the violation categories and other 
situations requiring a Tier 2 public notice. Appendix A to this subpart 
identifies the tier assignment for each specific violation or situation.

[[Page 628]]



  Table 1 to Sec.   141.203--Violation Categories and Other Situations
                    Requiring a Tier 2 Public Notice
(1) All violations of the MCL, MRDL, and treatment technique
 requirements, except where a Tier 1 notice is required under Sec.
 141.202(a) or where the primacy agency determines that a Tier 1 notice
 is required;
(2) Violations of the monitoring and testing procedure requirements,
 where the primacy agency determines that a Tier 2 rather than a Tier 3
 public notice is required, taking into account potential health impacts
 and persistence of the violation; and
(3) Failure to comply with the terms and conditions of any variance or
 exemption in place.
(4) Failure to take corrective action or failure to maintain at least 4-
 log treatment of viruses (using inactivation, removal, or a State-
 approved combination of 4-log virus inactivation and removal) before or
 at the first customer under Sec.   141.403(a).
------------------------------------------------------------------------

    (b) When is the Tier 2 public notice to be provided? (1) Public 
water systems must provide the public notice as soon as practical, but 
no later than 30 days after the system learns of the violation. If the 
public notice is posted, the notice must remain in place for as long as 
the violation or situation persists, but in no case for less than seven 
days, even if the violation or situation is resolved. The primacy agency 
may, in appropriate circumstances, allow additional time for the initial 
notice of up to three months from the date the system learns of the 
violation. It is not appropriate for the primacy agency to grant an 
extension to the 30-day deadline for any unresolved violation or to 
allow across-the-board extensions by rule or policy for other violations 
or situations requiring a Tier 2 public notice. Extensions granted by 
the primacy agency must be in writing.
    (2) The public water system must repeat the notice every three 
months as long as the violation or situation persists, unless the 
primacy agency determines that appropriate circumstances warrant a 
different repeat notice frequency. In no circumstance may the repeat 
notice be given less frequently than once per year. It is not 
appropriate for the primacy agency to allow less frequent repeat notice 
for an MCL or treatment technique violation under the Total Coliform 
Rule or subpart Y of this part or a treatment technique violation under 
the Surface Water Treatment Rule or Interim Enhanced Surface Water 
Treatment Rule. It is also not appropriate for the primacy agency to 
allow through its rules or policies across-the-board reductions in the 
repeat notice frequency for other ongoing violations requiring a Tier 2 
repeat notice. Primacy agency determinations allowing repeat notices to 
be given less frequently than once every three months must be in 
writing.
    (3) For the turbidity violations specified in this paragraph, public 
water systems must consult with the primacy agency as soon as practical 
but no later than 24 hours after the public water system learns of the 
violation, to determine whether a Tier 1 public notice under Sec.  
141.202(a) is required to protect public health. When consultation does 
not take place within the 24-hour period, the water system must 
distribute a Tier 1 notice of the violation within the next 24 hours 
(i.e., no later than 48 hours after the system learns of the violation), 
following the requirements under Sec.  141.202(b) and (c). Consultation 
with the primacy agency is required for:
    (i) Violation of the turbidity MCL under Sec.  141.13(b); or
    (ii) Violation of the SWTR, IESWTR or LT1ESWTR treatment technique 
requirement resulting from a single exceedance of the maximum allowable 
turbidity limit.
    (c) What is the form and manner of the Tier 2 public notice? Public 
water systems must provide the initial public notice and any repeat 
notices in a form and manner that is reasonably calculated to reach 
persons served in the required time period. The form and manner of the 
public notice may vary based on the specific situation and type of water 
system, but it must at a minimum meet the following requirements:
    (1) Unless directed otherwise by the primacy agency in writing, 
community water systems must provide notice by:
    (i) Mail or other direct delivery to each customer receiving a bill 
and to other service connections to which

[[Page 629]]

water is delivered by the public water system; and
    (ii) Any other method reasonably calculated to reach other persons 
regularly served by the system, if they would not normally be reached by 
the notice required in paragraph (c)(1)(i) of this section. Such persons 
may include those who do not pay water bills or do not have service 
connection addresses (e.g., house renters, apartment dwellers, 
university students, nursing home patients, prison inmates, etc.). Other 
methods may include: Publication in a local newspaper; delivery of 
multiple copies for distribution by customers that provide their 
drinking water to others (e.g., apartment building owners or large 
private employers); posting in public places served by the system or on 
the Internet; or delivery to community organizations.
    (2) Unless directed otherwise by the primacy agency in writing, non-
community water systems must provide notice by:
    (i) Posting the notice in conspicuous locations throughout the 
distribution system frequented by persons served by the system, or by 
mail or direct delivery to each customer and service connection (where 
known); and
    (ii) Any other method reasonably calculated to reach other persons 
served by the system if they would not normally be reached by the notice 
required in paragraph (c)(2)(i) of this section. Such persons may 
include those served who may not see a posted notice because the posted 
notice is not in a location they routinely pass by. Other methods may 
include: Publication in a local newspaper or newsletter distributed to 
customers; use of E-mail to notify employees or students; or, delivery 
of multiple copies in central locations (e.g., community centers).

[65 FR 26035, May 4, 2000, as amended at 67 FR 1836, Jan. 14, 2002; 71 
FR 65652, Nov. 8, 2006; 78 FR 10350, Feb. 13, 2013]



Sec.  141.204  Tier 3 Public Notice--Form, manner, and frequency of notice.

    (a) Which violations or situations require a Tier 3 public notice? 
Table 1 of this section lists the violation categories and other 
situations requiring a Tier 3 public notice. Appendix A to this subpart 
identifies the tier assignment for each specific violation or situation.

  Table 1 to Sec.   141.204--Violation Categories and Other Situations
                    Requiring a Tier 3 Public Notice
------------------------------------------------------------------------
 
-------------------------------------------------------------------------
(1) Monitoring violations under 40 CFR part 141, except where a Tier 1
 notice is required under Sec.   141.202(a) or where the primacy agency
 determines that a Tier 2 notice is required;
(2) Failure to comply with a testing procedure established in 40 CFR
 part 141, except where a Tier 1 notice is required under Sec.
 141.202(a)) or where the primacy agency determines that a Tier 2 notice
 is required;
(3) Operation under a variance granted under Section 1415 or an
 exemption granted under Section 1416 of the Safe Drinking Water Act;
(4) Availability of unregulated contaminant monitoring results, as
 required under Sec.   141.207;
(5) Exceedance of the fluoride secondary maximum contaminant level
 (SMCL), as required under Sec.   141.208; and
(6) Reporting and Recordkeeping violations under subpart Y of 40 CFR
 part 141.
------------------------------------------------------------------------

    (b) When is the Tier 3 public notice to be provided? (1) Public 
water systems must provide the public notice not later than one year 
after the public water system learns of the violation or situation or 
begins operating under a variance or exemption. Following the initial 
notice, the public water system must repeat the notice annually for as 
long as the violation, variance, exemption, or other situation persists. 
If the public notice is posted, the notice must remain in place for as 
long as the violation, variance, exemption, or other situation persists, 
but in no case less than seven days (even if the violation or situation 
is resolved).
    (2) Instead of individual Tier 3 public notices, a public water 
system may use an annual report detailing all violations and situations 
that occurred during the previous twelve months, as long as the timing 
requirements of paragraph (b)(1) of this section are met.
    (c) What is the form and manner of the Tier 3 public notice? Public 
water systems must provide the initial notice and any repeat notices in 
a form and manner that is reasonably calculated

[[Page 630]]

to reach persons served in the required time period. The form and manner 
of the public notice may vary based on the specific situation and type 
of water system, but it must at a minimum meet the following 
requirements:
    (1) Unless directed otherwise by the primacy agency in writing, 
community water systems must provide notice by:
    (i) Mail or other direct delivery to each customer receiving a bill 
and to other service connections to which water is delivered by the 
public water system; and
    (ii) Any other method reasonably calculated to reach other persons 
regularly served by the system, if they would not normally be reached by 
the notice required in paragraph (c)(1)(i) of this section. Such persons 
may include those who do not pay water bills or do not have service 
connection addresses (e.g., house renters, apartment dwellers, 
university students, nursing home patients, prison inmates, etc.). Other 
methods may include: Publication in a local newspaper; delivery of 
multiple copies for distribution by customers that provide their 
drinking water to others (e.g., apartment building owners or large 
private employers); posting in public places or on the Internet; or 
delivery to community organizations.
    (2) Unless directed otherwise by the primacy agency in writing, non-
community water systems must provide notice by:
    (i) Posting the notice in conspicuous locations throughout the 
distribution system frequented by persons served by the system, or by 
mail or direct delivery to each customer and service connection (where 
known); and
    (ii) Any other method reasonably calculated to reach other persons 
served by the system, if they would not normally be reached by the 
notice required in paragraph (c)(2)(i) of this section. Such persons may 
include those who may not see a posted notice because the notice is not 
in a location they routinely pass by. Other methods may include: 
Publication in a local newspaper or newsletter distributed to customers; 
use of E-mail to notify employees or students; or, delivery of multiple 
copies in central locations (e.g., community centers).
    (d) In what situations may the Consumer Confidence Report be used to 
meet the Tier 3 public notice requirements? For community water systems, 
the Consumer Confidence Report (CCR) required under Subpart O of this 
part may be used as a vehicle for the initial Tier 3 public notice and 
all required repeat notices, as long as:
    (1) The CCR is provided to persons served no later than 12 months 
after the system learns of the violation or situation as required under 
Sec.  141.204(b);
    (2) The Tier 3 notice contained in the CCR follows the content 
requirements under Sec.  141.205; and
    (3) The CCR is distributed following the delivery requirements under 
Sec.  141.204(c).

[65 FR 26035, May 4, 2000; 65 FR 38629, June 21, 2000, as amended at 78 
FR 10350, Feb. 13, 2013]



Sec.  141.205  Content of the public notice.

    (a) What elements must be included in the public notice for 
violations of National Primary Drinking Water Regulations (NPDWR) or 
other situations requiring a public notice? When a public water system 
violates a NPDWR or has a situation requiring public notification, each 
public notice must include the following elements:
    (1) A description of the violation or situation, including the 
contaminant(s) of concern, and (as applicable) the contaminant level(s);
    (2) When the violation or situation occurred;
    (3) Any potential adverse health effects from the violation or 
situation, including the standard language under paragraph (d)(1) or 
(d)(2) of this section, whichever is applicable;
    (4) The population at risk, including subpopulations particularly 
vulnerable if exposed to the contaminant in their drinking water;
    (5) Whether alternative water supplies should be used;
    (6) What actions consumers should take, including when they should 
seek medical help, if known;
    (7) What the system is doing to correct the violation or situation;
    (8) When the water system expects to return to compliance or resolve 
the situation;
    (9) The name, business address, and phone number of the water system

[[Page 631]]

owner, operator, or designee of the public water system as a source of 
additional information concerning the notice; and
    (10) A statement to encourage the notice recipient to distribute the 
public notice to other persons served, using the standard language under 
paragraph (d)(3) of this section, where applicable.
    (b) What elements must be included in the public notice for public 
water systems operating under a variance or exemption? (1) If a public 
water system has been granted a variance or an exemption, the public 
notice must contain:
    (i) An explanation of the reasons for the variance or exemption;
    (ii) The date on which the variance or exemption was issued;
    (iii) A brief status report on the steps the system is taking to 
install treatment, find alternative sources of water, or otherwise 
comply with the terms and schedules of the variance or exemption; and
    (iv) A notice of any opportunity for public input in the review of 
the variance or exemption.
    (2) If a public water system violates the conditions of a variance 
or exemption, the public notice must contain the ten elements listed in 
paragraph (a) of this section.
    (c) How is the public notice to be presented? (1) Each public notice 
required by this section:
    (i) Must be displayed in a conspicuous way when printed or posted;
    (ii) Must not contain overly technical language or very small print;
    (iii) Must not be formatted in a way that defeats the purpose of the 
notice;
    (iv) Must not contain language which nullifies the purpose of the 
notice.
    (2) Each public notice required by this section must comply with 
multilingual requirements, as follows:
    (i) For public water systems serving a large proportion of non-
English speaking consumers, as determined by the primacy agency, the 
public notice must contain information in the appropriate language(s) 
regarding the importance of the notice or contain a telephone number or 
address where persons served may contact the water system to obtain a 
translated copy of the notice or to request assistance in the 
appropriate language.
    (ii) In cases where the primacy agency has not determined what 
constitutes a large proportion of non-English speaking consumers, the 
public water system must include in the public notice the same 
information as in paragraph (c)(2)(i) of this section, where appropriate 
to reach a large proportion of non-English speaking persons served by 
the water system.
    (d) What standard language must public water systems include in 
their public notice? Public water systems are required to include the 
following standard language in their public notice:
    (1) Standard health effects language for MCL or MRDL violations, 
treatment technique violations, and violations of the condition of a 
variance or exemption. Public water systems must include in each public 
notice the health effects language specified in appendix B to this 
subpart corresponding to each MCL, MRDL, and treatment technique 
violation listed in appendix A to this subpart, and for each violation 
of a condition of a variance or exemption.
    (2) Standard language for monitoring and testing procedure 
violations. Public water systems must include the following language in 
their notice, including the language necessary to fill in the blanks, 
for all monitoring and testing procedure violations listed in appendix A 
to this subpart:

    We are required to monitor your drinking water for specific 
contaminants on a regular basis. Results of regular monitoring are an 
indicator of whether or not your drinking water meets health standards. 
During [compliance period], we ``did not monitor or test'' or ``did not 
complete all monitoring or testing'' for [contaminant(s)], and therefore 
cannot be sure of the quality of your drinking water during that time.

    (3) Standard language to encourage the distribution of the public 
notice to all persons served. Public water systems must include in their 
notice the following language (where applicable):

    Please share this information with all the other people who drink 
this water, especially those who may not have received this notice 
directly (for example, people in apartments, nursing homes, schools, and 
businesses). You can do this by posting this notice in a public place or 
distributing copies by hand or mail.

[[Page 632]]



Sec.  141.206  Notice to new billing units or new customers.

    (a) What is the requirement for community water systems? Community 
water systems must give a copy of the most recent public notice for any 
continuing violation, the existence of a variance or exemption, or other 
ongoing situations requiring a public notice to all new billing units or 
new customers prior to or at the time service begins.
    (b) What is the requirement for non-community water systems? Non-
community water systems must continuously post the public notice in 
conspicuous locations in order to inform new consumers of any continuing 
violation, variance or exemption, or other situation requiring a public 
notice for as long as the violation, variance, exemption, or other 
situation persists.



Sec.  141.207  Special notice of the availability of unregulated contaminant 
monitoring results.

    (a) When is the special notice to be given? The owner or operator of 
a community water system or non-transient, non-community water system 
required to monitor under Sec.  141.40 must notify persons served by the 
system of the availability of the results of such sampling no later than 
12 months after the monitoring results are known.
    (b) What is the form and manner of the special notice? The form and 
manner of the public notice must follow the requirements for a Tier 3 
public notice prescribed in Sec. Sec.  141.204(c), (d)(1), and (d)(3). 
The notice must also identify a person and provide the telephone number 
to contact for information on the monitoring results.



Sec.  141.208  Special notice for exceedance of the SMCL for fluoride.

    (a) When is the special notice to be given? Community water systems 
that exceed the fluoride secondary maximum contaminant level (SMCL) of 2 
mg/l as specified in Sec.  143.3 (determined by the last single sample 
taken in accordance with Sec.  141.23), but do not exceed the maximum 
contaminant level (MCL) of 4 mg/l for fluoride (as specified in Sec.  
141.62), must provide the public notice in paragraph (c) of this section 
to persons served. Public notice must be provided as soon as practical 
but no later than 12 months from the day the water system learns of the 
exceedance. A copy of the notice must also be sent to all new billing 
units and new customers at the time service begins and to the State 
public health officer. The public water system must repeat the notice at 
least annually for as long as the SMCL is exceeded. If the public notice 
is posted, the notice must remain in place for as long as the SMCL is 
exceeded, but in no case less than seven days (even if the exceedance is 
eliminated). On a case-by-case basis, the primacy agency may require an 
initial notice sooner than 12 months and repeat notices more frequently 
than annually.
    (b) What is the form and manner of the special notice? The form and 
manner of the public notice (including repeat notices) must follow the 
requirements for a Tier 3 public notice in Sec.  141.204(c) and (d)(1) 
and (d)(3).
    (c) What mandatory language must be contained in the special notice? 
The notice must contain the following language, including the language 
necessary to fill in the blanks:

    This is an alert about your drinking water and a cosmetic dental 
problem that might affect children under nine years of age. At low 
levels, fluoride can help prevent cavities, but children drinking water 
containing more than 2 milligrams per liter (mg/l) of fluoride may 
develop cosmetic discoloration of their permanent teeth (dental 
fluorosis). The drinking water provided by your community water system 
[name] has a fluoride concentration of [insert value] mg/l.
    Dental fluorosis, in its moderate or severe forms, may result in a 
brown staining and/or pitting of the permanent teeth. This problem 
occurs only in developing teeth, before they erupt from the gums. 
Children under nine should be provided with alternative sources of 
drinking water or water that has been treated to remove the fluoride to 
avoid the possibility of staining and pitting of their permanent teeth. 
You may also want to contact your dentist about proper use by young 
children of fluoride-containing products. Older children and adults may 
safely drink the water.
    Drinking water containing more than 4 mg/L of fluoride (the U.S. 
Environmental Protection Agency's drinking water standard) can increase 
your risk of developing bone disease. Your drinking water does not 
contain more than 4 mg/l of fluoride, but we're required to notify you 
when we discover that the fluoride levels in your drinking water exceed 
2 mg/l because of this cosmetic dental problem.

[[Page 633]]

    For more information, please call [name of water system contact] of 
[name of community water system] at [phone number]. Some home water 
treatment units are also available to remove fluoride from drinking 
water. To learn more about available home water treatment units, you may 
call NSF International at 1-877-8-NSF-HELP.''



Sec.  141.209  Special notice for nitrate exceedances above MCL 
by non-community water systems (NCWS), where granted permission 
by the primacy agency under Sec.  141.11(d).

    (a) When is the special notice to be given? The owner or operator of 
a non-community water system granted permission by the primacy agency 
under Sec.  141.11(d) to exceed the nitrate MCL must provide notice to 
persons served according to the requirements for a Tier 1 notice under 
Sec.  141.202(a) and (b).
    (b) What is the form and manner of the special notice? Non-community 
water systems granted permission by the primacy agency to exceed the 
nitrate MCL under Sec.  141.11(d) must provide continuous posting of the 
fact that nitrate levels exceed 10 mg/l and the potential health effects 
of exposure, according to the requirements for Tier 1 notice delivery 
under Sec.  141.202(c) and the content requirements under Sec.  141.205.



Sec.  141.210  Notice by primacy agency on behalf of the public water system.

    (a) May the primacy agency give the notice on behalf of the public 
water system? The primacy agency may give the notice required by this 
subpart on behalf of the owner and operator of the public water system 
if the primacy agency complies with the requirements of this subpart.
    (b) What is the responsibility of the public water system when 
notice is given by the primacy agency? The owner or operator of the 
public water system remains responsible for ensuring that the 
requirements of this subpart are met.



Sec.  141.211  Special notice for repeated failure to conduct monitoring 
of the source water for Cryptosporidium and for failure to determine 
bin classification or mean Cryptosporidium level.

    (a) When is the special notice for repeated failure to monitor to be 
given? The owner or operator of a community or non-community water 
system that is required to monitor source water under Sec.  141.701 must 
notify persons served by the water system that monitoring has not been 
completed as specified no later than 30 days after the system has failed 
to collect any 3 months of monitoring as specified in Sec.  141.701(c). 
The notice must be repeated as specified in Sec.  141.203(b).
    (b) When is the special notice for failure to determine bin 
classification or mean Cryptosporidium level to be given? The owner or 
operator of a community or non-community water system that is required 
to determine a bin classification under Sec.  141.710, or to determine 
mean Cryptosporidium level under Sec.  141.712, must notify persons 
served by the water system that the determination has not been made as 
required no later than 30 days after the system has failed report the 
determination as specified in Sec.  141.710(e) or Sec.  141.712(a), 
respectively. The notice must be repeated as specified in Sec.  
141.203(b). The notice is not required if the system is complying with a 
State-approved schedule to address the violation.
    (c) What is the form and manner of the special notice? The form and 
manner of the public notice must follow the requirements for a Tier 2 
public notice prescribed in Sec.  141.203(c). The public notice must be 
presented as required in Sec.  141.205(c).
    (d) What mandatory language must be contained in the special notice? 
The notice must contain the following language, including the language 
necessary to fill in the blanks.
    (1) The special notice for repeated failure to conduct monitoring 
must contain the following language:

    We are required to monitor the source of your drinking water for 
Cryptosporidium. Results of the monitoring are to be used to determine 
whether water treatment at the (treatment plant name) is sufficient to 
adequately remove Cryptosporidium from your drinking water. We are 
required to complete this monitoring and make this determination by 
(required bin determination date). We ``did not monitor or test'' or 
``did not complete all monitoring or testing'' on schedule and, 
therefore, we may not be able to determine by the required date what 
treatment modifications, if any, must be made to ensure adequate 
Cryptosporidium removal. Missing this deadline may, in turn, jeopardize 
our ability to have the required

[[Page 634]]

treatment modifications, if any, completed by the deadline required, 
(date).
    For more information, please call (name of water system contact) of 
(name of water system) at (phone number).

    (2) The special notice for failure to determine bin classification 
or mean Cryptosporidium level must contain the following language:

    We are required to monitor the source of your drinking water for 
Cryptosporidium in order to determine by (date) whether water treatment 
at the (treatment plant name) is sufficient to adequately remove 
Cryptosporidium from your drinking water. We have not made this 
determination by the required date. Our failure to do this may 
jeopardize our ability to have the required treatment modifications, if 
any, completed by the required deadline of (date). For more information, 
please call (name of water system contact) of (name of water system) at 
(phone number).

    (3) Each special notice must also include a description of what the 
system is doing to correct the violation and when the system expects to 
return to compliance or resolve the situation.

[71 FR 768, Jan. 5, 2006]

[[Page 635]]

    Appendix A to Subpart Q of Part 141--NPDWR Violations and Other 
                 Situations Requiring Public Notice \1\

----------------------------------------------------------------------------------------------------------------
                                           MCL/MRDL/TT violations \2\          Monitoring & testing procedure
                                     --------------------------------------              violations
             Contaminant                                                   -------------------------------------
                                        Tier of public        Citation        Tier of public
                                       notice required                       notice required        Citation
----------------------------------------------------------------------------------------------------------------
I. Violations of National Primary
 Drinking Water Regulations (NPDWR):
 \3\................................
A. Microbiological Contaminants.....
    1.a Total coliform bacteria                       2          141.63(a)                  3     141.21(a)-(e).
     [dagger].......................
    1.b Total coliform (TT                            2      141.860(b)(1)                  3     141.860(c)(1).
     violations resulting from
     failure to perform assessments
     or corrective actions,
     monitoring violations, and
     reporting violations) [Dagger].
                                      .................  .................  .................     141.860(d)(1).
    1.c Seasonal system failure to                    2      141.860(b)(2)                  3     141.860(d)(3).
     follow State-approved start-up
     plan prior to serving water to
     the public or failure to
     provide certification to State
     [Dagger].......................
    2.a Fecal coliform/E. coli                        1          141.63(b)            \4\ 1,3          141.21(e)
     [dagger].......................
    2.b E. coli (MCL, monitoring,                     1        141.860 (a)                  3      141.860(c)(2)
     and reporting violations)
     [Dagger].......................
                                      .................  .................  .................     141.860(d)(1).
                                      .................  .................  .................     141.860(d)(2).
    2.c E. coli (TT violations                        2      141.860(b)(1)
     resulting from failure to
     perform level 2 Assessments or
     corrective action) [Dagger]....
    3. Turbidity MCL................                  2          141.13(a)                  3             141.22
    4. Turbidity MCL (average of 2             \5\ 2, 1          141.13(b)                  3             141.22
     days' samples 5 NTU)
    5. Turbidity (for TT violations            \6\ 2, 1      141.71(a)(2),                  3      141.74(a)(1),
     resulting from a single                              141.71(c)(2)(i),                         141.74(b)(2),
     exceedance of maximum allowable                         141.73(a)(2),                         141.74(c)(1),
     turbidity level)...............                        141.73 (b)(2),                              141.174,
                                                            141.73 (c)(2),                       141.560(a)-(c),
                                                                141.73(d),                              141.561.
                                                            141.173(a)(2),
                                                               141.173(b),
                                                                141.551(b)
    6. Surface Water Treatment Rule                   2      141.70-141.73                  3             141.74
     violations, other than
     violations resulting from
     single exceedance of max.
     allowable turbidity level (TT).
    7. Interim Enhanced Surface                   \7\ 2   141.170-141.173,                  3  141.172, 141.174,
     Water Treatment Rule                                  141.500-141.553                      141.530-141.544,
     violations, other than                                                                     141.560-141.564.
     violations resulting from
     single exceedance of max.
     turbidity level (TT)...........
    8. Filter Backwash Recycling                      2          141.76(c)                  3     141.76(b), (d)
     Rule violations................
    9. Long Term 1 Enhanced Surface                   2    141.500-141.553                  3   141.530-141.544,
     Water Treatment Rule violations                                                            141.560-141.564.
    10. LT2ESWTR violations.........                  2    141.710-141.720          \22\ 2, 3    141.701-141.705
                                                                                                    and 141.708-
                                                                                                        141.709.
    11. Ground Water Rule violations                  2            141.404                  3        141.402(h),
                                                                                                     141.403(d).
B. Inorganic Chemicals (IOCs)
    1. Antimony.....................                  2          141.62(b)                  3     141.23(a), (c)

[[Page 636]]

 
    2. Arsenic......................                  2      \8\ 141.62(b)                  3    \11\ 141.23(a),
                                                                                                             (c)
    3. Asbestos (fibers 10 [micro]m)................
    4. Barium.......................                  2          141.62(b)                  3     141.23(a), (c)
    5. Beryllium....................                  2          141.62(b)                  3     141.23(a), (c)
    6. Cadmium......................                  2          141.62(b)                  3     141.23(a), (c)
    7. Chromium (total).............                  2          141.62(b)                  3     141.23(a), (c)
    8. Cyanide......................                  2          141.62(b)                  3     141.23(a), (c)
    9. Fluoride.....................                  2          141.62(b)                  3     141.23(a), (c)
    10. Mercury (inorganic).........                  2          141.62(b)                  3     141.23(a), (c)
    11. Nitrate.....................                  1          141.62(b)          \12\ 1, 3    141.23(a), (d),
                                                                                                    141.23(f)(2)
    12. Nitrite.....................                  1          141.62(b)          \12\ 1, 3    141.23(a), (e),
                                                                                                    141.23(f)(2)
    13. Total Nitrate and Nitrite...                  1          141.62(b)                  3          141.23(a)
    14. Selenium....................                  2          141.62(b)                  3     141.23(a), (c)
    15. Thallium....................                  2          141.62(b)                  3     141.23(a), (c)
C. Lead and Copper Rule (Action
 Level for lead is 0.015 mg/L, for
 copper is 1.3 mg/L)
    1. Lead and Copper Rule (TT)....                  2      141.80-141.85                  3      141.86-141.89
D. Synthetic Organic Chemicals
 (SOCs)
    1. 2,4-D........................                  2          141.61(c)                  3          141.24(h)
    2. 2,4,5-TP (Silvex)............                  2          141.61(c)                  3          141.24(h)
    3. Alachlor.....................                  2          141.61(c)                  3          141.24(h)
    4. Atrazine.....................                  2          141.61(c)                  3          141.24(h)
    5. Benzo(a)pyrene (PAHs)........                  2          141.61(c)                  3          141.24(h)
    6. Carbofuran...................                  2          141.61(c)                  3          141.24(h)
    7. Chlordane....................                  2          141.61(c)                  3          141.24(h)
    8. Dalapon......................                  2          141.61(c)                  3          141.24(h)
    9. Di (2-ethylhexyl) adipate....                  2          141.61(c)                  3          141.24(h)
    10. Di (2-ethylhexyl) phthalate.                  2          141.61(c)                  3          141.24(h)
    11. Dibromochloropropane........                  2          141.61(c)                  3          141.24(h)
    12. Dinoseb.....................                  2          141.61(c)                  3          141.24(h)
    13. Dioxin (2,3,7,8-TCDD).......                  2          141.61(c)                  3          141.24(h)
    14. Diquat......................                  2          141.61(c)                  3          141.24(h)
    15. Endothall...................                  2          141.61(c)                  3          141.24(h)
    16. Endrin......................                  2          141.61(c)                  3          141.24(h)
    17. Ethylene dibromide..........                  2          141.61(c)                  3          141.24(h)
    18. Glyphosate..................                  2          141.61(c)                  3          141.24(h)
    19. Heptachlor..................                  2          141.61(c)                  3          141.24(h)
    20. Heptachlor epoxide..........                  2          141.61(c)                  3          141.24(h)
    21. Hexachlorobenzene...........                  2          141.61(c)                  3          141.24(h)
    22. Hexachlorocyclo-pentadiene..                  2          141.61(c)                  3          141.24(h)
    23. Lindane.....................                  2          141.61(c)                  3          141.24(h)
    24. Methoxychlor................                  2          141.61(c)                  3          141.24(h)
    25. Oxamyl (Vydate).............                  2          141.61(c)                  3          141.24(h)
    26. Pentachlorophenol...........                  2          141.61(c)                  3          141.24(h)

[[Page 637]]

 
    27. Picloram....................                  2          141.61(c)                  3          141.24(h)
    28. Polychlorinated biphenyls                     2          141.61(c)                  3          141.24(h)
     (PCBs).........................
    29. Simazine....................                  2          141.61(c)                  3          141.24(h)
    30. Toxaphene...................                  2          141.61(c)                  3          141.24(h)
E. Volatile Organic Chemicals (VOCs)
    1. Benzene......................                  2          141.61(a)                  3          141.24(f)
    2. Carbon tetrachloride.........                  2          141.61(a)                  3          141.24(f)
    3. Chlorobenzene                                  2          141.61(a)                  3          141.24(f)
     (monochlorobenzene)............
    4. o-Dichlorobenzene............                  2          141.61(a)                  3          141.24(f)
    5. p-Dichlorobenzene............                  2          141.61(a)                  3          141.24(f)
    6. 1,2-Dichloroethane...........                  2          141.61(a)                  3          141.24(f)
    7. 1,1-Dichloroethylene.........                  2          141.61(a)                  3          141.24(f)
    8. cis-1,2-Dichloroethylene.....                  2          141.61(a)                  3          141.24(f)
    9. trans-1,2-Dichloroethylene...                  2          141.61(a)                  3          141.24(f)
    10. Dichloromethane.............                  2          141.61(a)                  3          141.24(f)
    11. 1,2-Dichloropropane.........                  2          141.61(a)                  3          141.24(f)
    12. Ethylbenzene................                  2          141.61(a)                  3          141.24(f)
    13. Styrene.....................                  2          141.61(a)                  3          141.24(f)
    14. Tetrachloroethylene.........                  2          141.61(a)                  3          141.24(f)
    15. Toluene.....................                  2          141.61(a)                  3          141.24(f)
    16. 1,2,4-Trichlorobenzene......                  2          141.61(a)                  3          141.24(f)
    17. 1,1,1-Trichloroethane.......                  2          141.61(a)                  3          141.24(f)
    18. 1,1,2-Trichloroethane.......                  2          141.61(a)                  3          141.24(f)
    19. Trichloroethylene...........                  2          141.61(a)                  3          141.24(f)
    20. Vinyl chloride..............                  2          141.61(a)                  3          141.24(f)
    21. Xylenes (total).............                  2          141.61(a)                  3          141.24(f)
F. Radioactive Contaminants
    1. Beta/photon emitters.........                  2          141.66(d)                  3          141.25(a)
                                                                                                       141.26(b)
    2. Alpha emitters...............                  2          141.66(c)                  3          141.25(a)
                                                                                                       141.26(a)
    3. Combined radium (226 and 228)                  2          141.66(b)                  3          141.25(a)
                                                                                                       141.26(a)
    4. Uranium......................              \9\ 2          141.66(e)             \10\ 3          141.25(a)
                                                                                                       141.26(a)
G. Disinfection Byproducts (DBPs),
 Byproduct Precursors, Disinfectant
 Residuals. Where disinfection is
 used in the treatment of drinking
 water, disinfectants combine with
 organic and inorganic matter
 present in water to form chemicals
 called disinfection byproducts
 (DBPs). EPA sets standards for
 controlling the levels of
 disinfectants and DBPs in drinking
 water, including trihalomethanes
 (THMs) and haloacetic acids (HAAs).
 \13\
    1. Total trihalomethanes (TTHMs)                  2     \14\ 141.64(b)                  3    141.132(a)-(b),
                                                                                                141.600-141.605,
                                                                                                 141.620-141.629
    2. Haloacetic Acids (HAA5)......                  2          141.64(b)                  3    141.132(a)-(b),
                                                                                                141.600-141.605,
                                                                                                 141.620-141.629
    3. Bromate......................                  2          141.64(a)                  3     141.132(a)-(b)
    4. Chlorite.....................                  2          141.64(a)                  3     141.132(a)-(b)
    5. Chlorine (MRDL)..............                  2          141.65(a)                  3    141.132(a), (c)
    6. Chloramine (MRDL)............                  2          141.65(a)                  3    141.132(a), (c)

[[Page 638]]

 
    7. Chlorine dioxide (MRDL),                       2         141.65(a),          2 \15\, 3   141.132(a), (c),
     where any 2 consecutive daily                           141.133(c)(3)                         141.133(c)(2)
     samples at entrance to
     distribution system only are
     above MRDL.....................
    8. Chlorine dioxide (MRDL),                  \16\ 1         141.65(a),                  1   141.132(a), (c),
     where sample(s) in distribution                         141.133(c)(3)                         141.133(c)(2)
     system the next day are also
     above MRDL.....................
    9. Control of DBP precursors--                    2     141.135(a)-(b)                  3    141.132(a), (d)
     TOC (TT).......................
    10. Bench marking and                           N/A                N/A                  3   141.172 141.530-
     disinfection profiling.........                                                                    141.544.
    11. Development of monitoring                   N/A                N/A                  3         141.132(f)
     plan...........................
H. Other Treatment Techniques
    1. Acrylamide (TT)..............                  2            141.111                N/A                N/A
    2. Epichlorohydrin (TT).........                  2            141.111                N/A                N/A
II. Unregulated Contaminant
 Monitoring: \17\
A. Unregulated contaminants.........                N/A                N/A                  3             141.40
B. Nickel...........................                N/A                N/A                  3     141.23(c), (k)
III. Public Notification for
 Variances and Exemptions:
A. Operation under a variance or                      3   \18\ 1415, 1416,                N/A                N/A
 exemption..........................
B. Violation of conditions of a                       2   1415, 1416, \19\                N/A                N/A
 variance or exemption..............                               142.307
IV. Other Situations Requiring
 Public Notification:
A. Fluoride secondary maximum                         3              143.3                N/A                N/A
 contaminant level (SMCL) exceedance
B. Exceedance of nitrate MCL for non-                 1          141.11(d)                N/A                N/A
 community systems, as allowed by
 primacy agency.....................
C. Availability of unregulated                        3             141.40                N/A                N/A
 contaminant monitoring data........
D. Waterborne disease outbreak......                  1             141.2,                N/A                N/A
                                                          141.71(c)(2)(ii)
E. Other waterborne emergency \20\..                  1                N/A                N/A                N/A
F. Source Water Sample Positive for                   1         141.402(g)                N/A                N/A
 GWR Fecal indicators: E. coli,
 enterococci, or coliphage..........
G. Other situations as determined by       \21\ 1, 2, 3                N/A                N/A                N/A
 primacy agency.....................
----------------------------------------------------------------------------------------------------------------


[[Page 639]]

                          Appendix A--Endnotes

    [dagger] Until March 31, 2016.
    [Dagger] Beginning April 1, 2016.
    1. Violations and other situations not listed in this table (e.g., 
failure to prepare Consumer Confidence Reports), do not require notice, 
unless otherwise determined by the primacy agency. Primacy agencies may, 
at their option, also require a more stringent public notice tier (e.g., 
Tier 1 instead of Tier 2 or Tier 2 instead of Tier 3) for specific 
violations and situations listed in this Appendix, as authorized under 
Sec.  141.202(a) and Sec.  141.203(a).
    2. MCL--Maximum contaminant level, MRDL--Maximum residual 
disinfectant level, TT--Treatment technique
    3. The term Violations of National Primary Drinking Water 
Regulations (NPDWR) is used here to include violations of MCL, MRDL, 
treatment technique, monitoring, and testing procedure requirements.
    4. Failure to test for fecal coliform or E. coli is a Tier 1 
violation if testing is not done after any repeat sample tests positive 
for coliform. All other total coliform monitoring and testing procedure 
violations are Tier 3.
    5. Systems that violate the turbidity MCL of 5 NTU based on an 
average of measurements over two consecutive days must consult with the 
primacy agency within 24 hours after learning of the violation. Based on 
this consultation, the primacy agency may subsequently decide to elevate 
the violation to Tier 1. If a system is unable to make contact with the 
primacy agency in the 24-hour period, the violation is automatically 
elevated to Tier 1.
    6. Systems with treatment technique violations involving a single 
exceedance of a maximum turbidity limit under the Surface Water 
Treatment Rule (SWTR), the Interim Enhanced Surface Water Treatment Rule 
(IESWTR), or the Long Term 1 Enhanced Surface Water Treatment Rule 
(LT1ESWTR) are required to consult with the primacy agency within 24 
hours after learning of the violation. Based on this consultation, the 
primacy agency may subsequently decide to elevate the violation to Tier 
1. If a system is unable to make contact with the primacy agency in the 
24-hour period, the violation is automatically elevated to Tier 1.
    7. Most of the requirements of the Interim Enhanced Surface Water 
Treatment Rule (63 FR 69477) (Sec. Sec.  141.170-141.171, 141.173-
141.174) become effective January 1, 2002 for Subpart H systems (surface 
water systems and ground water systems under the direct influence of 
surface water) serving at least 10,000 persons. However, Sec.  141.172 
has some requirements that become effective as early as April 16, 1999. 
The Surface Water Treatment Rule remains in effect for systems serving 
at least 10,000 persons even after 2002; the Interim Enhanced Surface 
Water Treatment Rule adds additional requirements and does not in many 
cases supercede the SWTR.
    8. The arsenic MCL citations are effective January 23, 2006. Until 
then, the citations are Sec.  141.11(b) and Sec.  141.23(n).
    9. The uranium MCL Tier 2 violation citations are effective December 
8, 2003 for all community water systems.
    10. The uranium Tier 3 violation citations are effective December 8, 
2000 for all community water systems.
    11. The arsenic Tier 3 violation MCL citations are effective January 
23, 2006. Until then, the citations are Sec.  141.23(a), (l).
    12. Failure to take a confirmation sample within 24 hours for 
nitrate or nitrite after an initial sample exceeds the MCL is a Tier 1 
violation. Other monitoring violations for nitrate are Tier 3.
    13. Subpart H community and non-transient non-community systems 
serving =10,000 must comply with new DBP MCLs, disinfectant 
MRDLs, and related monitoring requirements beginning January 1, 2002. 
All other community and non-transient non-community systems must meet 
the MCLs and MRDLs beginning January 1, 2004. Subpart H transient non-
community systems serving 10,000 or more persons and using chlorine 
dioxide as a disinfectant or oxidant must comply with the chlorine 
dioxide MRDL beginning January 1, 2002. Subpart H transient non-
community systems serving fewer than 10,000 persons and using only 
ground water not under the direct influence of surface water and using 
chlorine dioxide as a disinfectant or oxidant must comply with the 
chlorine dioxide MRDL beginning January 1, 2004.
    14. Sec. Sec.  141.64(b)(1) 141.132(a)-(b) apply until Sec. Sec.  
141.620-141.630 take effect under the schedule in Sec.  141.620(c).
    15. Failure to monitor for chlorine dioxide at the entrance to the 
distribution system the day after exceeding the MRDL at the entrance to 
the distribution system is a Tier 2 violation.
    16. If any daily sample taken at the entrance to the distribution 
system exceeds the MRDL for chlorine dioxide and one or more samples 
taken in the distribution system the next day exceed the MRDL, Tier 1 
notification is required. Failure to take the required samples in the 
distribution system after the MRDL is exceeded at the entry point also 
triggers Tier 1 notification.
    17. Some water systems must monitor for certain unregulated 
contaminants listed in Sec.  141.40.
    18. This citation refers to Sec. Sec.  1415 and 1416 of the Safe 
Drinking Water Act. Sec. Sec.  1415 and 1416 require that ``a schedule 
prescribed. . . for a public water system granted a variance [or 
exemption] shall require compliance by the system. . .''

[[Page 640]]

    19. In addition to Sec. Sec.  1415 and 1416 of the Safe Drinking 
Water Act, 40 CFR 142.307 specifies the items and schedule milestones 
that must be included in a variance for small systems.
    20. Other waterborne emergencies require a Tier 1 public notice 
under Sec.  141.202(a) for situations that do not meet the definition of 
a waterborne disease outbreak given in 40 CFR 141.2 but that still have 
the potential to have serious adverse effects on health as a result of 
short-term exposure. These could include outbreaks not related to 
treatment deficiencies, as well as situations that have the potential to 
cause outbreaks, such as failures or significant interruption in water 
treatment processes, natural disasters that disrupt the water supply or 
distribution system, chemical spills, or unexpected loading of possible 
pathogens into the source water.
    21. Primacy agencies may place other situations in any tier they 
believe appropriate, based on threat to public health.
    22. Failure to collect three or more samples for Cryptosporidium 
analysis is a Tier 2 violation requiring special notice as specified in 
Sec.  141.211. All other monitoring and testing procedure violations are 
Tier 3.

[65 FR 26035, May 4, 2000, as amended at 65 FR 76750, Dec. 7, 2000; 66 
FR 7065, Jan. 22, 2001; 66 FR 31104, June 8, 2001; 67 FR 1836, Jan. 14, 
2002; 69 FR 38856, June 29, 2004; 71 FR 483, Jan. 4, 2006; 71 FR 768, 
Jan. 5, 2006; 71 FR 65652, Nov. 8, 2006; 78 FR 10350, Feb. 13, 2013; 79 
FR 10669, Feb. 26, 2014]

[[Page 641]]

 Appendix B to Subpart Q of Part 141--Standard Health Effects Language 
                         for Public Notification

----------------------------------------------------------------------------------------------------------------
                                                                          Standard health effects language for
          Contaminant              MCLG \1\ mg/L       MCL \2\ mg/L               public notification
----------------------------------------------------------------------------------------------------------------
                               National Primary Drinking Water Regulations (NPDWR)
                                         A. Microbiological Contaminants
----------------------------------------------------------------------------------------------------------------
1a. Total coliform [dagger]...  Zero                See footnote \3\   Coliforms are bacteria that are naturally
                                                                        present in the environment and are used
                                                                        as an indicator that other, potentially-
                                                                        harmful, bacteria may be present.
                                                                        Coliforms were found in more samples
                                                                        than allowed and this was a warning of
                                                                        potential problems.
1b. Fecal coliform/E. coli      Zero                Zero               Fecal coliforms and E. coli are bacteria
 [dagger].                                                              whose presence indicates that the water
                                                                        may be contaminated with human or animal
                                                                        wastes. Microbes in these wastes can
                                                                        cause short-term effects, such as
                                                                        diarrhea, cramps, nausea, headaches, or
                                                                        other symptoms. They may pose a special
                                                                        health risk for infants, young children,
                                                                        some of the elderly, and people with
                                                                        severely compromised immune systems.
1c. Fecal indicators (GWR):...  Zero                TT                 Fecal indicators are microbes whose
i. E. coli....................  None                TT                  presence indicates that the water may be
ii. enterococci...............  None                TT                  contaminated with human or animal
iii. coliphage................                                          wastes. Microbes in these wastes can
                                                                        cause short-term health effects, such as
                                                                        diarrhea, cramps, nausea, headaches, or
                                                                        other symptoms. They may pose a special
                                                                        health risk for infants, young children,
                                                                        some of the elderly, and people with
                                                                        severely compromised immune systems.
1d. Ground Water Rule (GWR) TT  None                TT                 Inadequately treated or inadequately
 violations.                                                            protected water may contain disease-
                                                                        causing organisms. These organisms can
                                                                        cause symptoms such as diarrhea, nausea,
                                                                        cramps, and associated headaches.
1e. Subpart Y Coliform          N/A                 TT                 Coliforms are bacteria that are naturally
 Assessment and/or Corrective                                           present in the environment and are used
 Action Violations [Dagger].                                            as an indicator that other, potentially
                                                                        harmful, waterborne pathogens may be
                                                                        present or that a potential pathway
                                                                        exists through which contamination may
                                                                        enter the drinking water distribution
                                                                        system. We found coliforms indicating
                                                                        the need to look for potential problems
                                                                        in water treatment or distribution. When
                                                                        this occurs, we are required to conduct
                                                                        assessments to identify problems and to
                                                                        correct any problems that are found.
                                                                       [THE SYSTEM MUST USE THE FOLLOWING
                                                                        APPLICABLE SENTENCES.]
                                                                       We failed to conduct the required
                                                                        assessment.
                                                                       We failed to correct all identified
                                                                        sanitary defects that were found during
                                                                        the assessment(s).
1f. Subpart Y E.coli            N/A                 TT                 E. coli are bacteria whose presence
 Assessment and/or Corrective                                           indicates that the water may be
 Action Violations [Dagger].                                            contaminated with human or animal
                                                                        wastes. Human pathogens in these wastes
                                                                        can cause short-term effects, such as
                                                                        diarrhea, cramps, nausea, headaches, or
                                                                        other symptoms. They may pose a greater
                                                                        health risk for infants, young children,
                                                                        the elderly, and people with severely
                                                                        compromised immune systems. We violated
                                                                        the standard for E. coli, indicating the
                                                                        need to look for potential problems in
                                                                        water treatment or distribution. When
                                                                        this occurs, we are required to conduct
                                                                        a detailed assessment to identify
                                                                        problems and to correct any problems
                                                                        that are found.
                                                                       [THE SYSTEM MUST USE THE FOLLOWING
                                                                        APPLICABLE SENTENCES.]
                                                                       We failed to conduct the required
                                                                        assessment.
                                                                       We failed to correct all identified
                                                                        sanitary defects that were found during
                                                                        the assessment that we conducted.

[[Page 642]]

 
1g. E. coli [Dagger]..........  Zero                In compliance      E. coli are bacteria whose presence
                                                     unless one of      indicates that the water may be
                                                     the following      contaminated with human or animal
                                                     conditions         wastes. Human pathogens in these wastes
                                                     occurs:            can cause short-term effects, such as
                                                    (1) The system      diarrhea, cramps, nausea, headaches, or
                                                     has an E. coli-    other symptoms. They may pose a greater
                                                     positive repeat    health risk for infants, young children,
                                                     sample following   the elderly, and people with severely
                                                     a total coliform-  compromised immune systems.
                                                     positive routine
                                                     sample.
                                                    (2) The system
                                                     has a total
                                                     coliform-
                                                     positive repeat
                                                     sample following
                                                     an E. coli-
                                                     positive routine
                                                     sample.
                                                    (3) The system
                                                     fails to take
                                                     all required
                                                     repeat samples
                                                     following an E.
                                                     coli-positive
                                                     routine sample.
                                                    (4) The system
                                                     fails to test
                                                     for E. coli when
                                                     any repeat
                                                     sample tests
                                                     positive for
                                                     total coliform.
1h. Subpart Y Seasonal System   N/A                 TT                 When this violation includes the failure
 TT Violations [Dagger].                                                to monitor for total coliforms or E.
                                                                        coli prior to serving water to the
                                                                        public, the mandatory language found at
                                                                        141.205(d)(2) must be used.
                                                                       When this violation includes failure to
                                                                        complete other actions, the appropriate
                                                                        elements found in 141.205(a) to describe
                                                                        the violation must be used.
2a. Turbidity (MCL) \4\.......  None                1 NTU \5\/5 NTU    Turbidity has no health effects. However,
                                                                        turbidity can interfere with
                                                                        disinfection and provide a medium for
                                                                        microbial growth. Turbidity may indicate
                                                                        the presence of disease-causing
                                                                        organisms. These organisms include
                                                                        bacteria, viruses, and parasites that
                                                                        can cause symptoms such as nausea,
                                                                        cramps, diarrhea and associated
                                                                        headaches.
2b. Turbidity (SWTR TT) \6\...  None                TT \7\             Turbidity has no health effects. However,
                                                                        turbidity can interfere with
                                                                        disinfection and provide a medium for
                                                                        microbial growth. Turbidity may indicate
                                                                        the presence of disease-causing
                                                                        organisms. These organisms include
                                                                        bacteria, viruses, and parasites that
                                                                        can cause symptoms such as nausea,
                                                                        cramps, diarrhea and associated
                                                                        headaches.

[[Page 643]]

 
2c. Turbidity (IESWTR TT and    None                TT                 Turbidity has no health effects. However,
 LT1ESWTR TT) \8\.                                                      turbidity can interfere with
                                                                        disinfection and provide a medium for
                                                                        microbial growth. Turbidity may indicate
                                                                        the presence of disease-causing
                                                                        organisms. These organisms include
                                                                        bacteria, viruses, and parasites that
                                                                        can cause symptoms such as nausea,
                                                                        cramps, diarrhea and associated
                                                                        headaches.
----------------------------------------------------------------------------------------------------------------
   B. Surface Water Treatment Rule (SWTR), Interim Enhanced Surface Water Treatment Rule (IESWTR), Long Term 1
    Enhanced Surface Water Treatment Rule (LT1ESWTR) and the Filter Backwash Recycling Rule (FBRR) violations
----------------------------------------------------------------------------------------------------------------
3. Giardia lamblia (SWTR/       Zero                TT \10\            Inadequately treated water may contain
 IESWTR/LT1ESWTR).                                                      disease-causing organisms. These
                                                                        organisms include bacteria, viruses, and
                                                                        parasites which can cause symptoms such
                                                                        as nausea, cramps, diarrhea, and
                                                                        associated headaches.
4. Viruses (SWTR/IESWTR/
 LT1ESWTR).
5. Heterotrophic plate count
 (HPC) bacteria \9\ (SWTR/
 IESWTR/LT1ESWTR).
6. Legionella (SWTR/IESWTR/
 LT1ESWTR).
7. Cryptosporidium (IESWTR/
 FBRR/LT1ESWTR).
----------------------------------------------------------------------------------------------------------------
                                          C. Inorganic Chemicals (IOCs)
----------------------------------------------------------------------------------------------------------------
8. Antimony...................  0.006               0.006              Some people who drink water containing
                                                                        antimony well in excess of the MCL over
                                                                        many years could experience increases in
                                                                        blood cholesterol and decreases in blood
                                                                        sugar.
9. Arsenic \11\...............  0                   0.010              Some people who drink water containing
                                                                        arsenic in excess of the MCL over many
                                                                        years could experience skin damage or
                                                                        problems with their circulatory system,
                                                                        and may have an increased risk of
                                                                        getting cancer.
10. Asbestos (10 [micro]m)....  7 MFL \12\          7 MFL              Some people who drink water containing
                                                                        asbestos in excess of the MCL over many
                                                                        years may have an increased risk of
                                                                        developing benign intestinal polyps.
11. Barium....................  2                   2                  Some people who drink water containing
                                                                        barium in excess of the MCL over many
                                                                        years could experience an increase in
                                                                        their blood pressure.
12. Beryllium.................  0.004               0.004              Some people who drink water containing
                                                                        beryllium well in excess of the MCL over
                                                                        many years could develop intestinal
                                                                        lesions.
13. Cadmium...................  0.005               0.005              Some people who drink water containing
                                                                        cadmium in excess of the MCL over many
                                                                        years could experience kidney damage.
14. Chromium (total)..........  0.1                 0.1                Some people who use water containing
                                                                        chromium well in excess of the MCL over
                                                                        many years could experience allergic
                                                                        dermatitis.
15. Cyanide...................  0.2                 0.2                Some people who drink water containing
                                                                        cyanide well in excess of the MCL over
                                                                        many years could experience nerve damage
                                                                        or problems with their thyroid.
16. Fluoride..................  4.0                 4.0                Some people who drink water containing
                                                                        fluoride in excess of the MCL over many
                                                                        years could get bone disease, including
                                                                        pain and tenderness of the bones.
                                                                        Fluoride in drinking water at half the
                                                                        MCL or more may cause mottling of
                                                                        children's teeth, usually in children
                                                                        less than nine years old. Mottling, also
                                                                        known as dental fluorosis, may include
                                                                        brown staining and/or pitting of the
                                                                        teeth, and occurs only in developing
                                                                        teeth before they erupt from the gums.
17. Mercury (inorganic).......  0.002               0.002              Some people who drink water containing
                                                                        inorganic mercury well in excess of the
                                                                        MCL over many years could experience
                                                                        kidney damage.
18. Nitrate...................  10                  10                 Infants below the age of six months who
                                                                        drink water containing nitrate in excess
                                                                        of the MCL could become seriously ill
                                                                        and, if untreated, may die. Symptoms
                                                                        include shortness of breath and blue
                                                                        baby syndrome.
19. Nitrite...................  1                   1                  Infants below the age of six months who
                                                                        drink water containing nitrite in excess
                                                                        of the MCL could become seriously ill
                                                                        and, if untreated, may die. Symptoms
                                                                        include shortness of breath and blue
                                                                        baby syndrome.

[[Page 644]]

 
20. Total Nitrate and Nitrite.  10                  10                 Infants below the age of six months who
                                                                        drink water containing nitrate and
                                                                        nitrite in excess of the MCL could
                                                                        become seriously ill and, if untreated,
                                                                        may die. Symptoms include shortness of
                                                                        breath and blue baby syndrome.
21. Selenium..................  0.05                0.05               Selenium is an essential nutrient.
                                                                        However, some people who drink water
                                                                        containing selenium in excess of the MCL
                                                                        over many years could experience hair or
                                                                        fingernail losses, numbness in fingers
                                                                        or toes, or problems with their
                                                                        circulation.
22. Thallium..................  0.0005              0.002              Some people who drink water containing
                                                                        thallium in excess of the MCL over many
                                                                        years could experience hair loss,
                                                                        changes in their blood, or problems with
                                                                        their kidneys, intestines, or liver.
----------------------------------------------------------------------------------------------------------------
                                             D. Lead and Copper Rule
----------------------------------------------------------------------------------------------------------------
23. Lead......................  Zero                TT \13\            Infants and children who drink water
                                                                        containing lead in excess of the action
                                                                        level could experience delays in their
                                                                        physical or mental development. Children
                                                                        could show slight deficits in attention
                                                                        span and learning abilities. Adults who
                                                                        drink this water over many years could
                                                                        develop kidney problems or high blood
                                                                        pressure.
24. Copper....................  1.3                 TT \14\            Copper is an essential nutrient, but some
                                                                        people who drink water containing copper
                                                                        in excess of the action level over a
                                                                        relatively short amount of time could
                                                                        experience gastrointestinal distress.
                                                                        Some people who drink water containing
                                                                        copper in excess of the action level
                                                                        over many years could suffer liver or
                                                                        kidney damage. People with Wilson's
                                                                        Disease should consult their personal
                                                                        doctor.
----------------------------------------------------------------------------------------------------------------
                                      E. Synthetic Organic Chemicals (SOCs)
----------------------------------------------------------------------------------------------------------------
25. 2,4-D.....................  0.07                0.07               Some people who drink water containing
                                                                        the weed killer 2,4-D well in excess of
                                                                        the MCL over many years could experience
                                                                        problems with their kidneys, liver, or
                                                                        adrenal glands.
26. 2,4,5-TP (Silvex).........  0.05                0.05               Some people who drink water containing
                                                                        silvex in excess of the MCL over many
                                                                        years could experience liver problems.
27. Alachlor..................  Zero                0.002              Some people who drink water containing
                                                                        alachlor in excess of the MCL over many
                                                                        years could have problems with their
                                                                        eyes, liver, kidneys, or spleen, or
                                                                        experience anemia, and may have an
                                                                        increased risk of getting cancer.
28. Atrazine..................  0.003               0.003              Some people who drink water containing
                                                                        atrazine well in excess of the MCL over
                                                                        many years could experience problems
                                                                        with their cardiovascular system or
                                                                        reproductive difficulties.
29. Benzo(a)pyrene (PAHs).....  Zero                0.0002             Some people who drink water containing
                                                                        benzo(a)pyrene in excess of the MCL over
                                                                        many years may experience reproductive
                                                                        difficulties and may have an increased
                                                                        risk of getting cancer.
30. Carbofuran................  0.04                0.04               Some people who drink water containing
                                                                        carbofuran in excess of the MCL over
                                                                        many years could experience problems
                                                                        with their blood, or nervous or
                                                                        reproductive systems.
31. Chlordane.................  Zero                0.002              Some people who drink water containing
                                                                        chlordane in excess of the MCL over many
                                                                        years could experience problems with
                                                                        their liver or nervous system, and may
                                                                        have an increased risk of getting
                                                                        cancer.
32. Dalapon...................  0.2                 0.2                Some people who drink water containing
                                                                        dalapon well in excess of the MCL over
                                                                        many years could experience minor kidney
                                                                        changes.
33. Di(2-ethylhexyl) adipate..  0.4                 0.4                Some people who drink water containing
                                                                        di(2-ethylhexyl) adipate well in excess
                                                                        of the MCL over many years could
                                                                        experience toxic effects such as weight
                                                                        loss, liver enlargement or possible
                                                                        reproductive difficulties.

[[Page 645]]

 
34. Di(2-ethylhexyl) phthalate  Zero                0.006              Some people who drink water containing
                                                                        di(2-ethylhexyl) phthalate well in
                                                                        excess of the MCL over many years may
                                                                        have problems with their liver, or
                                                                        experience reproductive difficulties,
                                                                        and may have an increased risk of
                                                                        getting cancer.
35. Dibromochloropropane        Zero                0.0002             Some people who drink water containing
 (DBCP).                                                                DBCP in excess of the MCL over many
                                                                        years could experience reproductive
                                                                        difficulties and may have an increased
                                                                        risk of getting cancer.
36. Dinoseb...................  0.007               0.007              Some people who drink water containing
                                                                        dinoseb well in excess of the MCL over
                                                                        many years could experience reproductive
                                                                        difficulties.
37. Dioxin (2,3,7,8-TCDD).....  Zero                3 x 10 -8          Some people who drink water containing
                                                                        dioxin in excess of the MCL over many
                                                                        years could experience reproductive
                                                                        difficulties and may have an increased
                                                                        risk of getting cancer.
38. Diquat....................  0.02                0.02               Some people who drink water containing
                                                                        diquat in excess of the MCL over many
                                                                        years could get cataracts.
39. Endothall.................  0.1                 0.1                Some people who drink water containing
                                                                        endothall in excess of the MCL over many
                                                                        years could experience problems with
                                                                        their stomach or intestines.
40. Endrin....................  0.002               0.002              Some people who drink water containing
                                                                        endrin in excess of the MCL over many
                                                                        years could experience liver problems.
41. Ethylene dibromide........  Zero                0.00005            Some people who drink water containing
                                                                        ethylene dibromide in excess of the MCL
                                                                        over many years could experience
                                                                        problems with their liver, stomach,
                                                                        reproductive system, or kidneys, and may
                                                                        have an increased risk of getting
                                                                        cancer.
42. Glyphosate................  0.7                 0.7                Some people who drink water containing
                                                                        glyphosate in excess of the MCL over
                                                                        many years could experience problems
                                                                        with their kidneys or reproductive
                                                                        difficulties.
43. Heptachlor................  Zero                0.0004             Some people who drink water containing
                                                                        heptachlor in excess of the MCL over
                                                                        many years could experience liver damage
                                                                        and may have an increased risk of
                                                                        getting cancer.
44. Heptachlor epoxide........  Zero                0.0002             Some people who drink water containing
                                                                        heptachlor epoxide in excess of the MCL
                                                                        over many years could experience liver
                                                                        damage, and may have an increased risk
                                                                        of getting cancer.
45. Hexachlorobenzene.........  Zero                0.001              Some people who drink water containing
                                                                        hexachlorobenzene in excess of the MCL
                                                                        over many years could experience
                                                                        problems with their liver or kidneys, or
                                                                        adverse reproductive effects, and may
                                                                        have an increased risk of getting
                                                                        cancer.
46. Hexachlorocyclo-pentadiene  0.05                0.05               Some people who drink water containing
                                                                        hexachlorocyclopentadiene well in excess
                                                                        of the MCL over many years could
                                                                        experience problems with their kidneys
                                                                        or stomach.
47. Lindane...................  0.0002              0.0002             Some people who drink water containing
                                                                        lindane in excess of the MCL over many
                                                                        years could experience problems with
                                                                        their kidneys or liver.
48. Methoxychlor..............  0.04                0.04               Some people who drink water containing
                                                                        methoxychlor in excess of the MCL over
                                                                        many years could experience reproductive
                                                                        difficulties.
49. Oxamyl (Vydate)...........  0.2                 0.2                Some people who drink water containing
                                                                        oxamyl in excess of the MCL over many
                                                                        years could experience slight nervous
                                                                        system effects.
50. Pentachlorophenol.........  Zero                0.001              Some people who drink water containing
                                                                        pentachlorophenol in excess of the MCL
                                                                        over many years could experience
                                                                        problems with their liver or kidneys,
                                                                        and may have an increased risk of
                                                                        getting cancer.
51. Picloram..................  0.5                 0.5                Some people who drink water containing
                                                                        picloram in excess of the MCL over many
                                                                        years could experience problems with
                                                                        their liver.
52. Polychlorinated biphenyls   Zero                0.0005             Some people who drink water containing
 (PCBs).                                                                PCBs in excess of the MCL over many
                                                                        years could experience changes in their
                                                                        skin, problems with their thymus gland,
                                                                        immune deficiencies, or reproductive or
                                                                        nervous system difficulties, and may
                                                                        have an increased risk of getting
                                                                        cancer.
53. Simazine..................  0.004               0.004              Some people who drink water containing
                                                                        simazine in excess of the MCL over many
                                                                        years could experience problems with
                                                                        their blood.
54. Toxaphene.................  Zero                0.003              Some people who drink water containing
                                                                        toxaphene in excess of the MCL over many
                                                                        years could have problems with their
                                                                        kidneys, liver, or thyroid, and may have
                                                                        an increased risk of getting cancer.
----------------------------------------------------------------------------------------------------------------

[[Page 646]]

 
                                      F. Volatile Organic Chemicals (VOCs)
----------------------------------------------------------------------------------------------------------------
55. Benzene...................  Zero                0.005              Some people who drink water containing
                                                                        benzene in excess of the MCL over many
                                                                        years could experience anemia or a
                                                                        decrease in blood platelets, and may
                                                                        have an increased risk of getting
                                                                        cancer.
56. Carbon tetrachloride......  Zero                0.005              Some people who drink water containing
                                                                        carbon tetrachloride in excess of the
                                                                        MCL over many years could experience
                                                                        problems with their liver and may have
                                                                        an increased risk of getting cancer.
57. Chlorobenzene (monochloro-  0.1                 0.1                Some people who drink water containing
 benzene).                                                              chlorobenzene in excess of the MCL over
                                                                        many years could experience problems
                                                                        with their liver or kidneys.
58. o-Dichlorobenzene.........  0.6                 0.6                Some people who drink water containing o-
                                                                        dichlorobenzene well in excess of the
                                                                        MCL over many years could experience
                                                                        problems with their liver, kidneys, or
                                                                        circulatory systems.
59. p-Dichlorobenzene.........  0.075               0.075              Some people who drink water containing p-
                                                                        dichlorobenzene in excess of the MCL
                                                                        over many years could experience anemia,
                                                                        damage to their liver, kidneys, or
                                                                        spleen, or changes in their blood.
60. 1,2-Dichloroethane........  Zero                0.005              Some people who drink water containing
                                                                        1,2-dichloroethane in excess of the MCL
                                                                        over many years may have an increased
                                                                        risk of getting cancer.
61. 1,1-Dichloroethylene......  0.007               0.007              Some people who drink water containing
                                                                        1,1-dichloroethylene in excess of the
                                                                        MCL over many years could experience
                                                                        problems with their liver.
62. cis-1,2-Dichloroethylene..  0.07                0.07               Some people who drink water containing
                                                                        cis-1,2-dichloroethylene in excess of
                                                                        the MCL over many years could experience
                                                                        problems with their liver.
63. trans-1,2-Dichloroethylene  0.1                 0.1                Some people who drink water containing
                                                                        trans-1,2-dichloroethylene well in
                                                                        excess of the MCL over many years could
                                                                        experience problems with their liver.
64. Dichloromethane...........  Zero                0.005              Some people who drink water containing
                                                                        dichloromethane in excess of the MCL
                                                                        over many years could have liver
                                                                        problems and may have an increased risk
                                                                        of getting cancer.
65. 1,2-Dichloropropane.......  Zero                0.005              Some people who drink water containing
                                                                        1,2-dichloropropane in excess of the MCL
                                                                        over many years may have an increased
                                                                        risk of getting cancer.
66. Ethylbenzene..............  0.7                 0.7                Some people who drink water containing
                                                                        ethylbenzene well in excess of the MCL
                                                                        over many years could experience
                                                                        problems with their liver or kidneys.
67. Styrene...................  0.1                 0.1                Some people who drink water containing
                                                                        styrene well in excess of the MCL over
                                                                        many years could have problems with
                                                                        their liver, kidneys, or circulatory
                                                                        system.
68. Tetrachloroethylene.......  Zero                0.005              Some people who drink water containing
                                                                        tetrachloroethylene in excess of the MCL
                                                                        over many years could have problems with
                                                                        their liver, and may have an increased
                                                                        risk of getting cancer.
69. Toluene...................  1                   1                  Some people who drink water containing
                                                                        toluene well in excess of the MCL over
                                                                        many years could have problems with
                                                                        their nervous system, kidneys, or liver.
70. 1,2,4-Trichlorobenzene....  0.07                0.07               Some people who drink water containing
                                                                        1,2,4-trichlorobenzene well in excess of
                                                                        the MCL over many years could experience
                                                                        changes in their adrenal glands.
71. 1,1,1-Trichloroethane.....  0.2                 0.2                Some people who drink water containing
                                                                        1,1,1-trichloroethane in excess of the
                                                                        MCL over many years could experience
                                                                        problems with their liver, nervous
                                                                        system, or circulatory system.
72. 1,1,2-Trichloroethane.....  0.003               0.005              Some people who drink water containing
                                                                        1,1,2-trichloroethane well in excess of
                                                                        the MCL over many years could have
                                                                        problems with their liver, kidneys, or
                                                                        immune systems.
73. Trichloroethylene.........  Zero                0.005              Some people who drink water containing
                                                                        trichloroethylene in excess of the MCL
                                                                        over many years could experience
                                                                        problems with their liver and may have
                                                                        an increased risk of getting cancer.
74. Vinyl chloride............  Zero                0.002              Some people who drink water containing
                                                                        vinyl chloride in excess of the MCL over
                                                                        many years may have an increased risk of
                                                                        getting cancer.

[[Page 647]]

 
75. Xylenes (total)...........  10                  10                 Some people who drink water containing
                                                                        xylenes in excess of the MCL over many
                                                                        years could experience damage to their
                                                                        nervous system.
----------------------------------------------------------------------------------------------------------------
                                           G. Radioactive Contaminants
----------------------------------------------------------------------------------------------------------------
76. Beta/photon emitters......  Zero                4 mrem/yr \15\     Certain minerals are radioactive and may
                                                                        emit forms of radiation known as photons
                                                                        and beta radiation. Some people who
                                                                        drink water containing beta and photon
                                                                        emitters in excess of the MCL over many
                                                                        years may have an increased risk of
                                                                        getting cancer.
77. Alpha emitters............  Zero                17 pCi/L \17\      Certain minerals are radioactive and may
                                                                        emit a form of radiation known as alpha
                                                                        radiation. Some people who drink water
                                                                        containing alpha emitters in excess of
                                                                        the MCL over many years may have an
                                                                        increased risk of getting cancer.
78. Combined radium (226 &      Zero                5 pCi/L            Some people who drink water containing
 228).                                                                  radium 226 or 228 in excess of the MCL
                                                                        over many years may have an increased
                                                                        risk of getting cancer.
79. Uranium \16\..............  Zero                30 [micro]g/L      Some people who drink water containing
                                                                        uranium in excess of the MCL over many
                                                                        years may have an increased risk of
                                                                        getting cancer and kidney toxicity.
----------------------------------------------------------------------------------------------------------------
 H. Disinfection Byproducts (DBPs), Byproduct Precursors, and Disinfectant Residuals: Where disinfection is used
 in the treatment of drinking water, disinfectants combine with organic and inorganic matter present in water to
     form chemicals called disinfection byproducts (DBPs). EPA sets standards for controlling the levels of
   disinfectants and DBPs in drinking water, including trihalomethanes (THMs) and haloacetic acids (HAAs) \18\
----------------------------------------------------------------------------------------------------------------
80. Total trihalomethanes       N/A                 0.080 \19 20\      Some people who drink water containing
 (TTHMs).                                                               trihalomethanes in excess of the MCL
                                                                        over many years may experience problems
                                                                        with their liver, kidneys, or central
                                                                        nervous system, and may have an
                                                                        increased risk of getting cancer.
81. Haloacetic Acids (HAA)....  N/A                 0.060 \21\         Some people who drink water containing
                                                                        haloacetic acids in excess of the MCL
                                                                        over many years may have an increased
                                                                        risk of getting cancer.
82. Bromate...................  Zero                0.010              Some people who drink water containing
                                                                        bromate in excess of the MCL over many
                                                                        years may have an increased risk of
                                                                        getting cancer.
83. Chlorite..................  0.08                1.0                Some infants and young children who drink
                                                                        water containing chlorite in excess of
                                                                        the MCL could experience nervous system
                                                                        effects. Similar effects may occur in
                                                                        fetuses of pregnant women who drink
                                                                        water containing chlorite in excess of
                                                                        the MCL. Some people may experience
                                                                        anemia.
84. Chlorine..................  4 (MRDLG) \22\      4.0 (MRDL) \23\    Some people who use water containing
                                                                        chlorine well in excess of the MRDL
                                                                        could experience irritating effects to
                                                                        their eyes and nose. Some people who
                                                                        drink water containing chlorine well in
                                                                        excess of the MRDL could experience
                                                                        stomach discomfort.
85. Chloramines...............  4 (MRDLG)           4.0 (MRDL)         Some people who use water containing
                                                                        chloramines well in excess of the MRDL
                                                                        could experience irritating effects to
                                                                        their eyes and nose. Some people who
                                                                        drink water containing chloramines well
                                                                        in excess of the MRDL could experience
                                                                        stomach discomfort or anemia.
86a. Chlorine dioxide, where    0.8 (MRDLG)         0.8 (MRDL)         Some infants and young children who drink
 any 2 consecutive daily                                                water containing chlorine dioxide in
 samples taken at the entrance                                          excess of the MRDL could experience
 to the distribution system                                             nervous system effects. Similar effects
 are above the MRDL.                                                    may occur in fetuses of pregnant women
                                                                        who drink water containing chlorine
                                                                        dioxide in excess of the MRDL. Some
                                                                        people may experience anemia.
                                                                       Add for public notification only: The
                                                                        chlorine dioxide violations reported
                                                                        today are the result of exceedances at
                                                                        the treatment facility only, not within
                                                                        the distribution system which delivers
                                                                        water to consumers. Continued compliance
                                                                        with chlorine dioxide levels within the
                                                                        distribution system minimizes the
                                                                        potential risk of these violations to
                                                                        consumers.
86b. Chlorine dioxide, where    0.8 (MRDLG)         0.8 (MRDL)         Some infants and young children who drink
 one or more distribution                                               water containing chlorine dioxide in
 system samples are above the                                           excess of the MRDL could experience
 MRDL.                                                                  nervous system effects. Similar effects
                                                                        may occur in fetuses of pregnant women
                                                                        who drink water containing chlorine
                                                                        dioxide in excess of the MRDL. Some
                                                                        people may experience anemia.

[[Page 648]]

 
                                                                       Add for public notification only: The
                                                                        chlorine dioxide violations reported
                                                                        today include exceedances of the EPA
                                                                        standard within the distribution system
                                                                        which delivers water to consumers.
                                                                        Violations of the chlorine dioxide
                                                                        standard within the distribution system
                                                                        may harm human health based on short-
                                                                        term exposures. Certain groups,
                                                                        including fetuses, infants, and young
                                                                        children, may be especially susceptible
                                                                        to nervous system effects from excessive
                                                                        chlorine dioxide exposure.
87. Control of DBP precursors   None                TT                 Total organic carbon (TOC) has no health
 (TOC).                                                                 effects. However, total organic carbon
                                                                        provides a medium for the formation of
                                                                        disinfection byproducts. These
                                                                        byproducts include trihalomethanes
                                                                        (THMs) and haloacetic acids (HAAs).
                                                                        Drinking water containing these
                                                                        byproducts in excess of the MCL may lead
                                                                        to adverse health effects, liver or
                                                                        kidney problems, or nervous system
                                                                        effects, and may lead to an increased
                                                                        risk of getting cancer.
----------------------------------------------------------------------------------------------------------------
                                          I. Other Treatment Techniques
----------------------------------------------------------------------------------------------------------------
88. Acrylamide................  Zero                TT                 Some people who drink water containing
                                                                        high levels of acrylamide over a long
                                                                        period of time could have problems with
                                                                        their nervous system or blood, and may
                                                                        have an increased risk of getting
                                                                        cancer.
89. Epichlorohydrin...........  Zero                TT                 Some people who drink water containing
                                                                        high levels of epichlorohydrin over a
                                                                        long period of time could experience
                                                                        stomach problems, and may have an
                                                                        increased risk of getting cancer.
----------------------------------------------------------------------------------------------------------------


[[Page 649]]

                          Appendix B--Endnotes

    [dagger] Until March 31, 2016.
    [Dagger] Beginning April 1, 2016.
    1. MCLG--Maximum contaminant level goal
    2. MCL--Maximum contaminant level
    3. For water systems analyzing at least 40 samples per month, no 
more than 5.0 percent of the monthly samples may be positive for total 
coliforms. For systems analyzing fewer than 40 samples per month, no 
more than one sample per month may be positive for total coliforms.
    4. There are various regulations that set turbidity standards for 
different types of systems, including 40 CFR 141.13, and the 1989 
Surface Water Treatment Rule, the 1998 Interim Enhanced Surface Water 
Treatment Rule and the 2002 Long Term 1 Enhanced Surface Water Treatment 
Rule. The MCL for the monthly turbidity average is 1 NTU; the MCL for 
the 2-day average is 5 NTU for systems that are required to filter but 
have not yet installed filtration (40 CFR 141.13).
    5. NTU--Nephelometric turbidity unit
    6. There are various regulations that set turbidity standards for 
different types of systems, including 40 CFR 141.13, and the 1989 
Surface Water Treatment Rule, the 1998 Interim Enhanced Surface Water 
Treatment Rule and the 2001 Long Term 1 Enhanced Surface Water Treatment 
Rule. Systems subject to the Surface Water Treatment Rule (both filtered 
and unfiltered) may not exceed 5 NTU. In addition, in filtered systems, 
95 percent of samples each month must not exceed 0.5 NTU in systems 
using conventional or direct filtration and must not exceed 1 NTU in 
systems using slow sand or diatomaceous earth filtration or other 
filtration technologies approved by the primacy agency.
    7. TT--Treatment technique
    8. There are various regulations that set turbidity standards for 
different types of systems, including 40 CFR 141.13, the 1989 Surface 
Water Treatment Rule (SWTR), the 1998 Interim Enhanced Surface Water 
Treatment Rule (IESWTR) and the 2002 Long Term 1 Enhanced Surface Water 
Treatment Rule (LT1ESWTR). For systems subject to the IESWTR (systems 
serving at least 10,000 people, using surface water or ground water 
under the direct influence of surface water), that use conventional 
filtration or direct filtration, after January 1, 2002, the turbidity 
level of a system's combined filter effluent may not exceed 0.3 NTU in 
at least 95 percent of monthly measurements, and the turbidity level of 
a system's combined filter effluent must not exceed 1 NTU at any time. 
Systems subject to the IESWTR using technologies other than 
conventional, direct, slow sand, or diatomaceous earth filtration must 
meet turbidity limits set by the primacy agency. For systems subject to 
the LT1ESWTR (systems serving fewer than 10,000 people, using surface 
water or ground water under the direct influence of surface water) that 
use conventional filtration or direct filtration, after January 1, 2005, 
the turbidity level of a system's combined filter effluent may not 
exceed 0.3 NTU in at least 95 percent of monthly measurements, and the 
turbidity level of a system's combined filter effluent must not exceed 1 
NTU at any time. Systems subject to the LT1ESWTR using technologies 
other than conventional, direct, slow sand, or diatomaceous earth 
filtration must meet turbidity limits set by the primacy agency.
    9. The bacteria detected by heterotrophic plate count (HPC) are not 
necessarily harmful. HPC is simply an alternative method of determining 
disinfectant residual levels. The number of such bacteria is an 
indicator of whether there is enough disinfectant in the distribution 
system.
    10. SWTR, IESWTR, and LT1ESWTR treatment technique violations that 
involve turbidity exceedances may use the health effects language for 
turbidity instead.
    11. These arsenic values are effective January 23, 2006. Until then, 
the MCL is 0.05 mg/L and there is no MCLG.
    12. Millions fibers per liter.
    13. Action Level = 0.015 mg/L
    14. Action Level = 1.3 mg/L
    15. Millirems per years
    16. The uranium MCL is effective December 8, 2003 for all community 
water systems.
    17. Picocuries per liter
    18. Surface water systems and ground water systems under the direct 
influence of surface water are regulated under subpart H of 40 CFR 141. 
Subpart H community and non-transient non-community systems serving 
=10,000 must comply with subpart L DBP MCLs and disinfectant 
maximum residual disinfectant levels (MRDLs) beginning January 1, 2002. 
All other community and non-transient non-community systems must comply 
with subpart L DBP MCLs and disinfectant MRDLs beginning January 1, 
2004. Subpart H transient non-community systems serving 
=10,000 that use chlorine dioxide as a disinfectant or 
oxidant must comply with the chlorine dioxide MRDL beginning January 1, 
2002. All other transient non-community systems that use chlorine 
dioxide as a disinfectant or oxidant must comply with the chlorine 
dioxide MRDL beginning January 1, 2004.
    19. Community and non-transient non-community systems must comply 
with subpart V TTHM and HAA5 MCLs of 0.080 mg/L and 0.060 mg/L, 
respectively (with compliance calculated as a locational running annual 
average) on the schedule in Sec.  141.620.
    20. The MCL for total trihalomethanes is the sum of the 
concentrations of the individual trihalomethanes.

[[Page 650]]

    21. The MCL for haloacetic acids is the sum of the concentrations of 
the individual haloacetic acids.
    22. MRDLG--Maximum residual disinfectant level goal.
    23. MRDL--Maximum residual disinfectant level.

[65 FR 26043, May 4, 2000; 65 FR 38629, June 21, 2000; 65 FR 40521, 
40522, June 30, 2000, as amended at 65 FR 76751, Dec. 7, 2000; 66 FR 
7065, Jan. 22, 2001; 66 FR 31104, June 8, 2001; 67 FR 1838, Jan. 14, 
2002; 67 FR 70857, Nov. 27, 2002; 68 FR 14507, Mar. 25, 2003; 69 FR 
38856, June 29, 2004; 71 FR 483, Jan. 4, 2006; 71 FR 65653, Nov. 8, 
2006; 78 FR 10351, Feb. 13, 2013]



   Sec. Appendix C to Subpart Q of Part 141--List of Acronyms Used in 
                     Public Notification Regulation

CCR Consumer Confidence Report
CWS Community Water System
DBP Disinfection Byproduct
EPA Environmental Protection Agency
GWR Ground Water Rule
HPC Heterotrophic Plate Count
IESWTR Interim Enhanced Surface Water Treatment Rule
IOC Inorganic Chemical
LCR Lead and Copper Rule
MCL Maximum Contaminant Level
MCLG Maximum Contaminant Level Goal
MRDL Maximum Residual Disinfectant Level
MRDLG Maximum Residual Disinfectant Level Goal
NCWS Non-Community Water System
NPDWR National Primary Drinking Water Regulation
NTNCWS Non-Transient Non-Community Water System
NTU Nephelometric Turbidity Unit
OGWDW Office of Ground Water and Drinking Water
OW Office of Water
PN Public Notification
PWS Public Water System
SDWA Safe Drinking Water Act
SMCL Secondary Maximum Contaminant Level
SOC Synthetic Organic Chemical
SWTR Surface Water Treatment Rule
TCR Total Coliform Rule
TT Treatment Technique
TWS Transient Non-Community Water System
VOC Volatile Organic Chemical

[65 FR 26035, May 4, 2000, as amended at 71 FR 65653, Nov. 8, 2006]

Subpart R [Reserved]



                       Subpart S_Ground Water Rule

    Source: 71 FR 65653, Nov. 8, 2006, unless otherwise noted.



Sec.  141.400  General requirements and applicability.

    (a) Scope of this subpart. The requirements of this subpart S 
constitute National Primary Drinking Water Regulations.
    (b) Applicability. This subpart applies to all public water systems 
that use ground water except that it does not apply to public water 
systems that combine all of their ground water with surface water or 
with ground water under the direct influence of surface water prior to 
treatment under subpart H. For the purposes of this subpart, ``ground 
water system'' is defined as any public water system meeting this 
applicability statement, including consecutive systems receiving 
finished ground water.
    (c) General requirements. Systems subject to this subpart must 
comply with the following requirements:
    (1) Sanitary survey information requirements for all ground water 
systems as described in Sec.  141.401.
    (2) Microbial source water monitoring requirements for ground water 
systems that do not treat all of their ground water to at least 99.99 
percent (4-log) treatment of viruses (using inactivation, removal, or a 
State-approved combination of 4-log virus inactivation and removal) 
before or at the first customer as described in Sec.  141.402.
    (3) Treatment technique requirements, described in Sec.  141.403, 
that apply to ground water systems that have fecally contaminated source 
waters, as determined by source water monitoring conducted under Sec.  
141.402, or that have significant deficiencies that are identified by 
the State or that are identified by EPA under SDWA section 1445. A 
ground water system with fecally contaminated source water or with 
significant deficiencies subject to the treatment technique requirements 
of this subpart must implement one or more of the following corrective 
action options: correct all significant deficiencies; provide an 
alternate source of water; eliminate the source of contamination; or 
provide treatment that

[[Page 651]]

reliably achieves at least 4-log treatment of viruses (using 
inactivation, removal, or a State-approved combination of 4-log virus 
inactivation and removal) before or at the first customer.
    (4) Ground water systems that provide at least 4-log treatment of 
viruses (using inactivation, removal, or a State-approved combination of 
4-log virus inactivation and removal) before or at the first customer 
are required to conduct compliance monitoring to demonstrate treatment 
effectiveness, as described in Sec.  141.403(b).
    (5) If requested by the State, ground water systems must provide the 
State with any existing information that will enable the State to 
perform a hydrogeologic sensitivity assessment. For the purposes of this 
subpart, ``hydrogeologic sensitivity assessment'' is a determination of 
whether ground water systems obtain water from hydrogeologically 
sensitive settings.
    (d) Compliance date. Ground water systems must comply, unless 
otherwise noted, with the requirements of this subpart beginning 
December 1, 2009.



Sec.  141.401  Sanitary surveys for ground water systems.

    (a) Ground water systems must provide the State, at the State's 
request, any existing information that will enable the State to conduct 
a sanitary survey.
    (b) For the purposes of this subpart, a ``sanitary survey,'' as 
conducted by the State, includes but is not limited to, an onsite review 
of the water source(s) (identifying sources of contamination by using 
results of source water assessments or other relevant information where 
available), facilities, equipment, operation, maintenance, and 
monitoring compliance of a public water system to evaluate the adequacy 
of the system, its sources and operations and the distribution of safe 
drinking water.
    (c) The sanitary survey must include an evaluation of the applicable 
components listed in paragraphs (c)(1) through (8) of this section:
    (1) Source,
    (2) Treatment,
    (3) Distribution system,
    (4) Finished water storage,
    (5) Pumps, pump facilities, and controls,
    (6) Monitoring, reporting, and data verification,
    (7) System management and operation, and
    (8) Operator compliance with State requirements.



Sec.  141.402  Ground water source microbial monitoring and analytical methods.

    (a) Triggered source water monitoring--
    (1) General requirements. A ground water system must conduct 
triggered source water monitoring if the conditions identified in 
paragraphs (a)(1)(i) and either (a)(1)(ii) or (a)(1)(iii) of this 
section exist.
    (i) The system does not provide at least 4-log treatment of viruses 
(using inactivation, removal, or a State-approved combination of 4-log 
virus inactivation and removal) before or at the first customer for each 
ground water source; and either
    (ii) The system is notified that a sample collected under Sec.  
141.21(a) is total coliform-positive and the sample is not invalidated 
under Sec.  141.21(c) until March 31, 2016, or
    (iii) The system is notified that a sample collected under 
Sec. Sec.  141.854 through 141.857 is total coliform-positive and the 
sample is not invalidated under Sec.  141.853(c) beginning April 1, 
2016.
    (2) Sampling requirements. A ground water system must collect, 
within 24 hours of notification of the total coliform-positive sample, 
at least one ground water source sample from each ground water source in 
use at the time the total coliform-positive sample was collected under 
Sec.  141.21(a) until March 31, 2016, or collected under Sec. Sec.  
141.854 through 141.857 beginning April 1, 2016, except as provided in 
paragraph (a)(2)(ii) of this section.
    (i) The State may extend the 24-hour time limit on a case-by-case 
basis if the system cannot collect the ground water source water sample 
within 24 hours due to circumstances beyond its control. In the case of 
an extension, the State must specify how much time the system has to 
collect the sample.
    (ii) If approved by the State, systems with more than one ground 
water

[[Page 652]]

source may meet the requirements of this paragraph (a)(2) by sampling a 
representative ground water source or sources. If directed by the State, 
systems must submit for State approval a triggered source water 
monitoring plan that identifies one or more ground water sources that 
are representative of each monitoring site in the system's sample siting 
plan under Sec.  141.21(a) until March 31, 2016, or under Sec.  141.853 
beginning April 1, 2016, and that the system intends to use for 
representative sampling under this paragraph.
    (iii) Until March 31, 2016, a ground water system serving 1,000 or 
fewer people may use a repeat sample collected from a ground water 
source to meet both the requirements of Sec.  141.21(b) and to satisfy 
the monitoring requirements of paragraph (a)(2) of this section for that 
ground water source only if the State approves the use of E. coli as a 
fecal indicator for source water monitoring under this paragraph (a). If 
the repeat sample collected from the ground water source is E. coli-
positive, the system must comply with paragraph (a)(3) of this section.
    (iv) Beginning April 1, 2016, a ground water system serving 1,000 or 
fewer people may use a repeat sample collected from a ground water 
source to meet both the requirements of subpart Y and to satisfy the 
monitoring requirements of paragraph (a)(2) of this section for that 
ground water source only if the State approves the use of E. coli as a 
fecal indicator for source water monitoring under this paragraph (a) and 
approves the use of a single sample for meeting both the triggered 
source water monitoring requirements in this paragraph (a) and the 
repeat monitoring requirements in Sec.  141.858. If the repeat sample 
collected from the ground water source is E. coli- positive, the system 
must comply with paragraph (a)(3) of this section.
    (3) Additional requirements. If the State does not require 
corrective action under Sec.  141.403(a)(2) for a fecal indicator-
positive source water sample collected under paragraph (a)(2) of this 
section that is not invalidated under paragraph (d) of this section, the 
system must collect five additional source water samples from the same 
source within 24 hours of being notified of the fecal indicator-positive 
sample.
    (4) Consecutive and wholesale systems. (i) In addition to the other 
requirements of this paragraph (a), a consecutive ground water system 
that has a total coliform-positive sample collected under Sec.  
141.21(a) until March 31, 2016, or under Sec. Sec.  141.854 through 
141.857 beginning April 1, 2016, must notify the wholesale system(s) 
within 24 hours of being notified of the total coliform-positive sample.
    (ii) In addition to the other requirements of this paragraph (a), a 
wholesale ground water system must comply with paragraphs (a)(4)(ii)(A) 
and (a)(4)(ii)(B) of this section.
    (A) A wholesale ground water system that receives notice from a 
consecutive system it serves that a sample collected under Sec.  
141.21(a) until March 31, 2016, or collected under Sec. Sec.  141.854 
through 141.857 beginning April 1, 2016, is total coliform-positive 
must, within 24 hours of being notified, collect a sample from its 
ground water source(s) under paragraph (a)(2) of this section and 
analyze it for a fecal indicator under paragraph (c) of this section.
    (B) If the sample collected under paragraph (a)(4)(ii)(A) of this 
section is fecal indicator-positive, the wholesale ground water system 
must notify all consecutive systems served by that ground water source 
of the fecal indicator source water positive within 24 hours of being 
notified of the ground water source sample monitoring result and must 
meet the requirements of paragraph (a)(3) of this section.
    (5) Exceptions to the triggered source water monitoring 
requirements. A ground water system is not required to comply with the 
source water monitoring requirements of paragraph (a) of this section if 
either of the following conditions exists:
    (i) The State determines, and documents in writing, that the total 
coliform-positive sample collected under Sec.  141.21(a) until March 31, 
2016, or under Sec. Sec.  141.854 through 141.857 beginning April 1, 
2016, is caused by a distribution system deficiency; or
    (ii) The total coliform-positive sample collected under Sec.  
141.21(a) until March 31, 2016, or under Sec. Sec.  141.854 through 
141.857 beginning April 1, 2016,

[[Page 653]]

is collected at a location that meets State criteria for distribution 
system conditions that will cause total coliform-positive samples.
    (b) Assessment source water monitoring. If directed by the State, 
ground water systems must conduct assessment source water monitoring 
that meets State-determined requirements for such monitoring. A ground 
water system conducting assessment source water monitoring may use a 
triggered source water sample collected under paragraph (a)(2) of this 
section to meet the requirements of paragraph (b) of this section. 
State-determined assessment source water monitoring requirements may 
include:
    (1) Collection of a total of 12 ground water source samples that 
represent each month the system provides ground water to the public,
    (2) Collection of samples from each well unless the system obtains 
written State approval to conduct monitoring at one or more wells within 
the ground water system that are representative of multiple wells used 
by that system and that draw water from the same hydrogeologic setting,
    (3) Collection of a standard sample volume of at least 100 mL for 
fecal indicator analysis regardless of the fecal indicator or analytical 
method used,
    (4) Analysis of all ground water source samples using one of the 
analytical methods listed in the in paragraph (c)(2) of this section for 
the presence of E. coli, enterococci, or coliphage,
    (5) Collection of ground water source samples at a location prior to 
any treatment of the ground water source unless the State approves a 
sampling location after treatment, and
    (6) Collection of ground water source samples at the well itself 
unless the system's configuration does not allow for sampling at the 
well itself and the State approves an alternate sampling location that 
is representative of the water quality of that well.
    (c) Analytical methods. (1) A ground water system subject to the 
source water monitoring requirements of paragraph (a) of this section 
must collect a standard sample volume of at least 100 mL for fecal 
indicator analysis regardless of the fecal indicator or analytical 
method used.
    (2) A ground water system must analyze all ground water source 
samples collected under paragraph (a) of this section using one of the 
analytical methods listed in the following table in paragraph (c)(2) of 
this section or one of the alternative methods listed in appendix A to 
subpart C of this part for the presence of E. coli, enterococci, or 
coliphage:

             Analytical Methods for Source Water Monitoring
------------------------------------------------------------------------
      Fecal indicator \1\             Methodology        Method citation
------------------------------------------------------------------------
E. coli.......................  Colilert \3\..........  9223 B.\2\
                                Colisure \3\..........  9223 B.\2\
                                Membrane Filter Method  EPA Method
                                 with MI Agar.           1604.\4\
                                m-ColiBlue24 Test \5\.
                                E*Colite Test \6\.....
                                EC-MUG \7\............  9221 F.\2\
                                NA-MUG \7\............  9222 G.\2\
Enterococci                     Multiple-Tube           9230B.\2\
                                 Technique.
                                Membrane Filter         9230C.\2\
                                 Technique.
                                Membrane Filter         EPA Method
                                 Technique.              1600.\8\
                                Enterolert \9\........
Coliphage.....................  Two-Step Enrichment     EPA Method
                                 Presence-Absence        1601.\10\
                                 Procedure.
                                Single Agar Layer       EPA Method
                                 Procedure.              1602.\11\
------------------------------------------------------------------------
Analyses must be conducted in accordance with the documents listed
  below. The Director of the Federal Register approves the incorporation
  by reference of the documents listed in footnotes 2-11 in accordance
  with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be
  obtained from the sources listed below. Copies may be inspected at
  EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW.,
  EPA West, Room B102, Washington DC 20460 (Telephone: 202-566-2426); or
  at the National Archives and Records Administration (NARA). For
  information on the availability of this material at NARA, call 202-741-
  6030, or go to: http://www.archives.gov/federal_register/
  code_of_federal_regulations/ibr_locations.html.
\1\ The time from sample collection to initiation of analysis may not
  exceed 30 hours. The ground water system is encouraged but is not
  required to hold samples below 10 [deg]C during transit.
\2\ Methods are described in Standard Methods for the Examination of
  Water and Wastewater 20th edition (1998) and copies may be obtained
  from the American Public Health Association, 1015 Fifteenth Street,
  NW., Washington, DC 20005-2605.
\3\ Medium is available through IDEXX Laboratories, Inc., One IDEXX
  Drive, Westbrook, Maine 04092.

[[Page 654]]

 
\4\ EPA Method 1604: Total Coliforms and Escherichia coli in Water by
  Membrane Filtration Using a Simultaneous Detection Technique (MI
  Medium); September 2002, EPA 821-R-02-024. Method is available at
  http://www.epa.gov/nerlcwww/1604sp02.pdf or from EPA's Water Resource
  Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington, DC
  20460.
\5\ A description of the m-ColiBlue24 Test, ``Total Coliforms and E.
  coli Membrane Filtration Method with m-ColiBlue24 [supreg] Broth,''
  Method No. 10029 Revision 2, August 17, 1999, is available from Hach
  Company, 100 Dayton Ave., Ames, IA 50010 or from EPA's Water Resource
  Center (RC-4100T), 1200 Pennsylvania Avenue, NW., Washington, DC
  20460.
\6\ A description of the E*Colite Test, ``Charm E*Colite Presence/
  Absence Test for Detection and Identification of Coliform Bacteria and
  Escherichia coli in Drinking Water, January 9, 1998, is available from
  Charm Sciences, Inc., 659 Andover St., Lawrence, MA 01843-1032 or from
  EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue, NW.,
  Washington, DC 20460.
\7\ EC-MUG (Method 9221F) or NA-MUG (Method 9222G) can be used for E.
  coli testing step as described in Sec.   141.21(f)(6)(i) or (ii) after
  use of Standard Methods 9221 B, 9221 D, 9222 B, or 9222 C.
\8\ EPA Method 1600: Enterococci in Water by Membrane Filtration Using
  membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI) EPA 821-R-
  02-022 (September 2002) is an approved variation of Standard Method
  9230C. The method is available at http://www.epa.gov/nerlcwww/
  1600sp02.pdf or from EPA's Water Resource Center (RC-4100T), 1200
  Pennsylvania Avenue, NW., Washington, DC 20460. The holding time and
  temperature for ground water samples are specified in footnote 1
  above, rather than as specified in Section 8 of EPA Method 1600.
\9\ Medium is available through IDEXX Laboratories, Inc., One IDEXX
  Drive, Westbrook, Maine 04092. Preparation and use of the medium is
  set forth in the article ``Evaluation of Enterolert for Enumeration of
  Enterococci in Recreational Waters,'' by Budnick, G.E., Howard, R.T.,
  and Mayo, D.R., 1996, Applied and Environmental Microbiology, 62:3881-
  3884.
\10\ EPA Method 1601: Male-specific (F + ) and Somatic Coliphage in
  Water by Two-step Enrichment Procedure; April 2001, EPA 821-R-01-030.
  Method is available at http://www.epa.gov/nerlcwww/1601ap01.pdf or
  from EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania Avenue,
  NW., Washington, DC 20460.
\11\ EPA Method 1602: Male-specific (F + ) and Somatic Coliphage in
  Water by Single Agar Layer (SAL) Procedure; April 2001, EPA 821-R-01-
  029. Method is available at http://www.epa.gov/nerlcwww/1602ap01.pdf
  or from EPA's Water Resource Center (RC-4100T), 1200 Pennsylvania
  Avenue, NW., Washington, DC 20460.

    (d) Invalidation of a fecal indicator-positive ground water source 
sample. (1) A ground water system may obtain State invalidation of a 
fecal indicator-positive ground water source sample collected under 
paragraph (a) of this section only under the conditions specified in 
paragraphs (d)(1)(i) and (ii) of this section.
    (i) The system provides the State with written notice from the 
laboratory that improper sample analysis occurred; or
    (ii) The State determines and documents in writing that there is 
substantial evidence that a fecal indicator-positive ground water source 
sample is not related to source water quality.
    (2) If the State invalidates a fecal indicator-positive ground water 
source sample, the ground water system must collect another source water 
sample under paragraph (a) of this section within 24 hours of being 
notified by the State of its invalidation decision and have it analyzed 
for the same fecal indicator using the analytical methods in paragraph 
(c) of this section. The State may extend the 24-hour time limit on a 
case-by-case basis if the system cannot collect the source water sample 
within 24 hours due to circumstances beyond its control. In the case of 
an extension, the State must specify how much time the system has to 
collect the sample.
    (e) Sampling location. (1) Any ground water source sample required 
under paragraph (a) of this section must be collected at a location 
prior to any treatment of the ground water source unless the State 
approves a sampling location after treatment.
    (2) If the system's configuration does not allow for sampling at the 
well itself, the system may collect a sample at a State-approved 
location to meet the requirements of paragraph (a) of this section if 
the sample is representative of the water quality of that well.
    (f) New sources. If directed by the State, a ground water system 
that places a new ground water source into service after November 30, 
2009, must conduct assessment source water monitoring under paragraph 
(b) of this section. If directed by the State, the system must begin 
monitoring before the ground water source is used to provide water to 
the public.
    (g) Public notification. A ground water system with a ground water 
source sample collected under paragraph (a) or (b) of this section that 
is fecal indicator-positive and that is not invalidated under paragraph 
(d) of this section, including consecutive systems served by the ground 
water source, must conduct public notification under Sec.  141.202.
    (h) Monitoring violations. Failure to meet the requirements of 
paragraphs (a)-(f) of this section is a monitoring violation and 
requires the ground water system to provide public notification under 
Sec.  141.204.

[71 FR 65653, Nov. 8, 2006; 71 FR 67427, Nov. 21, 2006, as amended at 74 
FR 30958, June 29, 2009; 78 FR 10353, Feb. 13, 2013]

[[Page 655]]



Sec.  141.403  Treatment technique requirements for ground water systems.

    (a) Ground water systems with significant deficiencies or source 
water fecal contamination. (1) The treatment technique requirements of 
this section must be met by ground water systems when a significant 
deficiency is identified or when a ground water source sample collected 
under Sec.  141.402(a)(3) is fecal indicator-positive.
    (2) If directed by the State, a ground water system with a ground 
water source sample collected under Sec.  141.402(a)(2), Sec.  
141.402(a)(4), or Sec.  141.402(b) that is fecal indicator-positive must 
comply with the treatment technique requirements of this section.
    (3) When a significant deficiency is identified at a Subpart H 
public water system that uses both ground water and surface water or 
ground water under the direct influence of surface water, the system 
must comply with provisions of this paragraph except in cases where the 
State determines that the significant deficiency is in a portion of the 
distribution system that is served solely by surface water or ground 
water under the direct influence of surface water.
    (4) Unless the State directs the ground water system to implement a 
specific corrective action, the ground water system must consult with 
the State regarding the appropriate corrective action within 30 days of 
receiving written notice from the State of a significant deficiency, 
written notice from a laboratory that a ground water source sample 
collected under Sec.  141.402(a)(3) was found to be fecal indicator-
positive, or direction from the State that a fecal indicator'positive 
collected under Sec.  141.402(a)(2), Sec.  141.402(a)(4), or Sec.  
141.402(b) requires corrective action. For the purposes of this subpart, 
significant deficiencies include, but are not limited to, defects in 
design, operation, or maintenance, or a failure or malfunction of the 
sources, treatment, storage, or distribution system that the State 
determines to be causing, or have potential for causing, the 
introduction of contamination into the water delivered to consumers.
    (5) Within 120 days (or earlier if directed by the State) of 
receiving written notification from the State of a significant 
deficiency, written notice from a laboratory that a ground water source 
sample collected under Sec.  141.402(a)(3) was found to be fecal 
indicator-positive, or direction from the State that a fecal indicator-
positive sample collected under Sec.  141.402(a)(2), Sec.  
141.402(a)(4), or Sec.  141.402(b) requires corrective action, the 
ground water system must either:
    (i) Have completed corrective action in accordance with applicable 
State plan review processes or other State guidance or direction, if 
any, including State-specified interim measures; or
    (ii) Be in compliance with a State-approved corrective action plan 
and schedule subject to the conditions specified in paragraphs 
(a)(5)(ii)(A) and (a)(5)(ii)(B) of this section.
    (A) Any subsequent modifications to a State-approved corrective 
action plan and schedule must also be approved by the State.
    (B) If the State specifies interim measures for protection of the 
public health pending State approval of the corrective action plan and 
schedule or pending completion of the corrective action plan, the system 
must comply with these interim measures as well as with any schedule 
specified by the State.
    (6) Corrective action alternatives. Ground water systems that meet 
the conditions of paragraph (a)(1) or (a)(2) of this section must 
implement one or more of the following corrective action alternatives:
    (i) Correct all significant deficiencies;
    (ii) Provide an alternate source of water;
    (iii) Eliminate the source of contamination; or
    (iv) Provide treatment that reliably achieves at least 4-log 
treatment of viruses (using inactivation, removal, or a State-approved 
combination of 4-log virus inactivation and removal) before or at the 
first customer for the ground water source.
    (7) Special notice to the public of significant deficiencies or 
source water fecal contamination. (i) In addition to the applicable 
public notification requirements of Sec.  141.202, a community ground 
water system that receives notice from

[[Page 656]]

the State of a significant deficiency or notification of a fecal 
indicator-positive ground water source sample that is not invalidated by 
the State under Sec.  141.402(d) must inform the public served by the 
water system under Sec.  141.153(h)(6) of the fecal indicator-positive 
source sample or of any significant deficiency that has not been 
corrected. The system must continue to inform the public annually until 
the significant deficiency is corrected or the fecal contamination in 
the ground water source is determined by the State to be corrected under 
paragraph (a)(5) of this section.
    (ii) In addition to the applicable public notification requirements 
of Sec.  141.202, a non-community ground water system that receives 
notice from the State of a significant deficiency must inform the public 
served by the water system in a manner approved by the State of any 
significant deficiency that has not been corrected within 12 months of 
being notified by the State, or earlier if directed by the State. The 
system must continue to inform the public annually until the significant 
deficiency is corrected. The information must include:
    (A) The nature of the significant deficiency and the date the 
significant deficiency was identified by the State;
    (B) The State-approved plan and schedule for correction of the 
significant deficiency, including interim measures, progress to date, 
and any interim measures completed; and
    (C) For systems with a large proportion of non-English speaking 
consumers, as determined by the State, information in the appropriate 
language(s) regarding the importance of the notice or a telephone number 
or address where consumers may contact the system to obtain a translated 
copy of the notice or assistance in the appropriate language.
    (iii) If directed by the State, a non-community water system with 
significant deficiencies that have been corrected must inform its 
customers of the significant deficiencies, how the deficiencies were 
corrected, and the dates of correction under paragraph (a)(7)(ii) of 
this section.
    (b) Compliance monitoring--(1) Existing ground water sources. A 
ground water system that is not required to meet the source water 
monitoring requirements of this subpart for any ground water source 
because it provides at least 4-log treatment of viruses (using 
inactivation, removal, or a State-approved combination of 4-log virus 
inactivation and removal) before or at the first customer for any ground 
water source before December 1, 2009, must notify the State in writing 
that it provides at least 4-log treatment of viruses (using 
inactivation, removal, or a State-approved combination of 4-log virus 
inactivation and removal) before or at the first customer for the 
specified ground water source and begin compliance monitoring in 
accordance with paragraph (b)(3) of this section by December 1, 2009. 
Notification to the State must include engineering, operational, or 
other information that the State requests to evaluate the submission. If 
the system subsequently discontinues 4-log treatment of viruses (using 
inactivation, removal, or a State-approved combination of 4-log virus 
inactivation and removal) before or at the first customer for a ground 
water source, the system must conduct ground water source monitoring as 
required under Sec.  141.402.
    (2) New ground water sources. A ground water system that places a 
ground water source in service after November 30, 2009, that is not 
required to meet the source water monitoring requirements of this 
subpart because the system provides at least 4-log treatment of viruses 
(using inactivation, removal, or a State-approved combination of 4-log 
virus inactivation and removal) before or at the first customer for the 
ground water source must comply with the requirements of paragraphs 
(b)(2)(i), (b)(2)(ii) and (b)(2)(iii) of this section.
    (i) The system must notify the State in writing that it provides at 
least 4-log treatment of viruses (using inactivation, removal, or a 
State-approved combination of 4-log virus inactivation and removal) 
before or at the first customer for the ground water source. 
Notification to the State must include engineering, operational, or 
other information that the State requests to evaluate the submission.

[[Page 657]]

    (ii) The system must conduct compliance monitoring as required under 
Sec.  141.403(b)(3) of this subpart within 30 days of placing the source 
in service.
    (iii) The system must conduct ground water source monitoring under 
Sec.  141.402 if the system subsequently discontinues 4-log treatment of 
viruses (using inactivation, removal, or a State-approved combination of 
4-log virus inactivation and removal) before or at the first customer 
for the ground water source.
    (3) Monitoring requirements. A ground water system subject to the 
requirements of paragraphs (a), (b)(1) or (b)(2) of this section must 
monitor the effectiveness and reliability of treatment for that ground 
water source before or at the first customer as follows:
    (i) Chemical disinfection--(A) Ground water systems serving greater 
than 3,300 people. A ground water system that serves greater than 3,300 
people must continuously monitor the residual disinfectant concentration 
using analytical methods specified in Sec.  141.74(a)(2) at a location 
approved by the State and must record the lowest residual disinfectant 
concentration each day that water from the ground water source is served 
to the public. The ground water system must maintain the State-
determined residual disinfectant concentration every day the ground 
water system serves water from the ground water source to the public. If 
there is a failure in the continuous monitoring equipment, the ground 
water system must conduct grab sampling every four hours until the 
continuous monitoring equipment is returned to service. The system must 
resume continuous residual disinfectant monitoring within 14 days.
    (B) Ground water systems serving 3,300 or fewer people. A ground 
water system that serves 3,300 or fewer people must monitor the residual 
disinfectant concentration using analytical methods specified in Sec.  
141.74(a)(2) at a location approved by the State and record the residual 
disinfection concentration each day that water from the ground water 
source is served to the public. The ground water system must maintain 
the State-determined residual disinfectant concentration every day the 
ground water system serves water from the ground water source to the 
public. The ground water system must take a daily grab sample during the 
hour of peak flow or at another time specified by the State. If any 
daily grab sample measurement falls below the State-determined residual 
disinfectant concentration, the ground water system must take follow-up 
samples every four hours until the residual disinfectant concentration 
is restored to the State-determined level. Alternatively, a ground water 
system that serves 3,300 or fewer people may monitor continuously and 
meet the requirements of paragraph (b)(3)(i)(A) of this section.
    (ii) Membrane filtration. A ground water system that uses membrane 
filtration to meet the requirements of this subpart must monitor the 
membrane filtration process in accordance with all State-specified 
monitoring requirements and must operate the membrane filtration in 
accordance with all State-specified compliance requirements. A ground 
water system that uses membrane filtration is in compliance with the 
requirement to achieve at least 4-log removal of viruses when:
    (A) The membrane has an absolute molecular weight cut-off (MWCO), or 
an alternate parameter that describes the exclusion characteristics of 
the membrane, that can reliably achieve at least 4-log removal of 
viruses;
    (B) The membrane process is operated in accordance with State-
specified compliance requirements; and
    (C) The integrity of the membrane is intact.
    (iii) Alternative treatment. A ground water system that uses a 
State-approved alternative treatment to meet the requirements of this 
subpart by providing at least 4-log treatment of viruses (using 
inactivation, removal, or a State-approved combination of 4-log virus 
inactivation and removal) before or at the first customer must:
    (A) Monitor the alternative treatment in accordance with all State-
specified monitoring requirements; and
    (B) Operate the alternative treatment in accordance with all 
compliance requirements that the State determines to be necessary to 
achieve at least 4-log treatment of viruses.
    (c) Discontinuing treatment. A ground water system may discontinue 
4-log

[[Page 658]]

treatment of viruses (using inactivation, removal, or a State-approved 
combination of 4-log virus inactivation and removal) before or at the 
first customer for a ground water source if the State determines and 
documents in writing that 4-log treatment of viruses is no longer 
necessary for that ground water source. A system that discontinues 4-log 
treatment of viruses is subject to the source water monitoring and 
analytical methods requirements of Sec.  141.402 of this subpart.
    (d) Failure to meet the monitoring requirements of paragraph (b) of 
this section is a monitoring violation and requires the ground water 
system to provide public notification under Sec.  141.204.



Sec.  141.404  Treatment technique violations for ground water systems.

    (a) A ground water system with a significant deficiency is in 
violation of the treatment technique requirement if, within 120 days (or 
earlier if directed by the State) of receiving written notice from the 
State of the significant deficiency, the system:
    (1) Does not complete corrective action in accordance with any 
applicable State plan review processes or other State guidance and 
direction, including State specified interim actions and measures, or
    (2) Is not in compliance with a State-approved corrective action 
plan and schedule.
    (b) Unless the State invalidates a fecal indicator-positive ground 
water source sample under Sec.  141.402(d), a ground water system is in 
violation of the treatment technique requirement if, within 120 days (or 
earlier if directed by the State) of meeting the conditions of Sec.  
141.403(a)(1) or Sec.  141.403(a)(2), the system:
    (1) Does not complete corrective action in accordance with any 
applicable State plan review processes or other State guidance and 
direction, including State-specified interim measures, or
    (2) Is not in compliance with a State-approved corrective action 
plan and schedule.
    (c) A ground water system subject to the requirements of Sec.  
141.403(b)(3) that fails to maintain at least 4-log treatment of viruses 
(using inactivation, removal, or a State-approved combination of 4-log 
virus inactivation and removal) before or at the first customer for a 
ground water source is in violation of the treatment technique 
requirement if the failure is not corrected within four hours of 
determining the system is not maintaining at least 4-log treatment of 
viruses before or at the first customer.
    (d) Ground water system must give public notification under Sec.  
141.203 for the treatment technique violations specified in paragraphs 
(a), (b) and (c) of this section.



Sec.  141.405  Reporting and recordkeeping for ground water systems.

    (a) Reporting. In addition to the requirements of Sec.  141.31, a 
ground water system regulated under this subpart must provide the 
following information to the State:
    (1) A ground water system conducting compliance monitoring under 
Sec.  141.403(b) must notify the State any time the system fails to meet 
any State-specified requirements including, but not limited to, minimum 
residual disinfectant concentration, membrane operating criteria or 
membrane integrity, and alternative treatment operating criteria, if 
operation in accordance with the criteria or requirements is not 
restored within four hours. The ground water system must notify the 
State as soon as possible, but in no case later than the end of the next 
business day.
    (2) After completing any corrective action under Sec.  141.403(a), a 
ground water system must notify the State within 30 days of completion 
of the corrective action.
    (3) If a ground water system subject to the requirements of Sec.  
141.402(a) does not conduct source water monitoring under Sec.  
141.402(a)(5)(ii), the system must provide documentation to the State 
within 30 days of the total coliform positive sample that it met the 
State criteria.
    (b) Recordkeeping. In addition to the requirements of Sec.  141.33, 
a ground water system regulated under this subpart must maintain the 
following information in its records:

[[Page 659]]

    (1) Documentation of corrective actions. Documentation shall be kept 
for a period of not less than ten years.
    (2) Documentation of notice to the public as required under Sec.  
141.403(a)(7). Documentation shall be kept for a period of not less than 
three years.
    (3) Records of decisions under Sec.  141.402(a)(5)(ii) and records 
of invalidation of fecal indicator-positive ground water source samples 
under Sec.  141.402(d). Documentation shall be kept for a period of not 
less than five years.
    (4) For consecutive systems, documentation of notification to the 
wholesale system(s) of total coliform-positive samples that are not 
invalidated under Sec.  141.21(c) until March 31, 2016, or under Sec.  
141.853 beginning April 1, 2016. Documentation shall be kept for a 
period of not less than five years.
    (5) For systems, including wholesale systems, that are required to 
perform compliance monitoring under Sec.  141.403(b):
    (i) Records of the State-specified minimum disinfectant residual. 
Documentation shall be kept for a period of not less than ten years.
    (ii) Records of the lowest daily residual disinfectant concentration 
and records of the date and duration of any failure to maintain the 
State-prescribed minimum residual disinfectant concentration for a 
period of more than four hours. Documentation shall be kept for a period 
of not less than five years.
    (iii) Records of State-specified compliance requirements for 
membrane filtration and of parameters specified by the State for State-
approved alternative treatment and records of the date and duration of 
any failure to meet the membrane operating, membrane integrity, or 
alternative treatment operating requirements for more than four hours. 
Documentation shall be kept for a period of not less than five years.

[71 FR 65653, Nov. 8, 2006, as amended at 78 FR 10353, Feb. 13, 2013]



  Subpart T_Enhanced Filtration and Disinfection_Systems Serving Fewer 
                           Than 10,000 People

    Source: 67 FR 1839, Jan. 14, 2002, unless otherwise noted.

                          General Requirements



Sec.  141.500  General requirements.

    The requirements of this subpart constitute national primary 
drinking water regulations. These regulations establish requirements for 
filtration and disinfection that are in addition to criteria under which 
filtration and disinfection are required under subpart H of this part. 
The regulations in this subpart establish or extend treatment technique 
requirements in lieu of maximum contaminant levels for the following 
contaminants: Giardia lamblia, viruses, heterotrophic plate count 
bacteria, Legionella, Cryptosporidium and turbidity. The treatment 
technique requirements consist of installing and properly operating 
water treatment processes which reliably achieve:
    (a) At least 99 percent (2 log) removal of Cryptosporidium between a 
point where the raw water is not subject to recontamination by surface 
water runoff and a point downstream before or at the first customer for 
filtered systems, or Cryptosporidium control under the watershed control 
plan for unfiltered systems; and
    (b) Compliance with the profiling and benchmark requirements in 
Sec. Sec.  141.530 through 141.544.



Sec.  141.501  Who is subject to the requirements of subpart T?

    You are subject to these requirements if your system:
    (a) Is a public water system;
    (b) Uses surface water or GWUDI as a source; and
    (c) Serves fewer than 10,000 persons.



Sec.  141.502  When must my system comply with these requirements?

    You must comply with these requirements in this subpart beginning 
January 1, 2005, except where otherwise noted.

[69 FR 38856, June 29, 2004]

[[Page 660]]



Sec.  141.503  What does subpart T require?

    There are seven requirements of this subpart, and you must comply 
with all requirements that are applicable to your system. These 
requirements are:
    (a) You must cover any finished water reservoir that you began to 
construct on or after March 15, 2002 as described in Sec. Sec.  141.510 
and 141.511;
    (b) If your system is an unfiltered system, you must comply with the 
updated watershed control requirements described in Sec. Sec.  141.520-
141.522;
    (c) If your system is a community or non-transient non-community 
water systems you must develop a disinfection profile as described in 
Sec. Sec.  141.530-141.536;
    (d) If your system is considering making a significant change to its 
disinfection practices, you must develop a disinfection benchmark and 
consult with the State for approval of the change as described in 
Sec. Sec.  141.540-141.544;
    (e) If your system is a filtered system, you must comply with the 
combined filter effluent requirements as described in Sec. Sec.  
141.550-141.553;
    (f) If your system is a filtered system that uses conventional or 
direct filtration, you must comply with the individual filter turbidity 
requirements as described in Sec. Sec.  141.560-141.564; and
    (g) You must comply with the applicable reporting and recordkeeping 
requirements as described in Sec. Sec.  141.570 and 141.571.

                        Finished Water Reservoirs



Sec.  141.510  Is my system subject to the new finished 
water reservoir requirements?

    All subpart H systems which serve fewer than 10,000 are subject to 
this requirement.



Sec.  141.511  What is required of new finished water reservoirs?

    If your system begins construction of a finished water reservoir on 
or after March 15, 2002 the reservoir must be covered. Finished water 
reservoirs for which your system began construction prior to March 15, 
2002 are not subject to this requirement.

    Additional Watershed Control Requirements for Unfiltered Systems



Sec.  141.520  Is my system subject to the updated watershed 
control requirements?

    If you are a subpart H system serving fewer than 10,000 persons 
which does not provide filtration, you must continue to comply with all 
of the filtration avoidance criteria in Sec.  141.71, as well as the 
additional watershed control requirements in Sec.  141.521.



Sec.  141.521  What updated watershed control requirements must my unfiltered 
system implement to continue to avoid filtration?

    Your system must take any additional steps necessary to minimize the 
potential for contamination by Cryptosporidium oocysts in the source 
water. Your system's watershed control program must, for 
Cryptosporidium:
    (a) Identify watershed characteristics and activities which may have 
an adverse effect on source water quality; and
    (b) Monitor the occurrence of activities which may have an adverse 
effect on source water quality.



Sec.  141.522  How does the State determine whether my system's watershed 
control requirements are adequate?

    During an onsite inspection conducted under the provisions of Sec.  
141.71(b)(3), the State must determine whether your watershed control 
program is adequate to limit potential contamination by Cryptosporidium 
oocysts. The adequacy of the program must be based on the 
comprehensiveness of the watershed review; the effectiveness of your 
program to monitor and control detrimental activities occurring in the 
watershed; and the extent to which your system has maximized land 
ownership and/or controlled land use within the watershed.

                          Disinfection Profile



Sec.  141.530  What is a disinfection profile and who must develop one?

    A disinfection profile is a graphical representation of your 
system's level of Giardia lamblia or virus inactivation

[[Page 661]]

measured during the course of a year. If you are a subpart H community 
or non-transient non-community water system which serves fewer than 
10,000 persons, your system must develop a disinfection profile unless 
your State determines that your system's profile is unnecessary. Your 
State may approve the use of a more representative data set for 
disinfection profiling than the data set required under Sec. Sec.  
141.532-141.536.

[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38856, June 29, 2004]



Sec.  141.531  What criteria must a State use to determine that a profile 
is unnecessary?

    States may only determine that a system's profile is unnecessary if 
a system's TTHM and HAA5 levels are below 0.064 mg/L and 0.048 mg/L, 
respectively. To determine these levels, TTHM and HAA5 samples must be 
collected after January 1, 1998, during the month with the warmest water 
temperature, and at the point of maximum residence time in your 
distribution system. Your State may approve a more representative TTHM 
and HAA5 data set to determine these levels.

[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38856, June 29, 2004]



Sec.  141.532  How does my system develop a disinfection profile 
and when must it begin?

    A disinfection profile consists of three steps:
    (a) First, your system must collect data for several parameters from 
the plant as discussed in Sec.  141.533 over the course of 12 months. If 
your system serves between 500 and 9,999 persons you must begin to 
collect data no later than July 1, 2003. If your system serves fewer 
than 500 persons you must begin to collect data no later than January 1, 
2004.
    (b) Second, your system must use this data to calculate weekly log 
inactivation as discussed in Sec. Sec.  141.534 and 141.535; and
    (c) Third, your system must use these weekly log inactivations to 
develop a disinfection profile as specified in Sec.  141.536.



Sec.  141.533  What data must my system collect to calculate 
a disinfection profile?

    Your system must monitor the following parameters to determine the 
total log inactivation using the analytical methods in Sec.  141.74 (a), 
once per week on the same calendar day, over 12 consecutive months:
    (a) The temperature of the disinfected water at each residual 
disinfectant concentration sampling point during peak hourly flow;
    (b) If your system uses chlorine, the pH of the disinfected water at 
each residual disinfectant concentration sampling point during peak 
hourly flow;
    (c) The disinfectant contact time(s) (``T'') during peak hourly 
flow; and
    (d) The residual disinfectant concentration(s) (``C'') of the water 
before or at the first customer and prior to each additional point of 
disinfection during peak hourly flow.



Sec.  141.534  How does my system use this data to calculate 
an inactivation ratio?

    Use the tables in Sec.  141.74(b)(3)(v) to determine the appropriate 
CT99.9 value. Calculate the total inactivation ratio as follows, and 
multiply the value by 3.0 to determine log inactivation of Giardia 
lamblia:

------------------------------------------------------------------------
       If your system * * *           Your system must determine * * *
------------------------------------------------------------------------
(a) Uses only one point of          (1) One inactivation ratio (CTcalc/
 disinfectant application.           CT99.9) before or at the first
                                     customer during peak hourly flow
                                     or
                                    (2) Successive CTcalc/CT99.9 values,
                                     representing sequential
                                     inactivation ratios, between the
                                     point of disinfectant application
                                     and a point before or at the first
                                     customer during peak hourly flow.
                                     Under this alternative, your system
                                     must calculate the total
                                     inactivation ratio by determining
                                     (CTcalc/CT99.9) for each sequence
                                     and then adding the (CTcalc/CT99.9)
                                     values together to determine
                                     ([Sigma]CTcalc/CT99.9).
(b) Uses more than one point of     The (CTcalc/CT99.9) value of each
 disinfectant application before     disinfection segment immediately
 the first customer.                 prior to the next point of
                                     disinfectant application, or for
                                     the final segment, before or at the
                                     first customer, during peak hourly
                                     flow using the procedure specified
                                     in paragraph (a)(2) of this
                                     section.
------------------------------------------------------------------------


[[Page 662]]


[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38856, June 29, 2004]



Sec.  141.535  What if my system uses chloramines, ozone, or chlorine dioxide 
for primary disinfection?

    If your system uses chloramines, ozone, or chlorine dioxide for 
primary disinfection, you must also calculate the logs of inactivation 
for viruses and develop an additional disinfection profile for viruses 
using methods approved by the State.



Sec.  141.536  My system has developed an inactivation ratio; 
what must we do now?

    Each log inactivation serves as a data point in your disinfection 
profile. Your system will have obtained 52 measurements (one for every 
week of the year). This will allow your system and the State the 
opportunity to evaluate how microbial inactivation varied over the 
course of the year by looking at all 52 measurements (your Disinfection 
Profile). Your system must retain the Disinfection Profile data in 
graphic form, such as a spreadsheet, which must be available for review 
by the State as part of a sanitary survey. Your system must use this 
data to calculate a benchmark if you are considering changes to 
disinfection practices.

                         Disinfection Benchmark



Sec.  141.540  Who has to develop a disinfection benchmark?

    If you are a subpart H system required to develop a disinfection 
profile under Sec. Sec.  141.530 through 141.536, your system must 
develop a Disinfection Benchmark if you decide to make a significant 
change to your disinfection practice. Your system must consult with the 
State for approval before you can implement a significant disinfection 
practice change.



Sec.  141.541  What are significant changes to disinfection practice?

    Significant changes to disinfection practice include:
    (a) Changes to the point of disinfection;
    (b) Changes to the disinfectant(s) used in the treatment plant;
    (c) Changes to the disinfection process; or
    (d) Any other modification identified by the State.



Sec.  141.542  What must my system do if we are considering a significant 
change to disinfection practices?

    If your system is considering a significant change to its 
disinfection practice, your system must calculate a disinfection 
benchmark(s) as described in Sec. Sec.  141.543 and 141.544 and provide 
the benchmark(s) to your State. Your system may only make a significant 
disinfection practice change after consulting with the State for 
approval. Your system must submit the following information to the State 
as part of the consultation and approval process:
    (a) A description of the proposed change;
    (b) The disinfection profile for Giardia lamblia (and, if necessary, 
viruses) and disinfection benchmark;
    (c) An analysis of how the proposed change will affect the current 
levels of disinfection; and
    (d) Any additional information requested by the State.



Sec.  141.543  How is the disinfection benchmark calculated?

    If your system is making a significant change to its disinfection 
practice, it must calculate a disinfection benchmark using the procedure 
specified in the following table.

------------------------------------------------------------------------
   To calculate a disinfection benchmark your system must perform the
                             following steps
-------------------------------------------------------------------------
Step 1: Using the data your system collected to develop the Disinfection
 Profile, determine the average Giardia lamblia inactivation for each
 calendar month by dividing the sum of all Giardia lamblia inactivations
 for that month by the number of values calculated for that month.
Step 2: Determine the lowest monthly average value out of the twelve
 values. This value becomes the disinfection benchmark.
------------------------------------------------------------------------


[[Page 663]]



Sec.  141.544  What if my system uses chloramines, ozone, 
or chlorine dioxide for primary disinfection?

    If your system uses chloramines, ozone or chlorine dioxide for 
primary disinfection your system must calculate the disinfection 
benchmark from the data your system collected for viruses to develop the 
disinfection profile in addition to the Giardia lamblia disinfection 
benchmark calculated under Sec.  141.543. This viral benchmark must be 
calculated in the same manner used to calculate the Giardia lamblia 
disinfection benchmark in Sec.  141.543.

                  Combined Filter Effluent Requirements



Sec.  141.550  Is my system required to meet subpart T combined filter 
effluent turbidity limits?

    All subpart H systems which serve populations fewer than 10,000, are 
required to filter, and utilize filtration other than slow sand 
filtration or diatomaceous earth filtration must meet the combined 
filter effluent turbidity requirements of Sec. Sec.  141.551-141.553 . 
If your system uses slow sand or diatomaceous earth filtration you are 
not required to meet the combined filter effluent turbidity limits of 
subpart T, but you must continue to meet the combined filter effluent 
turbidity limits in Sec.  141.73.



Sec.  141.551  What strengthened combined filter effluent turbidity limits 
must my system meet?

    Your system must meet two strengthened combined filter effluent 
turbidity limits.
    (a) The first combined filter effluent turbidity limit is a ``95th 
percentile'' turbidity limit that your system must meet in at least 95 
percent of the turbidity measurements taken each month. Measurements 
must continue to be taken as described in Sec.  141.74(a) and (c). 
Monthly reporting must be completed according to Sec.  141.570. The 
following table describes the required limits for specific filtration 
technologies.

------------------------------------------------------------------------
                                                Your 95th percentile
     If your system consists of * * *         turbidity value is * * *
------------------------------------------------------------------------
(1) Conventional Filtration or Direct       0.3 NTU.
 Filtration.
(2) All other ``Alternative'' Filtration..  A value determined by the
                                             State (not to exceed 1 NTU)
                                             based on the demonstration
                                             described in Sec.
                                             141.552.
------------------------------------------------------------------------

    (b) The second combined filter effluent turbidity limit is a 
``maximum'' turbidity limit which your system may at no time exceed 
during the month. Measurements must continue to be taken as described in 
Sec.  141.74(a) and (c). Monthly reporting must be completed according 
to Sec.  141.570. The following table describes the required limits for 
specific filtration technologies.

------------------------------------------------------------------------
                                            Your maximum turbidity value
     If your system consists of * * *                 is * * *
------------------------------------------------------------------------
(1) Conventional Filtration or Direct       1 NTU.
 Filtration.
(2) All other ``Alternative Filtration''..  A value determined by the
                                             State (not to exceed 5 NTU)
                                             based on the demonstration
                                             as described in Sec.
                                             141.552.
------------------------------------------------------------------------


[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38856, June 29, 2004]



Sec.  141.552  My system consists of ``alternative filtration'' 
and is required to conduct a demonstration--what is required of my system 
and how does the State establish my turbidity limits?

    (a) If your system consists of alternative filtration(filtration 
other than slow sand filtration, diatomaceous earth filtration, 
conventional filtration, or direct filtration) you are required to 
conduct a demonstration (see tables in Sec.  141.551). Your system must 
demonstrate to the State, using pilot plant studies or other means, that 
your system's filtration, in combination with disinfection treatment, 
consistently achieves:
    (1) 99 percent removal of Cryptosporidium oocysts;
    (2) 99.9 percent removal and/or inactivation of Giardia lamblia 
cysts; and
    (3) 99.99 percent removal and/or inactivation of viruses.

[[Page 664]]

    (b) [Reserved]



Sec.  141.553  My system practices lime softening--is there any special 
provision regarding my combined filter effluent?

    If your system practices lime softening, you may acidify 
representative combined filter effluent turbidity samples prior to 
analysis using a protocol approved by the State.

                Individual Filter Turbidity Requirements



Sec.  141.560  Is my system subject to individual filter 
turbidity requirements?

    If your system is a subpart H system serving fewer than 10,000 
people and utilizing conventional filtration or direct filtration, you 
must conduct continuous monitoring of turbidity for each individual 
filter at your system. The following requirements apply to continuous 
turbidity monitoring:
    (a) Monitoring must be conducted using an approved method in Sec.  
141.74(a);
    (b) Calibration of turbidimeters must be conducted using procedures 
specified by the manufacturer;
    (c) Results of turbidity monitoring must be recorded at least every 
15 minutes;
    (d) Monthly reporting must be completed according to Sec.  141.570; 
and
    (e) Records must be maintained according to Sec.  141.571.



Sec.  141.561  What happens if my system's turbidity monitoring 
equipment fails?

    If there is a failure in the continuous turbidity monitoring 
equipment, your system must conduct grab sampling every four hours in 
lieu of continuous monitoring until the turbidimeter is back on-line. 
Your system has 14 days to resume continuous monitoring before a 
violation is incurred.



Sec.  141.562  My system only has two or fewer filters--is there any special 
provision regarding individual filter turbidity monitoring?

    Yes, if your system only consists of two or fewer filters, you may 
conduct continuous monitoring of combined filter effluent turbidity in 
lieu of individual filter effluent turbidity monitoring. Continuous 
monitoring must meet the same requirements set forth in Sec.  141.560(a) 
through (d) and Sec.  141.561.



Sec.  141.563  What follow-up action is my system required to take based 
on continuous turbidity monitoring?

    Follow-up action is required according to the following tables:

------------------------------------------------------------------------
                If * * *                      Your system must * * *
------------------------------------------------------------------------
(a) The turbidity of an individual       Report to the State by the 10th
 filter (or the turbidity of combined     of the following month and
 filter effluent (CFE) for systems with   include the filter number(s),
 2 filters that monitor CFE in lieu of    corresponding date(s),
 individual filters) exceeds 1.0 NTU in   turbidity value(s) which
 two consecutive recordings 15 minutes    exceeded 1.0 NTU, and the
 apart.                                   cause (if known) for the
                                          exceedance(s).
------------------------------------------------------------------------


------------------------------------------------------------------------
 If a system was required to report to
            the State * * *                   Your system must * * *
------------------------------------------------------------------------
(b) For three months in a row and        Conduct a self-assessment of
 turbidity exceeded 1.0 NTU in two        the filter(s) within 14 days
 consecutive recordings 15 minutes        of the day the filter exceeded
 apart at the same filter (or CFE for     1.0 NTU in two consecutive
 systems with 2 filters that monitor      measurements for the third
 CFE in lieu of individual filters).      straight month unless a CPE as
                                          specified in paragraph (c) of
                                          this section was required.
                                          Systems with 2 filters that
                                          monitor CFE in lieu of
                                          individual filters must
                                          conduct a self assessment on
                                          both filters. The self-
                                          assessment must consist of at
                                          least the following
                                          components: assessment of
                                          filter performance;
                                          development of a filter
                                          profile; identification and
                                          prioritization of factors
                                          limiting filter performance;
                                          assessment of the
                                          applicability of corrections;
                                          and preparation of a filter
                                          self-assessment report.
(c) For two months in a row and          Arrange to have a comprehensive
 turbidity exceeded 2.0 NTU in 2          performance evaluation (CPE)
 consecutive recordings 15 minutes        conducted by the State or a
 apart at the same filter (or CFE for     third party approved by the
 systems with 2 filters that monitor      State not later than 60 days
 CFE in lieu of individual filters).      following the day the filter
                                          exceeded 2.0 NTU in two
                                          consecutive measurements for
                                          the second straight month. If
                                          a CPE has been completed by
                                          the State or a third party
                                          approved by the State within
                                          the 12 prior months or the
                                          system and State are jointly
                                          participating in an ongoing
                                          Comprehensive Technical
                                          Assistance (CTA) project at
                                          the system, a new CPE is not
                                          required. If conducted, a CPE
                                          must be completed and
                                          submitted to the State no
                                          later than 120 days following
                                          the day the filter exceeded
                                          2.0 NTU in two consecutive
                                          measurements for the second
                                          straight month.
------------------------------------------------------------------------


[[Page 665]]


[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38856, June 29, 2004]



Sec.  141.564  My system practices lime softening--is there any special 
provision regarding my individual filter turbidity monitoring?

    If your system utilizes lime softening, you may apply to the State 
for alternative turbidity exceedance levels for the levels specified in 
the table in Sec.  141.563. You must be able to demonstrate to the State 
that higher turbidity levels are due to lime carryover only, and not due 
to degraded filter performance.

                Reporting and Recordkeeping Requirements



Sec.  141.570  What does subpart T require that my system report to the State?

    This subpart T requires your system to report several items to the 
State. The following table describes the items which must be reported 
and the frequency of reporting. Your system is required to report the 
information described in the following table, if it is subject to the 
specific requirement shown in the first column.

------------------------------------------------------------------------
                                    Description of
   Corresponding requirement        information to         Frequency
                                        report
------------------------------------------------------------------------
(a) Combined Filter Effluent     (1) The total        By the 10th of the
 Requirements.                    number of filtered   following month.
(Sec.  Sec.   141.550-141.553).   water turbidity
                                  measurements taken
                                  during the month.
                                 (2) The number and   By the 10th of the
                                  percentage of        following month.
                                  filtered water
                                  turbidity
                                  measurements taken
                                  during the month
                                  which are less
                                  than or equal to
                                  your system's
                                  required 95th
                                  percentile limit.
                                 (3) The date and     By the 10th of the
                                  value of any         following month.
                                  turbidity
                                  measurements taken
                                  during the month
                                  which exceed the
                                  maximum turbidity
                                  value for your
                                  filtration system.
(b) Individual Turbidity         (1) That your        By the 10th of the
 Requirements.                    system conducted     following month.
(Sec.  Sec.   141.560-141.564).   individual filter
                                  turbidity
                                  monitoring during
                                  the month.
                                 (2) The filter       By the 10th of the
                                  number(s),           following month.
                                  corresponding
                                  date(s), and the
                                  turbidity value(s)
                                  which exceeded 1.0
                                  NTU during the
                                  month, and the
                                  cause (if known)
                                  for the
                                  exceedance(s), but
                                  only if 2
                                  consecutive
                                  measurements
                                  exceeded 1.0 NTU.
                                 (3) If a self-       By the 10th of the
                                  assessment is        following month
                                  required, the date   (or 14 days after
                                  that it was          the self-
                                  triggered and the    assessment was
                                  date that it was     triggered only if
                                  completed.           the self-
                                                       assessment was
                                                       triggered during
                                                       the last four
                                                       days of the
                                                       month)
                                 (4) If a CPE is      By the 10th of the
                                  required, that the   following month.
                                  CPE is required
                                  and the date that
                                  it was triggered.
                                 (5) Copy of          Within 120 days
                                  completed CPE        after the CPE was
                                  report.              triggered.
(c) Disinfection Profiling.....  (1) Results of       (i) For systems
(Sec.  Sec.   141.530-141.536).   optional             serving 500-9,999
                                  monitoring which     by July 1, 2003;
                                  show TTHM levels    (ii) For systems
                                  <0.064 mg/l and      serving fewer
                                  HAA5 levels <0.048   than 500 by
                                  mg/l (Only if your   January 1, 2004.
                                  system wishes to
                                  forgo profiling)
                                  or that your
                                  system has begun
                                  disinfection
                                  profiling.
(d) Disinfection Benchmarking..  (1) A description    Anytime your
(Sec.  Sec.   141.540-141.544).   of the proposed      system is
                                  change in            considering a
                                  disinfection, your   significant
                                  system's             change to its
                                  disinfection         disinfection
                                  profile for          practice.
                                  Giardia lamblia
                                  (and, if
                                  necessary,
                                  viruses) and
                                  disinfection
                                  benchmark, and an
                                  analysis of how
                                  the proposed
                                  change will affect
                                  the current levels
                                  of disinfection.
------------------------------------------------------------------------


[67 FR 1839, Jan. 14, 2002, as amended at 69 FR 38857, June 29, 2004]



Sec.  141.571  What records does subpart T require my system to keep?

    Your system must keep several types of records based on the 
requirements of subpart T, in addition to recordkeeping requirements 
under Sec.  141.75. The following table describes the necessary records, 
the length of time these records must be kept, and for which requirement 
the records pertain. Your

[[Page 666]]

system is required to maintain records described in this table, if it is 
subject to the specific requirement shown in the first column.

------------------------------------------------------------------------
                                                        Duration of time
    Corresponding requirement        Description of     records must be
                                   necessary records          kept
------------------------------------------------------------------------
(a) Individual Filter Turbidity   Results of           At least 3 years.
 Requirements.                     individual filter
(Sec.  Sec.   141.560-141.564)..   monitoring.
(b) Disinfection Profiling......  Results of Profile   Indefinitely.
(Sec.  Sec.   141.530-141.536)..   (including raw
                                   data and analysis).
(c) Disinfection Benchmarking...  Benchmark            Indefinitely.
(Sec.  Sec.   141.540-141.544)..   (including raw
                                   data and analysis).
------------------------------------------------------------------------



            Subpart U_Initial Distribution System Evaluations

    Source: 71 FR 483, Jan. 4, 2006, unless otherwise noted.



Sec.  141.600  General requirements.

    (a) The requirements of subpart U of this part constitute national 
primary drinking water regulations. The regulations in this subpart 
establish monitoring and other requirements for identifying subpart V 
compliance monitoring locations for determining compliance with maximum 
contaminant levels for total trihalomethanes (TTHM) and haloacetic acids 
(five)(HAA5). You must use an Initial Distribution System Evaluation 
(IDSE) to determine locations with representative high TTHM and HAA5 
concentrations throughout your distribution system. IDSEs are used in 
conjunction with, but separate from, subpart L compliance monitoring, to 
identify and select subpart V compliance monitoring locations.
    (b) Applicability. You are subject to these requirements if your 
system is a community water system that uses a primary or residual 
disinfectant other than ultraviolet light or delivers water that has 
been treated with a primary or residual disinfectant other than 
ultraviolet light; or if your system is a nontransient noncommunity 
water system that serves at least 10,000 people and uses a primary or 
residual disinfectant other than ultraviolet light or delivers water 
that has been treated with a primary or residual disinfectant other than 
ultraviolet light.
    (c) Schedule. (1) You must comply with the requirements of this 
subpart on the schedule in the table in this paragraph (c)(1).

----------------------------------------------------------------------------------------------------------------
                                        You must submit your
                                      standard monitoring plan
                                      or system specific study   You must complete your
                                          plan \1\ or 40/30      standard monitoring or    You must submit your
    If you serve this population      certification \2\ to the   system specific study      IDSE report to the
                                      State by or receive very             by                  State by \3\
                                      small system waiver from
                                                State
----------------------------------------------------------------------------------------------------------------
Systems that are not part of a combined distribution system and systems that serve the largest population in the
                                          combined distribution system
----------------------------------------------------------------------------------------------------------------
(i) =100,000.............  October 1, 2006.........  September 30, 2008.....  January 1, 2009.
(ii) 50,000-99,999..................  April 1, 2007...........  March 31, 2009.........  July 1, 2009.
(iii) 10,000-49,999.................  October 1, 2007.........  September 30, 2009.....  January 1, 2010.
(iv) <10,000 (CWS Only).............  April 1, 2008...........  March 31, 2010.........  July 1, 2010.
----------------------------------------------------------------------------------------------------------------
                          Other systems that are part of a combined distribution system
----------------------------------------------------------------------------------------------------------------
(v) Wholesale system or consecutive   --at the same time as     --at the same time as    --at the same time as
 system.                               the system with the       the system with the      the system with the
                                       earliest compliance       earliest compliance      earliest compliance
                                       date in the combined      date in the combined     date in the combined
                                       distribution system.      distribution system.     distribution system.
----------------------------------------------------------------------------------------------------------------
\1\ If, within 12 months after the date identified in this column, the State does not approve your plan or
  notify you that it has not yet completed its review, you may consider the plan that you submitted as approved.
  You must implement that plan and you must complete standard monitoring or a system specific study no later
  than the date identified in the third column.
\2\ You must submit your 40/30 certification under Sec.   141.603 by the date indicated.
\3\ If, within three months after the date identified in this column (nine months after the date identified in
  this column if you must comply on the schedule in paragraph (c)(1)(iii) of this section), the State does not
  approve your IDSE report or notify you that it has not yet completed its review, you may consider the report
  that you submitted as approved and you must implement the recommended subpart V monitoring as required.


[[Page 667]]

    (2) For the purpose of the schedule in paragraph (c)(1) of this 
section, the State may determine that the combined distribution system 
does not include certain consecutive systems based on factors such as 
receiving water from a wholesale system only on an emergency basis or 
receiving only a small percentage and small volume of water from a 
wholesale system. The State may also determine that the combined 
distribution system does not include certain wholesale systems based on 
factors such as delivering water to a consecutive system only on an 
emergency basis or delivering only a small percentage and small volume 
of water to a consecutive system.
    (d) You must conduct standard monitoring that meets the requirements 
in Sec.  141.601, or a system specific study that meets the requirements 
in Sec.  141.602, or certify to the State that you meet 40/30 
certification criteria under Sec.  141.603, or qualify for a very small 
system waiver under Sec.  141.604.
    (1) You must have taken the full complement of routine TTHM and HAA5 
compliance samples required of a system with your population and source 
water under subpart L of this part (or you must have taken the full 
complement of reduced TTHM and HAA5 compliance samples required of a 
system with your population and source water under subpart L if you meet 
reduced monitoring criteria under subpart L of this part) during the 
period specified in Sec.  141.603(a) to meet the 40/30 certification 
criteria in Sec.  141.603. You must have taken TTHM and HAA5 samples 
under Sec. Sec.  141.131 and 141.132 to be eligible for the very small 
system waiver in Sec.  141.604.
    (2) If you have not taken the required samples, you must conduct 
standard monitoring that meets the requirements in Sec.  141.601, or a 
system specific study that meets the requirements in Sec.  141.602.
    (e) You must use only the analytical methods specified in Sec.  
141.131, or otherwise approved by EPA for monitoring under this subpart, 
to demonstrate compliance with the requirements of this subpart.
    (f) IDSE results will not be used for the purpose of determining 
compliance with MCLs in Sec.  141.64.



Sec.  141.601  Standard monitoring.

    (a) Standard monitoring plan. Your standard monitoring plan must 
comply with paragraphs (a)(1) through (a)(4) of this section. You must 
prepare and submit your standard monitoring plan to the State according 
to the schedule in Sec.  141.600(c).
    (1) Your standard monitoring plan must include a schematic of your 
distribution system (including distribution system entry points and 
their sources, and storage facilities), with notes indicating locations 
and dates of all projected standard monitoring, and all projected 
subpart L compliance monitoring.
    (2) Your standard monitoring plan must include justification of 
standard monitoring location selection and a summary of data you relied 
on to justify standard monitoring location selection.
    (3) Your standard monitoring plan must specify the population served 
and system type (subpart H or ground water).
    (4) You must retain a complete copy of your standard monitoring plan 
submitted under this paragraph (a), including any State modification of 
your standard monitoring plan, for as long as you are required to retain 
your IDSE report under paragraph (c)(4) of this section.
    (b) Standard monitoring. (1) You must monitor as indicated in the 
table in this paragraph (b)(1). You must collect dual sample sets at 
each monitoring location. One sample in the dual sample set must be 
analyzed for TTHM. The other sample in the dual sample set must be 
analyzed for HAA5. You must conduct one monitoring period during the 
peak historical month for TTHM levels or HAA5 levels or the month of 
warmest water temperature. You must review available compliance, study, 
or operational data to determine the peak historical month for TTHM or 
HAA5 levels or warmest water temperature.

[[Page 668]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                       Distribution system monitoring locations \1\
                                                                                                 -------------------------------------------------------
            Source water type              Population size category     Monitoring periods and     Total per     Near     Average
                                                                         frequency of sampling    monitoring    entry    residence  High TTHM  High HAA5
                                                                                                    period      points      time    locations  locations
--------------------------------------------------------------------------------------------------------------------------------------------------------
Subpart H
                                          <500 consecutive systems..  one (during peak                     2          1  .........          1
                                                                       historical month) \2\.
                                          <500 non-consecutive        ..........................           2  .........  .........          1          1
                                           systems.
                                          500-3,300 consecutive       four (every 90 days)......           2          1  .........          1
                                           systems.
                                          500-3,300 non-consecutive   ..........................           2  .........  .........          1          1
                                           systems.
                                          3,301-9,999...............  ..........................           4  .........          1          2          1
                                          10,000-49,999.............  six (every 60 days).......           8          1          2          3          2
                                          50,000-249,999............  ..........................          16          3          4          5          4
                                          250,000-999,999...........  ..........................          24          4          6          8          6
                                          1,000,000-4,999,999.......  ..........................          32          6          8         10          8
                                          =5,000,000.....  ..........................          40          8         10         12         10
Ground Water
                                          <500 consecutive systems..  one (during peak                     2          1  .........          1
                                                                       historical month) \2\.
                                          <500 non-consecutive        ..........................           2  .........  .........          1          1
                                           systems.
                                          500-9,999.................  four (every 90 days)......           2  .........  .........          1          1
                                          10,000-99,999.............  ..........................           6          1          1          2          2
                                          100,000-499,999...........  ..........................           8          1          1          3          3
                                          =500,000.......  ..........................          12          2          2          4          4
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ A dual sample set (i.e., a TTHM and an HAA5 sample) must be taken at each monitoring location during each monitoring period.
\2\ The peak historical month is the month with the highest TTHM or HAA5 levels or the warmest water temperature.

    (2) You must take samples at locations other than the existing 
subpart L monitoring locations. Monitoring locations must be distributed 
throughout the distribution system.
    (3) If the number of entry points to the distribution system is 
fewer than the specified number of entry point monitoring locations, 
excess entry point samples must be replaced equally at high TTHM and 
HAA5 locations. If there is an odd extra location number, you must take 
a sample at a high TTHM location. If the number of entry points to the 
distribution system is more than the specified number of entry point 
monitoring locations, you must take samples at entry points to the 
distribution system having the highest annual water flows.
    (4) Your monitoring under this paragraph (b) may not be reduced 
under the provisions of Sec.  141.29 and the State may not reduce your 
monitoring using the provisions of Sec.  142.16(m).
    (c) IDSE report. Your IDSE report must include the elements required 
in paragraphs (c)(1) through (c)(4) of this section. You must submit 
your IDSE report to the State according to the schedule in Sec.  
141.600(c).
    (1) Your IDSE report must include all TTHM and HAA5 analytical 
results from subpart L compliance monitoring and all standard monitoring 
conducted during the period of the IDSE as individual analytical results 
and LRAAs presented in a tabular or spreadsheet format acceptable to the 
State. If changed from your standard monitoring plan submitted under 
paragraph (a) of this section, your report must also include a schematic 
of your distribution system, the population served, and system type 
(subpart H or ground water).
    (2) Your IDSE report must include an explanation of any deviations 
from your approved standard monitoring plan.
    (3) You must recommend and justify subpart V compliance monitoring 
locations and timing based on the protocol in Sec.  141.605.
    (4) You must retain a complete copy of your IDSE report submitted 
under this section for 10 years after the date that you submitted your 
report. If the

[[Page 669]]

State modifies the subpart V monitoring requirements that you 
recommended in your IDSE report or if the State approves alternative 
monitoring locations, you must keep a copy of the State's notification 
on file for 10 years after the date of the State's notification. You 
must make the IDSE report and any State notification available for 
review by the State or the public.



Sec.  141.602  System specific studies.

    (a) System specific study plan. Your system specific study plan must 
be based on either existing monitoring results as required under 
paragraph (a)(1) of this section or modeling as required under paragraph 
(a)(2) of this section. You must prepare and submit your system specific 
study plan to the State according to the schedule in Sec.  141.600(c).
    (1) Existing monitoring results. You may comply by submitting 
monitoring results collected before you are required to begin monitoring 
under Sec.  141.600(c). The monitoring results and analysis must meet 
the criteria in paragraphs (a)(1)(i) and (a)(1)(ii) of this section.
    (i) Minimum requirements. (A) TTHM and HAA5 results must be based on 
samples collected and analyzed in accordance with Sec.  141.131. Samples 
must be collected no earlier than five years prior to the study plan 
submission date.
    (B) The monitoring locations and frequency must meet the conditions 
identified in this paragraph (a)(1)(i)(B). Each location must be sampled 
once during the peak historical month for TTHM levels or HAA5 levels or 
the month of warmest water temperature for every 12 months of data 
submitted for that location. Monitoring results must include all subpart 
L compliance monitoring results plus additional monitoring results as 
necessary to meet minimum sample requirements.

----------------------------------------------------------------------------------------------------------------
                                                                               Number of      Number of samples
                        System Type                           Population      monitoring   ---------------------
                                                             size category     locations       TTHM       HAA5
----------------------------------------------------------------------------------------------------------------
Subpart H:
                                                                      <500               3          3          3
                                                                 500-3,300               3          9          9
                                                               3,301-9,999               6         36         36
                                                             10,000-49,999              12         72         72
                                                            50,000-249,999              24        144        144
                                                            250,000-999,99              36        216        216
                                                                         9
                                                            1,000,000-4,99              48        288        288
                                                                     9,999
                                                            =5,              60        360        360
                                                                   000,000
Ground Water:
                                                                      <500               3          3          3
                                                                 500-9,999               3          9          9
                                                             10,000-99,999              12         48         48
                                                            100,000-499,99              18         72         72
                                                                         9
                                                            =50              24         96         96
                                                                     0,000
----------------------------------------------------------------------------------------------------------------

    (ii) Reporting monitoring results. You must report the information 
in this paragraph (a)(1)(ii).
    (A) You must report previously collected monitoring results and 
certify that the reported monitoring results include all compliance and 
non-compliance results generated during the time period beginning with 
the first reported result and ending with the most recent subpart L 
results.
    (B) You must certify that the samples were representative of the 
entire distribution system and that treatment, and distribution system 
have not changed significantly since the samples were collected.
    (C) Your study monitoring plan must include a schematic of your 
distribution system (including distribution system entry points and 
their sources, and storage facilities), with notes indicating the 
locations and dates of all completed or planned system specific study 
monitoring.

[[Page 670]]

    (D) Your system specific study plan must specify the population 
served and system type (subpart H or ground water).
    (E) You must retain a complete copy of your system specific study 
plan submitted under this paragraph (a)(1), including any State 
modification of your system specific study plan, for as long as you are 
required to retain your IDSE report under paragraph (b)(5) of this 
section.
    (F) If you submit previously collected data that fully meet the 
number of samples required under paragraph (a)(1)(i)(B) of this section 
and the State rejects some of the data, you must either conduct 
additional monitoring to replace rejected data on a schedule the State 
approves or conduct standard monitoring under Sec.  141.601.
    (2) Modeling. You may comply through analysis of an extended period 
simulation hydraulic model. The extended period simulation hydraulic 
model and analysis must meet the criteria in this paragraph (a)(2).
    (i) Minimum requirements. (A) The model must simulate 24 hour 
variation in demand and show a consistently repeating 24 hour pattern of 
residence time.
    (B) The model must represent the criteria listed in paragraphs 
(a)(2)(i)(B)(1) through (9) of this section.
    (1) 75% of pipe volume;
    (2) 50% of pipe length;
    (3) All pressure zones;
    (4) All 12-inch diameter and larger pipes;
    (5) All 8-inch and larger pipes that connect pressure zones, 
influence zones from different sources, storage facilities, major demand 
areas, pumps, and control valves, or are known or expected to be 
significant conveyors of water;
    (6) All 6-inch and larger pipes that connect remote areas of a 
distribution system to the main portion of the system;
    (7) All storage facilities with standard operations represented in 
the model; and
    (8) All active pump stations with controls represented in the model; 
and
    (9) All active control valves.
    (C) The model must be calibrated, or have calibration plans, for the 
current configuration of the distribution system during the period of 
high TTHM formation potential. All storage facilities must be evaluated 
as part of the calibration process. All required calibration must be 
completed no later than 12 months after plan submission.
    (ii) Reporting modeling. Your system specific study plan must 
include the information in this paragraph (a)(2)(ii).
    (A) Tabular or spreadsheet data demonstrating that the model meets 
requirements in paragraph (a)(2)(i)(B) of this section.
    (B) A description of all calibration activities undertaken, and if 
calibration is complete, a graph of predicted tank levels versus 
measured tank levels for the storage facility with the highest residence 
time in each pressure zone, and a time series graph of the residence 
time at the longest residence time storage facility in the distribution 
system showing the predictions for the entire simulation period (i.e., 
from time zero until the time it takes to for the model to reach a 
consistently repeating pattern of residence time).
    (C) Model output showing preliminary 24 hour average residence time 
predictions throughout the distribution system.
    (D) Timing and number of samples representative of the distribution 
system planned for at least one monitoring period of TTHM and HAA5 dual 
sample monitoring at a number of locations no less than would be 
required for the system under standard monitoring in Sec.  141.601 
during the historical month of high TTHM. These samples must be taken at 
locations other than existing subpart L compliance monitoring locations.
    (E) Description of how all requirements will be completed no later 
than 12 months after you submit your system specific study plan.
    (F) Schematic of your distribution system (including distribution 
system entry points and their sources, and storage facilities), with 
notes indicating the locations and dates of all completed system 
specific study monitoring (if calibration is complete) and all subpart L 
compliance monitoring.
    (G) Population served and system type (subpart H or ground water).

[[Page 671]]

    (H) You must retain a complete copy of your system specific study 
plan submitted under this paragraph (a)(2), including any State 
modification of your system specific study plan, for as long as you are 
required to retain your IDSE report under paragraph (b)(7) of this 
section.
    (iii) If you submit a model that does not fully meet the 
requirements under paragraph (a)(2) of this section, you must correct 
the deficiencies and respond to State inquiries concerning the model. If 
you fail to correct deficiencies or respond to inquiries to the State's 
satisfaction, you must conduct standard monitoring under Sec.  141.601.
    (b) IDSE report. Your IDSE report must include the elements required 
in paragraphs (b)(1) through (b)(6) of this section. You must submit 
your IDSE report according to the schedule in Sec.  141.600(c).
    (1) Your IDSE report must include all TTHM and HAA5 analytical 
results from subpart L compliance monitoring and all system specific 
study monitoring conducted during the period of the system specific 
study presented in a tabular or spreadsheet format acceptable to the 
State. If changed from your system specific study plan submitted under 
paragraph (a) of this section, your IDSE report must also include a 
schematic of your distribution system, the population served, and system 
type (subpart H or ground water).
    (2) If you used the modeling provision under paragraph (a)(2) of 
this section, you must include final information for the elements 
described in paragraph (a)(2)(ii) of this section, and a 24-hour time 
series graph of residence time for each subpart V compliance monitoring 
location selected.
    (3) You must recommend and justify subpart V compliance monitoring 
locations and timing based on the protocol in Sec.  141.605.
    (4) Your IDSE report must include an explanation of any deviations 
from your approved system specific study plan.
    (5) Your IDSE report must include the basis (analytical and modeling 
results) and justification you used to select the recommended subpart V 
monitoring locations.
    (6) You may submit your IDSE report in lieu of your system specific 
study plan on the schedule identified in Sec.  141.600(c) for submission 
of the system specific study plan if you believe that you have the 
necessary information by the time that the system specific study plan is 
due. If you elect this approach, your IDSE report must also include all 
information required under paragraph (a) of this section.
    (7) You must retain a complete copy of your IDSE report submitted 
under this section for 10 years after the date that you submitted your 
IDSE report. If the State modifies the subpart V monitoring requirements 
that you recommended in your IDSE report or if the State approves 
alternative monitoring locations, you must keep a copy of the State's 
notification on file for 10 years after the date of the State's 
notification. You must make the IDSE report and any State notification 
available for review by the State or the public.



Sec.  141.603  40/30 certification.

    (a) Eligibility. You are eligible for 40/30 certification if you had 
no TTHM or HAA5 monitoring violations under subpart L of this part and 
no individual sample exceeded 0.040 mg/L for TTHM or 0.030 mg/L for HAA5 
during an eight consecutive calendar quarter period beginning no earlier 
than the date specified in this paragraph (a).

------------------------------------------------------------------------
                                         Then your eligibility for 40/30
                                         certification is based on eight
                                          consecutive calendar quarters
   If your 40/30 certification is due        of subpart L compliance
                                         monitoring results beginning no
                                                 earlier than \1\
------------------------------------------------------------------------
(1) October 1, 2006....................  January 2004.
(2) April 1, 2007......................  January 2004.
(3) October 1, 2007....................  January 2005.
(4) April 1, 2008......................  January 2005.
------------------------------------------------------------------------
\1\ Unless you are on reduced monitoring under subpart L of this part
  and were not required to monitor during the specified period. If you
  did not monitor during the specified period, you must base your
  eligibility on compliance samples taken during the 12 months preceding
  the specified period.

    (b) 40/30 certification. (1) You must certify to your State that 
every individual compliance sample taken under subpart L of this part 
during the periods specified in paragraph (a) of this section were 
<=0.040 mg/L for TTHM and <=0.030 mg/L for HAA5, and that you have not 
had any TTHM or HAA5 monitoring violations during the period

[[Page 672]]

specified in paragraph (a) of this section.
    (2) The State may require you to submit compliance monitoring 
results, distribution system schematics, and/or recommended subpart V 
compliance monitoring locations in addition to your certification. If 
you fail to submit the requested information, the State may require 
standard monitoring under Sec.  141.601 or a system specific study under 
Sec.  141.602.
    (3) The State may still require standard monitoring under Sec.  
141.601 or a system specific study under Sec.  141.602 even if you meet 
the criteria in paragraph (a) of this section.
    (4) You must retain a complete copy of your certification submitted 
under this section for 10 years after the date that you submitted your 
certification. You must make the certification, all data upon which the 
certification is based, and any State notification available for review 
by the State or the public.



Sec.  141.604  Very small system waivers.

    (a) If you serve fewer than 500 people and you have taken TTHM and 
HAA5 samples under subpart L of this part, you are not required to 
comply with this subpart unless the State notifies you that you must 
conduct standard monitoring under Sec.  141.601 or a system specific 
study under Sec.  141.602.
    (b) If you have not taken TTHM and HAA5 samples under subpart L of 
this part or if the State notifies you that you must comply with this 
subpart, you must conduct standard monitoring under Sec.  141.601 or a 
system specific study under Sec.  141.602.



Sec.  141.605  Subpart V compliance monitoring location recommendations.

    (a) Your IDSE report must include your recommendations and 
justification for where and during what month(s) TTHM and HAA5 
monitoring for subpart V of this part should be conducted. You must base 
your recommendations on the criteria in paragraphs (b) through (e) of 
this section.
    (b) You must select the number of monitoring locations specified in 
the table in this paragraph (b). You will use these recommended 
locations as subpart V routine compliance monitoring locations, unless 
State requires different or additional locations. You should distribute 
locations throughout the distribution system to the extent possible.

--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                            Distribution system monitoring location
                                                                                                     ---------------------------------------------------
                                                                                                                                               Existing
            Source water type               Population size category      Monitoring frequency \1\     Total per     Highest      Highest     subpart L
                                                                                                       monitoring      TTHM         HAA5      compliance
                                                                                                       period \2\   locations    locations    locations
--------------------------------------------------------------------------------------------------------------------------------------------------------
Subpart H:
                                          <500                          per year                                2            1            1
                                          500-3,300                     per quarter                             2            1            1
                                          3,301-9,999                   per quarter                             2            1            1
                                          10,000-49,999                 per quarter                             4            2            1            1
                                          50,000-249,999                per quarter                             8            3            3            2
                                          250,000-999,999               per quarter                            12            5            4            3
                                          1,000,000-4,999,999           per quarter                            16            6            6            4
                                          =5,000,000         per quarter                            20            8            7            5
Ground water:
                                          <500                          per year                                2            1            1
                                          500-9,999                     per year                                2            1            1
                                          10,000-99,999                 per quarter                             4            2            1            1
                                          100,000-499,999               per quarter                             6            3            2            1
                                          =500,000           per quarter                             8            3            3           2
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ All systems must monitor during month of highest DBP concentrations.
\2\ Systems on quarterly monitoring must take dual sample sets every 90 days at each monitoring location, except for subpart H systems serving 500-
  3,300. Ground water systems serving 500-9,999 on annual monitoring must take dual sample sets at each monitoring location. All other systems on annual
  monitoring and subpart H systems serving 500-3,300 are required to take individual TTHM and HAA5 samples (instead of a dual sample set) at the
  locations with the highest TTHM and HAA5 concentrations, respectively. For systems serving fewer than 500 people, only one location with a dual sample
  set per monitoring period is needed if the highest TTHM and HAA5 concentrations occur at the same location and month.


[[Page 673]]

    (c) You must recommend subpart V compliance monitoring locations 
based on standard monitoring results, system specific study results, and 
subpart L compliance monitoring results. You must follow the protocol in 
paragraphs (c)(1) through (c)(8) of this section. If required to monitor 
at more than eight locations, you must repeat the protocol as necessary. 
If you do not have existing subpart L compliance monitoring results or 
if you do not have enough existing subpart L compliance monitoring 
results, you must repeat the protocol, skipping the provisions of 
paragraphs (c)(3) and (c)(7) of this section as necessary, until you 
have identified the required total number of monitoring locations.
    (1) Location with the highest TTHM LRAA not previously selected as a 
subpart V monitoring location.
    (2) Location with the highest HAA5 LRAA not previously selected as a 
subpart V monitoring location.
    (3) Existing subpart L average residence time compliance monitoring 
location (maximum residence time compliance monitoring location for 
ground water systems) with the highest HAA5 LRAA not previously selected 
as a subpart V monitoring location.
    (4) Location with the highest TTHM LRAA not previously selected as a 
subpart V monitoring location.
    (5) Location with the highest TTHM LRAA not previously selected as a 
subpart V monitoring location.
    (6) Location with the highest HAA5 LRAA not previously selected as a 
subpart V monitoring location.
    (7) Existing subpart L average residence time compliance monitoring 
location (maximum residence time compliance monitoring location for 
ground water systems) with the highest TTHM LRAA not previously selected 
as a subpart V monitoring location.
    (8) Location with the highest HAA5 LRAA not previously selected as a 
subpart V monitoring location.
    (d) You may recommend locations other than those specified in 
paragraph (c) of this section if you include a rationale for selecting 
other locations. If the State approves the alternate locations, you must 
monitor at these locations to determine compliance under subpart V of 
this part.
    (e) Your recommended schedule must include subpart V monitoring 
during the peak historical month for TTHM and HAA5 concentration, unless 
the State approves another month. Once you have identified the peak 
historical month, and if you are required to conduct routine monitoring 
at least quarterly, you must schedule subpart V compliance monitoring at 
a regular frequency of every 90 days or fewer.

[71 FR 483, Jan. 4, 2006, as amended at 74 FR 30958, June 29, 2009]



         Subpart V_Stage 2 Disinfection Byproducts Requirements

    Source: 71 FR 488, Jan. 4, 2006, unless otherwise noted.



Sec.  141.620  General requirements.

    (a) General. The requirements of subpart V of this part constitute 
national primary drinking water regulations. The regulations in this 
subpart establish monitoring and other requirements for achieving 
compliance with maximum contaminant levels based on locational running 
annual averages (LRAA) for total trihalomethanes (TTHM) and haloacetic 
acids (five)(HAA5), and for achieving compliance with maximum residual 
disinfectant residuals for chlorine and chloramine for certain 
consecutive systems.
    (b) Applicability. You are subject to these requirements if your 
system is a community water system or a nontransient noncommunity water 
system that uses a primary or residual disinfectant other than 
ultraviolet light or delivers water that has been treated with a primary 
or residual disinfectant other than ultraviolet light.
    (c) Schedule. You must comply with the requirements in this subpart 
on the schedule in the following table based on your system type.

[[Page 674]]



------------------------------------------------------------------------
                                       You must comply with subpart V
  If you are this type of system             monitoring by: \1\
------------------------------------------------------------------------
 Systems that are not part of a combined distribution system and systems
  that serve the largest population in the combined distribution system
------------------------------------------------------------------------
(1) System serving =100,000.
(2) System serving 50,000-99,999..  October 1, 2012.
(3) System serving 10,000-49,999..  October 1, 2013.
(4) System serving <10,000........  October 1, 2013 if no
                                     Cryptosporidium monitoring is
                                     required under Sec.   141.701(a)(4)
                                     or
                                    October 1, 2014 if Cryptosporidium
                                     monitoring is required under Sec.
                                     141.701(a)(4) or (a)(6)
------------------------------------------------------------------------
      Other systems that are part of a combined distribution system
------------------------------------------------------------------------
(5) Consecutive system or           --at the same time as the system
 wholesale system.                   with the earliest compliance date
                                     in the combined distribution
                                     system.
------------------------------------------------------------------------
\1\ The State may grant up to an additional 24 months for compliance
  with MCLs and operational evaluation levels if you require capital
  improvements to comply with an MCL.

    (6) Your monitoring frequency is specified in Sec.  141.621(a)(2).
    (i) If you are required to conduct quarterly monitoring, you must 
begin monitoring in the first full calendar quarter that includes the 
compliance date in the table in this paragraph (c).
    (ii) If you are required to conduct monitoring at a frequency that 
is less than quarterly, you must begin monitoring in the calendar month 
recommended in the IDSE report prepared under Sec.  141.601 or Sec.  
141.602 or the calendar month identified in the subpart V monitoring 
plan developed under Sec.  141.622 no later than 12 months after the 
compliance date in this table.
    (7) If you are required to conduct quarterly monitoring, you must 
make compliance calculations at the end of the fourth calendar quarter 
that follows the compliance date and at the end of each subsequent 
quarter (or earlier if the LRAA calculated based on fewer than four 
quarters of data would cause the MCL to be exceeded regardless of the 
monitoring results of subsequent quarters). If you are required to 
conduct monitoring at a frequency that is less than quarterly, you must 
make compliance calculations beginning with the first compliance sample 
taken after the compliance date.
    (8) For the purpose of the schedule in this paragraph (c), the State 
may determine that the combined distribution system does not include 
certain consecutive systems based on factors such as receiving water 
from a wholesale system only on an emergency basis or receiving only a 
small percentage and small volume of water from a wholesale system. The 
State may also determine that the combined distribution system does not 
include certain wholesale systems based on factors such as delivering 
water to a consecutive system only on an emergency basis or delivering 
only a small percentage and small volume of water to a consecutive 
system.
    (d) Monitoring and compliance--(1) Systems required to monitor 
quarterly. To comply with subpart V MCLs in Sec.  141.64(b)(2), you must 
calculate LRAAs for TTHM and HAA5 using monitoring results collected 
under this subpart and determine that each LRAA does not exceed the MCL. 
If you fail to complete four consecutive quarters of monitoring, you 
must calculate compliance with the MCL based on the average of the 
available data from the most recent four quarters. If you take more than 
one sample per quarter at a monitoring location, you must average all 
samples taken in the quarter at that location to determine a quarterly 
average to be used in the LRAA calculation.
    (2) Systems required to monitor yearly or less frequently. To 
determine compliance with subpart V MCLs in Sec.  141.64(b)(2), you must 
determine that each sample taken is less than the MCL. If any sample 
exceeds the MCL, you must comply with the requirements of Sec.  141.625. 
If no sample exceeds the MCL, the sample result for each monitoring 
location is considered the LRAA for that monitoring location.
    (e) Violation. You are in violation of the monitoring requirements 
for each quarter that a monitoring result would

[[Page 675]]

be used in calculating an LRAA if you fail to monitor.

[71 FR 488, Jan. 4, 2006; 71 FR 4645, Jan. 27, 2006]



Sec.  141.621  Routine monitoring.

    (a) Monitoring. (1) If you submitted an IDSE report, you must begin 
monitoring at the locations and months you have recommended in your IDSE 
report submitted under Sec.  141.605 following the schedule in Sec.  
141.620(c), unless the State requires other locations or additional 
locations after its review. If you submitted a 40/30 certification under 
Sec.  141.603 or you qualified for a very small system waiver under 
Sec.  141.604 or you are a nontransient noncommunity water system 
serving <10,000, you must monitor at the location(s) and dates 
identified in your monitoring plan in Sec.  141.132(f), updated as 
required by Sec.  141.622.
    (2) You must monitor at no fewer than the number of locations 
identified in this paragraph (a)(2).

----------------------------------------------------------------------------------------------------------------
                                                                                                   Distribution
                                                                                                      system
                                                                                                    monitoring
            Source water type              Population size category    Monitoring Frequency \1\   location total
                                                                                                  per monitoring
                                                                                                    period \2\
----------------------------------------------------------------------------------------------------------------
Subpart H:
                                          <500......................  per year..................               2
                                          500-3,300.................  per quarter...............               2
                                          3,301-9,999...............  per quarter...............               2
                                          10,000-49,999.............  per quarter...............               4
                                          50,000-249,999............  per quarter...............               8
                                          250,000-999,999...........  per quarter...............              12
                                          1,000,000-4,999,999.......  per quarter...............              16
                                          =5,000,000.....  per quarter...............              20
Ground Water:
                                          <500......................  per year..................               2
                                          500-9,999.................  per year..................               2
                                          10,000-99,999.............  per quarter...............               4
                                          100,000-499,999...........  per quarter...............               6
                                          =500,000.......  per quarter...............               8
----------------------------------------------------------------------------------------------------------------
\1\ All systems must monitor during month of highest DBP concentrations.
\2\ Systems on quarterly monitoring must take dual sample sets every 90 days at each monitoring location, except
  for subpart H systems serving 500-3,300. Ground water systems serving 500-9,999 on annual monitoring must take
  dual sample sets at each monitoring location. All other systems on annual monitoring and subpart H systems
  serving 500-3,300 are required to take individual TTHM and HAA5 samples (instead of a dual sample set) at the
  locations with the highest TTHM and HAA5 concentrations, respectively. For systems serving fewer than 500
  people, only one location with a dual sample set per monitoring period is needed if the highest TTHM and HAA5
  concentrations occur at the same location and month.

    (3) If you are an undisinfected system that begins using a 
disinfectant other than UV light after the dates in subpart U of this 
part for complying with the Initial Distribution System Evaluation 
requirements, you must consult with the State to identify compliance 
monitoring locations for this subpart. You must then develop a 
monitoring plan under Sec.  141.622 that includes those monitoring 
locations.
    (b) Analytical methods. You must use an approved method listed in 
Sec.  141.131 for TTHM and HAA5 analyses in this subpart. Analyses must 
be conducted by laboratories that have received certification by EPA or 
the State as specified in Sec.  141.131.

[71 FR 488, Jan. 4, 2006, as amended at 74 FR 30958, June 29, 2009]



Sec.  141.622  Subpart V monitoring plan.

    (a)(1) You must develop and implement a monitoring plan to be kept 
on file for State and public review. The monitoring plan must contain 
the elements in paragraphs (a)(1)(i) through (a)(1)(iv) of this section 
and be complete no later than the date you conduct your initial 
monitoring under this subpart.
    (i) Monitoring locations;
    (ii) Monitoring dates;
    (iii) Compliance calculation procedures; and
    (iv) Monitoring plans for any other systems in the combined 
distribution system if the State has reduced monitoring requirements 
under the State authority in Sec.  142.16(m).
    (2) If you were not required to submit an IDSE report under either 
Sec.  141.601 or

[[Page 676]]

Sec.  141.602, and you do not have sufficient subpart L monitoring 
locations to identify the required number of subpart V compliance 
monitoring locations indicated in Sec.  141.605(b), you must identify 
additional locations by alternating selection of locations representing 
high TTHM levels and high HAA5 levels until the required number of 
compliance monitoring locations have been identified. You must also 
provide the rationale for identifying the locations as having high 
levels of TTHM or HAA5. If you have more subpart L monitoring locations 
than required for subpart V compliance monitoring in Sec.  141.605(b), 
you must identify which locations you will use for subpart V compliance 
monitoring by alternating selection of locations representing high TTHM 
levels and high HAA5 levels until the required number of subpart V 
compliance monitoring locations have been identified.
    (b) If you are a subpart H system serving 3,300 people, 
you must submit a copy of your monitoring plan to the State prior to the 
date you conduct your initial monitoring under this subpart, unless your 
IDSE report submitted under subpart U of this part contains all the 
information required by this section.
    (c) You may revise your monitoring plan to reflect changes in 
treatment, distribution system operations and layout (including new 
service areas), or other factors that may affect TTHM or HAA5 formation, 
or for State-approved reasons, after consultation with the State 
regarding the need for changes and the appropriateness of changes. If 
you change monitoring locations, you must replace existing compliance 
monitoring locations with the lowest LRAA with new locations that 
reflect the current distribution system locations with expected high 
TTHM or HAA5 levels. The State may also require modifications in your 
monitoring plan. If you are a subpart H system serving 3,300 
people, you must submit a copy of your modified monitoring plan to the 
State prior to the date you are required to comply with the revised 
monitoring plan.



Sec.  141.623  Reduced monitoring.

    (a) You may reduce monitoring to the level specified in the table in 
this paragraph (a) any time the LRAA is <=0.040 mg/L for TTHM and 
<=0.030 mg/L for HAA5 at all monitoring locations. You may only use data 
collected under the provisions of this subpart or subpart L of this part 
to qualify for reduced monitoring. In addition, the source water annual 
average TOC level, before any treatment, must be <=4.0 mg/L at each 
treatment plant treating surface water or ground water under the direct 
influence of surface water, based on monitoring conducted under either 
Sec.  141.132(b)(1)(iii) or Sec.  141.132(d).

----------------------------------------------------------------------------------------------------------------
                                                                                          Distribution system
            Source water type               Population     Monitoring frequency \1\     monitoring location per
                                           size category                                   monitoring period
----------------------------------------------------------------------------------------------------------------
Subpart H:
                                                    <500  ..........................  monitoring may not be
                                                                                       reduced.
                                               500-3,300  per year..................  1 TTHM and 1 HAA5 sample:
                                                                                       one at the location and
                                                                                       during the quarter with
                                                                                       the highest TTHM single
                                                                                       measurement, one at the
                                                                                       location and during the
                                                                                       quarter with the highest
                                                                                       HAA5 single measurement;
                                                                                       1 dual sample set per
                                                                                       year if the highest TTHM
                                                                                       and HAA5 measurements
                                                                                       occurred at the same
                                                                                       location and quarter.
                                             3,301-9,999  per year..................  2 dual sample sets: one at
                                                                                       the location and during
                                                                                       the quarter with the
                                                                                       highest TTHM single
                                                                                       measurement, one at the
                                                                                       location and during the
                                                                                       quarter with the highest
                                                                                       HAA5 single measurement.
                                           10,000-49,999  per quarter...............  2 dual sample sets at the
                                                                                       locations with the
                                                                                       highest TTHM and highest
                                                                                       HAA5 LRAAs.
                                          50,000-249,999  per quarter...............  4 dual sample sets--at the
                                                                                       locations with the two
                                                                                       highest TTHM and two
                                                                                       highest HAA5 LRAAs.
                                          250,000-999,99  per quarter...............  6 dual sample sets--at the
                                                       9                               locations with the three
                                                                                       highest TTHM and three
                                                                                       highest HAA5 LRAAs.

[[Page 677]]

 
                                          1,000,000-4,99  per quarter...............  8 dual sample sets--at the
                                                   9,999                               locations with the four
                                                                                       highest TTHM and four
                                                                                       highest HAA5 LRAAs.
                                          =5,  per quarter...............  10 dual sample sets--at
                                                 000,000                               the locations with the
                                                                                       five highest TTHM and
                                                                                       five highest HAA5 LRAAs.
Ground Water:
                                                    <500  every third year..........  1 TTHM and 1 HAA5 sample:
                                                                                       one at the location and
                                                                                       during the quarter with
                                                                                       the highest TTHM single
                                                                                       measurement, one at the
                                                                                       location and during the
                                                                                       quarter with the highest
                                                                                       HAA5 single measurement;
                                                                                       1 dual sample set per
                                                                                       year if the highest TTHM
                                                                                       and HAA5 measurements
                                                                                       occurred at the same
                                                                                       location and quarter.
                                               500-9,999  per year..................  1 TTHM and 1 HAA5 sample:
                                                                                       one at the location and
                                                                                       during the quarter with
                                                                                       the highest TTHM single
                                                                                       measurement, one at the
                                                                                       location and during the
                                                                                       quarter with the highest
                                                                                       HAA5 single measurement;
                                                                                       1 dual sample set per
                                                                                       year if the highest TTHM
                                                                                       and HAA5 measurements
                                                                                       occurred at the same
                                                                                       location and quarter.
                                           10,000-99,999  per year..................  2 dual sample sets: one at
                                                                                       the location and during
                                                                                       the quarter with the
                                                                                       highest TTHM single
                                                                                       measurement, one at the
                                                                                       location and during the
                                                                                       quarter with the highest
                                                                                       HAA5 single measurement.
                                          100,000-499,99  per quarter...............  2 dual sample sets; at the
                                                       9                               locations with the
                                                                                       highest TTHM and highest
                                                                                       HAA5 LRAAs.
                                          =50  per quarter...............  4 dual sample sets at the
                                                   0,000                               locations with the two
                                                                                       highest TTHM and two
                                                                                       highest HAA5 LRAAs.
----------------------------------------------------------------------------------------------------------------
\1\ Systems on quarterly monitoring must take dual sample sets every 90 days.

    (b) You may remain on reduced monitoring as long as the TTHM LRAA 
<=0.040 mg/L and the HAA5 LRAA <=0.030 mg/L at each monitoring location 
(for systems with quarterly reduced monitoring) or each TTHM sample 
<=0.060 mg/L and each HAA5 sample <=0.045 mg/L (for systems with annual 
or less frequent monitoring). In addition, the source water annual 
average TOC level, before any treatment, must be <=4.0 mg/L at each 
treatment plant treating surface water or ground water under the direct 
influence of surface water, based on monitoring conducted under either 
Sec.  141.132(b)(1)(iii) or Sec.  141.132(d).
    (c) If the LRAA based on quarterly monitoring at any monitoring 
location exceeds either 0.040 mg/L for TTHM or 0.030 mg/L for HAA5 or if 
the annual (or less frequent) sample at any location exceeds either 
0.060 mg/L for TTHM or 0.045 mg/L for HAA5, or if the source water 
annual average TOC level, before any treatment, 4.0 mg/L at 
any treatment plant treating surface water or ground water under the 
direct influence of surface water, you must resume routine monitoring 
under Sec.  141.621 or begin increased monitoring if Sec.  141.625 
applies.
    (d) The State may return your system to routine monitoring at the 
State's discretion.



Sec.  141.624  Additional requirements for consecutive systems.

    If you are a consecutive system that does not add a disinfectant but 
delivers water that has been treated with a primary or residual 
disinfectant other than ultraviolet light, you must comply with 
analytical and monitoring requirements for chlorine and chloramines in 
Sec.  141.131 (c) and Sec.  141.132(c)(1) and the compliance 
requirements in Sec.  141.133(c)(1) beginning April 1, 2009, unless 
required earlier by the State, and report monitoring results under Sec.  
141.134(c).



Sec.  141.625  Conditions requiring increased monitoring.

    (a) If you are required to monitor at a particular location annually 
or less frequently than annually under Sec.  141.621

[[Page 678]]

or Sec.  141.623, you must increase monitoring to dual sample sets once 
per quarter (taken every 90 days) at all locations if a TTHM sample is 
0.080 mg/L or a HAA5 sample is 0.060 mg/L at any 
location.
    (b) You are in violation of the MCL when the LRAA exceeds the 
subpart V MCLs in Sec.  141.64(b)(2), calculated based on four 
consecutive quarters of monitoring (or the LRAA calculated based on 
fewer than four quarters of data if the MCL would be exceeded regardless 
of the monitoring results of subsequent quarters). You are in violation 
of the monitoring requirements for each quarter that a monitoring result 
would be used in calculating an LRAA if you fail to monitor.
    (c) You may return to routine monitoring once you have conducted 
increased monitoring for at least four consecutive quarters and the LRAA 
for every monitoring location is <=0.060 mg/L for TTHM and <=0.045 mg/L 
for HAA5.



Sec.  141.626  Operational evaluation levels.

    (a) You have exceeded the operational evaluation level at any 
monitoring location where the sum of the two previous quarters' TTHM 
results plus twice the current quarter's TTHM result, divided by 4 to 
determine an average, exceeds 0.080 mg/L, or where the sum of the two 
previous quarters' HAA5 results plus twice the current quarter's HAA5 
result, divided by 4 to determine an average, exceeds 0.060 mg/L.
    (b)(1) If you exceed the operational evaluation level, you must 
conduct an operational evaluation and submit a written report of the 
evaluation to the State no later than 90 days after being notified of 
the analytical result that causes you to exceed the operational 
evaluation level. The written report must be made available to the 
public upon request.
    (2) Your operational evaluation must include an examination of 
system treatment and distribution operational practices, including 
storage tank operations, excess storage capacity, distribution system 
flushing, changes in sources or source water quality, and treatment 
changes or problems that may contribute to TTHM and HAA5 formation and 
what steps could be considered to minimize future exceedences.
    (i) You may request and the State may allow you to limit the scope 
of your evaluation if you are able to identify the cause of the 
operational evaluation level exceedance.
    (ii) Your request to limit the scope of the evaluation does not 
extend the schedule in paragraph (b)(1) of this section for submitting 
the written report. The State must approve this limited scope of 
evaluation in writing and you must keep that approval with the completed 
report.



Sec.  141.627  Requirements for remaining on reduced TTHM and HAA5 
monitoring based on subpart L results.

    You may remain on reduced monitoring after the dates identified in 
Sec.  141.620(c) for compliance with this subpart only if you qualify 
for a 40/30 certification under Sec.  141.603 or have received a very 
small system waiver under Sec.  141.604, plus you meet the reduced 
monitoring criteria in Sec.  141.623(a), and you do not change or add 
monitoring locations from those used for compliance monitoring under 
subpart L of this part. If your monitoring locations under this subpart 
differ from your monitoring locations under subpart L of this part, you 
may not remain on reduced monitoring after the dates identified in Sec.  
141.620(c) for compliance with this subpart.



Sec.  141.628  Requirements for remaining on increased TTHM and HAA5 
monitoring based on subpart L results.

    If you were on increased monitoring under Sec.  141.132(b)(1), you 
must remain on increased monitoring until you qualify for a return to 
routine monitoring under Sec.  141.625(c). You must conduct increased 
monitoring under Sec.  141.625 at the monitoring locations in the 
monitoring plan developed under Sec.  141.622 beginning at the date 
identified in Sec.  141.620(c) for compliance with this subpart and 
remain on increased monitoring until you qualify for a return to routine 
monitoring under Sec.  141.625(c).

[[Page 679]]



Sec.  141.629  Reporting and recordkeeping requirements.

    (a) Reporting. (1) You must report the following information for 
each monitoring location to the State within 10 days of the end of any 
quarter in which monitoring is required:
    (i) Number of samples taken during the last quarter.
    (ii) Date and results of each sample taken during the last quarter.
    (iii) Arithmetic average of quarterly results for the last four 
quarters for each monitoring location (LRAA), beginning at the end of 
the fourth calendar quarter that follows the compliance date and at the 
end of each subsequent quarter. If the LRAA calculated based on fewer 
than four quarters of data would cause the MCL to be exceeded regardless 
of the monitoring results of subsequent quarters, you must report this 
information to the State as part of the first report due following the 
compliance date or anytime thereafter that this determination is made. 
If you are required to conduct monitoring at a frequency that is less 
than quarterly, you must make compliance calculations beginning with the 
first compliance sample taken after the compliance date, unless you are 
required to conduct increased monitoring under Sec.  141.625.
    (iv) Whether, based on Sec.  141.64(b)(2) and this subpart, the MCL 
was violated at any monitoring location.
    (v) Any operational evaluation levels that were exceeded during the 
quarter and, if so, the location and date, and the calculated TTHM and 
HAA5 levels.
    (2) If you are a subpart H system seeking to qualify for or remain 
on reduced TTHM/HAA5 monitoring, you must report the following source 
water TOC information for each treatment plant that treats surface water 
or ground water under the direct influence of surface water to the State 
within 10 days of the end of any quarter in which monitoring is 
required:
    (i) The number of source water TOC samples taken each month during 
last quarter.
    (ii) The date and result of each sample taken during last quarter.
    (iii) The quarterly average of monthly samples taken during last 
quarter or the result of the quarterly sample.
    (iv) The running annual average (RAA) of quarterly averages from the 
past four quarters.
    (v) Whether the RAA exceeded 4.0 mg/L.
    (3) The State may choose to perform calculations and determine 
whether the MCL was exceeded or the system is eligible for reduced 
monitoring in lieu of having the system report that information
    (b) Recordkeeping. You must retain any subpart V monitoring plans 
and your subpart V monitoring results as required by Sec.  141.33.



            Subpart W_Enhanced Treatment for Cryptosporidium

    Source: 71 FR 769, Jan. 5, 2006, unless otherwise noted.

                          General Requirements



Sec.  141.700  General requirements.

    (a) The requirements of this subpart W are national primary drinking 
water regulations. The regulations in this subpart establish or extend 
treatment technique requirements in lieu of maximum contaminant levels 
for Cryptosporidium. These requirements are in addition to requirements 
for filtration and disinfection in subparts H, P, and T of this part.
    (b) Applicability. The requirements of this subpart apply to all 
subpart H systems, which are public water systems supplied by a surface 
water source and public water systems supplied by a ground water source 
under the direct influence of surface water.
    (1) Wholesale systems, as defined in Sec.  141.2, must comply with 
the requirements of this subpart based on the population of the largest 
system in the combined distribution system.
    (2) The requirements of this subpart for filtered systems apply to 
systems required by National Primary Drinking Water Regulations to 
provide filtration treatment, whether or not the system is currently 
operating a filtration system.
    (3) The requirements of this subpart for unfiltered systems apply 
only to unfiltered systems that timely met and

[[Page 680]]

continue to meet the filtration avoidance criteria in subparts H, P, and 
T of this part, as applicable.
    (c) Requirements. Systems subject to this subpart must comply with 
the following requirements:
    (1) Systems must conduct an initial and a second round of source 
water monitoring for each plant that treats a surface water or GWUDI 
source. This monitoring may include sampling for Cryptosporidium, E. 
coli, and turbidity as described in Sec. Sec.  141.701 through 141.706, 
to determine what level, if any, of additional Cryptosporidium treatment 
they must provide.
    (2) Systems that plan to make a significant change to their 
disinfection practice must develop disinfection profiles and calculate 
disinfection benchmarks, as described in Sec. Sec.  141.708 through 
141.709.
    (3) Filtered systems must determine their Cryptosporidium treatment 
bin classification as described in Sec.  141.710 and provide additional 
treatment for Cryptosporidium, if required, as described in Sec.  
141.711. All unfiltered systems must provide treatment for 
Cryptosporidium as described in Sec.  141.712. Filtered and unfiltered 
systems must implement Cryptosporidium treatment according to the 
schedule in Sec.  141.713.
    (4) Systems with uncovered finished water storage facilities must 
comply with the requirements to cover the facility or treat the 
discharge from the facility as described in Sec.  141.714.
    (5) Systems required to provide additional treatment for 
Cryptosporidium must implement microbial toolbox options that are 
designed and operated as described in Sec. Sec.  141.715 through 
141.720.
    (6) Systems must comply with the applicable recordkeeping and 
reporting requirements described in Sec. Sec.  141.721 through 141.722.
    (7) Systems must address significant deficiencies identified in 
sanitary surveys performed by EPA as described in Sec.  141.723.

                  Source Water Monitoring Requirements



Sec.  141.701  Source water monitoring.

    (a) Initial round of source water monitoring. Systems must conduct 
the following monitoring on the schedule in paragraph (c) of this 
section unless they meet the monitoring exemption criteria in paragraph 
(d) of this section.
    (1) Filtered systems serving at least 10,000 people must sample 
their source water for Cryptosporidium, E. coli, and turbidity at least 
monthly for 24 months.
    (2) Unfiltered systems serving at least 10,000 people must sample 
their source water for Cryptosporidium at least monthly for 24 months.
    (3)(i) Filtered systems serving fewer than 10,000 people must sample 
their source water for E. coli at least once every two weeks for 12 
months.
    (ii) A filtered system serving fewer than 10,000 people may avoid E. 
coli monitoring if the system notifies the State that it will monitor 
for Cryptosporidium as described in paragraph (a)(4) of this section. 
The system must notify the State no later than 3 months prior to the 
date the system is otherwise required to start E. coli monitoring under 
Sec.  141.701(c).
    (4) Filtered systems serving fewer than 10,000 people must sample 
their source water for Cryptosporidium at least twice per month for 12 
months or at least monthly for 24 months if they meet one of the 
following, based on monitoring conducted under paragraph (a)(3) of this 
section:
    (i) For systems using lake/reservoir sources, the annual mean E. 
coli concentration is greater than 10 E. coli/100 mL.
    (ii) For systems using flowing stream sources, the annual mean E. 
coli concentration is greater than 50 E. coli/100 mL.
    (iii) The system does not conduct E. coli monitoring as described in 
paragraph (a)(3) of this section.
    (iv) Systems using ground water under the direct influence of 
surface water (GWUDI) must comply with the requirements of paragraph 
(a)(4) of this section based on the E. coli level that applies to the 
nearest surface water body. If no surface water body is nearby, the 
system must comply based on the requirements that apply to systems using 
lake/reservoir sources.
    (5) For filtered systems serving fewer than 10,000 people, the State 
may approve monitoring for an indicator

[[Page 681]]

other than E. coli under paragraph (a)(3) of this section. The State 
also may approve an alternative to the E. coli concentration in 
paragraph (a)(4)(i), (ii) or (iv) of this section to trigger 
Cryptosporidium monitoring. This approval by the State must be provided 
to the system in writing and must include the basis for the State's 
determination that the alternative indicator and/or trigger level will 
provide a more accurate identification of whether a system will exceed 
the Bin 1 Cryptosporidium level in Sec.  141.710.
    (6) Unfiltered systems serving fewer than 10,000 people must sample 
their source water for Cryptosporidium at least twice per month for 12 
months or at least monthly for 24 months.
    (7) Systems may sample more frequently than required under this 
section if the sampling frequency is evenly spaced throughout the 
monitoring period.
    (b) Second round of source water monitoring. Systems must conduct a 
second round of source water monitoring that meets the requirements for 
monitoring parameters, frequency, and duration described in paragraph 
(a) of this section, unless they meet the monitoring exemption criteria 
in paragraph (d) of this section. Systems must conduct this monitoring 
on the schedule in paragraph (c) of this section.
    (c) Monitoring schedule. Systems must begin the monitoring required 
in paragraphs (a) and (b) of this section no later than the month 
beginning with the date listed in this table:

              Source Water Monitoring Starting Dates Table
------------------------------------------------------------------------
                                                     And must begin the
                              Must begin the first     second round of
                                 round of source        source water
  Systems that serve . . .     water monitoring no   monitoring no later
                              later than the month     than the month
                                 beginning . . .       beginning . . .
------------------------------------------------------------------------
(1) At least 100,000 people.  (i) October 1, 2006.  (ii) April 1, 2015.
(2) From 50,000 to 99,999     (i) April 1, 2007...  (ii) October 1,
 people.                                             2015.
(3) From 10,000 to 49,999     (i) April 1, 2008...  (ii) October 1,
 people.                                             2016.
(4) Fewer than 10,000 and     (i) October 1, 2008.  (ii) October 1,
 monitor for E. coli \a\.                            2017.
(5) Fewer than 10,000 and     (i) April 1, 2010...  (ii) April 1, 2019.
 monitor for Cryptosporidium
 \b\.
------------------------------------------------------------------------
\a\ Applies only to filtered systems.
\b\ Applies to filtered systems that meet the conditions of paragraph
  (a)(4) of this section and unfiltered systems.

    (d) Monitoring avoidance. (1) Filtered systems are not required to 
conduct source water monitoring under this subpart if the system will 
provide a total of at least 5.5-log of treatment for Cryptosporidium, 
equivalent to meeting the treatment requirements of Bin 4 in Sec.  
141.711.
    (2) Unfiltered systems are not required to conduct source water 
monitoring under this subpart if the system will provide a total of at 
least 3-log Cryptosporidium inactivation, equivalent to meeting the 
treatment requirements for unfiltered systems with a mean 
Cryptosporidium concentration of greater than 0.01 oocysts/L in Sec.  
141.712.
    (3) If a system chooses to provide the level of treatment in 
paragraph (d)(1) or (2) of this section, as applicable, rather than 
start source water monitoring, the system must notify the State in 
writing no later than the date the system is otherwise required to 
submit a sampling schedule for monitoring under Sec.  141.702. 
Alternatively, a system may choose to stop sampling at any point after 
it has initiated monitoring if it notifies the State in writing that it 
will provide this level of treatment. Systems must install and operate 
technologies to provide this level of treatment by the applicable 
treatment compliance date in Sec.  141.713.
    (e) Plants operating only part of the year. Systems with subpart H 
plants that operate for only part of the year must conduct source water 
monitoring in accordance with this subpart, but with the following 
modifications:
    (1) Systems must sample their source water only during the months 
that the plant operates unless the State specifies another monitoring 
period based on plant operating practices.
    (2) Systems with plants that operate less than six months per year 
and that

[[Page 682]]

monitor for Cryptosporidium must collect at least six Cryptosporidium 
samples per year during each of two years of monitoring. Samples must be 
evenly spaced throughout the period the plant operates.
    (f)(1) New sources. A system that begins using a new source of 
surface water or GWUDI after the system is required to begin monitoring 
under paragraph (c) of this section must monitor the new source on a 
schedule the State approves. Source water monitoring must meet the 
requirements of this subpart. The system must also meet the bin 
classification and Cryptosporidium treatment requirements of Sec. Sec.  
141.710 and 141.711 or Sec.  141.712, as applicable, for the new source 
on a schedule the State approves.
    (2) The requirements of Sec.  141.701(f) apply to subpart H systems 
that begin operation after the monitoring start date applicable to the 
system's size under paragraph (c) of this section.
    (3) The system must begin a second round of source water monitoring 
no later than 6 years following initial bin classification under Sec.  
141.710 or determination of the mean Cryptosporidium level under Sec.  
141.712, as applicable.
    (g) Failure to collect any source water sample required under this 
section in accordance with the sampling schedule, sampling location, 
analytical method, approved laboratory, and reporting requirements of 
Sec. Sec.  141.702 through 141.706 is a monitoring violation.
    (h) Grandfathering monitoring data. Systems may use (grandfather) 
monitoring data collected prior to the applicable monitoring start date 
in paragraph (c) of this section to meet the initial source water 
monitoring requirements in paragraph (a) of this section. Grandfathered 
data may substitute for an equivalent number of months at the end of the 
monitoring period. All data submitted under this paragraph must meet the 
requirements in Sec.  141.707.



Sec.  141.702  Sampling schedules.

    (a) Systems required to conduct source water monitoring under Sec.  
141.701 must submit a sampling schedule that specifies the calendar 
dates when the system will collect each required sample.
    (1) Systems must submit sampling schedules no later than 3 months 
prior to the applicable date listed in Sec.  141.701(c) for each round 
of required monitoring.
    (2)(i) Systems serving at least 10,000 people must submit their 
sampling schedule for the initial round of source water monitoring under 
Sec.  141.701(a) to EPA electronically at https://intranet.epa.gov/lt2/.
    (ii) If a system is unable to submit the sampling schedule 
electronically, the system may use an alternative approach for 
submitting the sampling schedule that EPA approves.
    (3) Systems serving fewer than 10,000 people must submit their 
sampling schedules for the initial round of source water monitoring 
Sec.  141.701(a) to the State.
    (4) Systems must submit sampling schedules for the second round of 
source water monitoring Sec.  141.701(b) to the State.
    (5) If EPA or the State does not respond to a system regarding its 
sampling schedule, the system must sample at the reported schedule.
    (b) Systems must collect samples within two days before or two days 
after the dates indicated in their sampling schedule (i.e., within a 
five-day period around the schedule date) unless one of the conditions 
of paragraph (b)(1) or (2) of this section applies.
    (1) If an extreme condition or situation exists that may pose danger 
to the sample collector, or that cannot be avoided and causes the system 
to be unable to sample in the scheduled five-day period, the system must 
sample as close to the scheduled date as is feasible unless the State 
approves an alternative sampling date. The system must submit an 
explanation for the delayed sampling date to the State concurrent with 
the shipment of the sample to the laboratory.
    (2)(i) If a system is unable to report a valid analytical result for 
a scheduled sampling date due to equipment failure, loss of or damage to 
the sample, failure to comply with the analytical method requirements, 
including the quality control requirements in Sec.  141.704, or the 
failure of an approved

[[Page 683]]

laboratory to analyze the sample, then the system must collect a 
replacement sample.
    (ii) The system must collect the replacement sample not later than 
21 days after receiving information that an analytical result cannot be 
reported for the scheduled date unless the system demonstrates that 
collecting a replacement sample within this time frame is not feasible 
or the State approves an alternative resampling date. The system must 
submit an explanation for the delayed sampling date to the State 
concurrent with the shipment of the sample to the laboratory.
    (c) Systems that fail to meet the criteria of paragraph (b) of this 
section for any source water sample required under Sec.  141.701 must 
revise their sampling schedules to add dates for collecting all missed 
samples. Systems must submit the revised schedule to the State for 
approval prior to when the system begins collecting the missed samples.



Sec.  141.703  Sampling locations.

    (a) Systems required to conduct source water monitoring under Sec.  
141.701 must collect samples for each plant that treats a surface water 
or GWUDI source. Where multiple plants draw water from the same 
influent, such as the same pipe or intake, the State may approve one set 
of monitoring results to be used to satisfy the requirements of Sec.  
141.701 for all plants.
    (b)(1) Systems must collect source water samples prior to chemical 
treatment, such as coagulants, oxidants and disinfectants, unless the 
system meets the condition of paragraph (b)(2) of this section.
    (2) The State may approve a system to collect a source water sample 
after chemical treatment. To grant this approval, the State must 
determine that collecting a sample prior to chemical treatment is not 
feasible for the system and that the chemical treatment is unlikely to 
have a significant adverse effect on the analysis of the sample.
    (c) Systems that recycle filter backwash water must collect source 
water samples prior to the point of filter backwash water addition.
    (d) Bank filtration. (1) Systems that receive Cryptosporidium 
treatment credit for bank filtration under Sec.  141.173(b) or Sec.  
141.552(a), as applicable, must collect source water samples in the 
surface water prior to bank filtration.
    (2) Systems that use bank filtration as pretreatment to a filtration 
plant must collect source water samples from the well (i.e., after bank 
filtration). Use of bank filtration during monitoring must be consistent 
with routine operational practice. Systems collecting samples after a 
bank filtration process may not receive treatment credit for the bank 
filtration under Sec.  141.717(c).
    (e) Multiple sources. Systems with plants that use multiple water 
sources, including multiple surface water sources and blended surface 
water and ground water sources, must collect samples as specified in 
paragraph (e)(1) or (2) of this section. The use of multiple sources 
during monitoring must be consistent with routine operational practice.
    (1) If a sampling tap is available where the sources are combined 
prior to treatment, systems must collect samples from the tap.
    (2) If a sampling tap where the sources are combined prior to 
treatment is not available, systems must collect samples at each source 
near the intake on the same day and must follow either paragraph 
(e)(2)(i) or (ii) of this section for sample analysis.
    (i) Systems may composite samples from each source into one sample 
prior to analysis. The volume of sample from each source must be 
weighted according to the proportion of the source in the total plant 
flow at the time the sample is collected.
    (ii) Systems may analyze samples from each source separately and 
calculate a weighted average of the analysis results for each sampling 
date. The weighted average must be calculated by multiplying the 
analysis result for each source by the fraction the source contributed 
to total plant flow at the time the sample was collected and then 
summing these values.
    (f) Additional Requirements. Systems must submit a description of 
their sampling location(s) to the State at

[[Page 684]]

the same time as the sampling schedule required under Sec.  141.702. 
This description must address the position of the sampling location in 
relation to the system's water source(s) and treatment processes, 
including pretreatment, points of chemical treatment, and filter 
backwash recycle. If the State does not respond to a system regarding 
sampling location(s), the system must sample at the reported 
location(s).



Sec.  141.704  Analytical methods.

    (a) Cryptosporidium. Systems must analyze for Cryptosporidium using 
Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA, 
2005, United States Environmental Protection Agency, EPA-815-R-05-002 or 
Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, 2005, United 
States Environmental Protection Agency, EPA-815-R-05-001, which are 
incorporated by reference, or alternative methods listed in appendix A 
to subpart C of this part. The Director of the Federal Register approves 
this incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 
CFR part 51. You may obtain a copy of these methods online from http://
www.epa.gov/safewater/disinfection/lt2 or from the United States 
Environmental Protection Agency, Office of Ground Water and Drinking 
Water, 1201 Constitution Ave., NW., Washington, DC 20460 (Telephone: 
800-426-4791). You may inspect a copy at the Water Docket in the EPA 
Docket Center, 1301 Constitution Ave., NW., Washington, DC (Telephone: 
202-566-2426) or at the National Archives and Records Administration 
(NARA). For information on the availability of this material at NARA, 
call 202-741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Systems must analyze at least a 10 L sample or a packed pellet 
volume of at least 2 mL as generated by the methods listed in paragraph 
(a) of this section. Systems unable to process a 10 L sample must 
analyze as much sample volume as can be filtered by two filters approved 
by EPA for the methods listed in paragraph (a) of this section, up to a 
packed pellet volume of at least 2 mL.
    (2)(i) Matrix spike (MS) samples, as required by the methods in 
paragraph (a) of this section, must be spiked and filtered by a 
laboratory approved for Cryptosporidium analysis under Sec.  141.705.
    (ii) If the volume of the MS sample is greater than 10 L, the system 
may filter all but 10 L of the MS sample in the field, and ship the 
filtered sample and the remaining 10 L of source water to the 
laboratory. In this case, the laboratory must spike the remaining 10 L 
of water and filter it through the filter used to collect the balance of 
the sample in the field.
    (3) Flow cytometer-counted spiking suspensions must be used for MS 
samples and ongoing precision and recovery (OPR) samples.
    (b) E. coli. System must use methods for enumeration of E. coli in 
source water approved in Sec.  136.3(a) of this chapter or alternative 
methods listed in appendix A to subpart C of this part.
    (1) The time from sample collection to initiation of analysis may 
not exceed 30 hours unless the system meets the condition of paragraph 
(b)(2) of this section.
    (2) The State may approve on a case-by-case basis the holding of an 
E. coli sample for up to 48 hours between sample collection and 
initiation of analysis if the State determines that analyzing an E. coli 
sample within 30 hours is not feasible. E. coli samples held between 30 
to 48 hours must be analyzed by the Colilert reagent version of Standard 
Method 9223B as listed in Sec.  136.3(a) of this title.
    (3) Systems must maintain samples between 0 [deg]C and 10 [deg]C 
during storage and transit to the laboratory.
    (c) Turbidity. Systems must use methods for turbidity measurement 
approved in Sec.  141.74(a)(1).

[71 FR 769, Jan. 5, 2006, as amended at 74 FR 30959, June 29, 2009]



Sec.  141.705  Approved laboratories.

    (a) Cryptosporidium. Systems must have Cryptosporidium samples 
analyzed by a laboratory that is approved under EPA's Laboratory Quality 
Assurance Evaluation Program for Analysis of Cryptosporidium in Water or 
a laboratory that has been certified for

[[Page 685]]

Cryptosporidium analysis by an equivalent State laboratory certification 
program.
    (b) E. coli. Any laboratory certified by the EPA, the National 
Environmental Laboratory Accreditation Conference or the State for total 
coliform or fecal coliform analysis under Sec.  141.74 is approved for 
E. coli analysis under this subpart when the laboratory uses the same 
technique for E. coli that the laboratory uses for Sec.  141.74.
    (c) Turbidity. Measurements of turbidity must be made by a party 
approved by the State.



Sec.  141.706  Reporting source water monitoring results.

    (a) Systems must report results from the source water monitoring 
required under Sec.  141.701 no later than 10 days after the end of the 
first month following the month when the sample is collected.
    (b)(1) All systems serving at least 10,000 people must report the 
results from the initial source water monitoring required under Sec.  
141.701(a) to EPA electronically at https://intranet.epa.gov/lt2/.
    (2) If a system is unable to report monitoring results 
electronically, the system may use an alternative approach for reporting 
monitoring results that EPA approves.
    (c) Systems serving fewer than 10,000 people must report results 
from the initial source water monitoring required under Sec.  141.701(a) 
to the State.
    (d) All systems must report results from the second round of source 
water monitoring required under Sec.  141.701(b) to the State.
    (e) Systems must report the applicable information in paragraphs 
(e)(1) and (2) of this section for the source water monitoring required 
under Sec.  141.701.
    (1) Systems must report the following data elements for each 
Cryptosporidium analysis:

1. PWS ID.
2. Facility ID.
3. Sample collection date.
4. Sample type (field or matrix spike).
5. Sample volume filtered (L), to nearest \1/4\ L.
6. Was 100% of filtered volume examined.
7. Number of oocysts counted.
 

    (i) For matrix spike samples, systems must also report the sample 
volume spiked and estimated number of oocysts spiked. These data are not 
required for field samples.
    (ii) For samples in which less than 10 L is filtered or less than 
100% of the sample volume is examined, systems must also report the 
number of filters used and the packed pellet volume.
    (iii) For samples in which less than 100% of sample volume is 
examined, systems must also report the volume of resuspended concentrate 
and volume of this resuspension processed through immunomagnetic 
separation.
    (2) Systems must report the following data elements for each E. coli 
analysis:

Data element.
 
1. PWS ID.
2. Facility ID.
3. Sample collection date.
4. Analytical method number.
5. Method type.
6. Source type (flowing stream, lake/reservoir, GWUDI).
7. E. coli/100 mL.
8. Turbidity. \1\
 
\1\ Systems serving fewer than 10,000 people that are not required to
  monitor for turbidity under Sec.   141.701 are not required to report
  turbidity with their E. coli results.



Sec.  141.707  Grandfathering previously collected data.

    (a)(1) Systems may comply with the initial source water monitoring 
requirements of Sec.  141.701(a) by grandfathering sample results 
collected before the system is required to begin monitoring (i.e., 
previously collected data). To be grandfathered, the sample results and 
analysis must meet the criteria in this section and the State must 
approve.
    (2) A filtered system may grandfather Cryptosporidium samples to 
meet the requirements of Sec.  141.701(a) when the system does not have 
corresponding E. coli and turbidity samples. A system that grandfathers 
Cryptosporidium samples without E. coli and turbidity samples is not 
required to collect E. coli and turbidity samples when the system 
completes the requirements for Cryptosporidium monitoring under Sec.  
141.701(a).
    (b) E. coli sample analysis. The analysis of E. coli samples must 
meet the analytical method and approved laboratory requirements of 
Sec. Sec.  141.704 through 141.705.

[[Page 686]]

    (c) Cryptosporidium sample analysis. The analysis of Cryptosporidium 
samples must meet the criteria in this paragraph.
    (1) Laboratories analyzed Cryptosporidium samples using one of the 
analytical methods in paragraphs (c)(1)(i) through (vi) of this section, 
which are incorporated by reference. The Director of the Federal 
Register approves this incorporation by reference in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. You may obtain a copy of these methods 
on-line from the United States Environmental Protection Agency, Office 
of Ground Water and Drinking Water, 1201 Constitution Ave, NW, 
Washington, DC 20460 (Telephone: 800-426-4791). You may inspect a copy 
at the Water Docket in the EPA Docket Center, 1301 Constitution Ave., 
NW, Washington, DC, (Telephone: 202-566-2426) or at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (i) Method 1623: Cryptosporidium and Giardia in Water by Filtration/
IMS/FA, 2005, United States Environmental Protection Agency, EPA-815-R-
05-002.
    (ii) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, 
2005, United States Environmental Protection Agency, EPA-815-R-05-001.
    (iii) Method 1623: Cryptosporidium and Giardia in Water by 
Filtration/IMS/FA, 2001, United States Environmental Protection Agency, 
EPA-821-R-01-025.
    (iv) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, 
2001, United States Environmental Protection Agency, EPA-821--R-01-026.
    (v) Method 1623: Cryptosporidium and Giardia in Water by Filtration/
IMS/FA, 1999, United States Environmental Protection Agency, EPA-821-R-
99-006.
    (vi) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, 
1999, United States Environmental Protection Agency, EPA-821-R-99-001.
    (2) For each Cryptosporidium sample, the laboratory analyzed at 
least 10 L of sample or at least 2 mL of packed pellet or as much volume 
as could be filtered by 2 filters that EPA approved for the methods 
listed in paragraph (c)(1) of this section.
    (d) Sampling location. The sampling location must meet the 
conditions in Sec.  141.703.
    (e) Sampling frequency. Cryptosporidium samples were collected no 
less frequently than each calendar month on a regular schedule, 
beginning no earlier than January 1999. Sample collection intervals may 
vary for the conditions specified in Sec.  141.702(b)(1) and (2) if the 
system provides documentation of the condition when reporting monitoring 
results.
    (1) The State may approve grandfathering of previously collected 
data where there are time gaps in the sampling frequency if the system 
conducts additional monitoring the State specifies to ensure that the 
data used to comply with the initial source water monitoring 
requirements of Sec.  141.701(a) are seasonally representative and 
unbiased.
    (2) Systems may grandfather previously collected data where the 
sampling frequency within each month varied. If the Cryptosporidium 
sampling frequency varied, systems must follow the monthly averaging 
procedure in Sec.  141.710(b)(5) or Sec.  141.712(a)(3), as applicable, 
when calculating the bin classification for filtered systems or the mean 
Cryptosporidium concentration for unfiltered systems.
    (f) Reporting monitoring results for grandfathering. Systems that 
request to grandfather previously collected monitoring results must 
report the following information by the applicable dates listed in this 
paragraph. Systems serving at least 10,000 people must report this 
information to EPA unless the State approves reporting to the State 
rather than EPA. Systems serving fewer than 10,000 people must report 
this information to the State.
    (1) Systems must report that they intend to submit previously 
collected monitoring results for grandfathering. This report must 
specify the number of previously collected results the system will 
submit, the dates of the first and last sample, and whether a system 
will conduct additional source water monitoring to meet the requirements 
of Sec.  141.701(a). Systems must report this information no later than 
the date the

[[Page 687]]

sampling schedule under Sec.  141.702 is required.
    (2) Systems must report previously collected monitoring results for 
grandfathering, along with the associated documentation listed in 
paragraphs (f)(2)(i) through (iv) of this section, no later than two 
months after the applicable date listed in Sec.  141.701(c).
    (i) For each sample result, systems must report the applicable data 
elements in Sec.  141.706.
    (ii) Systems must certify that the reported monitoring results 
include all results the system generated during the time period 
beginning with the first reported result and ending with the final 
reported result. This applies to samples that were collected from the 
sampling location specified for source water monitoring under this 
subpart, not spiked, and analyzed using the laboratory's routine process 
for the analytical methods listed in this section.
    (iii) Systems must certify that the samples were representative of a 
plant's source water(s) and the source water(s) have not changed. 
Systems must report a description of the sampling location(s), which 
must address the position of the sampling location in relation to the 
system's water source(s) and treatment processes, including points of 
chemical addition and filter backwash recycle.
    (iv) For Cryptosporidium samples, the laboratory or laboratories 
that analyzed the samples must provide a letter certifying that the 
quality control criteria specified in the methods listed in paragraph 
(c)(1) of this section were met for each sample batch associated with 
the reported results. Alternatively, the laboratory may provide bench 
sheets and sample examination report forms for each field, matrix spike, 
IPR, OPR, and method blank sample associated with the reported results.
    (g) If the State determines that a previously collected data set 
submitted for grandfathering was generated during source water 
conditions that were not normal for the system, such as a drought, the 
State may disapprove the data. Alternatively, the State may approve the 
previously collected data if the system reports additional source water 
monitoring data, as determined by the State, to ensure that the data set 
used under Sec.  141.710 or Sec.  141.712 represents average source 
water conditions for the system.
    (h) If a system submits previously collected data that fully meet 
the number of samples required for initial source water monitoring under 
Sec.  141.701(a) and some of the data are rejected due to not meeting 
the requirements of this section, systems must conduct additional 
monitoring to replace rejected data on a schedule the State approves. 
Systems are not required to begin this additional monitoring until two 
months after notification that data have been rejected and additional 
monitoring is necessary.

          Disinfection Profiling and Benchmarking Requirements



Sec.  141.708  Requirements when making a significant change 
in disinfection practice.

    (a) Following the completion of initial source water monitoring 
under Sec.  141.701(a), a system that plans to make a significant change 
to its disinfection practice, as defined in paragraph (b) of this 
section, must develop disinfection profiles and calculate disinfection 
benchmarks for Giardia lamblia and viruses as described in Sec.  
141.709. Prior to changing the disinfection practice, the system must 
notify the State and must include in this notice the information in 
paragraphs (a)(1) through (3) of this section.
    (1) A completed disinfection profile and disinfection benchmark for 
Giardia lamblia and viruses as described in Sec.  141.709.
    (2) A description of the proposed change in disinfection practice.
    (3) An analysis of how the proposed change will affect the current 
level of disinfection.
    (b) Significant changes to disinfection practice are defined as 
follows:
    (1) Changes to the point of disinfection;
    (2) Changes to the disinfectant(s) used in the treatment plant;
    (3) Changes to the disinfection process; or
    (4) Any other modification identified by the State as a significant 
change to disinfection practice.

[[Page 688]]



Sec.  141.709  Developing the disinfection profile and benchmark.

    (a) Systems required to develop disinfection profiles under Sec.  
141.708 must follow the requirements of this section. Systems must 
monitor at least weekly for a period of 12 consecutive months to 
determine the total log inactivation for Giardia lamblia and viruses. If 
systems monitor more frequently, the monitoring frequency must be evenly 
spaced. Systems that operate for fewer than 12 months per year must 
monitor weekly during the period of operation. Systems must determine 
log inactivation for Giardia lamblia through the entire plant, based on 
CT99.9 values in Tables 1.1 through 1.6, 2.1 and 3.1 of Sec.  
141.74(b) as applicable. Systems must determine log inactivation for 
viruses through the entire treatment plant based on a protocol approved 
by the State.
    (b) Systems with a single point of disinfectant application prior to 
the entrance to the distribution system must conduct the monitoring in 
paragraphs (b)(1) through (4) of this section. Systems with more than 
one point of disinfectant application must conduct the monitoring in 
paragraphs (b)(1) through (4) of this section for each disinfection 
segment. Systems must monitor the parameters necessary to determine the 
total inactivation ratio, using analytical methods in Sec.  141.74(a).
    (1) For systems using a disinfectant other than UV, the temperature 
of the disinfected water must be measured at each residual disinfectant 
concentration sampling point during peak hourly flow or at an 
alternative location approved by the State.
    (2) For systems using chlorine, the pH of the disinfected water must 
be measured at each chlorine residual disinfectant concentration 
sampling point during peak hourly flow or at an alternative location 
approved by the State.
    (3) The disinfectant contact time(s) (t) must be determined during 
peak hourly flow.
    (4) The residual disinfectant concentration(s) (C) of the water 
before or at the first customer and prior to each additional point of 
disinfectant application must be measured during peak hourly flow.
    (c) In lieu of conducting new monitoring under paragraph (b) of this 
section, systems may elect to meet the requirements of paragraphs (c)(1) 
or (2) of this section.
    (1) Systems that have at least one year of existing data that are 
substantially equivalent to data collected under the provisions of 
paragraph (b) of this section may use these data to develop disinfection 
profiles as specified in this section if the system has neither made a 
significant change to its treatment practice nor changed sources since 
the data were collected. Systems may develop disinfection profiles using 
up to three years of existing data.
    (2) Systems may use disinfection profile(s) developed under Sec.  
141.172 or Sec. Sec.  141.530 through 141.536 in lieu of developing a 
new profile if the system has neither made a significant change to its 
treatment practice nor changed sources since the profile was developed. 
Systems that have not developed a virus profile under Sec.  141.172 or 
Sec. Sec.  141.530 through 141.536 must develop a virus profile using 
the same monitoring data on which the Giardia lamblia profile is based.
    (d) Systems must calculate the total inactivation ratio for Giardia 
lamblia as specified in paragraphs (d)(1) through (3) of this section.
    (1) Systems using only one point of disinfectant application may 
determine the total inactivation ratio for the disinfection segment 
based on either of the methods in paragraph (d)(1)(i) or (ii) of this 
section.
    (i) Determine one inactivation ratio (CTcalc/CT99.9) 
before or at the first customer during peak hourly flow.
    (ii) Determine successive CTcalc/CT99.9 values, 
representing sequential inactivation ratios, between the point of 
disinfectant application and a point before or at the first customer 
during peak hourly flow. The system must calculate the total 
inactivation ratio by determining (CTcalc/CT99.9) for each 
sequence and then adding the (CTcalc/CT99.9) values together 
to determine ([Sigma] (CTcalc/CT99.9)).
    (2) Systems using more than one point of disinfectant application 
before the first customer must determine the CT value of each 
disinfection segment

[[Page 689]]

immediately prior to the next point of disinfectant application, or for 
the final segment, before or at the first customer, during peak hourly 
flow. The (CTcalc/CT99.9) value of each segment and ([Sigma] 
(CTcalc/CT99.9)) must be calculated using the method in 
paragraph (d)(1)(ii) of this section.
    (3) The system must determine the total logs of inactivation by 
multiplying the value calculated in paragraph (d)(1) or (d)(2) of this 
section by 3.0.
    (4) Systems must calculate the log of inactivation for viruses using 
a protocol approved by the State.
    (e) Systems must use the procedures specified in paragraphs (e)(1) 
and (2) of this section to calculate a disinfection benchmark.
    (1) For each year of profiling data collected and calculated under 
paragraphs (a) through (d) of this section, systems must determine the 
lowest mean monthly level of both Giardia lamblia and virus 
inactivation. Systems must determine the mean Giardia lamblia and virus 
inactivation for each calendar month for each year of profiling data by 
dividing the sum of daily or weekly Giardia lamblia and virus log 
inactivation by the number of values calculated for that month.
    (2) The disinfection benchmark is the lowest monthly mean value (for 
systems with one year of profiling data) or the mean of the lowest 
monthly mean values (for systems with more than one year of profiling 
data) of Giardia lamblia and virus log inactivation in each year of 
profiling data.

                    Treatment Technique Requirements



Sec.  141.710  Bin classification for filtered systems.

    (a) Following completion of the initial round of source water 
monitoring required under Sec.  141.701(a), filtered systems must 
calculate an initial Cryptosporidium bin concentration for each plant 
for which monitoring was required. Calculation of the bin concentration 
must use the Cryptosporidium results reported under Sec.  141.701(a) and 
must follow the procedures in paragraphs (b)(1) through (5) of this 
section.
    (b)(1) For systems that collect a total of at least 48 samples, the 
bin concentration is equal to the arithmetic mean of all sample 
concentrations.
    (2) For systems that collect a total of at least 24 samples, but not 
more than 47 samples, the bin concentration is equal to the highest 
arithmetic mean of all sample concentrations in any 12 consecutive 
months during which Cryptosporidium samples were collected.
    (3) For systems that serve fewer than 10,000 people and monitor for 
Cryptosporidium for only one year (i.e., collect 24 samples in 12 
months), the bin concentration is equal to the arithmetic mean of all 
sample concentrations.
    (4) For systems with plants operating only part of the year that 
monitor fewer than 12 months per year under Sec.  141.701(e), the bin 
concentration is equal to the highest arithmetic mean of all sample 
concentrations during any year of Cryptosporidium monitoring.
    (5) If the monthly Cryptosporidium sampling frequency varies, 
systems must first calculate a monthly average for each month of 
monitoring. Systems must then use these monthly average concentrations, 
rather than individual sample concentrations, in the applicable 
calculation for bin classification in paragraphs (b)(1) through (4) of 
this section.
    (c) Filtered systems must determine their initial bin classification 
from the following table and using the Cryptosporidium bin concentration 
calculated under paragraphs (a)-(b) of this section:

              Bin Classification Table for Filtered Systems
------------------------------------------------------------------------
                                With a Cryptosporidium       The bin
     For systems that are:      bin concentration of .   classification
                                        . . \1\             is . . .
------------------------------------------------------------------------
. . . required to monitor for   Cryptosporidium <0.075  Bin 1.
 Cryptosporidium under Sec.      oocyst/L.
 141.701.
                                 0.075 oocysts/L        Bin 2.
                                 <=Cryptosporidium
                                 <1.0 oocysts/L.

[[Page 690]]

 
                                 1.0 oocysts/L          Bin 3.
                                 <=Cryptosporidium
                                 <3.0 oocysts/L.
                                 Cryptosporidium =3.0 oocysts/L.
. . . serving fewer than        NA....................  Bin 1.
 10,000 people and NOT
 required to monitor for
 Cryptosporidium under Sec.
 141.701(a)(4).
------------------------------------------------------------------------
\1\ Based on calculations in paragraph (a) or (d) of this section, as
  applicable.

    (d) Following completion of the second round of source water 
monitoring required under Sec.  141.701(b), filtered systems must 
recalculate their Cryptosporidium bin concentration using the 
Cryptosporidium results reported under Sec.  141.701(b) and following 
the procedures in paragraphs (b)(1) through (4) of this section. Systems 
must then redetermine their bin classification using this bin 
concentration and the table in paragraph (c) of this section.
    (e)(1) Filtered systems must report their initial bin classification 
under paragraph (c) of this section to the State for approval no later 
than 6 months after the system is required to complete initial source 
water monitoring based on the schedule in Sec.  141.701(c).
    (2) Systems must report their bin classification under paragraph (d) 
of this section to the State for approval no later than 6 months after 
the system is required to complete the second round of source water 
monitoring based on the schedule in Sec.  141.701(c).
    (3) The bin classification report to the State must include a 
summary of source water monitoring data and the calculation procedure 
used to determine bin classification.
    (f) Failure to comply with the conditions of paragraph (e) of this 
section is a violation of the treatment technique requirement.



Sec.  141.711  Filtered system additional Cryptosporidium 
treatment requirements.

    (a) Filtered systems must provide the level of additional treatment 
for Cryptosporidium specified in this paragraph based on their bin 
classification as determined under Sec.  141.710 and according to the 
schedule in Sec.  141.713.

----------------------------------------------------------------------------------------------------------------
                         And the system uses the following filtration treatment in full compliance with subparts
                         H, P, and T of this part (as applicable), then the additional Cryptosporidium treatment
   If the system bin                                     requirements are . . .
 classification is . . -----------------------------------------------------------------------------------------
           .                 Conventional                                 Slow sand or           Alternative
                         filtration treatment    Direct filtration     diatomaceous earth        filtration
                        (including softening)                              filtration           technologies
----------------------------------------------------------------------------------------------------------------
Bin 1.................  No additional          No additional          No additional         No additional
                         treatment.             treatment.             treatment.            treatment.
Bin 2.................  1-log treatment......  1.5-log treatment....  1-log treatment.....  (\1\)
Bin 3.................  2-log treatment......  2.5-log treatment....  2-log treatment.....  (\2\)
Bin 4.................  2.5-log treatment....  3-log treatment......  2.5-log treatment...  (\3\)
----------------------------------------------------------------------------------------------------------------
\1\ As determined by the State such that the total Cryptosporidium removal and inactivation is at least 4.0-log.
\2\ As determined by the State such that the total Cryptosporidium removal and inactivation is at least 5.0-log.
\3\ As determined by the State such that the total Cryptosporidium removal and inactivation is at least 5.5-log.

    (b)(1) Filtered systems must use one or more of the treatment and 
management options listed in Sec.  141.715, termed the microbial 
toolbox, to comply with the additional Cryptosporidium treatment 
required in paragraph (a) of this section.
    (2) Systems classified in Bin 3 and Bin 4 must achieve at least 1-
log of the additional Cryptosporidium treatment required under paragraph 
(a) of this section using either one or a combination of the following: 
bag filters, bank filtration, cartridge filters, chlorine dioxide, 
membranes, ozone, or UV, as described in Sec. Sec.  141.716 through 
141.720.
    (c) Failure by a system in any month to achieve treatment credit by 
meeting criteria in Sec. Sec.  141.716 through 141.720 for microbial 
toolbox options that is at

[[Page 691]]

least equal to the level of treatment required in paragraph (a) of this 
section is a violation of the treatment technique requirement.
    (d) If the State determines during a sanitary survey or an 
equivalent source water assessment that after a system completed the 
monitoring conducted under Sec.  141.701(a) or Sec.  141.701(b), 
significant changes occurred in the system's watershed that could lead 
to increased contamination of the source water by Cryptosporidium, the 
system must take actions specified by the State to address the 
contamination. These actions may include additional source water 
monitoring and/or implementing microbial toolbox options listed in Sec.  
141.715.



Sec.  141.712  Unfiltered system Cryptosporidium treatment requirements.

    (a) Determination of mean Cryptosporidium level. (1) Following 
completion of the initial source water monitoring required under Sec.  
141.701(a), unfiltered systems must calculate the arithmetic mean of all 
Cryptosporidium sample concentrations reported under Sec.  141.701(a). 
Systems must report this value to the State for approval no later than 6 
months after the month the system is required to complete initial source 
water monitoring based on the schedule in Sec.  141.701(c).
    (2) Following completion of the second round of source water 
monitoring required under Sec.  141.701(b), unfiltered systems must 
calculate the arithmetic mean of all Cryptosporidium sample 
concentrations reported under Sec.  141.701(b). Systems must report this 
value to the State for approval no later than 6 months after the month 
the system is required to complete the second round of source water 
monitoring based on the schedule in Sec.  141.701(c).
    (3) If the monthly Cryptosporidium sampling frequency varies, 
systems must first calculate a monthly average for each month of 
monitoring. Systems must then use these monthly average concentrations, 
rather than individual sample concentrations, in the calculation of the 
mean Cryptosporidium level in paragraphs (a)(1) or (2) of this section.
    (4) The report to the State of the mean Cryptosporidium levels 
calculated under paragraphs (a)(1) and (2) of this section must include 
a summary of the source water monitoring data used for the calculation.
    (5) Failure to comply with the conditions of paragraph (a) of this 
section is a violation of the treatment technique requirement.
    (b) Cryptosporidium inactivation requirements. Unfiltered systems 
must provide the level of inactivation for Cryptosporidium specified in 
this paragraph, based on their mean Cryptosporidium levels as determined 
under paragraph (a) of this section and according to the schedule in 
Sec.  141.713.
    (1) Unfiltered systems with a mean Cryptosporidium level of 0.01 
oocysts/L or less must provide at least 2-log Cryptosporidium 
inactivation.
    (2) Unfiltered systems with a mean Cryptosporidium level of greater 
than 0.01 oocysts/L must provide at least 3-log Cryptosporidium 
inactivation.
    (c) Inactivation treatment technology requirements. Unfiltered 
systems must use chlorine dioxide, ozone, or UV as described in Sec.  
141.720 to meet the Cryptosporidium inactivation requirements of this 
section.
    (1) Systems that use chlorine dioxide or ozone and fail to achieve 
the Cryptosporidium inactivation required in paragraph (b) of this 
section on more than one day in the calendar month are in violation of 
the treatment technique requirement.
    (2) Systems that use UV light and fail to achieve the 
Cryptosporidium inactivation required in paragraph (b) of this section 
by meeting the criteria in Sec.  141.720(d)(3)(ii) are in violation of 
the treatment technique requirement.
    (d) Use of two disinfectants. Unfiltered systems must meet the 
combined Cryptosporidium inactivation requirements of this section and 
Giardia lamblia and virus inactivation requirements of Sec.  141.72(a) 
using a minimum of two disinfectants, and each of two disinfectants must 
separately achieve the total inactivation required for either 
Cryptosporidium, Giardia lamblia, or viruses.

[[Page 692]]



Sec.  141.713  Schedule for compliance with Cryptosporidium 
treatment requirements.

    (a) Following initial bin classification under Sec.  141.710(c), 
filtered systems must provide the level of treatment for Cryptosporidium 
required under Sec.  141.711 according to the schedule in paragraph (c) 
of this section.
    (b) Following initial determination of the mean Cryptosporidium 
level under Sec.  141.712(a)(1), unfiltered systems must provide the 
level of treatment for Cryptosporidium required under Sec.  141.712 
according to the schedule in paragraph (c) of this section.
    (c) Cryptosporidium treatment compliance dates.

            Cryptosporidium Treatment Compliance Dates Table
------------------------------------------------------------------------
                                                  Must comply with
                                              Cryptosporidium treatment
         Systems that serve . . .           requirements no later than .
                                                       . . \a\
------------------------------------------------------------------------
(1) At least 100,000 people...............  (i) April 1, 2012.
(2) From 50,000 to 99,999 people..........  (i) October 1, 2012.
(3) From 10,000 to 49,999 people..........  (i) October 1, 2013.
(4) Fewer than 10,000 people..............  (i) October 1, 2014.
------------------------------------------------------------------------
\a\ States may allow up to an additional two years for complying with
  the treatment requirement for systems making capital improvements.

    (d) If the bin classification for a filtered system changes 
following the second round of source water monitoring, as determined 
under Sec.  141.710(d), the system must provide the level of treatment 
for Cryptosporidium required under Sec.  141.711 on a schedule the State 
approves.
    (e) If the mean Cryptosporidium level for an unfiltered system 
changes following the second round of monitoring, as determined under 
Sec.  141.712(a)(2), and if the system must provide a different level of 
Cryptosporidium treatment under Sec.  141.712 due to this change, the 
system must meet this treatment requirement on a schedule the State 
approves.



Sec.  141.714  Requirements for uncovered finished water storage facilities.

    (a) Systems using uncovered finished water storage facilities must 
comply with the conditions of this section.
    (b) Systems must notify the State of the use of each uncovered 
finished water storage facility no later than April 1, 2008.
    (c) Systems must meet the conditions of paragraph (c)(1) or (2) of 
this section for each uncovered finished water storage facility or be in 
compliance with a State-approved schedule to meet these conditions no 
later than April 1, 2009.
    (1) Systems must cover any uncovered finished water storage 
facility.
    (2) Systems must treat the discharge from the uncovered finished 
water storage facility to the distribution system to achieve 
inactivation and/or removal of at least 4-log virus, 3-log Giardia 
lamblia, and 2-log Cryptosporidium using a protocol approved by the 
State.
    (d) Failure to comply with the requirements of this section is a 
violation of the treatment technique requirement.

              Requirements for Microbial Toolbox Components



Sec.  141.715  Microbial toolbox options for meeting Cryptosporidium 
treatment requirements.

    (a)(1) Systems receive the treatment credits listed in the table in 
paragraph (b) of this section by meeting the conditions for microbial 
toolbox options described in Sec. Sec.  141.716 through 141.720. Systems 
apply these treatment credits to meet the treatment requirements in 
Sec.  141.711 or Sec.  141.712, as applicable.
    (2) Unfiltered systems are eligible for treatment credits for the 
microbial toolbox options described in Sec.  141.720 only.
    (b) The following table summarizes options in the microbial toolbox:

Microbial Toolbox Summary Table: Options, Treatment Credits and Criteria
------------------------------------------------------------------------
                                 Cryptosporidium treatment credit with
        Toolbox Option             design and implementation criteria
------------------------------------------------------------------------
            Source Protection and Management Toolbox Options
------------------------------------------------------------------------
(1) Watershed control program  0.5-log credit for State-approved program
                                comprising required elements, annual
                                program status report to State, and
                                regular watershed survey. Unfiltered
                                systems are not eligible for credit.
                                Specific criteria are in Sec.
                                141.716(a).

[[Page 693]]

 
(2) Alternative source/intake  No prescribed credit. Systems may conduct
 management.                    simultaneous monitoring for treatment
                                bin classification at alternative intake
                                locations or under alternative intake
                                management strategies. Specific criteria
                                are in Sec.   141.716(b).
------------------------------------------------------------------------
                     Pre Filtration Toolbox Options
------------------------------------------------------------------------
(3) Presedimentation basin     0.5-log credit during any month that
 with coagulation.              presedimentation basins achieve a
                                monthly mean reduction of 0.5-log or
                                greater in turbidity or alternative
                                State-approved performance criteria. To
                                be eligible, basins must be operated
                                continuously with coagulant addition and
                                all plant flow must pass through basins.
                                Specific criteria are in Sec.
                                141.717(a).
(4) Two-stage lime softening.  0.5-log credit for two-stage softening
                                where chemical addition and hardness
                                precipitation occur in both stages. All
                                plant flow must pass through both
                                stages. Single-stage softening is
                                credited as equivalent to conventional
                                treatment. Specific criteria are in Sec.
                                  141.717(b).
(5) Bank filtration..........  0.5-log credit for 25-foot setback; 1.0-
                                log credit for 50-foot setback; aquifer
                                must be unconsolidated sand containing
                                at least 10 percent fines; average
                                turbidity in wells must be less than 1
                                NTU. Systems using wells followed by
                                filtration when conducting source water
                                monitoring must sample the well to
                                determine bin classification and are not
                                eligible for additional credit. Specific
                                criteria are in Sec.   141.717(c).
------------------------------------------------------------------------
                  Treatment Performance Toolbox Options
------------------------------------------------------------------------
(6) Combined filter            0.5-log credit for combined filter
 performance.                   effluent turbidity less than or equal to
                                0.15 NTU in at least 95 percent of
                                measurements each month. Specific
                                criteria are in Sec.   141.718(a).
(7) Individual filter          0.5-log credit (in addition to 0.5-log
 performance.                   combined filter performance credit) if
                                individual filter effluent turbidity is
                                less than or equal to 0.15 NTU in at
                                least 95 percent of samples each month
                                in each filter and is never greater than
                                0.3 NTU in two consecutive measurements
                                in any filter. Specific criteria are in
                                Sec.   141.718(b).
(8) Demonstration of           Credit awarded to unit process or
 performance.                   treatment train based on a demonstration
                                to the State with a State- approved
                                protocol. Specific criteria are in Sec.
                                 141.718(c).
------------------------------------------------------------------------
                  Additional Filtration Toolbox Options
------------------------------------------------------------------------
(9) Bag or cartridge filters   Up to 2-log credit based on the removal
 (individual filters).          efficiency demonstrated during challenge
                                testing with a 1.0-log factor of safety.
                                Specific criteria are in Sec.
                                141.719(a).
(10) Bag or cartridge filters  Up to 2.5-log credit based on the removal
 (in series).                   efficiency demonstrated during challenge
                                testing with a 0.5-log factor of safety.
                                Specific criteria are in Sec.
                                141.719(a).
(11) Membrane filtration.....  Log credit equivalent to removal
                                efficiency demonstrated in challenge
                                test for device if supported by direct
                                integrity testing. Specific criteria are
                                in Sec.   141.719(b).
(12) Second stage filtration.  0.5-log credit for second separate
                                granular media filtration stage if
                                treatment train includes coagulation
                                prior to first filter. Specific criteria
                                are in Sec.   141.719(c)
(13) Slow sand filters.......  2.5-log credit as a secondary filtration
                                step; 3.0-log credit as a primary
                                filtration process. No prior
                                chlorination for either option. Specific
                                criteria are in Sec.   141.719(d).
------------------------------------------------------------------------
                      Inactivation Toolbox Options
------------------------------------------------------------------------
(14) Chlorine dioxide........  Log credit based on measured CT in
                                relation to CT table. Specific criteria
                                in Sec.   141.720(b)
(15) Ozone...................  Log credit based on measured CT in
                                relation to CT table. Specific criteria
                                in Sec.   141.720(b).
(16) UV......................  Log credit based on validated UV dose in
                                relation to UV dose table; reactor
                                validation testing required to establish
                                UV dose and associated operating
                                conditions. Specific criteria in Sec.
                                141.720(d).
------------------------------------------------------------------------



Sec.  141.716  Source toolbox components.

    (a) Watershed control program. Systems receive 0.5-log 
Cryptosporidium treatment credit for implementing a watershed control 
program that meets the requirements of this section.
    (1) Systems that intend to apply for the watershed control program 
credit must notify the State of this intent no later than two years 
prior to the treatment compliance date applicable to the system in Sec.  
141.713.
    (2) Systems must submit to the State a proposed watershed control 
plan no later than one year before the applicable treatment compliance 
date in Sec.  141.713. The State must approve the

[[Page 694]]

watershed control plan for the system to receive watershed control 
program treatment credit. The watershed control plan must include the 
elements in paragraphs (a)(2)(i) through (iv) of this section.
    (i) Identification of an ``area of influence'' outside of which the 
likelihood of Cryptosporidium or fecal contamination affecting the 
treatment plant intake is not significant. This is the area to be 
evaluated in future watershed surveys under paragraph (a)(5)(ii) of this 
section.
    (ii) Identification of both potential and actual sources of 
Cryptosporidium contamination and an assessment of the relative impact 
of these sources on the system's source water quality.
    (iii) An analysis of the effectiveness and feasibility of control 
measures that could reduce Cryptosporidium loading from sources of 
contamination to the system's source water.
    (iv) A statement of goals and specific actions the system will 
undertake to reduce source water Cryptosporidium levels. The plan must 
explain how the actions are expected to contribute to specific goals, 
identify watershed partners and their roles, identify resource 
requirements and commitments, and include a schedule for plan 
implementation with deadlines for completing specific actions identified 
in the plan.
    (3) Systems with existing watershed control programs (i.e., programs 
in place on January 5, 2006) are eligible to seek this credit. Their 
watershed control plans must meet the criteria in paragraph (a)(2) of 
this section and must specify ongoing and future actions that will 
reduce source water Cryptosporidium levels.
    (4) If the State does not respond to a system regarding approval of 
a watershed control plan submitted under this section and the system 
meets the other requirements of this section, the watershed control 
program will be considered approved and 0.5 log Cryptosporidium 
treatment credit will be awarded unless and until the State subsequently 
withdraws such approval.
    (5) Systems must complete the actions in paragraphs (a)(5)(i) 
through (iii) of this section to maintain the 0.5-log credit.
    (i) Submit an annual watershed control program status report to the 
State. The annual watershed control program status report must describe 
the system's implementation of the approved plan and assess the adequacy 
of the plan to meet its goals. It must explain how the system is 
addressing any shortcomings in plan implementation, including those 
previously identified by the State or as the result of the watershed 
survey conducted under paragraph (a)(5)(ii) of this section. It must 
also describe any significant changes that have occurred in the 
watershed since the last watershed sanitary survey. If a system 
determines during implementation that making a significant change to its 
approved watershed control program is necessary, the system must notify 
the State prior to making any such changes. If any change is likely to 
reduce the level of source water protection, the system must also list 
in its notification the actions the system will take to mitigate this 
effect.
    (ii) Undergo a watershed sanitary survey every three years for 
community water systems and every five years for noncommunity water 
systems and submit the survey report to the State. The survey must be 
conducted according to State guidelines and by persons the State 
approves.
    (A) The watershed sanitary survey must meet the following criteria: 
encompass the region identified in the State-approved watershed control 
plan as the area of influence; assess the implementation of actions to 
reduce source water Cryptosporidium levels; and identify any significant 
new sources of Cryptosporidium.
    (B) If the State determines that significant changes may have 
occurred in the watershed since the previous watershed sanitary survey, 
systems must undergo another watershed sanitary survey by a date the 
State requires, which may be earlier than the regular date in paragraph 
(a)(5)(ii) of this section.
    (iii) The system must make the watershed control plan, annual status 
reports, and watershed sanitary survey reports available to the public 
upon request. These documents must be in a

[[Page 695]]

plain language style and include criteria by which to evaluate the 
success of the program in achieving plan goals. The State may approve 
systems to withhold from the public portions of the annual status 
report, watershed control plan, and watershed sanitary survey based on 
water supply security considerations.
    (6) If the State determines that a system is not carrying out the 
approved watershed control plan, the State may withdraw the watershed 
control program treatment credit.
    (b) Alternative source. (1) A system may conduct source water 
monitoring that reflects a different intake location (either in the same 
source or for an alternate source) or a different procedure for the 
timing or level of withdrawal from the source (alternative source 
monitoring). If the State approves, a system may determine its bin 
classification under Sec.  141.710 based on the alternative source 
monitoring results.
    (2) If systems conduct alternative source monitoring under paragraph 
(b)(1) of this section, systems must also monitor their current plant 
intake concurrently as described in Sec.  141.701.
    (3) Alternative source monitoring under paragraph (b)(1) of this 
section must meet the requirements for source monitoring to determine 
bin classification, as described in Sec. Sec.  141.701 through 141.706. 
Systems must report the alternative source monitoring results to the 
State, along with supporting information documenting the operating 
conditions under which the samples were collected.
    (4) If a system determines its bin classification under Sec.  
141.710 using alternative source monitoring results that reflect a 
different intake location or a different procedure for managing the 
timing or level of withdrawal from the source, the system must relocate 
the intake or permanently adopt the withdrawal procedure, as applicable, 
no later than the applicable treatment compliance date in Sec.  141.713.



Sec.  141.717  Pre-filtration treatment toolbox components.

    (a) Presedimentation. Systems receive 0.5-log Cryptosporidium 
treatment credit for a presedimentation basin during any month the 
process meets the criteria in this paragraph.
    (1) The presedimentation basin must be in continuous operation and 
must treat the entire plant flow taken from a surface water or GWUDI 
source.
    (2) The system must continuously add a coagulant to the 
presedimentation basin.
    (3) The presedimentation basin must achieve the performance criteria 
in paragraph (3)(i) or (ii) of this section.
    (i) Demonstrates at least 0.5-log mean reduction of influent 
turbidity. This reduction must be determined using daily turbidity 
measurements in the presedimentation process influent and effluent and 
must be calculated as follows: log10(monthly mean of daily 
influent turbidity)-log10(monthly mean of daily effluent 
turbidity).
    (ii) Complies with State-approved performance criteria that 
demonstrate at least 0.5-log mean removal of micron-sized particulate 
material through the presedimentation process.
    (b) Two-stage lime softening. Systems receive an additional 0.5-log 
Cryptosporidium treatment credit for a two-stage lime softening plant if 
chemical addition and hardness precipitation occur in two separate and 
sequential softening stages prior to filtration. Both softening stages 
must treat the entire plant flow taken from a surface water or GWUDI 
source.
    (c) Bank filtration. Systems receive Cryptosporidium treatment 
credit for bank filtration that serves as pretreatment to a filtration 
plant by meeting the criteria in this paragraph. Systems using bank 
filtration when they begin source water monitoring under Sec.  
141.701(a) must collect samples as described in Sec.  141.703(d) and are 
not eligible for this credit.
    (1) Wells with a ground water flow path of at least 25 feet receive 
0.5-log treatment credit; wells with a ground water flow path of at 
least 50 feet receive 1.0-log treatment credit. The ground water flow 
path must be determined as specified in paragraph (c)(4) of this 
section.
    (2) Only wells in granular aquifers are eligible for treatment 
credit. Granular aquifers are those comprised

[[Page 696]]

of sand, clay, silt, rock fragments, pebbles or larger particles, and 
minor cement. A system must characterize the aquifer at the well site to 
determine aquifer properties. Systems must extract a core from the 
aquifer and demonstrate that in at least 90 percent of the core length, 
grains less than 1.0 mm in diameter constitute at least 10 percent of 
the core material.
    (3) Only horizontal and vertical wells are eligible for treatment 
credit.
    (4) For vertical wells, the ground water flow path is the measured 
distance from the edge of the surface water body under high flow 
conditions (determined by the 100 year floodplain elevation boundary or 
by the floodway, as defined in Federal Emergency Management Agency flood 
hazard maps) to the well screen. For horizontal wells, the ground water 
flow path is the measured distance from the bed of the river under 
normal flow conditions to the closest horizontal well lateral screen.
    (5) Systems must monitor each wellhead for turbidity at least once 
every four hours while the bank filtration process is in operation. If 
monthly average turbidity levels, based on daily maximum values in the 
well, exceed 1 NTU, the system must report this result to the State and 
conduct an assessment within 30 days to determine the cause of the high 
turbidity levels in the well. If the State determines that microbial 
removal has been compromised, the State may revoke treatment credit 
until the system implements corrective actions approved by the State to 
remediate the problem.
    (6) Springs and infiltration galleries are not eligible for 
treatment credit under this section, but are eligible for credit under 
Sec.  141.718(c).
    (7) Bank filtration demonstration of performance. The State may 
approve Cryptosporidium treatment credit for bank filtration based on a 
demonstration of performance study that meets the criteria in this 
paragraph. This treatment credit may be greater than 1.0-log and may be 
awarded to bank filtration that does not meet the criteria in paragraphs 
(c)(1)-(5) of this section.
    (i) The study must follow a State-approved protocol and must involve 
the collection of data on the removal of Cryptosporidium or a surrogate 
for Cryptosporidium and related hydrogeologic and water quality 
parameters during the full range of operating conditions.
    (ii) The study must include sampling both from the production 
well(s) and from monitoring wells that are screened and located along 
the shortest flow path between the surface water source and the 
production well(s).



Sec.  141.718  Treatment performance toolbox components.

    (a) Combined filter performance. Systems using conventional 
filtration treatment or direct filtration treatment receive an 
additional 0.5-log Cryptosporidium treatment credit during any month the 
system meets the criteria in this paragraph. Combined filter effluent 
(CFE) turbidity must be less than or equal to 0.15 NTU in at least 95 
percent of the measurements. Turbidity must be measured as described in 
Sec.  141.74(a) and (c).
    (b) Individual filter performance. Systems using conventional 
filtration treatment or direct filtration treatment receive 0.5-log 
Cryptosporidium treatment credit, which can be in addition to the 0.5-
log credit under paragraph (a) of this section, during any month the 
system meets the criteria in this paragraph. Compliance with these 
criteria must be based on individual filter turbidity monitoring as 
described in Sec.  141.174 or Sec.  141.560, as applicable.
    (1) The filtered water turbidity for each individual filter must be 
less than or equal to 0.15 NTU in at least 95 percent of the 
measurements recorded each month.
    (2) No individual filter may have a measured turbidity greater than 
0.3 NTU in two consecutive measurements taken 15 minutes apart.
    (3) Any system that has received treatment credit for individual 
filter performance and fails to meet the requirements of paragraph 
(b)(1) or (2) of this section during any month does not receive a 
treatment technique violation under Sec.  141.711(c) if the State 
determines the following:
    (i) The failure was due to unusual and short-term circumstances that 
could not reasonably be prevented

[[Page 697]]

through optimizing treatment plant design, operation, and maintenance.
    (ii) The system has experienced no more than two such failures in 
any calendar year.
    (c) Demonstration of performance. The State may approve 
Cryptosporidium treatment credit for drinking water treatment processes 
based on a demonstration of performance study that meets the criteria in 
this paragraph. This treatment credit may be greater than or less than 
the prescribed treatment credits in Sec.  141.711 or Sec. Sec.  141.717 
through 141.720 and may be awarded to treatment processes that do not 
meet the criteria for the prescribed credits.
    (1) Systems cannot receive the prescribed treatment credit for any 
toolbox box option in Sec. Sec.  141.717 through 141.720 if that toolbox 
option is included in a demonstration of performance study for which 
treatment credit is awarded under this paragraph.
    (2) The demonstration of performance study must follow a State-
approved protocol and must demonstrate the level of Cryptosporidium 
reduction the treatment process will achieve under the full range of 
expected operating conditions for the system.
    (3) Approval by the State must be in writing and may include 
monitoring and treatment performance criteria that the system must 
demonstrate and report on an ongoing basis to remain eligible for the 
treatment credit. The State may designate such criteria where necessary 
to verify that the conditions under which the demonstration of 
performance credit was approved are maintained during routine operation.



Sec.  141.719  Additional filtration toolbox components.

    (a) Bag and cartridge filters. Systems receive Cryptosporidium 
treatment credit of up to 2.0-log for individual bag or cartridge 
filters and up to 2.5-log for bag or cartridge filters operated in 
series by meeting the criteria in paragraphs (a)(1) through (10) of this 
section. To be eligible for this credit, systems must report the results 
of challenge testing that meets the requirements of paragraphs (a)(2) 
through (9) of this section to the State. The filters must treat the 
entire plant flow taken from a subpart H source.
    (1) The Cryptosporidium treatment credit awarded to bag or cartridge 
filters must be based on the removal efficiency demonstrated during 
challenge testing that is conducted according to the criteria in 
paragraphs (a)(2) through (a)(9) of this section. A factor of safety 
equal to 1-log for individual bag or cartridge filters and 0.5-log for 
bag or cartridge filters in series must be applied to challenge testing 
results to determine removal credit. Systems may use results from 
challenge testing conducted prior to January 5, 2006 if the prior 
testing was consistent with the criteria specified in paragraphs (a)(2) 
through (9) of this section.
    (2) Challenge testing must be performed on full-scale bag or 
cartridge filters, and the associated filter housing or pressure vessel, 
that are identical in material and construction to the filters and 
housings the system will use for removal of Cryptosporidium. Bag or 
cartridge filters must be challenge tested in the same configuration 
that the system will use, either as individual filters or as a series 
configuration of filters.
    (3) Challenge testing must be conducted using Cryptosporidium or a 
surrogate that is removed no more efficiently than Cryptosporidium. The 
microorganism or surrogate used during challenge testing is referred to 
as the challenge particulate. The concentration of the challenge 
particulate must be determined using a method capable of discreetly 
quantifying the specific microorganism or surrogate used in the test; 
gross measurements such as turbidity may not be used.
    (4) The maximum feed water concentration that can be used during a 
challenge test must be based on the detection limit of the challenge 
particulate in the filtrate (i.e., filtrate detection limit) and must be 
calculated using the following equation:

Maximum Feed Concentration = 1 x 10 \4\ x (Filtrate Detection Limit)

    (5) Challenge testing must be conducted at the maximum design flow 
rate for the filter as specified by the manufacturer.
    (6) Each filter evaluated must be tested for a duration sufficient 
to reach 100 percent of the terminal pressure

[[Page 698]]

drop, which establishes the maximum pressure drop under which the filter 
may be used to comply with the requirements of this subpart.
    (7) Removal efficiency of a filter must be determined from the 
results of the challenge test and expressed in terms of log removal 
values using the following equation:

LRV = LOG10(Cf)-LOG10(Cp)

Where:

LRV = log removal value demonstrated during challenge testing; 
          Cf = the feed concentration measured during the 
          challenge test; and Cp = the filtrate concentration 
          measured during the challenge test. In applying this equation, 
          the same units must be used for the feed and filtrate 
          concentrations. If the challenge particulate is not detected 
          in the filtrate, then the term Cp must be set equal 
          to the detection limit.

    (8) Each filter tested must be challenged with the challenge 
particulate during three periods over the filtration cycle: within two 
hours of start-up of a new filter; when the pressure drop is between 45 
and 55 percent of the terminal pressure drop; and at the end of the 
cycle after the pressure drop has reached 100 percent of the terminal 
pressure drop. An LRV must be calculated for each of these challenge 
periods for each filter tested. The LRV for the filter 
(LRVfilter) must be assigned the value of the minimum LRV 
observed during the three challenge periods for that filter.
    (9) If fewer than 20 filters are tested, the overall removal 
efficiency for the filter product line must be set equal to the lowest 
LRVfilter among the filters tested. If 20 or more filters are 
tested, the overall removal efficiency for the filter product line must 
be set equal to the 10th percentile of the set of LRVfilter 
values for the various filters tested. The percentile is defined by (i/
(n + 1)) where i is the rank of n individual data points ordered lowest 
to highest. If necessary, the 10th percentile may be calculated using 
linear interpolation.
    (10) If a previously tested filter is modified in a manner that 
could change the removal efficiency of the filter product line, 
challenge testing to demonstrate the removal efficiency of the modified 
filter must be conducted and submitted to the State.
    (b) Membrane filtration. (1) Systems receive Cryptosporidium 
treatment credit for membrane filtration that meets the criteria of this 
paragraph. Membrane cartridge filters that meet the definition of 
membrane filtration in Sec.  141.2 are eligible for this credit. The 
level of treatment credit a system receives is equal to the lower of the 
values determined under paragraph (b)(1)(i) and (ii) of this section.
    (i) The removal efficiency demonstrated during challenge testing 
conducted under the conditions in paragraph (b)(2) of this section.
    (ii) The maximum removal efficiency that can be verified through 
direct integrity testing used with the membrane filtration process under 
the conditions in paragraph (b)(3) of this section.
    (2) Challenge testing. The membrane used by the system must undergo 
challenge testing to evaluate removal efficiency, and the system must 
report the results of challenge testing to the State. Challenge testing 
must be conducted according to the criteria in paragraphs (b)(2)(i) 
through (vii) of this section. Systems may use data from challenge 
testing conducted prior to January 5, 2006 if the prior testing was 
consistent with the criteria in paragraphs (b)(2)(i) through (vii) of 
this section.
    (i) Challenge testing must be conducted on either a full-scale 
membrane module, identical in material and construction to the membrane 
modules used in the system's treatment facility, or a smaller-scale 
membrane module, identical in material and similar in construction to 
the full-scale module. A module is defined as the smallest component of 
a membrane unit in which a specific membrane surface area is housed in a 
device with a filtrate outlet structure.
    (ii) Challenge testing must be conducted using Cryptosporidium 
oocysts or a surrogate that is removed no more efficiently than 
Cryptosporidium oocysts. The organism or surrogate used during challenge 
testing is referred to as the challenge particulate. The concentration 
of the challenge particulate, in both the feed and filtrate water, must 
be determined using a method capable of discretely quantifying the 
specific

[[Page 699]]

challenge particulate used in the test; gross measurements such as 
turbidity may not be used.
    (iii) The maximum feed water concentration that can be used during a 
challenge test is based on the detection limit of the challenge 
particulate in the filtrate and must be determined according to the 
following equation:

Maximum Feed Concentration = 3.16 x 106 x (Filtrate Detection 
Limit)

    (iv) Challenge testing must be conducted under representative 
hydraulic conditions at the maximum design flux and maximum design 
process recovery specified by the manufacturer for the membrane module. 
Flux is defined as the throughput of a pressure driven membrane process 
expressed as flow per unit of membrane area. Recovery is defined as the 
volumetric percent of feed water that is converted to filtrate over the 
course of an operating cycle uninterrupted by events such as chemical 
cleaning or a solids removal process (i.e., backwashing).
    (v) Removal efficiency of a membrane module must be calculated from 
the challenge test results and expressed as a log removal value 
according to the following equation:

LRV = LOG10(Cf) - LOG10(Cp)

Where:

LRV = log removal value demonstrated during the challenge test; 
          Cf = the feed concentration measured during the 
          challenge test; and Cp = the filtrate concentration 
          measured during the challenge test. Equivalent units must be 
          used for the feed and filtrate concentrations. If the 
          challenge particulate is not detected in the filtrate, the 
          term Cp is set equal to the detection limit for the 
          purpose of calculating the LRV. An LRV must be calculated for 
          each membrane module evaluated during the challenge test.

    (vi) The removal efficiency of a membrane filtration process 
demonstrated during challenge testing must be expressed as a log removal 
value (LRVC-Test). If fewer than 20 modules are tested, then 
LRVC-Test is equal to the lowest of the representative LRVs 
among the modules tested. If 20 or more modules are tested, then 
LRVC-Test is equal to the 10th percentile of the 
representative LRVs among the modules tested. The percentile is defined 
by (i/(n + 1)) where i is the rank of n individual data points ordered 
lowest to highest. If necessary, the 10th percentile may be calculated 
using linear interpolation.
    (vii) The challenge test must establish a quality control release 
value (QCRV) for a non-destructive performance test that demonstrates 
the Cryptosporidium removal capability of the membrane filtration 
module. This performance test must be applied to each production 
membrane module used by the system that was not directly challenge 
tested in order to verify Cryptosporidium removal capability. Production 
modules that do not meet the established QCRV are not eligible for the 
treatment credit demonstrated during the challenge test.
    (viii) If a previously tested membrane is modified in a manner that 
could change the removal efficiency of the membrane or the applicability 
of the non-destructive performance test and associated QCRV, additional 
challenge testing to demonstrate the removal efficiency of, and 
determine a new QCRV for, the modified membrane must be conducted and 
submitted to the State.
    (3) Direct integrity testing. Systems must conduct direct integrity 
testing in a manner that demonstrates a removal efficiency equal to or 
greater than the removal credit awarded to the membrane filtration 
process and meets the requirements described in paragraphs (b)(3)(i) 
through (vi) of this section. A direct integrity test is defined as a 
physical test applied to a membrane unit in order to identify and 
isolate integrity breaches (i.e., one or more leaks that could result in 
contamination of the filtrate).
    (i) The direct integrity test must be independently applied to each 
membrane unit in service. A membrane unit is defined as a group of 
membrane modules that share common valving that allows the unit to be 
isolated from the rest of the system for the purpose of integrity 
testing or other maintenance.
    (ii) The direct integrity method must have a resolution of 3 
micrometers or less, where resolution is defined as the size of the 
smallest integrity breach

[[Page 700]]

that contributes to a response from the direct integrity test.
    (iii) The direct integrity test must have a sensitivity sufficient 
to verify the log treatment credit awarded to the membrane filtration 
process by the State, where sensitivity is defined as the maximum log 
removal value that can be reliably verified by a direct integrity test. 
Sensitivity must be determined using the approach in either paragraph 
(b)(3)(iii)(A) or (B) of this section as applicable to the type of 
direct integrity test the system uses.
    (A) For direct integrity tests that use an applied pressure or 
vacuum, the direct integrity test sensitivity must be calculated 
according to the following equation:

LRVDIT = LOG10 (Qp /(VCF x 
Qbreach))

Where:

LRVDIT = the sensitivity of the direct integrity test; 
          Qp = total design filtrate flow from the membrane 
          unit; Qbreach = flow of water from an integrity 
          breach associated with the smallest integrity test response 
          that can be reliably measured, and VCF = volumetric 
          concentration factor. The volumetric concentration factor is 
          the ratio of the suspended solids concentration on the high 
          pressure side of the membrane relative to that in the feed 
          water.

    (B) For direct integrity tests that use a particulate or molecular 
marker, the direct integrity test sensitivity must be calculated 
according to the following equation:

LRVDIT = LOG10(Cf)-
LOG10(Cp)

Where:

LRVDIT = the sensitivity of the direct integrity test; 
          Cf = the typical feed concentration of the marker 
          used in the test; and Cp = the filtrate 
          concentration of the marker from an integral membrane unit.

    (iv) Systems must establish a control limit within the sensitivity 
limits of the direct integrity test that is indicative of an integral 
membrane unit capable of meeting the removal credit awarded by the 
State.
    (v) If the result of a direct integrity test exceeds the control 
limit established under paragraph (b)(3)(iv) of this section, the system 
must remove the membrane unit from service. Systems must conduct a 
direct integrity test to verify any repairs, and may return the membrane 
unit to service only if the direct integrity test is within the 
established control limit.
    (vi) Systems must conduct direct integrity testing on each membrane 
unit at a frequency of not less than once each day that the membrane 
unit is in operation. The State may approve less frequent testing, based 
on demonstrated process reliability, the use of multiple barriers 
effective for Cryptosporidium, or reliable process safeguards.
    (4) Indirect integrity monitoring. Systems must conduct continuous 
indirect integrity monitoring on each membrane unit according to the 
criteria in paragraphs (b)(4)(i) through (v) of this section. Indirect 
integrity monitoring is defined as monitoring some aspect of filtrate 
water quality that is indicative of the removal of particulate matter. A 
system that implements continuous direct integrity testing of membrane 
units in accordance with the criteria in paragraphs (b)(3)(i) through 
(v) of this section is not subject to the requirements for continuous 
indirect integrity monitoring. Systems must submit a monthly report to 
the State summarizing all continuous indirect integrity monitoring 
results triggering direct integrity testing and the corrective action 
that was taken in each case.
    (i) Unless the State approves an alternative parameter, continuous 
indirect integrity monitoring must include continuous filtrate turbidity 
monitoring.
    (ii) Continuous monitoring must be conducted at a frequency of no 
less than once every 15 minutes.
    (iii) Continuous monitoring must be separately conducted on each 
membrane unit.
    (iv) If indirect integrity monitoring includes turbidity and if the 
filtrate turbidity readings are above 0.15 NTU for a period greater than 
15 minutes (i.e., two consecutive 15-minute readings above 0.15 NTU), 
direct integrity testing must immediately be performed on the associated 
membrane unit as specified in paragraphs (b)(3)(i) through (v) of this 
section.
    (v) If indirect integrity monitoring includes a State-approved 
alternative

[[Page 701]]

parameter and if the alternative parameter exceeds a State-approved 
control limit for a period greater than 15 minutes, direct integrity 
testing must immediately be performed on the associated membrane units 
as specified in paragraphs (b)(3)(i) through (v) of this section.
    (c) Second stage filtration. Systems receive 0.5-log Cryptosporidium 
treatment credit for a separate second stage of filtration that consists 
of sand, dual media, GAC, or other fine grain media following granular 
media filtration if the State approves. To be eligible for this credit, 
the first stage of filtration must be preceded by a coagulation step and 
both filtration stages must treat the entire plant flow taken from a 
surface water or GWUDI source. A cap, such as GAC, on a single stage of 
filtration is not eligible for this credit. The State must approve the 
treatment credit based on an assessment of the design characteristics of 
the filtration process.
    (d) Slow sand filtration (as secondary filter). Systems are eligible 
to receive 2.5-log Cryptosporidium treatment credit for a slow sand 
filtration process that follows a separate stage of filtration if both 
filtration stages treat entire plant flow taken from a surface water or 
GWUDI source and no disinfectant residual is present in the influent 
water to the slow sand filtration process. The State must approve the 
treatment credit based on an assessment of the design characteristics of 
the filtration process. This paragraph does not apply to treatment 
credit awarded to slow sand filtration used as a primary filtration 
process.

[71 FR 769, Jan. 5, 2006; 71 FR 6136, Feb. 6, 2006]



Sec.  141.720  Inactivation toolbox components.

    (a) Calculation of CT values. (1) CT is the product of the 
disinfectant contact time (T, in minutes) and disinfectant concentration 
(C, in milligrams per liter). Systems with treatment credit for chlorine 
dioxide or ozone under paragraph (b) or (c) of this section must 
calculate CT at least once each day, with both C and T measured during 
peak hourly flow as specified in Sec. Sec.  141.74(a) through (b).
    (2) Systems with several disinfection segments in sequence may 
calculate CT for each segment, where a disinfection segment is defined 
as a treatment unit process with a measurable disinfectant residual 
level and a liquid volume. Under this approach, systems must add the 
Cryptosporidium CT values in each segment to determine the total CT for 
the treatment plant.
    (b) CT values for chlorine dioxide and ozone. (1) Systems receive 
the Cryptosporidium treatment credit listed in this table by meeting the 
corresponding chlorine dioxide CT value for the applicable water 
temperature, as described in paragraph (a) of this section.

                                  CT Values (mg[middot]min/L) for Cryptosporidium Inactivation by Chlorine Dioxide \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                 Water Temperature, [deg]C
                           Log credit                            ---------------------------------------------------------------------------------------
                                                                   <=0.5     1       2       3       5       7      10      15      20      25      30
--------------------------------------------------------------------------------------------------------------------------------------------------------
(i) 0.25........................................................     159     153     140     128     107      90      69      45      29      19      12
(ii) 0.5........................................................     319     305     279     256     214     180     138      89      58      38      24
(iii) 1.0.......................................................     637     610     558     511     429     360     277     179     116      75      49
(iv) 1.5........................................................     956     915     838     767     643     539     415     268     174     113      73
(v) 2.0.........................................................    1275    1220    1117    1023     858     719     553     357     232     150      98
(vi) 2.5........................................................    1594    1525    1396    1278    1072     899     691     447     289     188     122
(vii) 3.0.......................................................    1912    1830    1675    1534    1286    1079     830     536     347     226    147
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Systems may use this equation to determine log credit between the indicated values: Log credit = (0.001506 x (1.09116)\Temp\) x CT.

    (2) Systems receive the Cryptosporidium treatment credit listed in 
this table by meeting the corresponding ozone CT values for the 
applicable water temperature, as described in paragraph (a) of this 
section.

[[Page 702]]



                                        CT Values (mg[middot]min/L) for Cryptosporidium Inactivation by Ozone \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                 Water Temperature, [deg]C
                           Log credit                            ---------------------------------------------------------------------------------------
                                                                   <=0.5     1       2       3       5       7      10      15      20      25      30
--------------------------------------------------------------------------------------------------------------------------------------------------------
(i) 0.25........................................................     6.0     5.8     5.2     4.8     4.0     3.3     2.5     1.6     1.0     0.6    0.39
(ii) 0.5........................................................      12      12      10     9.5     7.9     6.5     4.9     3.1     2.0     1.2    0.78
(iii) 1.0.......................................................      24      23      21      19      16      13     9.9     6.2     3.9     2.5     1.6
(iv) 1.5........................................................      36      35      31      29      24      20      15     9.3     5.9     3.7     2.4
(v) 2.0.........................................................      48      46      42      38      32      26      20      12     7.8     4.9     3.1
(vi) 2.5........................................................      60      58      52      48      40      33      25      16     9.8     6.2     3.9
(vii) 3.0.......................................................      72      69      63      57      47      39      30      19      12     7.4    4.7
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Systems may use this equation to determine log credit between the indicated values: Log credit = (0.0397 x (1.09757)\Temp\) x CT.

    (c) Site-specific study. The State may approve alternative chlorine 
dioxide or ozone CT values to those listed in paragraph (b) of this 
section on a site-specific basis. The State must base this approval on a 
site-specific study a system conducts that follows a State-approved 
protocol.
    (d) Ultraviolet light. Systems receive Cryptosporidium, Giardia 
lamblia, and virus treatment credits for ultraviolet (UV) light reactors 
by achieving the corresponding UV dose values shown in paragraph (d)(1) 
of this section. Systems must validate and monitor UV reactors as 
described in paragraphs (d)(2) and (3) of this section to demonstrate 
that they are achieving a particular UV dose value for treatment credit.
    (1) UV dose table. The treatment credits listed in this table are 
for UV light at a wavelength of 254 nm as produced by a low pressure 
mercury vapor lamp. To receive treatment credit for other lamp types, 
systems must demonstrate an equivalent germicidal dose through reactor 
validation testing, as described in paragraph (d)(2) of this section. 
The UV dose values in this table are applicable only to post-filter 
applications of UV in filtered systems and to unfiltered systems.

                UV Dose Table for Cryptosporidium, Giardia lamblia, and Virus Inactivation Credit
----------------------------------------------------------------------------------------------------------------
                                                          Cryptosporidium    Giardia lamblia
                       Log credit                          UV dose (mJ/cm     UV dose (mJ/cm   Virus UV dose (mJ/
                                                                \2\)               \2\)             cm \2\)
----------------------------------------------------------------------------------------------------------------
(i) 0.5................................................                1.6                1.5                 39
(ii) 1.0...............................................                2.5                2.1                 58
(iii) 1.5..............................................                3.9                3.0                 79
(iv) 2.0...............................................                5.8                5.2                100
(v) 2.5................................................                8.5                7.7                121
(vi) 3.0...............................................                 12                 11                143
(vii) 3.5..............................................                 15                 15                163
(viii) 4.0.............................................                 22                 22                186
----------------------------------------------------------------------------------------------------------------

    (2) Reactor validation testing. Systems must use UV reactors that 
have undergone validation testing to determine the operating conditions 
under which the reactor delivers the UV dose required in paragraph 
(d)(1) of this section (i.e., validated operating conditions). These 
operating conditions must include flow rate, UV intensity as measured by 
a UV sensor, and UV lamp status.
    (i) When determining validated operating conditions, systems must 
account for the following factors: UV absorbance of the water; lamp 
fouling and aging; measurement uncertainty of on-line sensors; UV dose 
distributions arising from the velocity profiles through the reactor; 
failure of UV lamps or other critical system components; and inlet and 
outlet piping or channel configurations of the UV reactor.
    (ii) Validation testing must include the following: Full scale 
testing of a reactor that conforms uniformly to the UV reactors used by 
the system and inactivation of a test microorganism whose dose response 
characteristics

[[Page 703]]

have been quantified with a low pressure mercury vapor lamp.
    (iii) The State may approve an alternative approach to validation 
testing.
    (3) Reactor monitoring. (i) Systems must monitor their UV reactors 
to determine if the reactors are operating within validated conditions, 
as determined under paragraph (d)(2) of this section. This monitoring 
must include UV intensity as measured by a UV sensor, flow rate, lamp 
status, and other parameters the State designates based on UV reactor 
operation. Systems must verify the calibration of UV sensors and must 
recalibrate sensors in accordance with a protocol the State approves.
    (ii) To receive treatment credit for UV light, systems must treat at 
least 95 percent of the water delivered to the public during each month 
by UV reactors operating within validated conditions for the required UV 
dose, as described in paragraphs (d)(1) and (2) of this section. Systems 
must demonstrate compliance with this condition by the monitoring 
required under paragraph (d)(3)(i) of this section.

                Reporting and Recordkeeping Requirements



Sec.  141.721  Reporting requirements.

    (a) Systems must report sampling schedules under Sec.  141.702 and 
source water monitoring results under Sec.  141.706 unless they notify 
the State that they will not conduct source water monitoring due to 
meeting the criteria of Sec.  141.701(d).
    (b) Systems must report the use of uncovered finished water storage 
facilities to the State as described in Sec.  141.714.
    (c) Filtered systems must report their Cryptosporidium bin 
classification as described in Sec.  141.710.
    (d) Unfiltered systems must report their mean source water 
Cryptosporidium level as described in Sec.  141.712.
    (e) Systems must report disinfection profiles and benchmarks to the 
State as described in Sec. Sec.  141.708 through 141.709 prior to making 
a significant change in disinfection practice.
    (f) Systems must report to the State in accordance with the 
following table for any microbial toolbox options used to comply with 
treatment requirements under Sec.  141.711 or Sec.  141.712. 
Alternatively, the State may approve a system to certify operation 
within required parameters for treatment credit rather than reporting 
monthly operational data for toolbox options.

                                    Microbial Toolbox Reporting Requirements
----------------------------------------------------------------------------------------------------------------
                                                    Systems must submit the
                Toolbox option                       following information          On the following schedule
----------------------------------------------------------------------------------------------------------------
(1) Watershed control program (WCP)..........  (i) Notice of intention to        No later than two years before
                                                develop a new or continue an      the applicable treatment
                                                existing watershed control        compliance date in Sec.
                                                program.                          141.713
                                               (ii) Watershed control plan.....  No later than one year before
                                                                                  the applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713.
                                               (iii) Annual watershed control    Every 12 months, beginning one
                                                program status report.            year after the applicable
                                                                                  treatment compliance date in
                                                                                  Sec.   141.713.
                                               (iv) Watershed sanitary survey    For community water systems,
                                                report.                           every three years beginning
                                                                                  three years after the
                                                                                  applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713. For noncommunity
                                                                                  water systems, every five
                                                                                  years beginning five years
                                                                                  after the applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713.
(2) Alternative source/intake management.....  Verification that system has      No later than the applicable
                                                relocated the intake or adopted   treatment compliance date in
                                                the intake withdrawal procedure   Sec.   141.713.
                                                reflected in monitoring results.

[[Page 704]]

 
(3) Presedimentation.........................  Monthly verification of the       Monthly reporting within 10
                                                following: (i) Continuous basin   days following the month in
                                                operation (ii) Treatment of       which the monitoring was
                                                100% of the flow (iii)            conducted, beginning on the
                                                Continuous addition of a          applicable treatment
                                                coagulant (iv) At least 0.5-log   compliance date in Sec.
                                                mean reduction of influent        141.713.
                                                turbidity or compliance with
                                                alternative State-approved
                                                performance criteria.
(4) Two-stage lime softening.................  Monthly verification of the       Monthly reporting within 10
                                                following: (i) Chemical           days following the month in
                                                addition and hardness             which the monitoring was
                                                precipitation occurred in two     conducted, beginning on the
                                                separate and sequential           applicable treatment
                                                softening stages prior to         compliance date in Sec.
                                                filtration (ii) Both stages       141.713.
                                                treated 100% of the plant flow.
(5) Bank filtration..........................  (i) Initial demonstration of the  No later than the applicable
                                                following: (A) Unconsolidated,    treatment compliance date in
                                                predominantly sandy aquifer (B)   Sec.   141.713.
                                                Setback distance of at least 25
                                                ft. (0.5-log credit) or 50 ft.
                                                (1.0-log credit).
                                               (ii) If monthly average of daily  Report within 30 days following
                                                max turbidity is greater than 1   the month in which the
                                                NTU then system must report       monitoring was conducted,
                                                result and submit an assessment   beginning on the applicable
                                                of the cause..                    treatment compliance date in
                                                                                  Sec.   141.713.
(6) Combined filter performance..............  Monthly verification of combined  Monthly reporting within 10
                                                filter effluent (CFE) turbidity   days following the month in
                                                levels less than or equal to      which the monitoring was
                                                0.15 NTU in at least 95 percent   conducted, beginning on the
                                                of the 4 hour CFE measurements    applicable treatment
                                                taken each month.                 compliance date in Sec.
                                                                                  141.713.
(7) Individual filter performance............  Monthly verification of the       Monthly reporting within 10
                                                following: (i) Individual         days following the month in
                                                filter effluent (IFE) turbidity   which the monitoring was
                                                levels less than or equal to      conducted, beginning on the
                                                0.15 NTU in at least 95 percent   applicable treatment
                                                of samples each month in each     compliance date in Sec.
                                                filter (ii) No individual         141.713.]
                                                filter greater than 0.3 NTU in
                                                two consecutive readings 15
                                                minutes apart.
(8) Demonstration of performance.............  (i) Results from testing          No later than the applicable
                                                following a State approved        treatment compliance date in
                                                protocol.                         Sec.   141.713.
                                               (ii) As required by the State,    Within 10 days following the
                                                monthly verification of           month in which monitoring was
                                                operation within conditions of    conducted, beginning on the
                                                State approval for                applicable treatment
                                                demonstration of performance      compliance date in Sec.
                                                credit.                           141.713.
(9) Bag filters and cartridge filters........  (i) Demonstration that the        No later than the applicable
                                                following criteria are met: (A)   treatment compliance date in
                                                Process meets the definition of   Sec.   141.713.
                                                bag or cartridge filtration;
                                                (B) Removal efficiency
                                                established through challenge
                                                testing that meets criteria in
                                                this subpart.
                                               (ii) Monthly verification that    Within 10 days following the
                                                100% of plant flow was filtered.  month in which monitoring was
                                                                                  conducted, beginning on the
                                                                                  applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713.
(10) Membrane filtration.....................  (i) Results of verification       No later than the applicable
                                                testing demonstrating the         treatment compliance date in
                                                following: (A) Removal            Sec.   141.713.
                                                efficiency established through
                                                challenge testing that meets
                                                criteria in this subpart; (B)
                                                Integrity test method and
                                                parameters, including
                                                resolution, sensitivity, test
                                                frequency, control limits, and
                                                associated baseline.
                                               (ii) Monthly report summarizing   Within 10 days following the
                                                the following: (A) All direct     month in which monitoring was
                                                integrity tests above the         conducted, beginning on the
                                                control limit; (B) If             applicable treatment
                                                applicable, any turbidity or      compliance date in Sec.
                                                alternative state-approved        141.713.
                                                indirect integrity monitoring
                                                results triggering direct
                                                integrity testing and the
                                                corrective action that was
                                                taken.
(11) Second stage filtration.................  Monthly verification that 100%    Within 10 days following the
                                                of flow was filtered through      month in which monitoring was
                                                both stages and that first        conducted, beginning on the
                                                stage was preceded by             applicable treatment
                                                coagulation step.                 compliance date in Sec.
                                                                                  141.713.

[[Page 705]]

 
(12) Slow sand filtration (as secondary        Monthly verification that both a  Within 10 days following the
 filter).                                       slow sand filter and a            month in which monitoring was
                                                preceding separate stage of       conducted, beginning on the
                                                filtration treated 100% of flow   applicable treatment
                                                from subpart H sources..          compliance date in Sec.
                                                                                  141.713.
(13) Chlorine dioxide........................  Summary of CT values for each     Within 10 days following the
                                                day as described in Sec.          month in which monitoring was
                                                141.720..                         conducted, beginning on the
                                                                                  applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713.
(14) Ozone...................................  Summary of CT values for each     Within 10 days following the
                                                day as described in Sec.          month in which monitoring was
                                                141.720..                         conducted, beginning on the
                                                                                  applicable treatment
                                                                                  compliance date in Sec.
                                                                                  141.713.
(15) UV......................................  (i) Validation test results       No later than the applicable
                                                demonstrating operating           treatment compliance date in
                                                conditions that achieve           Sec.   141.713.
                                                required UV dose.                Within 10 days following the
                                               (ii) Monthly report summarizing    month in which monitoring was
                                                the percentage of water           conducted, beginning on the
                                                entering the distribution         applicable treatment
                                                system that was not treated by    compliance date in Sec.
                                                UV reactors operating within      141.713.
                                                validated conditions for the
                                                required dose as specified in
                                                141.720(d)..
----------------------------------------------------------------------------------------------------------------



Sec.  141.722  Recordkeeping requirements.

    (a) Systems must keep results from the initial round of source water 
monitoring under Sec.  141.701(a) and the second round of source water 
monitoring under Sec.  141.701(b) until 3 years after bin classification 
under Sec.  141.710 for filtered systems or determination of the mean 
Cryptosporidium level under Sec.  141.710 for unfiltered systems for the 
particular round of monitoring.
    (b) Systems must keep any notification to the State that they will 
not conduct source water monitoring due to meeting the criteria of Sec.  
141.701(d) for 3 years.
    (c) Systems must keep the results of treatment monitoring associated 
with microbial toolbox options under Sec. Sec.  141.716 through 141.720 
and with uncovered finished water reservoirs under Sec.  141.714, as 
applicable, for 3 years.

           Requirements for Sanitary Surveys Performed by EPA



Sec.  141.723  Requirements to respond to significant deficiencies identified 
in sanitary surveys performed by EPA.

    (a) A sanitary survey is an onsite review of the water source 
(identifying sources of contamination by using results of source water 
assessments where available), facilities, equipment, operation, 
maintenance, and monitoring compliance of a PWS to evaluate the adequacy 
of the PWS, its sources and operations, and the distribution of safe 
drinking water.
    (b) For the purposes of this section, a significant deficiency 
includes a defect in design, operation, or maintenance, or a failure or 
malfunction of the sources, treatment, storage, or distribution system 
that EPA determines to be causing, or has the potential for causing the 
introduction of contamination into the water delivered to consumers.
    (c) For sanitary surveys performed by EPA, systems must respond in 
writing to significant deficiencies identified in sanitary survey 
reports no later than 45 days after receipt of the report, indicating 
how and on what schedule the system will address significant 
deficiencies noted in the survey.
    (d) Systems must correct significant deficiencies identified in 
sanitary survey reports according to the schedule approved by EPA, or if 
there is no approved schedule, according to the schedule reported under 
paragraph (c) of this section if such deficiencies are within the 
control of the system.



                 Subpart X_Aircraft Drinking Water Rule

    Source: 74 FR 53618, Oct. 19, 2009, unless otherwise noted.

[[Page 706]]



Sec.  141.800  Applicability and compliance date.

    (a) Applicability. The requirements of this subpart constitute the 
National Primary Drinking Water Regulations for aircraft that are public 
water systems and that board only finished water for human consumption. 
Aircraft public water systems are considered transient non-community 
water systems (TNCWS). To the extent there is a conflict between the 
requirements in this subpart and the regulatory requirements established 
elsewhere in this part, this subpart governs.
    (b) Compliance date. Aircraft public water systems must comply, 
unless otherwise noted, with the requirements of this subpart beginning 
October 19, 2011. Until this compliance date, air carriers remain 
subject to existing national primary drinking water regulations.



Sec.  141.801  Definitions.

    As used in this subpart, the term:
    Administrator means the Administrator of the United States 
Environmental Protection Agency or his/her authorized representative.
    Air carrier means a person who undertakes directly by lease, or 
other arrangement, to engage in air transportation. The air carrier is 
responsible for ensuring all of the aircraft it owns or operates that 
are public water systems comply with all provisions of this subpart.
    Aircraft means a device that is used or intended to be used for 
flight in the air.
    Aircraft water system means an aircraft that qualifies as a public 
water system under the Safe Drinking Water Act and the national primary 
drinking water regulations. The components of an aircraft water system 
include the water service panel, the filler neck of the aircraft 
finished water storage tank, and all finished water storage tanks, 
piping, treatment equipment, and plumbing fixtures within the aircraft 
that supply water for human consumption to passengers or crew.
    Aircraft water system operations and maintenance plan means the 
schedules and procedures for operating, monitoring, and maintaining an 
aircraft water system that is included in an aircraft operation and 
maintenance program accepted by the Federal Aviation Administration. (14 
CFR part 43, 14 CFR part 91, 14 CFR part 121)
    Finished water means water that is introduced into the distribution 
system of a public water system and is intended for distribution and 
consumption without further treatment, except as treatment necessary to 
maintain water quality in the distribution system (e.g., supplemental 
disinfection, addition of corrosion control chemicals). (40 CFR 141.2)
    Human consumption means drinking, bathing, showering, hand washing, 
teeth brushing, food preparation, dishwashing, and maintaining oral 
hygiene.
    Self inspection means an onsite review of the aircraft water system, 
including the water service panel, the filler neck of the aircraft 
finished water storage tank; all finished water storage tanks, piping, 
treatment equipment, and plumbing fixtures; and a review of the aircraft 
operations, maintenance, monitoring, and recordkeeping for the purpose 
of evaluating the adequacy of such water system components and practices 
for providing safe drinking water to passengers and crew.
    Watering point means the water supply, methods, and facilities used 
for the delivery of finished water to the aircraft. These facilities may 
include water trucks, carts, cabinets, and hoses.



Sec.  141.802  Coliform sampling plan.

    (a) Each air carrier under this subpart must develop a coliform 
sampling plan covering each aircraft water system owned or operated by 
the air carrier that identifies the following:
    (1) Coliform sample collection procedures that are consistent with 
the requirements of Sec.  141.803(a) and (b).
    (2) Sample tap location(s) representative of the aircraft water 
system as specified in Sec.  141.803(b)(2) and (b)(4).
    (3) Frequency and number of routine coliform samples to be collected 
as specified in Sec.  141.803(b)(3).
    (4) Frequency of routine disinfection and flushing as specified in 
the operations and maintenance plan under Sec.  141.804.
    (5) Procedures for communicating sample results promptly so that any

[[Page 707]]

required actions, including repeat and follow-up sampling, corrective 
action, and notification of passengers and crew, will be conducted in a 
timely manner.
    (b) Each air carrier must develop a coliform sampling plan for each 
aircraft with a water system meeting the definition of a public water 
system by April 19, 2011.
    (c) The coliform sampling plan must be included in the Aircraft 
Water System Operations and Maintenance Plan required in Sec.  141.804. 
Any subsequent changes to the coliform sampling plan must also be 
included in the Aircraft Water System Operations and Maintenance Plan 
required in Sec.  141.804.



Sec.  141.803  Coliform sampling.

    (a) Analytical methodology. Air carriers must follow the sampling 
and analysis requirements under this section.
    (1) The standard sample volume required for total coliform analysis, 
regardless of analytical method used, is 100 mL.
    (2) Air carriers need determine only the presence or absence of 
total coliforms and/or E. coli; a determination of density of these 
organisms is not required.
    (3) Air carriers must conduct analyses for total coliform and E. 
coli in accordance with the analytical methods approved in Sec.  
141.21(f)(3) and 141.21(f)(6)) until March 31, 2016, and in accordance 
with the analytical methods approved in Sec.  141.852 beginning April 1, 
2016.
    (4) The time from sample collection to initiation of analysis may 
not exceed 30 hours. Systems are encouraged but not required to hold 
samples below 10 [deg]C during transit.
    (5) The invalidation of a total coliform sample result can be made 
only by the Administrator in accordance with Sec.  141.21(c)(1)(i), 
(ii), or (iii) or by the certified laboratory in accordance with Sec.  
141.21(c)(2) until March 31, 2016, or in accordance with Sec.  
141.853(c) beginning April 1, 2016, with the Administrator acting as the 
State.
    (6) Certified laboratories. For the purpose of determining 
compliance with this subpart, samples may be considered only if they 
have been analyzed by a laboratory certified by a State or EPA. For the 
purposes of this paragraph, ``State'' refers to a State or Tribe that 
has received primacy for public water systems (other than aircraft water 
systems) under section 1413 of SDWA.
    (b) Routine monitoring. For each aircraft water system, the sampling 
frequency must be determined by the disinfection and flushing frequency 
recommended by the aircraft water system manufacturer, when available, 
and as identified in the operations and maintenance plan in Sec.  
141.804.
    (1) Except as provided in paragraph (b)(2) of this section, the air 
carrier must collect two 100 mL total coliform routine samples at the 
frequency specified in the sampling plan in Sec.  141.802 and in 
accordance with paragraph (b)(3) of this section;
    (2) The air carrier may collect one 100 mL total coliform routine 
sample at the frequency specified in the sampling plan in Sec.  141.802 
for aircraft with a removable or portable tank that is drained every day 
of passenger service, and the aircraft has only one tap. Aircraft 
meeting the requirements of this paragraph do not have to comply with 
paragraph (b)(4) of this section.
    (3) Air carriers must perform routine monitoring for total coliform 
at a frequency corresponding to the frequency of routine disinfection 
and flushing as specified in the Table b-1 (Routine Disinfection and 
Flushing and Routine Sample Frequencies). Air carriers must follow the 
disinfection and flushing frequency recommended by the aircraft water 
system manufacturer, when available. Where the aircraft water system 
manufacturer does not specify a recommended routine disinfection and 
flushing frequency, the air carrier must choose a frequency from Table 
b-1 (Routine Disinfection and Flushing and Routine Sample Frequencies):

[[Page 708]]



     Table B-1--Routine Disinfection and Flushing and Routine Sample
                               Frequencies
------------------------------------------------------------------------
Minimum routine disinfection & flushing    Minimum frequency of routine
              per aircraft                     samples per aircraft
------------------------------------------------------------------------
At least 4 times per year = At least     At least 1 time per year = At
 once within every three-month period     least once within every twelve-
 (quarterly).                             month period (annually).
At least 3 times per year = At least     At least 2 times per year = At
 once within every four-month period.     least once within every six-
                                          month period (semi-annually).
At least 2 times per year = At least     At least 4 times per year = At
 once within every six-month period       least once within every three-
 (semi-annually).                         month period (quarterly).
At least 1 time per year or less = At    At least 12 times per year = At
 least once within every twelve-month     least once every month
 period (annually) or less.               (monthly).
------------------------------------------------------------------------

    (4) One sample must be taken from a lavatory and one from a galley; 
each sample must be analyzed for total coliform. If only one water tap 
is located in the aircraft water system due to aircraft model type and 
construction, then a single tap may be used to collect two separate 100 
mL samples.
    (5) If any routine, repeat, or follow-up coliform sample is total 
coliform-positive, the air carrier must analyze that total coliform-
positive culture medium to determine if E. coli is present.
    (6) Routine total coliform samples must not be collected within 72 
hours after completing routine disinfection and flushing procedures.
    (c) Routine coliform sample results--(1) Negative routine coliform 
sample results. If all routine sample results are total coliform-
negative, then the air carrier must maintain the routine monitoring 
frequency for total coliform as specified in the sampling plan in Sec.  
141.802.
    (2) Positive routine E. coli sample results. If any routine sample 
is E. coli-positive, the air carrier must perform all of the following:
    (i) Restrict public access. Restrict public access to the aircraft 
water system in accordance with paragraph (d) of this section as 
expeditiously as possible, but in no case later than 24 hours after the 
laboratory notifies the air carrier of the E. coli-positive result or 
discovery of the applicable failure as specified in paragraphs (g) and 
(h) of this section. All public access restrictions, including 
applicable public notification requirements, must remain in-place until 
the aircraft water system has been disinfected and flushed and a 
complete set of follow-up samples is total coliform-negative; and
    (ii) Disinfect and flush. Conduct disinfection and flushing in 
accordance with Sec.  141.804(b)(2). If the aircraft water system cannot 
be physically disconnected or shut-off, or the flow of water otherwise 
prevented through the tap(s), then the air carrier must disinfect and 
flush the system no later than 72 hours after the laboratory notifies 
the air carrier of the E. coli-positive result or discovery of the 
applicable failure as specified in paragraphs (g) and (h) of this 
section; and
    (iii) Follow-up sampling. Collect follow-up samples in accordance 
with paragraph (e) of this section. A complete set of follow-up sample 
results must be total coliform-negative before the air carrier provides 
water for human consumption from the aircraft water system and returns 
to the routine monitoring frequency as specified in the sampling plan 
required by Sec.  141.802.
    (3) Positive routine total coliform sample results. If any routine 
sample is total coliform-positive and E. coli-negative, then the air 
carrier must perform at least one of the following three corrective 
actions and continue through with that action until a complete set of 
follow-up or repeat samples is total coliform-negative:
    (i) Disinfect and flush. In accordance with Sec.  141.804(b)(2), 
conduct disinfection and flushing of the system no later than 72 hours 
after the laboratory notifies the air carrier of the total coliform-
positive and E. coli-negative result. After disinfection and flushing is 
completed, the air carrier must collect follow-up samples in accordance 
with paragraph (e) of this section prior to providing water for human 
consumption from the aircraft water system. A complete set of follow-up 
sample results must be total coliform-negative before the air carrier 
returns to the

[[Page 709]]

routine monitoring frequency as specified in the sampling plan required 
by Sec.  141.802; or
    (ii) Restrict public access. In accordance with paragraph (d) of 
this section, restrict public access to the aircraft water system as 
expeditiously as possible, but in no case later than 72 hours after the 
laboratory notifies the air carrier of the total coliform-positive and 
E. coli-negative result or discovery of the applicable failure as 
specified in paragraphs (f), (g), and, (i) of this section. All public 
access restrictions, including applicable public notification 
requirements, must remain in-place until the aircraft water system has 
been disinfected and flushed, and a complete set of follow-up samples 
has been collected. The air carrier must conduct disinfection and 
flushing in accordance with Sec.  141.804(b)(2). After disinfection and 
flushing is completed, the air carrier must collect follow-up samples in 
accordance with paragraph (e) of this section prior to providing water 
for human consumption from the aircraft water system. A complete set of 
follow-up sample results must be total coliform-negative before the air 
carrier returns to the routine monitoring frequency as specified in the 
sampling plan required by Sec.  141.802; or
    (iii) Repeat sampling. Collect three 100 mL repeat samples no later 
than 24 hours after the laboratory notifies the air carrier of the 
routine total coliform-positive and E. coli-negative result. Repeat 
samples must be collected and analyzed from three taps within the 
aircraft as follows: The tap which resulted in the total coliform-
positive sample, one other lavatory tap, and one other galley tap. If 
fewer than three taps exist, then a total of three 100 mL samples must 
be collected and analyzed from the available taps within the aircraft 
water system.
    (A) If all repeat samples are total coliform-negative, then the air 
carrier must maintain the routine monitoring frequency for total 
coliform as specified in the sampling plan in Sec.  141.802.
    (B) If any repeat sample is E. coli-positive, the air carrier must 
perform all the corrective actions as specified in paragraphs (c)(2)(i), 
(c)(2)(ii), and (c)(2)(iii) of this section.
    (C) If any repeat sample is total coliform-positive and E. coli-
negative, then the air carrier must perform the corrective actions 
specified in paragraphs (c)(3)(i) or (c)(3)(ii) of this section, and 
continue through with that action until a complete set of follow-up 
samples is total coliform-negative.
    (d) Restriction of public access. Restriction of public access to 
the aircraft water system includes, but need not be limited to, the 
following:
    (1) Physically disconnecting or shutting off the aircraft water 
system, where feasible, or otherwise preventing the flow of water 
through the tap(s);
    (2) Providing public notification to passengers and crew in 
accordance with Sec.  141.805.
    (3) Providing alternatives to water from the aircraft water system, 
such as bottled water for drinking and coffee or tea preparation; 
antiseptic hand gels or wipes in accordance with 21 CFR part 333--
``Topical Anti-microbial Drug Products for Over-the-Counter Human Use'' 
in the galleys and lavatories; and other feasible measures that reduce 
or eliminate the need to use the aircraft water system during the 
limited period before public use of the aircraft water system is 
unrestricted.
    (e) Post disinfection and flushing follow-up sampling. Following 
corrective action disinfection and flushing, air carriers must comply 
with post disinfection and flushing follow-up sampling procedures that, 
at a minimum, consist of the following:
    (1) For each aircraft water system, the air carrier must collect a 
complete set of total coliform follow-up samples consisting of two 100 
mL total coliform samples at the same routine sample locations as 
identified in paragraphs (b)(2) and (b)(4) of this section.
    (2) Follow-up samples must be collected prior to providing water to 
the public for human consumption from the aircraft water system.
    (3) If a complete set of follow-up samples is total coliform-
negative, the air carrier must return to the routine monitoring 
frequency for total coliform as specified in the sampling plan required 
by Sec.  141.802.
    (4) If any follow-up sample is E. coli-positive, the air carrier 
must perform all the corrective actions as specified

[[Page 710]]

in paragraphs (c)(2)(i), (c)(2)(ii), and (c)(2)(iii) of this section.
    (5) If any follow-up sample is total coliform-positive and E. coli-
negative the air carrier must restrict public access to the aircraft 
water system in accordance with paragraph (d) of this section as 
expeditiously as possible, but in no case later than 72 hours after the 
laboratory notifies the air carrier of the total coliform-positive and 
E. coli-negative result. All public access restrictions, including 
applicable public notification requirements, must remain in-place until 
the aircraft water system has been disinfected and flushed in accordance 
with Sec.  141.804(b)(2) and a complete set of follow-up samples is 
total coliform-negative. The air carrier must collect follow-up samples 
in accordance with paragraph (e) of this section. A complete set of 
follow-up sample results must be total coliform-negative before the air 
carrier provides water for human consumption from the aircraft water 
system and returns to the routine monitoring frequency for coliform as 
specified in Sec.  141.802.
    (f) Failure to perform required routine disinfection and flushing or 
failure to collect required routine samples. If the air carrier fails to 
perform routine disinfection and flushing or fails to collect and 
analyze the required number of routine coliform samples, the air carrier 
must perform all the corrective actions as specified in paragraph 
(c)(3)(ii) of this section.
    (g) Failure to collect repeat or follow-up samples. If the air 
carrier fails to collect and analyze the required follow-up samples as a 
result of an E. coli-positive result, then the air carrier must perform 
all the corrective actions as specified in paragraphs (c)(2)(i), 
(c)(2)(ii), and (c)(2)(iii) of this section. If the air carrier fails to 
collect and analyze the required repeat samples or follow-up samples as 
a result of a total coliform-positive and E. coli-negative result, then 
the air carrier must perform all the corrective actions as specified in 
paragraph (c)(3)(ii) of this section.
    (h) Failure to board water from a safe watering point (E. coli-
positive). For the aircraft water system, the air carrier must perform 
all the corrective actions specified in paragraphs (c)(2)(i), 
(c)(2)(ii), and (c)(2)(iii) of this section when it becomes aware of an 
E. coli-positive event resulting from:
    (1) Boarding water from a watering point not in accordance with FDA 
regulations (21 CFR part 1240 subpart E), or
    (2) Boarding water that does not meet NPDWRs applicable to transient 
non-community water systems (Sec. Sec.  141.62 and 141.63, as applied to 
TNCWS),
    (3) Boarding water that is otherwise determined to be unsafe due to 
non-compliance with the procedures specified in Sec.  141.804(b)(6).
    (i) Failure to board water from a safe watering point (non-E. coli-
positive). For the aircraft water system, the air carrier must perform 
all the corrective actions specified in paragraphs (c)(3)(ii) of this 
section when it becomes aware of a non-E. coli-positive event resulting 
from:
    (1) Boarding water from a watering point not in accordance with FDA 
regulations (21 CFR part 1240, subpart E),
    (2) Boarding water that does not meet NPDWRs applicable to transient 
non-community water systems (Sec. Sec.  141.62 and 141.63, as applied to 
TNCWS), or
    (3) Boarding water that is otherwise determined to be unsafe due to 
non-compliance with the procedures specified in Sec.  141.804(b)(6).

[74 FR 53618, Oct. 19, 2009, as amended at 78 FR 10354, Feb. 13, 2013]



Sec.  141.804  Aircraft water system operations and maintenance plan.

    (a) Each air carrier must develop and implement an aircraft water 
system operations and maintenance plan for each aircraft water system 
that it owns or operates. This plan must be included in a Federal 
Aviation Administration (FAA)-accepted air carrier operations and 
maintenance program (14 CFR part 43, 14 CFR part 91, 14 CFR part 121).
    (b) Each aircraft water system operations and maintenance plan must 
include the following:
    (1) Watering point selection requirement. All watering points must 
be selected in accordance with Food and Drug Administration (FDA) 
regulations (21 CFR part 1240, subpart E).

[[Page 711]]

    (2) Procedures for disinfection and flushing. The plan must include 
the following requirements for procedures for disinfection and flushing 
of aircraft water system.
    (i) The air carrier must conduct disinfection and flushing of the 
aircraft water system in accordance with, or is consistent with, the 
water system manufacturer's recommendations. The air carrier may conduct 
disinfection and flushing more frequently, but not less frequently, than 
the manufacturer recommends.
    (ii) The operations and maintenance plan must identify the 
disinfection frequency, type of disinfecting agent, disinfectant 
concentration to be used, and the disinfectant contact time, and 
flushing volume or flushing time.
    (iii) In cases where a recommended routine disinfection and flushing 
frequency is not specified by the aircraft water system manufacturer, 
the air carrier must choose a disinfection and flushing, and 
corresponding monitoring frequency specified in Sec.  141.803(b)(3).
    (3) Follow-up sampling. The plan must include the procedures for 
follow-up sampling in accordance with Sec.  141.803(e).
    (4) Training requirements. Training for all personnel involved with 
the aircraft water system operation and maintenance provisions of this 
regulation must include, but is not limited to the following:
    (i) Boarding water procedures;
    (ii) Sample collection procedures;
    (iii) Disinfection and flushing procedures;
    (iv) Public health and safety reasons for the requirements of this 
subpart.
    (5) Procedures for conducting self-inspections of the aircraft water 
system. Procedures must include, but are not limited to, inspection of 
storage tank, distribution system, supplemental treatment, fixtures, 
valves, and backflow prevention devices.
    (6) Procedures for boarding water. The plan must include the 
following requirements and procedures for boarding water:
    (i) Within the United States, the air carrier must board water from 
watering points in accordance with Food and Drug Administration (FDA) 
regulations (21 CFR part 1240, subpart E).
    (ii) A description of how the water will be transferred from the 
watering point to the aircraft in a manner that ensures it will not 
become contaminated during the transfer.
    (iii) A description of how the carrier will ensure that water 
boarded outside the United States is safe for human consumption.
    (iv) A description of emergency procedures that meet the 
requirements in Sec.  141.803(h) and (i) that must be used in the event 
that the air carrier becomes aware that water was boarded to operate 
essential systems, such as toilets, but was boarded from a watering 
point not in accordance with FDA regulations, does not meet NPDWRs 
applicable to transient non-community water systems (Sec. Sec.  141.62 
and 141.63, as applied to TNCWSs), or is otherwise unsafe.
    (7) Coliform sampling plan. The air carrier must include the 
coliform sampling plan prepared in accordance with Sec.  141.802.
    (8) Aircraft water system disconnect/shut-off, or prevent flow of 
water through the tap(s) statement. An explanation of whether the 
aircraft water system can be physically disconnected/shut-off, or the 
flow of water otherwise prevented through the tap(s) to the crew and 
passengers.
    (c) For existing aircraft, the air carrier must develop the water 
system operations and maintenance plan required by this section by April 
19, 2011;
    (d) For new aircraft, the air carrier must develop the operations 
and maintenance plan required in this section within the first calendar 
quarter of initial operation of the aircraft.
    (e) Any changes to the aircraft water system operations and 
maintenance plan must be included in the FAA-accepted air carrier 
operations and maintenance program.



Sec.  141.805  Notification to passengers and crew.

    (a) Air carriers must give public notice for each aircraft in all of 
the following situations:
    (1) Public access to the aircraft water system is restricted in 
response to a routine, repeat or follow-up total coliform-positive or E. 
coli-positive sample result in accordance with Sec.  141.803(d);

[[Page 712]]

    (2) Failure to perform required routine disinfection and flushing or 
failure to collect required routine samples in accordance with Sec.  
141.803(f);
    (3) Failure to collect the required follow-up samples in response to 
a sample result that is E. coli-positive in accordance with Sec.  
141.803(g);
    (4) Failure to collect the required repeat samples or failure to 
collect the required follow-up samples in response to a sample result 
that is total coliform-positive and E. coli-negative in accordance with 
Sec.  141.803(g);
    (5) In accordance with Sec.  141.803(h), the air carrier becomes 
aware of an E. coli-positive event resulting from water that has been 
boarded from a watering point not in accordance with FDA regulations (21 
CFR part 1240, subpart E), or that does not meet NPDWRs applicable to 
transient non-community water systems, or that is otherwise determined 
to be unsafe due to non-compliance with the procedures specified in 
Sec.  141.804(b)(6);
    (6) In accordance with Sec.  141.803(i), the air carrier becomes 
aware of a non-E. coli-positive event resulting from water that has been 
boarded from a watering point not in accordance with FDA regulations (21 
CFR part 1240, subpart E), or that does not meet NPDWRs applicable to 
transient non-community water systems, or that is otherwise determined 
to be unsafe due to non-compliance with the procedures specified in 
Sec.  141.804(b)(6).
    (7) The Administrator, the carrier, or the crew otherwise determines 
that notification is necessary to protect public health.
    (b) Public notification: (1) Must be displayed in a conspicuous way 
when printed or posted;
    (2) Must not contain overly technical language or very small print;
    (3) Must not be formatted in a way that defeats the purpose of the 
notice;
    (4) Must not contain language that nullifies the purpose of the 
notice;
    (5) Must contain information in the appropriate language(s) 
regarding the importance of the notice, reflecting a good faith effort 
to reach the non-English speaking population served, including, where 
applicable, an easily recognized symbol for non-potable water.
    (c) Public notification for paragraph (a)(1) of this section must 
meet the requirements of paragraph (b) of this section in addition to 
the following:
    (1) Public notification must include a prominently displayed, clear 
statement in each lavatory indicating that the water is non-potable and 
should not be used for drinking, food or beverage preparation, hand 
washing, teeth brushing, or any other consumptive use; and
    (2) A prominent notice in the galley directed at the crew which 
includes:
    (i) A clear statement that the water is non-potable and should not 
be used for drinking, food or beverage preparation, hand washing, teeth 
brushing, or any other consumptive use;
    (ii) A description of the violation or situation triggering the 
notice, including the contaminant(s) of concern;
    (iii) When the violation or situation occurred;
    (iv) Any potential adverse health effects from the violation or 
situation, as appropriate, under paragraph (g) of this section;
    (v) The population at risk, including sensitive subpopulations 
particularly vulnerable if exposed to the contaminant in the drinking 
water;
    (vi) What the air carrier is doing to correct the violation or 
situation; and
    (vii) When the air carrier expects to return the system to 
unrestricted public access.
    (3) If passenger access to the water system is physically prevented 
through disconnecting or shutting off the water, or the flow of water 
prevented through the tap(s), or if water is supplied only to lavatory 
toilets, and not to any lavatory or galley taps, then only the notice 
specified in paragraph (c)(2) of this section is required.
    (4) Air carriers must initiate public notification when restriction 
of public access is initiated in accordance with Sec.  141.803(d) and 
must continue until the aircraft water system is returned to 
unrestricted public access.
    (d) Public notification for paragraphs (a)(2), (a)(4), and (a)(6) of 
this section must meet the requirements of paragraph (b) of this section 
in addition to the following:
    (1) Public notification must include a prominently displayed, clear 
statement

[[Page 713]]

in each lavatory indicating that the water is non-potable and should not 
be used for drinking, food or beverage preparation, hand washing, teeth 
brushing, or any other consumptive use; and
    (2) A prominent notice in the galley directed at the crew which 
includes:
    (i) A clear statement that the water is non-potable and should not 
be used for drinking, food or beverage preparation, hand washing, teeth 
brushing, or any other consumptive use;
    (ii) A clear statement that it is not known whether the water is 
contaminated because there was a failure to perform required routine 
disinfection and flushing; or a failure to perform required monitoring; 
or water was boarded from a watering point not in accordance with FDA 
regulations, or that does not meet NPDWRs applicable to transient 
noncommunity water systems, or that is otherwise determined to be unsafe 
due to noncompliance with the procedures specified in Sec.  
141.804(b)(6);
    (iii) When and where the unsafe water was boarded or when the 
specific monitoring or disinfection and flushing requirement was not 
met;
    (iv) Any potential adverse health effects from exposure to 
waterborne pathogens that might be in the water, as appropriate, under 
paragraph (g) of this section;
    (v) The population at risk, including sensitive subpopulations 
particularly vulnerable if exposed to the contaminant in the drinking 
water; and
    (vi) A statement indicating when the system will be disinfected and 
flushed and returned to unrestricted public access.
    (3) If passenger access to the water system is physically prevented 
through disconnecting or shutting off the water, or the flow of water 
prevented through the tap(s), or if water is supplied only to lavatory 
toilets, and not to any lavatory or galley taps, then only the notice 
specified in paragraph (d)(2) of this section is required.
    (4) Air carriers must initiate public notification when restriction 
of public access is initiated in accordance with Sec.  141.803(d) and 
must continue until the aircraft water system is returned to 
unrestricted public access.
    (e) Public notification for paragraphs (a)(3) and (a)(5) of this 
section must meet the requirements of paragraph (b) of this section in 
addition to the following:
    (1) Public notification must include a prominently displayed, clear 
statement in each lavatory indicating that the water is non-potable and 
should not be used for drinking, food or beverage preparation, hand 
washing, teeth brushing, or any other consumptive use; and
    (2) A prominent notice in the galley directed at the crew which 
includes:
    (i) A clear statement that the water is non-potable and should not 
be used for drinking, food or beverage preparation, hand washing, teeth 
brushing, or any other consumptive use;
    (ii) A clear statement that the water is contaminated and there was 
a failure to conduct required monitoring; or a clear statement that 
water is contaminated because water was boarded from a watering point 
not in accordance with FDA regulations, or that does not meet NPDWRs 
applicable to transient noncommunity water systems, or that is otherwise 
determined to be unsafe due to noncompliance with the procedures 
specified in Sec.  141.804(b)(6);
    (iii) A description of the contaminant(s) of concern;
    (iv) When and where the unsafe water was boarded or when the 
specific monitoring requirement was not met;
    (v) Any potential adverse health effects from the situation, as 
appropriate, under paragraph (g) of this section;
    (vi) The population at risk, including sensitive subpopulations 
particularly vulnerable if exposed to the contaminant in the drinking 
water;
    (vii) A statement indicating what the air carrier is doing to 
correct the situation; and
    (viii) When the air carrier expects to return the system to 
unrestricted public access.
    (3) If passenger access to the water system is physically prevented 
through disconnecting or shutting off the water, or the flow of water 
prevented through the tap(s), or if water is supplied only to lavatory 
toilets, and not to any lavatory or galley taps, then

[[Page 714]]

only the notice specified in paragraph (e)(2) of this section is 
required.
    (4) Air carriers must initiate public notification when restriction 
of public access is initiated in accordance with Sec.  141.803(d) and 
must continue public notification until a complete set of required 
follow-up samples are total coliform-negative.
    (f) Public notification for paragraph (a)(7) of this section must 
meet the requirements of paragraph (b) of this section in addition to 
the following:
    (1) Notification must be in a form and manner reasonably calculated 
to reach all passengers and crew while on board the aircraft by using 
one or more of the following forms of delivery:
    (i) Broadcast over public announcement system on aircraft;
    (ii) Posting of the notice in conspicuous locations throughout the 
area served by the water system. These locations would normally be the 
galleys and in the lavatories of each aircraft requiring posting;
    (iii) Hand delivery of the notice to passengers and crew;
    (iv) Another delivery method approved in writing by the 
Administrator.
    (2) Air carriers must initiate public notification within 24 hours 
of being informed by EPA to perform notification and must continue 
notification for the duration determined by EPA.
    (g) In each public notice to the crew, air carriers must use the 
following standard health effects language that corresponds to the 
situations in paragraphs (a)(1) through (a)(6) of this section.
    (1) Health effects language to be used when public notice is 
initiated due to the detection of total coliforms only (not E. coli) in 
accordance with paragraph (a)(1) of this section:

    Coliform are bacteria that are naturally present in the environment 
and are used as an indicator that other, potentially harmful, bacteria 
may be present. Coliforms were found in [INSERT NUMBER OF SAMPLES 
DETECTED] samples collected and this is a warning of potential problems. 
If human pathogens are present, they can cause short-term health 
effects, such as diarrhea, cramps, nausea, headaches, or other symptoms. 
They may pose a special health risk for infants, young children, some of 
the elderly, and people with severely compromised immune systems.

    (2) Health effects language to be used when public notice is 
initiated due to any E. coli-positive routine, repeat, or follow-up 
sample in accordance with paragraph (a)(1) of this section:

    E. coli are bacteria whose presence indicates that the water may be 
contaminated with human or animal wastes. Microbes in these wastes can 
cause short-term health effects, such as diarrhea, cramps, nausea, 
headaches, or other symptoms. They may pose a special health risk for 
infants, young children, some of the elderly, and people with severely 
compromised immune systems.

    (3) Health effects language to be used when public notice is 
initiated due to a failure to conduct routine monitoring or routine 
disinfection and flushing in accordance with paragraph (a)(2) of this 
section; or when there is a failure to conduct repeat or follow-up 
sampling in accordance with paragraph (a)(4) of this section; or in 
accordance with paragraph (a)(6) of this section, when the air carrier 
becomes aware of a non-E. coli-positive event that is the result of 
water that was boarded from a watering point not in accordance with FDA 
regulations (21 CFR part 1240, subpart E), or that does not meet NPDWRs 
applicable to transient non-community water systems, or that is 
otherwise determined to be unsafe due to non-compliance with the 
procedures specified in Sec.  141.804(b)(6):

    Because [REQUIRED MONITORING AND ANALYSIS WAS NOT CONDUCTED], 
[REQUIRED DISINFECTION AND FLUSHING WAS NOT CONDUCTED] [WATER WAS 
BOARDED FROM A WATERING POINT NOT IN ACCORDANCE WITH FDA REGULATIONS (21 
CR 1240 SUBPART E)], or [OTHER APPROPRIATE EXPLANATION], we cannot be 
sure of the quality of the drinking water at this time. However, 
drinking water contaminated with human pathogens can cause short-term 
health effects, such as diarrhea, cramps, nausea, headaches, or other 
symptoms. They may pose a special health risk for infants, young 
children, some of the elderly, and people with severely compromised 
immune systems.

    (4) Health effects language to be used when public notice is 
initiated due to a failure to conduct required follow-up

[[Page 715]]

monitoring in response to a sample result that is E. coli-positive in 
accordance with paragraph (a)(3) of this section; or in accordance with 
paragraph (a)(5) of this section, when the air carrier becomes aware of 
an E. coli-positive event that is the result of water that was boarded 
from a watering point not in accordance with FDA regulations (21 CFR 
part 1240, subpart E), or that does not meet NPDWRs applicable to 
transient non-community water systems, or that is otherwise determined 
to be unsafe due to non-compliance with the procedures specified in 
Sec.  141.804(b)(6):

    Because required follow-up monitoring and analysis was not conducted 
after the aircraft water system tested positive for E. coli, we cannot 
be sure of the quality of the drinking water at this time. E. coli are 
bacteria whose presence indicates that the water may be contaminated 
with human or animal wastes. Microbes in these wastes can cause short-
term health effects, such as diarrhea, cramps, nausea, headaches, or 
other symptoms. They may pose a special health risk for infants, young 
children, some of the elderly, and people with severely compromised 
immune systems.

OR

    Water was boarded that is contaminated with E. coli because [WATER 
WAS BOARDED FROM A WATERING POINT NOT IN ACCORDANCE WITH FDA REGULATIONS 
(21 CR 1240 SUBPART E)], or [OTHER APPROPRIATE EXPLANATION]. E. coli are 
bacteria whose presence indicates that the water may be contaminated 
with human or animal wastes. Microbes in these wastes can cause short-
term health effects, such as diarrhea, cramps, nausea, headaches, or 
other symptoms. They may pose a special health risk for infants, young 
children, some of the elderly, and people with severely compromised 
immune systems.



Sec.  141.806  Reporting requirements.

    (a) The air carrier must comply with the following requirements 
regarding reporting of the development of the coliform sampling plan, 
the operations and maintenance plan, and the disinfection and flushing 
and coliform sampling frequencies.
    (1) The air carrier must report to the Administrator that it has 
developed the coliform sampling plan required by Sec.  141.802, which 
covers each existing aircraft water system, as well as report the 
frequency for routine coliform sampling identified in the coliform 
sampling plan by April 19, 2011. The air carrier must report to the 
Administrator that it has developed its operations and maintenance plan 
required by Sec.  141.804 and report the frequency for routine 
disinfection and flushing by April 19, 2011;
    (2) For each new aircraft meeting the definition of an aircraft 
water system, which becomes operational after publication of this 
subpart, the air carrier must report to the Administrator that it has 
developed the coliform sampling plan required by Sec.  141.802, as well 
as report the frequency for routine coliform sampling identified in the 
coliform sampling plan, within the first calendar quarter of initial 
operation of the aircraft. The air carrier must report to the 
Administrator that it has developed the aircraft water system operations 
and maintenance plan required by Sec.  141.804, and report the frequency 
for routine disinfection and flushing within the first calendar quarter 
of initial operation of the aircraft.
    (b) The air carrier must report the following information to the 
Administrator:
    (1) A complete inventory of aircraft that are public water systems 
by April 19, 2011. Inventory information includes, at a minimum, the 
following:
    (i) The unique aircraft identifier number;
    (ii) The status (active or inactive) of any aircraft as an aircraft 
water system as defined in Sec.  141.801;
    (iii) The type and location of any supplemental treatment equipment 
installed on the water system; and
    (iv) Whether the aircraft water system can be physically 
disconnected or shut-off, or the flow of water prevented through the 
tap(s).
    (2) Changes in aircraft inventory no later than 10 days following 
the calendar month in which the change occurred. Changes in inventory 
information include, at a minimum, the following:
    (i) Change in the unique identifier number for any new aircraft, or 
any aircraft removed from the carrier's fleet;
    (ii) Change in status (active or inactive) of any aircraft as an 
aircraft water system as defined in Sec.  141.801; and

[[Page 716]]

    (iii) Change to the type and location of any supplemental treatment 
equipment added to or removed from the water system.
    (iv) Change to whether the aircraft water system can be physically 
disconnected or shut-off, or the flow of water prevented through the 
tap(s).
    (3) All sampling results no later than 10 calendar days following 
the monitoring period in which the sampling occurred. The monitoring 
period is based on the monitoring frequency identified in the coliform 
sampling plan required under Sec.  141.802. Routine disinfection and 
flushing events must be reported no later than 10 calendar days 
following the disinfection and flushing period in which the disinfection 
and flushing occurred. The disinfection and flushing period is based on 
the frequency identified in the operations and maintenance plan required 
under Sec.  141.804.
    (4) All events requiring notification to passengers or crew, or non-
routine disinfection and flushing, or non-routine sampling, within 10 
days of the event (e.g., notification of positive sample result by 
laboratory), including information on whether required notification was 
provided to passengers or crew or both.
    (5) Failure to comply with the monitoring or disinfection and 
flushing requirements of this subpart within 10 calendar days of 
discovery of the failure.
    (6) Changes in disinfection and flushing and coliform sampling 
frequencies no later than 10 days following the calendar month in which 
the change occurred. Changes to an aircraft's routine coliform sampling 
frequency and routine disinfection and flushing frequency must be 
included in the aircraft water system operation and maintenance plan 
that is included in the air carrier operations and maintenance program 
accepted by FAA in accordance with Sec.  141.804.
    (c) The air carrier must provide evidence of a self-inspection to 
the Administrator within 90 days of completion of the self-inspection 
required under Sec.  141.808(b), including reporting whether all 
deficiencies were addressed in accordance with Sec.  141.808(c). The air 
carrier must also report to the Administrator within 90 days that any 
deficiency identified during a compliance audit conducted in accordance 
with Sec.  141.808(a) has been addressed. If any deficiency has not been 
addressed within 90 days of identification of the deficiency, the report 
must also include a description of the deficiency, an explanation as to 
why it has not yet been addressed, and a schedule for addressing it as 
expeditiously as possible.
    (d) All information required to be reported to the Administrator 
under this subpart must be in an electronic format established or 
approved by the Administrator. If an air carrier is unable to report 
electronically, the air carrier may use an alternative approach that the 
Administrator approves.



Sec.  141.807  Recordkeeping requirements.

    (a) The air carrier must keep records of bacteriological analyses 
for at least 5 years and must include the following information:
    (1) The date, time, and place of sampling, and the name of the 
person who collected the sample;
    (2) Identification of the sample as a routine, repeat, follow-up, or 
other special purpose sample;
    (3) Date of the analysis;
    (4) Laboratory and person responsible for performing the analysis;
    (5) The analytical technique/method used; and
    (6) The results of the analysis.
    (b) The air carrier must keep records of any disinfection and 
flushing for at least 5 years and must include the following 
information:
    (1) The date and time of the disinfection and flushing; and
    (2) The type of disinfection and flushing (i.e., routine or 
corrective action).
    (c) The air carrier must keep records of a self-inspection for at 
least 10 years and must include the following information:
    (1) The completion date of the self-inspection; and
    (2) Copies of any written reports, summaries, or communications 
related to the self-inspection.
    (d) The air carrier must maintain sampling plans and make such plans 
available for review by the Administrator upon request, including during 
compliance audits.

[[Page 717]]

    (e) The air carrier must maintain aircraft water system operations 
and maintenance plans in accordance with FAA requirements, and make such 
plans available for review by the Administrator upon request, including 
during compliance audits.
    (f) The air carrier must keep copies of public notices to passengers 
and crew issued as required by this subpart for at least 3 years after 
issuance.



Sec.  141.808  Audits and inspections.

    (a) The Administrator may conduct routine compliance audits as 
deemed necessary in providing regulatory oversight to ensure proper 
implementation of the requirements in this subpart. Compliance audits 
may include, but are not limited to:
    (1) Bacteriological sampling of aircraft water system;
    (2) Reviews and audits of records as they pertain to water system 
operations and maintenance such as log entries, disinfection and 
flushing procedures, and sampling results; and
    (3) Observation of procedures involving the handling of finished 
water, watering point selection, boarding of water, operation, 
disinfection and flushing, and general maintenance and self-inspections 
of aircraft water system.
    (b) Air carriers or their representatives must perform a self-
inspection of all water system components for each aircraft water system 
no less frequently than once every 5 years.
    (c) The air carrier must address any deficiency identified during 
compliance audits or routine self-inspections within 90 days of 
identification of the deficiency, or where such deficiency is identified 
during extended or heavy maintenance, before the aircraft is put back 
into service. This includes any deficiency in the water system's design, 
construction, operation, maintenance, or administration, as well as any 
failure or malfunction of any system component that has the potential to 
cause an unacceptable risk to health or that could affect the reliable 
delivery of safe drinking water.



Sec.  141.809  Supplemental treatment.

    (a) Any supplemental drinking water treatment units installed 
onboard existing or new aircraft must be acceptable to FAA and FDA; and 
must be installed, operated, and maintained in accordance with the 
manufacturer's plans and specifications and FAA requirements.
    (b) Water supplemental treatment and production equipment must 
produce water that meets the standards prescribed in this part.



Sec.  141.810  Violations.

    An air carrier is in violation of this subpart when, for any 
aircraft water system it owns or operates, any of the following occur:
    (a) It fails to perform any of the requirements in accordance with 
Sec.  141.803 or Sec.  141.804.
    (b) It has an E. coli-positive sample in any monitoring period 
(routine and repeat samples are used in this determination).
    (c) It fails to provide notification to passengers and crew in 
accordance with Sec.  141.805.
    (d) It fails to comply with the reporting and recordkeeping 
requirements of this subpart.
    (e) It fails to conduct a self-inspection or address a deficiency in 
accordance with Sec.  141.808.
    (f) It fails to develop a coliform sampling plan in accordance with 
Sec.  141.802, or fails to have and follow an operations and maintenance 
plan, which is included in a FAA accepted program in accordance with 
Sec.  141.804.



                  Subpart Y_Revised Total Coliform Rule

    Source: 78 FR 10354, Feb. 13, 2013, unless otherwise noted.



Sec.  141.851  General.

    (a) General. The provisions of this subpart include both maximum 
contaminant level and treatment technique requirements.
    (b) Applicability. The provisions of this subpart apply to all 
public water systems.
    (c) Compliance date. Systems must comply with the provisions of this 
subpart beginning April 1, 2016, unless otherwise specified in this 
subpart.
    (d) Implementation with EPA as State. Systems falling under direct 
oversight

[[Page 718]]

of EPA, where EPA acts as the State, must comply with decisions made by 
EPA for implementation of subpart Y. EPA has authority to establish such 
procedures and criteria as are necessary to implement subpart Y.
    (e) Violations of national primary drinking water regulations. 
Failure to comply with the applicable requirements of Sec. Sec.  141.851 
through 141.861, including requirements established by the State 
pursuant to these provisions, is a violation of the national primary 
drinking water regulations under subpart Y.



Sec.  141.852  Analytical methods and laboratory certification.

    (a) Analytical methodology. (1) The standard sample volume required 
for analysis, regardless of analytical method used, is 100 ml.
    (2) Systems need only determine the presence or absence of total 
coliforms and E. coli; a determination of density is not required.
    (3) The time from sample collection to initiation of test medium 
incubation may not exceed 30 hours. Systems are encouraged but not 
required to hold samples below 10 deg. C during transit.
    (4) If water having residual chlorine (measured as free, combined, 
or total chlorine) is to be analyzed, sufficient sodium thiosulfate 
(Na2S2O3) must be added to the sample 
bottle before sterilization to neutralize any residual chlorine in the 
water sample. Dechlorination procedures are addressed in Section 9060A.2 
of Standard Methods for the Examination of Water and Wastewater (20th 
and 21st editions).
    (5) Systems must conduct total coliform and E. coli analyses in 
accordance with one of the analytical methods in the following table or 
one of the alternative methods listed in Appendix A to subpart C of part 
141.

[[Page 719]]



----------------------------------------------------------------------------------------------------------------
             Organism                 Methodology category           Method \1\               Citation \1\
----------------------------------------------------------------------------------------------------------------
         Total Coliforms
                                   Lactose Fermentation       Standard Total Coliform   Standard Methods 9221
                                    Methods.                   Fermentation Technique.   B.1, B.2 (20th ed.;
                                                                                         21st ed.).2 3
                                   .........................  ........................  Standard Methods Online
                                                                                         9221 B.1, B.2-99.2 3
                                   .........................  Presence-Absence (P-A)    Standard Methods 9221
                                                               Coliform Test.            D.1, D.2 (20th ed.;
                                                                                         21st ed.).2 7
                                   .........................  ........................  Standard Methods Online
                                                                                         9221 D.1, D.2-99.2 7
                                   Membrane Filtration        Standard Total Coliform   Standard Methods 9222 B,
                                    Methods.                   Membrane Filter           C (20th ed.; 21st
                                                               Procedure.                ed.).2 4
                                   .........................  ........................  Standard Methods Online
                                                                                         9222 B-97 2 4, 9222 C-
                                                                                         97.2 4
                                   .........................  Membrane Filtration       EPA Method 1604.\2\
                                                               using MI medium.
                                   .........................  m-ColiBlue24[supreg]
                                                               Test 2 4.
                                   .........................  Chromocult 2 4..........
                                   Enzyme Substrate Methods.  Colilert[supreg]........  Standard Methods 9223 B
                                                                                         (20th ed.; 21st ed.).2
                                                                                         5
                                   .........................  ........................  Standard Methods Online
                                                                                         9223 B-97.2 5
                                   .........................  Colisure[supreg]........  Standard Methods 9223 B
                                                                                         (20th ed.; 21st ed.).2
                                                                                         5 6
                                   .........................  ........................  Standard Methods Online
                                                                                         9223 B-97.2 5 6
                                   .........................  E*Colite[supreg] Test
                                                               \2\.
                                   .........................  Readycult[supreg] Test
                                                               \2\.
                                   .........................  modified Colitag[supreg]
                                                               Test \2\.
Escherichia coli.................
                                   Escherichia coli           EC-MUG medium...........  Standard Methods 9221
                                    Procedure (following                                 F.1 (20th ed.; 21st
                                    Lactose Fermentation                                 ed.) \2\
                                    Methods).
                                   Escherichia coli           EC broth with MUG (EC-    Standard Methods 9222
                                    Partition Method.          MUG).                     G.1c(2) (20th ed.; 21st
                                                                                         ed.) \2 8\
                                                              NA-MUG medium...........  Standard Methods 9222
                                                                                         G.1c(1) (20th ed.; 21st
                                                                                         ed.) \2\
                                   Membrane Filtration        Membrane Filtration       EPA Method 1604 \2\
                                    Methods.                   using MI medium.
                                                              m-ColiBlue24[supreg]
                                                               Test \2 4\.
                                                              Chromocult \2 4\........
                                   Enzyme Substrate Methods.  Colilert[supreg]........  Standard Methods 9223 B
                                                                                         (20th ed.; 21st ed.) \2
                                                                                         5\
                                                                                        Standard Methods Online
                                                                                         9223 B-97 \2 5 6\
                                                              Colisure[supreg]........  Standard Methods 9223 B
                                                                                         (20th ed.; 21st ed.) \2
                                                                                         5 6\
                                                                                        Standard Methods Online
                                                                                        9223 B-97 \2 5 6\
                                                              E*Colite[supreg] Test
                                                               \2\.
                                                              Readycult[supreg] Test
                                                               \2\.
                                                              modified Colitag[supreg]
                                                               Test \2\.
----------------------------------------------------------------------------------------------------------------
\1\ The procedures must be done in accordance with the documents listed in paragraph (c) of this section. For
  Standard Methods, either editions, 20th (1998) or 21st (2005), may be used. For the Standard Methods Online,
  the year in which each method was approved by the Standard Methods Committee is designated by the last two
  digits following the hyphen in the method number. The methods listed are the only online versions that may be
  used. For vendor methods, the date of the method listed in paragraph (c) of this section is the date/version
  of the approved method. The methods listed are the only versions that may be used for compliance with this
  rule. Laboratories should be careful to use only the approved versions of the methods, as product package
  inserts may not be the same as the approved versions of the methods.

[[Page 720]]

 
\2\ Incorporated by reference. See paragraph (c) of this section.
\3\ Lactose broth, as commercially available, may be used in lieu of lauryl tryptose broth, if the system
  conducts at least 25 parallel tests between lactose broth and lauryl tryptose broth using the water normally
  tested, and if the findings from this comparison demonstrate that the false-positive rate and false-negative
  rate for total coliforms, using lactose broth, is less than 10 percent.
\4\ All filtration series must begin with membrane filtration equipment that has been sterilized by autoclaving.
  Exposure of filtration equipment to UV light is not adequate to ensure sterilization. Subsequent to the
  initial autoclaving, exposure of the filtration equipment to UV light may be used to sanitize the funnels
  between filtrations within a filtration series. Alternatively, membrane filtration equipment that is pre-
  sterilized by the manufacturer (i.e., disposable funnel units) may be used.
\5\ Multiple-tube and multi-well enumerative formats for this method are approved for use in presence-absence
  determination under this regulation.
\6\ Colisure[supreg] results may be read after an incubation time of 24 hours.
\7\ A multiple tube enumerative format, as described in Standard Methods for the Examination of Water and
  Wastewater 9221, is approved for this method for use in presence-absence determination under this regulation.
\8\ The following changes must be made to the EC broth with MUG (EC-MUG) formulation: Potassium dihydrogen
  phosphate, KH 2PO 4, must be 1.5g, and 4-methylumbelliferyl-Beta-D-glucuronide must be 0.05 g.


[[Page 721]]

    (b) Laboratory certification. Systems must have all compliance 
samples required under this subpart analyzed by a laboratory certified 
by the EPA or a primacy State to analyze drinking water samples. The 
laboratory used by the system must be certified for each method (and 
associated contaminant(s)) used for compliance monitoring analyses under 
this rule.
    (c) Incorporation by reference. The standards required in this 
section are incorporated by reference into this section with the 
approval of the Director of the Federal Register under 5 U.S.C. 552(a) 
and 1 CFR part 51. To enforce any edition other than that specified in 
this section, EPA must publish notice of change in the Federal Register 
and the material must be available to the public. All approved material 
is available for inspection either electronically at 
www.regulations.gov, in hard copy at the Water Docket, or from the 
sources indicated below. The Docket ID is EPA-HQ-OW-2008-0878. Hard 
copies of these documents may be viewed at the Water Docket in the EPA 
Docket Center, (EPA/DC) EPA West, Room 3334, 1301 Constitution Ave. NW., 
Washington, DC. The EPA Docket Center Public Reading Room is open from 
8:30 a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. 
The telephone number for the Public Reading Room is 1-202-566-1744, and 
the telephone number for the Water Docket is 1-202-566-2426. Copyrighted 
materials are only available for viewing in hard copy. These documents 
are also available for inspection at the National Archives and Records 
Administration (NARA). For information on the availability of this 
material at NARA, call 1-202-741-6030 or go to: http://www.archives.gov/
federal_register/code_of_federal_regulations/ibr_ locations.html.
    (1) American Public Health Association, 800 I Street, NW., 
Washington, DC 20001.
    (i) ``Standard Methods for the Examination of Water and 
Wastewater,'' 20th edition (1998):
    (A) Standard Methods 9221, ``Multiple-Tube Fermentation Technique 
for Members of the Coliform Group,'' B.1, B.2, ``Standard Total Coliform 
Fermentation Technique.''
    (B) Standard Methods 9221, ``Multiple-Tube Fermentation Technique 
for Members of the Coliform Group,'' D.1, D.2, ``Presence-Absence (P-A) 
Coliform Test.''
    (C) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' B, ``Standard Total Coliform Membrane Filter 
Procedure.''
    (D) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' C, ``Delayed-Incubation Total Coliform 
Procedure.''
    (E) Standard Methods 9223, ``Enzyme Substrate Coliform Test,'' B, 
``Enzyme Substrate Test,'' Colilert[supreg] and Colisure[supreg].
    (F) Standard Methods 9221, ``Multiple Tube Fermentation Technique 
for Members of the Coliform Group,'' F.1, ``Escherichia coli Procedure: 
EC-MUG medium.''
    (G) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' G.1.c(2), ``Escherichia coli Partition Method: 
EC broth with MUG (EC-MUG).''
    (H) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' G.1.c(1), ``Escherichia coli Partition Method: 
NA-MUG medium.''
    (ii) ``Standard Methods for the Examination of Water and 
Wastewater,'' 21st edition (2005):
    (A) Standard Methods 9221, ``Multiple-Tube Fermentation Technique 
for Members of the Coliform Group,'' B.1, B.2, ``Standard Total Coliform 
Fermentation Technique.''
    (B) Standard Methods 9221, ``Multiple-Tube Fermentation Technique 
for Members of the Coliform Group,'' D.1, D.2, ``Presence-Absence (P-A) 
Coliform Test.''
    (C) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' B, ``Standard Total Coliform Membrane Filter 
Procedure.''
    (D) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' C, ``Delayed-Incubation Total Coliform 
Procedure.''
    (E) Standard Methods 9223, ``Enzyme Substrate Coliform Test,'' B, 
``Enzyme Substrate Test,'' Colilert[supreg] and Colisure[supreg].

[[Page 722]]

    (F) Standard Methods 9221, ``Multiple Tube Fermentation Technique 
for Members of the Coliform Group,'' F.1, ``Escherichia coli Procedure: 
EC-MUG medium.''
    (G) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' G.1.c(2), ``Escherichia coli Partition Method: 
EC broth with MUG (EC-MUG).''
    (H) Standard Methods 9222, ``Membrane Filter Technique for Members 
of the Coliform Group,'' G.1.c(1), ``Escherichia coli Partition Method: 
NA-MUG medium.''
    (iii) ``Standard Methods Online'' available at http://
www.standardmethods.org:
    (A) Standard Methods Online 9221, ``Multiple-Tube Fermentation 
Technique for Members of the Coliform Group'' (1999), B.1, B.2-99, 
``Standard Total Coliform Fermentation Technique.''
    (B) Standard Methods Online 9221, ``Multiple-Tube Fermentation 
Technique for Members of the Coliform Group'' (1999), D.1, D.2-99, 
``Presence-Absence (P-A) Coliform Test.''
    (C) Standard Methods Online 9222, ``Membrane Filter Technique for 
Members of the Coliform Group'' (1997), B-97, ``Standard Total Coliform 
Membrane Filter Procedure.''
    (D) Standard Methods Online 9222, ``Membrane Filter Technique for 
Members of the Coliform Group'' (1997), C-97, ``Delayed-Incubation Total 
Coliform Procedure.''
    (E) Standard Methods Online 9223, ``Enzyme Substrate Coliform Test'' 
(1997), B-97, ``Enzyme Substrate Test'', Colilert[supreg] and 
Colisure[supreg].
    (2) Charm Sciences, Inc., 659 Andover Street, Lawrence, MA 01843-
1032, telephone 1-800-343-2170:
    (i) E*Colite[supreg]--``Charm E*Colite \TM\ Presence/Absence Test 
for Detection and Identification of Coliform Bacteria and Escherichia 
coli in Drinking Water,'' January 9, 1998.
    (ii) [Reserved]
    (3) CPI International, Inc., 5580 Skylane Blvd., Santa Rosa, CA, 
95403, telephone 1-800-878-7654:
    (i) modified Colitag[supreg], ATP D05-0035--``Modified Colitag \TM\ 
Test Method for the Simultaneous Detection of E. coli and other Total 
Coliforms in Water,'' August 28, 2009.
    (ii) [Reserved]
    (4) EMD Millipore (a division of Merck KGaA, Darmstadt Germany), 290 
Concord Road, Billerica, MA 01821, telephone 1-800-645-5476:
    (i) Chromocult--``Chromocult[supreg] Coliform Agar Presence/Absence 
Membrane Filter Test Method for Detection and Identification of Coliform 
Bacteria and Escherichia coli for Finished Waters,'' November 2000, 
Version 1.0.
    (ii) Readycult[supreg]--``Readycult[supreg] Coliforms 100 Presence/
Absence Test for Detection and Identification of Coliform Bacteria and 
Escherichia coli in Finished Waters,'' January 2007, Version 1.1.
    (5) EPA's Water Resource Center (MC-4100T), 1200 Pennsylvania Avenue 
NW., Washington, DC 20460, telephone 1-202-566-1729:
    (i) EPA Method 1604, EPA 821-R-02-024--``EPA Method 1604: Total 
Coliforms and Escherichia coli in Water by Membrane Filtration Using a 
Simultaneous Detection Technique (MI Medium),'' September 2002, http://
www.epa.gov/nerlcwww/1604sp02.pdf.
    (ii) [Reserved]
    (6) Hach Company, P.O. Box 389, Loveland, CO 80539, telephone 1-800-
604-3493:
    (i) m-ColiBlue24[supreg]--``Membrane Filtration Method m-
ColiBlue24[supreg] Broth,'' Revision 2, August 17, 1999.
    (ii) [Reserved]

[78 FR 10354, Feb. 13, 2013, as amended at 79 FR 10669, Feb. 26, 2014]



Sec.  141.853  General monitoring requirements for all public water systems.

    (a) Sample siting plans. (1) Systems must develop a written sample 
siting plan that identifies sampling sites and a sample collection 
schedule that are representative of water throughout the distribution 
system not later than March 31, 2016. These plans are subject to State 
review and revision. Systems must collect total coliform samples 
according to the written sample siting plan. Monitoring required by 
Sec. Sec.  141.854 through 141.858 may take place at a customer's 
premise, dedicated sampling station, or other designated compliance 
sampling location. Routine and repeat sample sites and any sampling

[[Page 723]]

points necessary to meet the requirements of subpart S must be reflected 
in the sampling plan.
    (2) Systems must collect samples at regular time intervals 
throughout the month, except that systems that use only ground water and 
serve 4,900 or fewer people may collect all required samples on a single 
day if they are taken from different sites.
    (3) Systems must take at least the minimum number of required 
samples even if the system has had an E. coli MCL violation or has 
exceeded the coliform treatment technique triggers in Sec.  141.859(a).
    (4) A system may conduct more compliance monitoring than is required 
by this subpart to investigate potential problems in the distribution 
system and use monitoring as a tool to assist in uncovering problems. A 
system may take more than the minimum number of required routine samples 
and must include the results in calculating whether the coliform 
treatment technique trigger in Sec.  141.859(a)(1)(i) and (ii) has been 
exceeded only if the samples are taken in accordance with the existing 
sample siting plan and are representative of water throughout the 
distribution system.
    (5) Systems must identify repeat monitoring locations in the sample 
siting plan. Unless the provisions of paragraphs (a)(5)(i) or (a)(5)(ii) 
of this section are met, the system must collect at least one repeat 
sample from the sampling tap where the original total coliform-positive 
sample was taken, and at least one repeat sample at a tap within five 
service connections upstream and at least one repeat sample at a tap 
within five service connections downstream of the original sampling 
site. If a total coliform-positive sample is at the end of the 
distribution system, or one service connection away from the end of the 
distribution system, the system must still take all required repeat 
samples. However, the State may allow an alternative sampling location 
in lieu of the requirement to collect at least one repeat sample 
upstream or downstream of the original sampling site. Except as provided 
for in paragraph (a)(5)(ii) of this section, systems required to conduct 
triggered source water monitoring under Sec.  141.402(a) must take 
ground water source sample(s) in addition to repeat samples required 
under this subpart.
    (i) Systems may propose repeat monitoring locations to the State 
that the system believes to be representative of a pathway for 
contamination of the distribution system. A system may elect to specify 
either alternative fixed locations or criteria for selecting repeat 
sampling sites on a situational basis in a standard operating procedure 
(SOP) in its sample siting plan. The system must design its SOP to focus 
the repeat samples at locations that best verify and determine the 
extent of potential contamination of the distribution system area based 
on specific situations. The State may modify the SOP or require 
alternative monitoring locations as needed.
    (ii) Ground water systems serving 1,000 or fewer people may propose 
repeat sampling locations to the State that differentiate potential 
source water and distribution system contamination (e.g., by sampling at 
entry points to the distribution system). A ground water system with a 
single well required to conduct triggered source water monitoring may, 
with written State approval, take one of its repeat samples at the 
monitoring location required for triggered source water monitoring under 
Sec.  141.402(a) if the system demonstrates to the State's satisfaction 
that the sample siting plan remains representative of water quality in 
the distribution system. If approved by the State, the system may use 
that sample result to meet the monitoring requirements in both Sec.  
141.402(a) and this section.
    (A) If a repeat sample taken at the monitoring location required for 
triggered source water monitoring is E. coli-positive, the system has 
violated the E. coli MCL and must also comply with Sec.  141.402(a)(3). 
If a system takes more than one repeat sample at the monitoring location 
required for triggered source water monitoring, the system may reduce 
the number of additional source water samples required under Sec.  
141.402(a)(3) by the number of repeat samples taken at that location 
that were not E. coli-positive.

[[Page 724]]

    (B) If a system takes more than one repeat sample at the monitoring 
location required for triggered source water monitoring under Sec.  
141.402(a), and more than one repeat sample is E. coli-positive, the 
system has violated the E. coli MCL and must also comply with Sec.  
141.403(a)(1).
    (C) If all repeat samples taken at the monitoring location required 
for triggered source water monitoring are E. coli-negative and a repeat 
sample taken at a monitoring location other than the one required for 
triggered source water monitoring is E. coli-positive, the system has 
violated the E. coli MCL, but is not required to comply with Sec.  
141.402(a)(3).
    (6) States may review, revise, and approve, as appropriate, repeat 
sampling proposed by systems under paragraphs (a)(5)(i) and (ii) of this 
section. The system must demonstrate that the sample siting plan remains 
representative of the water quality in the distribution system. The 
State may determine that monitoring at the entry point to the 
distribution system (especially for undisinfected ground water systems) 
is effective to differentiate between potential source water and 
distribution system problems.
    (b) Special purpose samples. Special purpose samples, such as those 
taken to determine whether disinfection practices are sufficient 
following pipe placement, replacement, or repair, must not be used to 
determine whether the coliform treatment technique trigger has been 
exceeded. Repeat samples taken pursuant to Sec.  141.858 are not 
considered special purpose samples, and must be used to determine 
whether the coliform treatment technique trigger has been exceeded.
    (c) Invalidation of total coliform samples. A total coliform-
positive sample invalidated under this paragraph (c) of this section 
does not count toward meeting the minimum monitoring requirements of 
this subpart.
    (1) The State may invalidate a total coliform-positive sample only 
if the conditions of paragraph (c)(1)(i), (ii), or (iii) of this section 
are met.
    (i) The laboratory establishes that improper sample analysis caused 
the total coliform-positive result.
    (ii) The State, on the basis of the results of repeat samples 
collected as required under Sec.  141.858(a), determines that the total 
coliform-positive sample resulted from a domestic or other non-
distribution system plumbing problem. The State cannot invalidate a 
sample on the basis of repeat sample results unless all repeat sample(s) 
collected at the same tap as the original total coliform-positive sample 
are also total coliform-positive, and all repeat samples collected at a 
location other than the original tap are total coliform-negative (e.g., 
a State cannot invalidate a total coliform-positive sample on the basis 
of repeat samples if all the repeat samples are total coliform-negative, 
or if the system has only one service connection).
    (iii) The State has substantial grounds to believe that a total 
coliform-positive result is due to a circumstance or condition that does 
not reflect water quality in the distribution system. In this case, the 
system must still collect all repeat samples required under Sec.  
141.858(a), and use them to determine whether a coliform treatment 
technique trigger in Sec.  141.859 has been exceeded. To invalidate a 
total coliform-positive sample under this paragraph, the decision and 
supporting rationale must be documented in writing, and approved and 
signed by the supervisor of the State official who recommended the 
decision. The State must make this document available to EPA and the 
public. The written documentation must state the specific cause of the 
total coliform-positive sample, and what action the system has taken, or 
will take, to correct this problem. The State may not invalidate a total 
coliform-positive sample solely on the grounds that all repeat samples 
are total coliform-negative.
    (2) A laboratory must invalidate a total coliform sample (unless 
total coliforms are detected) if the sample produces a turbid culture in 
the absence of gas production using an analytical method where gas 
formation is examined (e.g., the Multiple-Tube Fermentation Technique), 
produces a turbid culture in the absence of an acid reaction in the 
Presence-Absence (P-A) Coliform Test, or exhibits confluent

[[Page 725]]

growth or produces colonies too numerous to count with an analytical 
method using a membrane filter (e.g., Membrane Filter Technique). If a 
laboratory invalidates a sample because of such interference, the system 
must collect another sample from the same location as the original 
sample within 24 hours of being notified of the interference problem, 
and have it analyzed for the presence of total coliforms. The system 
must continue to re-sample within 24 hours and have the samples analyzed 
until it obtains a valid result. The State may waive the 24-hour time 
limit on a case-by-case basis. Alternatively, the State may implement 
criteria for waiving the 24-hour sampling time limit to use in lieu of 
case-by-case extensions.



Sec.  141.854  Routine monitoring requirements for non-community water systems 
serving 1,000 or fewer people using only ground water.

    (a) General. (1) The provisions of this section apply to non-
community water systems using only ground water (except ground water 
under the direct influence of surface water, as defined in Sec.  141.2) 
and serving 1,000 or fewer people.
    (2) Following any total coliform-positive sample taken under the 
provisions of this section, systems must comply with the repeat 
monitoring requirements and E. coli analytical requirements in Sec.  
141.858.
    (3) Once all monitoring required by this section and Sec.  141.858 
for a calendar month has been completed, systems must determine whether 
any coliform treatment technique triggers specified in Sec.  141.859 
have been exceeded. If any trigger has been exceeded, systems must 
complete assessments as required by Sec.  141.859.
    (4) For the purpose of determining eligibility for remaining on or 
qualifying for quarterly monitoring under the provisions of paragraphs 
(f)(4) and (g)(2), respectively, of this section for transient non-
community water systems, the State may elect to not count monitoring 
violations under Sec.  141.860(c)(1) of this part if the missed sample 
is collected no later than the end of the monitoring period following 
the monitoring period in which the sample was missed. The system must 
collect the make-up sample in a different week than the routine sample 
for that monitoring period and should collect the sample as soon as 
possible during the monitoring period. The State may not use this 
provision under paragraph (h) of this section. This authority does not 
affect the provisions of Sec. Sec.  141.860(c)(1) and 141.861(a)(4) of 
this part.
    (b) Monitoring frequency for total coliforms. Systems must monitor 
each calendar quarter that the system provides water to the public, 
except for seasonal systems or as provided under paragraphs (c) through 
(h) and (j) of this section. Seasonal systems must meet the monitoring 
requirements of paragraph (i) of this section.
    (c) Transition to subpart Y. (1) Systems, including seasonal 
systems, must continue to monitor according to the total coliform 
monitoring schedules under Sec.  141.21 that were in effect on March 31, 
2016, unless any of the conditions for increased monitoring in paragraph 
(f) of this section are triggered on or after April 1, 2016, or unless 
otherwise directed by the State.
    (2) Beginning April 1, 2016, the State must perform a special 
monitoring evaluation during each sanitary survey to review the status 
of the system, including the distribution system, to determine whether 
the system is on an appropriate monitoring schedule. After the State has 
performed the special monitoring evaluation during each sanitary survey, 
the State may modify the system's monitoring schedule, as necessary, or 
it may allow the system to stay on its existing monitoring schedule, 
consistent with the provisions of this section. The State may not allow 
systems to begin less frequent monitoring under the special monitoring 
evaluation unless the system has already met the applicable criteria for 
less frequent monitoring in this section. For seasonal systems on 
quarterly or annual monitoring, this evaluation must include review of 
the approved sample siting plan, which must designate the time period(s) 
for monitoring based on site-specific considerations (e.g., during 
periods of highest demand or highest vulnerability to contamination). 
The seasonal system

[[Page 726]]

must collect compliance samples during these time periods.
    (d) Annual site visits. Beginning no later than calendar year 2017, 
systems on annual monitoring, including seasonal systems, must have an 
initial and recurring annual site visit by the State that is equivalent 
to a Level 2 assessment or an annual voluntary Level 2 assessment that 
meets the criteria in Sec.  141.859(b) to remain on annual monitoring. 
The periodic required sanitary survey may be used to meet the 
requirement for an annual site visit for the year in which the sanitary 
survey was completed.
    (e) Criteria for annual monitoring. Beginning April 1, 2016, the 
State may reduce the monitoring frequency for a well-operated ground 
water system from quarterly routine monitoring to no less than annual 
monitoring, if the system demonstrates that it meets the criteria for 
reduced monitoring in paragraphs (e)(1) through (e)(3) of this section, 
except for a system that has been on increased monitoring under the 
provisions of paragraph (f) of this section. A system on increased 
monitoring under paragraph (f) of this section must meet the provisions 
of paragraph (g) of this section to go to quarterly monitoring and must 
meet the provisions of paragraph (h) of this section to go to annual 
monitoring.
    (1) The system has a clean compliance history for a minimum of 12 
months;
    (2) The most recent sanitary survey shows that the system is free of 
sanitary defects or has corrected all identified sanitary defects, has a 
protected water source, and meets approved construction standards; and
    (3) The State has conducted an annual site visit within the last 12 
months and the system has corrected all identified sanitary defects. The 
system may substitute a Level 2 assessment that meets the criteria in 
Sec.  141.859(b) for the State annual site visit.
    (f) Increased monitoring requirements for systems on quarterly or 
annual monitoring. A system on quarterly or annual monitoring that 
experiences any of the events identified in paragraphs (f)(1) through 
(f)(4) of this section must begin monthly monitoring the month following 
the event. A system on annual monitoring that experiences the event 
identified in paragraphs (f)(5) of this section must begin quarterly 
monitoring the quarter following the event. The system must continue 
monthly or quarterly monitoring until the requirements in paragraph (g) 
of this section for quarterly monitoring or paragraph (h) of this 
section for annual monitoring are met. A system on monthly monitoring 
for reasons other than those identified in paragraphs (f)(1) through 
(f)(4) of this section is not considered to be on increased monitoring 
for the purposes of paragraphs (g) and (h) of this section.
    (1) The system triggers a Level 2 assessment or two Level 1 
assessments under the provisions of Sec.  141.859 in a rolling 12-month 
period.
    (2) The system has an E. coli MCL violation.
    (3) The system has a coliform treatment technique violation.
    (4) The system has two subpart Y monitoring violations or one 
subpart Y monitoring violation and one Level 1 assessment under the 
provisions of Sec.  141.859 in a rolling 12-month period for a system on 
quarterly monitoring.
    (5) The system has one subpart Y monitoring violation for a system 
on annual monitoring.
    (g) Requirements for returning to quarterly monitoring. The State 
may reduce the monitoring frequency for a system on monthly monitoring 
triggered under paragraph (f) of this section to quarterly monitoring if 
the system meets the criteria in paragraphs (g)(1) and (g)(2) of this 
section.
    (1) Within the last 12 months, the system must have a completed 
sanitary survey or a site visit by the State or a voluntary Level 2 
assessment by a party approved by the State, be free of sanitary 
defects, and have a protected water source; and
    (2) The system must have a clean compliance history for a minimum of 
12 months.
    (h) Requirements for systems on increased monitoring to qualify for 
annual monitoring. The State may reduce the monitoring frequency for a 
system on increased monitoring under paragraph (f) of this section if 
the system meets

[[Page 727]]

the criteria in paragraph (g) of this section plus the criteria in 
paragraphs (h)(1) and (h)(2) of this section.
    (1) An annual site visit by the State and correction of all 
identified sanitary defects. The system may substitute a voluntary Level 
2 assessment by a party approved by the State for the State annual site 
visit in any given year.
    (2) The system must have in place or adopt one or more additional 
enhancements to the water system barriers to contamination in paragraphs 
(h)(2)(i) through (h)(2)(v) of this section.
    (i) Cross connection control, as approved by the State.
    (ii) An operator certified by an appropriate State certification 
program or regular visits by a circuit rider certified by an appropriate 
State certification program.
    (iii) Continuous disinfection entering the distribution system and a 
residual in the distribution system in accordance with criteria 
specified by the State.
    (iv) Demonstration of maintenance of at least a 4-log removal or 
inactivation of viruses as provided for under Sec.  141.403(b)(3).
    (v) Other equivalent enhancements to water system barriers as 
approved by the State.
    (i) Seasonal systems. (1) Beginning April 1, 2016, all seasonal 
systems must demonstrate completion of a State-approved start-up 
procedure, which may include a requirement for startup sampling prior to 
serving water to the public.
    (2) A seasonal system must monitor every month that it is in 
operation unless it meets the criteria in paragraphs (i)(2)(i) through 
(iii) of this section to be eligible for monitoring less frequently than 
monthly beginning April 1, 2016, except as provided under paragraph (c) 
of this section.
    (i) Seasonal systems monitoring less frequently than monthly must 
have an approved sample siting plan that designates the time period for 
monitoring based on site-specific considerations (e.g., during periods 
of highest demand or highest vulnerability to contamination). Seasonal 
systems must collect compliance samples during this time period.
    (ii) To be eligible for quarterly monitoring, the system must meet 
the criteria in paragraph (g) of this section.
    (iii) To be eligible for annual monitoring, the system must meet the 
criteria under paragraph (h) of this section.
    (3) The State may exempt any seasonal system from some or all of the 
requirements for seasonal systems if the entire distribution system 
remains pressurized during the entire period that the system is not 
operating, except that systems that monitor less frequently than monthly 
must still monitor during the vulnerable period designated by the State.
    (j) Additional routine monitoring the month following a total 
coliform-positive sample. Systems collecting samples on a quarterly or 
annual frequency must conduct additional routine monitoring the month 
following one or more total coliform-positive samples (with or without a 
Level 1 treatment technique trigger). Systems must collect at least 
three routine samples during the next month, except that the State may 
waive this requirement if the conditions of paragraph (j)(1), (2), or 
(3) of this section are met. Systems may either collect samples at 
regular time intervals throughout the month or may collect all required 
routine samples on a single day if samples are taken from different 
sites. Systems must use the results of additional routine samples in 
coliform treatment technique trigger calculations under Sec.  
141.859(a).
    (1) The State may waive the requirement to collect three routine 
samples the next month in which the system provides water to the public 
if the State, or an agent approved by the State, performs a site visit 
before the end of the next month in which the system provides water to 
the public. Although a sanitary survey need not be performed, the site 
visit must be sufficiently detailed to allow the State to determine 
whether additional monitoring and/or any corrective action is needed. 
The State cannot approve an employee of the system to perform this site 
visit, even if the employee is an agent approved by the State to perform 
sanitary surveys.
    (2) The State may waive the requirement to collect three routine 
samples

[[Page 728]]

the next month in which the system provides water to the public if the 
State has determined why the sample was total coliform-positive and has 
established that the system has corrected the problem or will correct 
the problem before the end of the next month in which the system serves 
water to the public. In this case, the State must document this decision 
to waive the following month's additional monitoring requirement in 
writing, have it approved and signed by the supervisor of the State 
official who recommends such a decision, and make this document 
available to the EPA and public. The written documentation must describe 
the specific cause of the total coliform-positive sample and what action 
the system has taken and/or will take to correct this problem.
    (3) The State may not waive the requirement to collect three 
additional routine samples the next month in which the system provides 
water to the public solely on the grounds that all repeat samples are 
total coliform-negative. If the State determines that the system has 
corrected the contamination problem before the system takes the set of 
repeat samples required in Sec.  141.858, and all repeat samples were 
total coliform-negative, the State may waive the requirement for 
additional routine monitoring the next month.



Sec.  141.855  Routine monitoring requirements for community water systems 
serving 1,000 or fewer people using only ground water.

    (a) General. (1) The provisions of this section apply to community 
water systems using only ground water (except ground water under the 
direct influence of surface water, as defined in Sec.  141.2) and 
serving 1,000 or fewer people.
    (2) Following any total coliform-positive sample taken under the 
provisions of this section, systems must comply with the repeat 
monitoring requirements and E. coli analytical requirements in Sec.  
141.858.
    (3) Once all monitoring required by this section and Sec.  141.858 
for a calendar month has been completed, systems must determine whether 
any coliform treatment technique triggers specified in Sec.  141.859 
have been exceeded. If any trigger has been exceeded, systems must 
complete assessments as required by Sec.  141.859.
    (b) Monitoring frequency for total coliforms. The monitoring 
frequency for total coliforms is one sample/month, except as provided 
for under paragraphs (c) through (f) of this section.
    (c) Transition to subpart Y. (1) All systems must continue to 
monitor according to the total coliform monitoring schedules under Sec.  
141.21 that were in effect on March 31, 2016, unless any of the 
conditions in paragraph (e) of this section are triggered on or after 
April 1, 2016, or unless otherwise directed by the State.
    (2) Beginning April 1, 2016, the State must perform a special 
monitoring evaluation during each sanitary survey to review the status 
of the system, including the distribution system, to determine whether 
the system is on an appropriate monitoring schedule. After the State has 
performed the special monitoring evaluation during each sanitary survey, 
the State may modify the system's monitoring schedule, as necessary, or 
it may allow the system to stay on its existing monitoring schedule, 
consistent with the provisions of this section. The State may not allow 
systems to begin less frequent monitoring under the special monitoring 
evaluation unless the system has already met the applicable criteria for 
less frequent monitoring in this section.
    (d) Criteria for reduced monitoring. (1) The State may reduce the 
monitoring frequency from monthly monitoring to no less than quarterly 
monitoring if the system is in compliance with State-certified operator 
provisions and demonstrates that it meets the criteria in paragraphs 
(d)(1)(i) through (d)(1)(iii) of this section. A system that loses its 
certified operator must return to monthly monitoring the month following 
that loss.
    (i) The system has a clean compliance history for a minimum of 12 
months.
    (ii) The most recent sanitary survey shows the system is free of 
sanitary defects (or has an approved plan and schedule to correct them 
and is in compliance with the plan and the schedule), has a protected 
water source and

[[Page 729]]

meets approved construction standards.
    (iii) The system meets at least one of the following criteria:
    (A) An annual site visit by the State that is equivalent to a Level 
2 assessment or an annual Level 2 assessment by a party approved by the 
State and correction of all identified sanitary defects (or an approved 
plan and schedule to correct them and is in compliance with the plan and 
schedule).
    (B) Cross connection control, as approved by the State.
    (C) Continuous disinfection entering the distribution system and a 
residual in the distribution system in accordance with criteria 
specified by the State.
    (D) Demonstration of maintenance of at least a 4-log removal or 
inactivation of viruses as provided for under Sec.  141.403(b)(3).
    (E) Other equivalent enhancements to water system barriers as 
approved by the State.
    (2) [Reserved]
    (e) Return to routine monthly monitoring requirements. Systems on 
quarterly monitoring that experience any of the events in paragraphs 
(e)(1) through (e)(4) of this section must begin monthly monitoring the 
month following the event. The system must continue monthly monitoring 
until it meets the reduced monitoring requirements in paragraph (d) of 
this section.
    (1) The system triggers a Level 2 assessment or two Level 1 
assessments in a rolling 12-month period.
    (2) The system has an E. coli MCL violation.
    (3) The system has a coliform treatment technique violation.
    (4) The system has two subpart Y monitoring violations in a rolling 
12-month period.
    (f) Additional routine monitoring the month following a total 
coliform-positive sample. Systems collecting samples on a quarterly 
frequency must conduct additional routine monitoring the month following 
one or more total coliform-positive samples (with or without a Level 1 
treatment technique trigger). Systems must collect at least three 
routine samples during the next month, except that the State may waive 
this requirement if the conditions of paragraph (f)(1), (2), or (3) of 
this section are met. Systems may either collect samples at regular time 
intervals throughout the month or may collect all required routine 
samples on a single day if samples are taken from different sites. 
Systems must use the results of additional routine samples in coliform 
treatment technique trigger calculations.
    (1) The State may waive the requirement to collect three routine 
samples the next month in which the system provides water to the public 
if the State, or an agent approved by the State, performs a site visit 
before the end of the next month in which the system provides water to 
the public. Although a sanitary survey need not be performed, the site 
visit must be sufficiently detailed to allow the State to determine 
whether additional monitoring and/or any corrective action is needed. 
The State cannot approve an employee of the system to perform this site 
visit, even if the employee is an agent approved by the State to perform 
sanitary surveys.
    (2) The State may waive the requirement to collect three routine 
samples the next month in which the system provides water to the public 
if the State has determined why the sample was total coliform-positive 
and has established that the system has corrected the problem or will 
correct the problem before the end of the next month in which the system 
serves water to the public. In this case, the State must document this 
decision to waive the following month's additional monitoring 
requirement in writing, have it approved and signed by the supervisor of 
the State official who recommends such a decision, and make this 
document available to the EPA and the public. The written documentation 
must describe the specific cause of the total coliform-positive sample 
and what action the system has taken and/or will take to correct this 
problem.
    (3) The State may not waive the requirement to collect three 
additional routine samples the next month in which the system provides 
water to the public solely on the grounds that all repeat samples are 
total coliform-negative. If the State determines that the

[[Page 730]]

system has corrected the contamination problem before the system takes 
the set of repeat samples required in Sec.  141.858, and all repeat 
samples were total coliform-negative, the State may waive the 
requirement for additional routine monitoring the next month.



Sec.  141.856  Routine monitoring requirements for subpart H public 
water systems serving 1,000 or fewer people.

    (a) General. (1) The provisions of this section apply to subpart H 
public water systems of this part serving 1,000 or fewer people.
    (2) Following any total coliform-positive sample taken under the 
provisions of this section, systems must comply with the repeat 
monitoring requirements and E. coli analytical requirements in Sec.  
141.858.
    (3) Once all monitoring required by this section and Sec.  141.858 
for a calendar month has been completed, systems must determine whether 
any coliform treatment technique triggers specified in Sec.  141.859 
have been exceeded. If any trigger has been exceeded, systems must 
complete assessments as required by Sec.  141.859.
    (4) Seasonal systems. (i) Beginning April 1, 2016, all seasonal 
systems must demonstrate completion of a State-approved start-up 
procedure, which may include a requirement for start-up sampling prior 
to serving water to the public.
    (ii) The State may exempt any seasonal system from some or all of 
the requirements for seasonal systems if the entire distribution system 
remains pressurized during the entire period that the system is not 
operating.
    (b) Routine monitoring frequency for total coliforms. Subpart H 
systems of this part (including consecutive systems) must monitor 
monthly. Systems may not reduce monitoring.
    (c) Unfiltered subpart H systems. A subpart H system of this part 
that does not practice filtration in compliance with subparts H, P, T, 
and W must collect at least one total coliform sample near the first 
service connection each day the turbidity level of the source water, 
measured as specified in Sec.  141.74(b)(2), exceeds 1 NTU. When one or 
more turbidity measurements in any day exceed 1 NTU, the system must 
collect this coliform sample within 24 hours of the first exceedance, 
unless the State determines that the system, for logistical reasons 
outside the system's control, cannot have the sample analyzed within 30 
hours of collection and identifies an alternative sample collection 
schedule. Sample results from this coliform monitoring must be included 
in determining whether the coliform treatment technique trigger in Sec.  
141.859 has been exceeded.



Sec.  141.857  Routine monitoring requirements for public water systems 
serving more than 1,000 people.

    (a) General. (1) The provisions of this section apply to public 
water systems serving more than 1,000 persons.
    (2) Following any total coliform-positive sample taken under the 
provisions of this section, systems must comply with the repeat 
monitoring requirements and E. coli analytical requirements in Sec.  
141.858.
    (3) Once all monitoring required by this section and Sec.  141.858 
for a calendar month has been completed, systems must determine whether 
any coliform treatment technique triggers specified in Sec.  141.859 
have been exceeded. If any trigger has been exceeded, systems must 
complete assessments as required by Sec.  141.859.
    (4) Seasonal systems. (i) Beginning April 1, 2016, all seasonal 
systems must demonstrate completion of a State-approved start-up 
procedure, which may include a requirement for start-up sampling prior 
to serving water to the public.
    (ii) The State may exempt any seasonal system from some or all of 
the requirements for seasonal systems if the entire distribution system 
remains pressurized during the entire period that the system is not 
operating.
    (b) Monitoring frequency for total coliforms. The monitoring 
frequency for total coliforms is based on the population served by the 
system, as follows:

[[Page 731]]



  Total Coliform Monitoring Frequency for Public Water Systems Serving
                         More Than 1,000 People
------------------------------------------------------------------------
                                                       Minimum number of
                  Population served                    samples per month
------------------------------------------------------------------------
1,001 to 2,500.......................................                  2
2,501 to 3,300.......................................                  3
3,301 to 4,100.......................................                  4
4,101 to 4,900.......................................                  5
4,901 to 5,800.......................................                  6
5,801 to 6,700.......................................                  7
6,701 to 7,600.......................................                  8
7,601 to 8,500.......................................                  9
8,501 to 12,900......................................                 10
12,901 to 17,200.....................................                 15
17,201 to 21,500.....................................                 20
21,501 to 25,000.....................................                 25
25,001 to 33,000.....................................                 30
33,001 to 41,000.....................................                 40
41,001 to 50,000.....................................                 50
50,001 to 59,000.....................................                 60
59,001 to 70,000.....................................                 70
70,001 to 83,000.....................................                 80
83,001 to 96,000.....................................                 90
96,001 to 130,000....................................                100
130,001 to 220,000...................................                120
220,001 to 320,000...................................                150
320,001 to 450,000...................................                180
450,001 to 600,000...................................                210
600,001 to 780,000...................................                240
780,001 to 970,000...................................                270
970,001 to 1,230,000.................................                300
1,230,001 to 1,520,000...............................                330
1,520,001 to 1,850,000...............................                360
1,850,001 to 2,270,000...............................                390
2,270,001 to 3,020,000...............................                420
3,020,001 to 3,960,000...............................                450
3,960,001 or more....................................                480
------------------------------------------------------------------------

    (c) Unfiltered subpart H systems. A subpart H system of this part 
that does not practice filtration in compliance with subparts H, P, T, 
and W must collect at least one total coliform sample near the first 
service connection each day the turbidity level of the source water, 
measured as specified in Sec.  141.74(b)(2), exceeds 1 NTU. When one or 
more turbidity measurements in any day exceed 1 NTU, the system must 
collect this coliform sample within 24 hours of the first exceedance, 
unless the State determines that the system, for logistical reasons 
outside the system's control, cannot have the sample analyzed within 30 
hours of collection and identifies an alternative sample collection 
schedule. Sample results from this coliform monitoring must be included 
in determining whether the coliform treatment technique trigger in Sec.  
141.859 has been exceeded.
    (d) Reduced monitoring. Systems may not reduce monitoring, except 
for non-community water systems using only ground water (and not ground 
water under the direct influence of surface water) serving 1,000 or 
fewer people in some months and more than 1,000 persons in other months. 
In months when more than 1,000 persons are served, the systems must 
monitor at the frequency specified in paragraph (a) of this section. In 
months when 1,000 or fewer people are served, the State may reduce the 
monitoring frequency, in writing, to a frequency allowed under Sec.  
141.854 for a similarly situated system that always serves 1,000 or 
fewer people, taking into account the provisions in Sec.  141.854(e) 
through (g).



Sec.  141.858  Repeat monitoring and E. coli requirements.

    (a) Repeat monitoring. (1) If a sample taken under Sec. Sec.  
141.854 though 141.857 is total coliform-positive, the system must 
collect a set of repeat samples within 24 hours of being notified of the 
positive result. The system must collect no fewer than three repeat 
samples for each total coliform-positive sample found. The State may 
extend the 24-hour limit on a case-by-case basis if the system has a 
logistical problem in collecting the repeat samples within 24 hours that 
is beyond its control. Alternatively, the State may implement criteria 
for the system to use in lieu of case-by-case extensions. In the case of 
an extension, the State must specify how much time the system has to 
collect the repeat samples. The State cannot waive the requirement for a 
system to collect repeat samples in paragraphs (a)(1) through (a)(3) of 
this section.
    (2) The system must collect all repeat samples on the same day, 
except that the State may allow a system with a single service 
connection to collect the required set of repeat samples over a three-
day period or to collect a larger volume repeat sample(s) in one or more 
sample containers of any size, as long as the total volume collected is 
at least 300 ml.
    (3) The system must collect an additional set of repeat samples in 
the manner specified in paragraphs (a)(1) through (a)(3) of this section 
if one or more repeat samples in the current set of repeat samples is 
total coliform-positive. The system must collect the additional set of 
repeat samples within

[[Page 732]]

24 hours of being notified of the positive result, unless the State 
extends the limit as provided in paragraph (a)(1) of this section. The 
system must continue to collect additional sets of repeat samples until 
either total coliforms are not detected in one complete set of repeat 
samples or the system determines that a coliform treatment technique 
trigger specified in Sec.  141.859(a) has been exceeded as a result of a 
repeat sample being total coliform-positive and notifies the State. If a 
trigger identified in Sec.  141.859 is exceeded as a result of a routine 
sample being total coliform-positive, systems are required to conduct 
only one round of repeat monitoring for each total coliform-positive 
routine sample.
    (4) After a system collects a routine sample and before it learns 
the results of the analysis of that sample, if it collects another 
routine sample(s) from within five adjacent service connections of the 
initial sample, and the initial sample, after analysis, is found to 
contain total coliforms, then the system may count the subsequent 
sample(s) as a repeat sample instead of as a routine sample.
    (5) Results of all routine and repeat samples taken under Sec. Sec.  
141.854 through 141.858 not invalidated by the State must be used to 
determine whether a coliform treatment technique trigger specified in 
Sec.  141.859 has been exceeded.
    (b) Escherichia coli (E. coli) testing. (1) If any routine or repeat 
sample is total coliform-positive, the system must analyze that total 
coliform-positive culture medium to determine if E. coli are present. If 
E. coli are present, the system must notify the State by the end of the 
day when the system is notified of the test result, unless the system is 
notified of the result after the State office is closed and the State 
does not have either an after-hours phone line or an alternative 
notification procedure, in which case the system must notify the State 
before the end of the next business day.
    (2) The State has the discretion to allow a system, on a case-by-
case basis, to forgo E. coli testing on a total coliform-positive sample 
if that system assumes that the total coliform-positive sample is E. 
coli-positive. Accordingly, the system must notify the State as 
specified in paragraph (b)(1) of this section and the provisions of 
Sec.  141.63(c) apply.



Sec.  141.859  Coliform treatment technique triggers and assessment 
requirements for protection against potential fecal contamination.

    (a) Treatment technique triggers. Systems must conduct assessments 
in accordance with paragraph (b) of this section after exceeding 
treatment technique triggers in paragraphs (a)(1) and (a)(2) of this 
section.
    (1) Level 1 treatment technique triggers.
    (i) For systems taking 40 or more samples per month, the system 
exceeds 5.0% total coliform-positive samples for the month.
    (ii) For systems taking fewer than 40 samples per month, the system 
has two or more total coliform-positive samples in the same month.
    (iii) The system fails to take every required repeat sample after 
any single total coliform-positive sample.
    (2) Level 2 treatment technique triggers.
    (i) An E. coli MCL violation, as specified in Sec.  141.860(a).
    (ii) A second Level 1 trigger as defined in paragraph (a)(1) of this 
section, within a rolling 12-month period, unless the State has 
determined a likely reason that the samples that caused the first Level 
1 treatment technique trigger were total coliform-positive and has 
established that the system has corrected the problem.
    (iii) For systems with approved annual monitoring, a Level 1 trigger 
in two consecutive years.
    (b) Requirements for assessments. (1) Systems must ensure that Level 
1 and 2 assessments are conducted in order to identify the possible 
presence of sanitary defects and defects in distribution system coliform 
monitoring practices. Level 2 assessments must be conducted by parties 
approved by the State.
    (2) When conducting assessments, systems must ensure that the 
assessor evaluates minimum elements that include review and 
identification of inadequacies in sample sites; sampling protocol; 
sample processing; atypical events that could affect distributed water 
quality or indicate that distributed water quality was impaired;

[[Page 733]]

changes in distribution system maintenance and operation that could 
affect distributed water quality (including water storage); source and 
treatment considerations that bear on distributed water quality, where 
appropriate (e.g., small ground water systems); and existing water 
quality monitoring data. The system must conduct the assessment 
consistent with any State directives that tailor specific assessment 
elements with respect to the size and type of the system and the size, 
type, and characteristics of the distribution system.
    (3) Level 1 assessments. A system must conduct a Level 1 assessment 
consistent with State requirements if the system exceeds one of the 
treatment technique triggers in paragraph (a)(1) of this section.
    (i) The system must complete a Level 1 assessment as soon as 
practical after any trigger in paragraph (a)(1) of this section. In the 
completed assessment form, the system must describe sanitary defects 
detected, corrective actions completed, and a proposed timetable for any 
corrective actions not already completed. The assessment form may also 
note that no sanitary defects were identified. The system must submit 
the completed Level 1 assessment form to the State within 30 days after 
the system learns that it has exceeded a trigger.
    (ii) If the State reviews the completed Level 1 assessment and 
determines that the assessment is not sufficient (including any proposed 
timetable for any corrective actions not already completed), the State 
must consult with the system. If the State requires revisions after 
consultation, the system must submit a revised assessment form to the 
State on an agreed-upon schedule not to exceed 30 days from the date of 
the consultation.
    (iii) Upon completion and submission of the assessment form by the 
system, the State must determine if the system has identified a likely 
cause for the Level 1 trigger and, if so, establish that the system has 
corrected the problem, or has included a schedule acceptable to the 
State for correcting the problem.
    (4) Level 2 assessments. A system must ensure that a Level 2 
assessment consistent with State requirements is conducted if the system 
exceeds one of the treatment technique triggers in paragraph (a)(2) of 
this section. The system must comply with any expedited actions or 
additional actions required by the State in the case of an E. coli MCL 
violation.
    (i) The system must ensure that a Level 2 assessment is completed by 
the State or by a party approved by the State as soon as practical after 
any trigger in paragraph (a)(2) of this section. The system must submit 
a completed Level 2 assessment form to the State within 30 days after 
the system learns that it has exceeded a trigger. The assessment form 
must describe sanitary defects detected, corrective actions completed, 
and a proposed timetable for any corrective actions not already 
completed. The assessment form may also note that no sanitary defects 
were identified.
    (ii) The system may conduct Level 2 assessments if the system has 
staff or management with the certification or qualifications specified 
by the State unless otherwise directed by the State.
    (iii) If the State reviews the completed Level 2 assessment and 
determines that the assessment is not sufficient (including any proposed 
timetable for any corrective actions not already completed), the State 
must consult with the system. If the State requires revisions after 
consultation, the system must submit a revised assessment form to the 
State on an agreed-upon schedule not to exceed 30 days.
    (iv) Upon completion and submission of the assessment form by the 
system, the State must determine if the system has identified a likely 
cause for the Level 2 trigger and determine whether the system has 
corrected the problem, or has included a schedule acceptable to the 
State for correcting the problem.
    (c) Corrective action. Systems must correct sanitary defects found 
through either Level 1 or 2 assessments conducted under paragraph (b) of 
this section. For corrections not completed by the time of submission of 
the assessment form, the system must complete the corrective action(s) 
in compliance with a timetable approved by the State in consultation 
with the system. The

[[Page 734]]

system must notify the State when each scheduled corrective action is 
completed.
    (d) Consultation. At any time during the assessment or corrective 
action phase, either the water system or the State may request a 
consultation with the other party to determine the appropriate actions 
to be taken. The system may consult with the State on all relevant 
information that may impact on its ability to comply with a requirement 
of this subpart, including the method of accomplishment, an appropriate 
timeframe, and other relevant information.



Sec.  141.860  Violations.

    (a) E. coli MCL Violation. A system is in violation of the MCL for 
E. coli when any of the conditions identified in paragraphs (a)(1) 
through (a)(4) of this section occur.
    (1) The system has an E. coli-positive repeat sample following a 
total coliform-positive routine sample.
    (2) The system has a total coliform-positive repeat sample following 
an E. coli-positive routine sample.
    (3) The system fails to take all required repeat samples following 
an E. coli-positive routine sample.
    (4) The system fails to test for E. coli when any repeat sample 
tests positive for total coliform.
    (b) Treatment technique violation. (1) A treatment technique 
violation occurs when a system exceeds a treatment technique trigger 
specified in Sec.  141.859(a) and then fails to conduct the required 
assessment or corrective actions within the timeframe specified in Sec.  
141.859(b) and (c).
    (2) A treatment technique violation occurs when a seasonal system 
fails to complete a State-approved start-up procedure prior to serving 
water to the public.
    (c) Monitoring violations. (1) Failure to take every required 
routine or additional routine sample in a compliance period is a 
monitoring violation.
    (2) Failure to analyze for E. coli following a total coliform-
positive routine sample is a monitoring violation.
    (d) Reporting violations. (1) Failure to submit a monitoring report 
or completed assessment form after a system properly conducts monitoring 
or assessment in a timely manner is a reporting violation.
    (2) Failure to notify the State following an E. coli-positive sample 
as required by Sec.  141.858(b)(1) in a timely manner is a reporting 
violation.
    (3) Failure to submit certification of completion of State-approved 
start-up procedure by a seasonal system is a reporting violation.



Sec.  141.861  Reporting and recordkeeping.

    (a) Reporting--(1) E. coli. (i) A system must notify the State by 
the end of the day when the system learns of an E. coli MCL violation, 
unless the system learns of the violation after the State office is 
closed and the State does not have either an after-hours phone line or 
an alternative notification procedure, in which case the system must 
notify the State before the end of the next business day, and notify the 
public in accordance with subpart Q of this part.
    (ii) A system must notify the State by the end of the day when the 
system is notified of an E. coli-positive routine sample, unless the 
system is notified of the result after the State office is closed and 
the State does not have either an after-hours phone line or an 
alternative notification procedure, in which case the system must notify 
the State before the end of the next business day.
    (2) A system that has violated the treatment technique for coliforms 
in Sec.  141.859 must report the violation to the State no later than 
the end of the next business day after it learns of the violation, and 
notify the public in accordance with subpart Q of this part.
    (3) A system required to conduct an assessment under the provisions 
of Sec.  141.859 of this part must submit the assessment report within 
30 days. The system must notify the State in accordance with Sec.  
141.859(c) when each scheduled corrective action is completed for 
corrections not completed by the time of submission of the assessment 
form.
    (4) A system that has failed to comply with a coliform monitoring 
requirement must report the monitoring violation to the State within 10 
days

[[Page 735]]

after the system discovers the violation, and notify the public in 
accordance with subpart Q of this part.
    (5) A seasonal system must certify, prior to serving water to the 
public, that it has complied with the State-approved start-up procedure.
    (b) Recordkeeping. (1) The system must maintain any assessment form, 
regardless of who conducts the assessment, and documentation of 
corrective actions completed as a result of those assessments, or other 
available summary documentation of the sanitary defects and corrective 
actions taken under Sec.  141.859 for State review. This record must be 
maintained by the system for a period not less than five years after 
completion of the assessment or corrective action.
    (2) The system must maintain a record of any repeat sample taken 
that meets State criteria for an extension of the 24-hour period for 
collecting repeat samples as provided for under Sec.  141.858(a)(1) of 
this part.

[78 FR 10354, Feb. 13, 2013, as amended at 79 FR 10670, Feb. 26, 2014]



PART 142_NATIONAL PRIMARY DRINKING WATER REGULATIONS IMPLEMENTATION--
Table of Contents



                      Subpart A_General Provisions

Sec.
142.1 Applicability.
142.2 Definitions.
142.3 Scope.
142.4 State and local authority.

              Subpart B_Primary Enforcement Responsibility

142.10 Requirements for a determination of primary enforcement 
          responsibility.
142.11 Initial determination of primary enforcement responsibility.
142.12 Revision of State programs.
142.13 Public hearing.
142.14 Records kept by States.
142.15 Reports by States.
142.16 Special primacy requirements.
142.17 Review of State programs and procedures for withdrawal of 
          approved primacy programs.
142.18 EPA review of State monitoring determinations.
142.19 EPA review of State implementation of national primary drinking 
          water regulations for lead and copper.

        Subpart C_Review of State-Issued Variances and Exemptions

142.20 State-issued variances and exemptions under Section 1415(a) and 
          Section 1416 of the Act.
142.21 State consideration of a variance or exemption request.
142.22 Review of State variances, exemptions and schedules.
142.23 Notice to State.
142.24 Administrator's rescission.

                      Subpart D_Federal Enforcement

142.30 Failure by State to assure enforcement.
142.31 [Reserved]
142.32 Petition for public hearing.
142.33 Public hearing.
142.34 Entry and inspection of public water systems.

Subpart E_Variances Issued by the Administrator Under Section 1415(a) of 
                                 the Act

142.40 Requirements for a variance.
142.41 Variance request.
142.42 Consideration of a variance request.
142.43 Disposition of a variance request.
142.44 Public hearings on variances and schedules.
142.45 Action after hearing.
142.46 Alternative treatment techniques.

            Subpart F_Exemptions Issued by the Administrator

142.50 Requirements for an exemption.
142.51 Exemption request.
142.52 Consideration of an exemption request.
142.53 Disposition of an exemption request.
142.54 Public hearings on exemption schedules.
142.55 Final schedule.
142.56 Extension of date for compliance.
142.57 Bottled water, point-of-use, and point-of-entry devices.

  Subpart G_Identification of Best Technology, Treatment Techniques or 
                     Other Means Generally Available

142.60 Variances from the maximum contaminant level for total 
          trihalomethanes.
142.61 Variances from the maximum contaminant level for fluoride.
142.62 Variances and exemptions from the maximum contaminant levels for 
          organic and inorganic chemicals.
142.63 Variances and exemptions from the maximum contaminant level for 
          total coliforms.

[[Page 736]]

142.64 Variances and exemptions from the requirements of part 141, 
          subpart H--Filtration and Disinfection.
142.65 Variances and exemptions from the maximum contaminant levels for 
          radionuclides.

                         Subpart H_Indian Tribes

142.72 Requirements for Tribal eligibility.
142.76 Request by an Indian Tribe for a determination of eligibility.
142.78 Procedure for processing an Indian Tribe's application.

   Subpart I_Administrator's Review of State Decisions that Implement 
               Criteria Under Which Filtration Is Required

142.80 Review procedures.
142.81 Notice to the State.

Subpart J [Reserved]

                  Subpart K_Variances for Small System

                           General Provisions

142.301 What is a small system variance?
142.302 Who can issue a small system variance?
142.303 Which size public water systems can receive a small system 
          variance?
142.304 For which of the regulatory requirements is a small system 
          variance available?
142.305 When can a small system variance be granted by a State?

               Review of Small System Variance Application

142.306 What are the responsibilities of the public water system, State 
          and the Administrator in ensuring that sufficient information 
          is available and for evaluation of a small system variance 
          application?
142.307 What terms and conditions must be included in a small system 
          variance?

                          Public Participation

142.308 What public notice is required before a State or the 
          Administrator proposes to issue a small system variance?
142.309 What are the public meeting requirements associated with the 
          proposal of a small system variance?
142.310 How can a person served by the public water system obtain EPA 
          review of a State proposed small system variance?

            EPA Review and Approval of Small System Variances

142.311 What procedures allow for the Administrator to object to a 
          proposed small system variance or overturn a granted small 
          system variance for a public water system serving 3,300 or 
          fewer persons?
142.312 What EPA action is necessary when a State proposes to grant a 
          small system variance to a public water system serving a 
          population of more than 3,300 and fewer than 10,000 persons?
142.313 How will the Administrator review a State's program under this 
          subpart?

    Authority: 42 U.S.C. 300f, 300g-1, 300g-2, 300g-3, 300g-4, 300g-5, 
300g-6, 300j-4, 300j-9, and 300j-11.

    Source: 41 FR 2918, Jan. 20, 1976, unless otherwise noted.



                      Subpart A_General Provisions



Sec.  142.1  Applicability.

    This part sets forth, pursuant to sections 1413 through 1416, 1445, 
and 1450 of the Public Health Service Act, as amended by the Safe 
Drinking Water Act, Public Law 93-523, regulations for the 
implementation and enforcement of the national primary drinking water 
regulations contained in part 141 of this chapter.



Sec.  142.2  Definitions.

    As used in this part, and except as otherwise specifically provided:
    Act means the Public Health Service Act.
    Administrator means the Administrator of the United States 
Environmental Protection Agency or his authorized representative.
    Agency means the United States Environmental Protection Agency.
    Approved State primacy program consists of those program elements 
listed in Sec.  142.11(a) that were submitted with the initial State 
application for primary enforcement authority and approved by the EPA 
Administrator and all State program revisions thereafter that were 
approved by the EPA Administrator.
    Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    Federal agency means any department, agency, or instrumentality of 
the United States.
    Indian Tribe means any Indian Tribe having a Federally recognized 
governing body carrying out substantial governmental duties and powers 
over a defined area.

[[Page 737]]

    Interstate Agency means an agency of two or more States established 
by or under an agreement or compact approved by the Congress, or any 
other agency of two or more States or Indian Tribes having substantial 
powers or duties pertaining to the control of pollution as determined 
and approved by the Administrator.
    Maximum contaminant level means the maximum permissible level of a 
contaminant in water which is delivered to the free flowing outlet of 
the ultimate user of a public water system; except in the case of 
turbidity where the maximum permissible level is measured at the point 
of entry to the distribution system. Contaminants added to the water 
under circumstances controlled by the user, except for those resulting 
from corrosion of piping and plumbing caused by water quality are 
excluded from this definition.
    Municipality means a city, town, or other public body created by or 
pursuant to State law, or an Indian Tribe which does not meet the 
requirements of subpart H of this part.
    National primary drinking water regulation means any primary 
drinking water regulation contained in part 141 of this chapter.
    Person means an individual; corporation; company; association; 
partnership; municipality; or State, federal, or Tribal agency.
    Primary enforcement responsibility means the primary responsibility 
for administration and enforcement of primary drinking water regulations 
and related requirements applicable to public water systems within a 
State.
    Public water system or PWS means a system for the provision to the 
public of water for human consumption through pipes or, after August 5, 
1998, other constructed conveyances, if such system has at least fifteen 
service connections or regularly serves an average of at least twenty-
five individuals daily at least 60 days out of the year. Such term 
includes:
    Any collection, treatment, storage, and distribution facilities 
under control of the operator of such system and used primarily in 
connection with such system; and any collection or pretreatment storage 
facilities not under such control which are used primarily in connection 
with such system. Such term does not include any ``special irrigation 
district.'' A public water system is either a ``community water system'' 
or a ``noncommunity water system'' as defined in Sec.  141.2.
    Sanitary survey means an onsite review of the water source, 
facilities, equipment, operation and maintenance of a public water 
system for the purpose of evaluating the adequacy of such source, 
facilities, equipment, operation and maintenance for producing and 
distributing safe drinking water.
    Service connection, as used in the definition of public water 
system, does not include a connection to a system that delivers water by 
a constructed conveyance other than a pipe if:
    (1) The water is used exclusively for purposes other than 
residential uses (consisting of drinking, bathing, and cooking, or other 
similar uses);
    (2) The Administrator or the State exercising primary enforcement 
responsibility for public water systems, determines that alternative 
water to achieve the equivalent level of public health protection 
provided by the applicable national primary drinking water regulation is 
provided for residential or similar uses for drinking and cooking; or
    (3) The Administrator or the State exercising primary enforcement 
responsibility for public water systems, determines that the water 
provided for residential or similar uses for drinking, cooking, and 
bathing is centrally treated or treated at the point of entry by the 
provider, a pass-through entity, or the user to achieve the equivalent 
level of protection provided by the applicable national primary drinking 
water regulations.
    Special irrigation district means an irrigation district in 
existence prior to May 18, 1994 that provides primarily agricultural 
service through a piped water system with only incidental residential or 
similar use where the system or the residential or similar users of the 
system comply with the exclusion provisions in section 1401(4)(B)(i)(II) 
or (III).
    State means one of the States of the United States, the District of 
Columbia, the Commonwealth of Puerto Rico, the Virgin Islands, Guam, 
American

[[Page 738]]

Samoa, the Commonwealth of the Northern Mariana Islands, the Trust 
Territory of the Pacific Islands, or an eligible Indian tribe.
    State primary drinking water regulation means a drinking water 
regulation of a State which is comparable to a national primary drinking 
water regulation.
    State program revision means a change in an approved State primacy 
program.
    Supplier of water means any person who owns or operates a public 
water system.
    Treatment technique requirement means a requirement of the national 
primary drinking water regulations which specifies for a contaminant a 
specific treatment technique(s) known to the Administrator which leads 
to a reduction in the level of such contaminant sufficient to comply 
with the requirements of part 141 of this chapter.

[41 FR 2918, Jan. 20, 1976, as amended at 53 FR 37410, Sept. 26, 1988; 
54 FR 52137, Dec. 20, 1989; 59 FR 64344, Dec. 14, 1994; 63 FR 23367, 
Apr. 28, 1998]



Sec.  142.3  Scope.

    (a) Except where otherwise provided, this part applies to each 
public water system in each State; except that this part shall not apply 
to a public water system which meets all of the following conditions:
    (1) Which consists only of distribution and storage facilities (and 
does not have any collection and treatment facilities);
    (2) Which obtains all of its water from, but is not owned or 
operated by, a public water system to which such regulations apply;
    (3) Which does not sell water to any person; and
    (4) Which is not a carrier which conveys passengers in interstate 
commerce.
    (b) In order to qualify for primary enforcement responsibility, a 
State's program for enforcement of primary drinking water regulations 
must apply to all other public water systems in the State, except for:
    (1) Public water systems on carriers which convey passengers in 
interstate commerce;
    (2) Public water systems on Indian land with respect to which the 
State does not have the necessary jurisdiction or its jurisdiction is in 
question; or
    (c) Section 1451 of the SDWA authorizes the Administrator to 
delegate primary enforcement responsibility for public water systems to 
Indian Tribes. An Indian Tribe must meet the statutory criteria at 42 
U.S.C. 300j-11(b)(1) before it is eligible to apply for Public Water 
System Supervision grants and primary enforcement responsibility. All 
primary enforcement responsibility requirements of parts 141 and 142 
apply to Indian Tribes except where specifically noted.

[41 FR 2918, Jan. 20, 1976, as amended at 53 FR 37410, Sept. 26, 1988; 
59 FR 64344, Dec. 14, 1994; 67 FR 70858, Nov. 27, 2002]



Sec.  142.4  State and local authority.

    Nothing in this part shall diminish any authority of a State or 
political subdivision to adopt or enforce any law or regulation 
respecting drinking water regulations or public water systems, but no 
such law or regulation shall relieve any person of any requirements 
otherwise applicable under this part.



              Subpart B_Primary Enforcement Responsibility



Sec.  142.10  Requirements for a determination of primary enforcement 
responsibility.

    A State has primary enforcement responsibility for public water 
systems in the State during any period for which the Administrator 
determines, based upon a submission made pursuant to Sec.  142.11, and 
submission under Sec.  142.12, that such State, pursuant to appropriate 
State legal authority:
    (a) Has adopted drinking water regulations which are no less 
stringent than the national primary drinking water regulations (NPDWRs) 
in effect under part 141 of this chapter;
    (b) Has adopted and is implementing adequate procedures for the 
enforcement of such State regulations, such procedures to include:
    (1) Maintenance of an inventory of public water systems.
    (2) A systematic program for conducting sanitary surveys of public

[[Page 739]]

water systems in the State, with priority given to sanitary surveys of 
public water systems not in compliance with State primary drinking water 
regulations.
    (3)(i) The establishment and maintenance of a State program for the 
certification of laboratories conducting analytical measurements of 
drinking water contaminants pursuant to the requirements of the State 
primary drinking water regulations including the designation by the 
State of a laboratory officer, or officers, certified by the 
Administrator, as the official(s) responsible for the State's 
certification program. The requirements of this paragraph may be waived 
by the Administrator for any State where all analytical measurements 
required by the State's primary drinking water regulations are conducted 
at laboratories operated by the State and certified by the Agency. Until 
such time as the Agency establishes a National quality assurance program 
for laboratory certification the State shall maintain an interim program 
for the purpose of approving those laboratories from which the required 
analytical measurements will be acceptable.
    (ii) Upon a showing by an Indian Tribe of an intergovernmental or 
other agreement to have all analytical tests performed by a certified 
laboratory, the Administrator may waive this requirement.
    (4) Assurance of the availability to the State of laboratory 
facilities certified by the Administrator and capable of performing 
analytical measurements of all contaminants specified in the State 
primary drinking water regulations. Until such time as the Agency 
establishes a National quality assurance program for laboratory 
certification the Administrator will approve such State laboratories on 
an interim basis.
    (5) The establishment and maintenance of an activity to assure that 
the design and construction of new or substantially modified public 
water system facilities will be capable of compliance with the State 
primary drinking water regulations.
    (6) Statutory or regulatory enforcement authority adequate to compel 
compliance with the State primary drinking water regulations in 
appropriate cases, such authority to include:
    (i) Authority to apply State primary drinking water regulations to 
all public water systems in the State covered by the national primary 
drinking water regulations, except for interstate carrier conveyances 
and systems on Indian land with respect to which the State does not have 
the necessary jurisdiction or its jurisdiction is in question.
    (ii) Authority to sue in courts of competent jurisdiction to enjoin 
any threatened or continuing violation of the State primary drinking 
water regulations.
    (iii) Right of entry and inspection of public water systems, 
including the right to take water samples, whether or not the State has 
evidence that the system is in violation of an applicable legal 
requirement.
    (iv) Authority to require suppliers of water to keep appropriate 
records and make appropriate reports to the State.
    (v) Authority to require public water systems to give public notice 
that is no less stringent than the EPA requirements in subpart Q of part 
141 of this chapter and Sec.  142.16(a).
    (vi) Authority to assess civil or criminal penalties for violation 
of the State's primary drinking water regulations and public 
notification requirements, including the authority to assess daily 
penalties or multiple penalties when a violation continues;
    (vii) Authority to require community water systems to provide 
consumer confidence reports as required under 40 CFR part 141, subpart 
O.
    (c) Has established and will maintain record keeping and reporting 
of its activities under paragraphs (a), (b) and (d) in compliance with 
Sec. Sec.  142.14 and 142.15;
    (d) Variances and exemptions. (1) If it permits small system 
variances pursuant to Section 1415(e) of the Act, it must provide 
procedures no less stringent than the Act and Subpart K of this part.
    (2) If it permits variances (other than small system variances) or 
exemptions, or both, from the requirements of the State primary drinking 
water regulations, it shall do so under conditions and in a manner no 
less stringent than

[[Page 740]]

the requirements of Sections 1415 and 1416 of the Act. In granting these 
variances, the State must adopt the Administrator's findings of best 
available technology, treatment techniques, or other means available as 
specified in Subpart G of this part. (States with primary enforcement 
responsibility may adopt procedures different from those set forth in 
Subparts E and F of this part, which apply to the issuance of variances 
(other than small system variances) and exemptions by the Administrator 
in States that do not have primary enforcement responsibility, provided 
that the State procedures meet the requirements of this paragraph); and
    (e) Has adopted and can implement an adequate plan for the provision 
of safe drinking water under emergency circumstances including, but not 
limited to, earthquakes, floods, hurricanes, and other natural 
disasters.
    (f)(1) Has adopted authority for assessing administrative penalties 
unless the constitution of the State prohibits the adoption of such 
authority. For public water systems serving a population of more than 
10,000 individuals, States must have the authority to impose a penalty 
of at least $1,000 per day per violation. For public water systems 
serving a population of 10,000 or fewer individuals, States must have 
penalties that are adequate to ensure compliance with the State 
regulations as determined by the State.
    (2) As long as criteria in paragraph (f)(1) of this section are met, 
States may establish a maximum administrative penalty per violation that 
may be assessed on a public water system.
    (g) Has adopted regulations consistent with 40 CFR part 3--
(Electronic reporting) if the state receives electronic documents.
    (h) An Indian Tribe shall not be required to exercise criminal 
enforcement jurisdiction to meet the requirements for primary 
enforcement responsibility.

[41 FR 2918, Jan. 20, 1976, as amended at 43 FR 5373, Feb. 8, 1978; 52 
FR 20675, June 2, 1987; 52 FR 41550, Oct. 28, 1987; 53 FR 37410, Sept. 
26, 1988; 54 FR 15188, Apr. 17, 1989; 54 FR 52138, Dec. 20, 1989; 63 FR 
23367, Apr. 28, 1998; 63 FR 43846, Aug. 14, 1998; 63 FR 44535, Aug. 19, 
1998; 65 FR 26048, May 4, 2000; 70 FR 59888, Oct. 13, 2005]



Sec.  142.11  Initial determination of primary enforcement responsibility.

    (a) A State may apply to the Administrator for a determination that 
the State has primary enforcement responsibility for public water 
systems in the State pursuant to section 1413 of the Act. The 
application shall be as concise as possible and include a side-by-side 
comparison of the Federal requirements and the corresponding State 
authorities, including citations to the specific statutes and 
administrative regulations or ordinances and, wherever appropriate, 
judicial decisions which demonstrate adequate authority to meet the 
requirements of Sec.  142.10. The following information is to be 
included with the State application.
    (1) The text of the State's primary drinking water regulations, with 
references to those State regulations that vary from comparable 
regulations set forth in part 141 of this chapter, and a demonstration 
that any different State regulation is at least as stringent as the 
comparable regulation contained in part 141.
    (2) A description, accompanied by appropriate documentation, of the 
State's procedures for the enforcement of the State primary drinking 
water regulations. The submission shall include:
    (i) A brief description of the State's program to maintain a current 
inventory of public water systems.
    (ii) A brief description of the State's program for conducting 
sanitary surveys, including an explanation of the priorities given to 
various classes of public water systems.
    (iii) A brief description of the State's laboratory approval or 
certification program, including the name(s) of the responsible State 
laboratory officer(s) certified by the Administrator.
    (iv) Identification of laboratory facilities, available to the 
State, certified or approved by the Administrator and capable of 
performing analytical measurements of all contaminants specified in the 
State's primary drinking water regulations.

[[Page 741]]

    (v) A brief description of the State's program activity to assure 
that the design and construction of new or substantially modified public 
water system facilities will be capable of compliance with the 
requirements of the State primary drinking water regulations.
    (vi) Copies of State statutory and regulatory provisions authorizing 
the adoption and enforcement of State primary drinking water 
regulations, and a brief description of State procedures for 
administrative or judicial action with respect to public water systems 
not in compliance with such regulations.
    (3) A statement that the State will make such reports and will keep 
such records as may be required pursuant to Sec. Sec.  142.14 and 
142.15.
    (4) If the State permits variances or exemptions from its primary 
drinking water regulations, the text of the State's statutory and 
regulatory provisions concerning variances and exemptions.
    (5) A brief description of the State's plan for the provision of 
safe drinking water under emergency conditions.

    Note: In satisfaction of this requirement, for public water supplies 
from groundwater sources, EPA will accept the contingency plan for 
providing alternate drinking water supplies that is part of a State's 
Wellhead Protection Program, where such program has been approved by EPA 
pursuant to section 1428 of the SDWA.

    (6)(i) A copy of the State statutory and regulatory provisions 
authorizing the executive branch of the State government to impose an 
administrative penalty on all public water systems, and a brief 
description of the State's authority for administrative penalties that 
will ensure adequate compliance of systems serving a population of 
10,000 or fewer individuals.
    (ii) In instances where the State constitution prohibits the 
executive branch of the State government from assessing any penalty, the 
State shall submit a copy of the applicable part of its constitution and 
a statement from its Attorney General confirming this interpretation.
    (7)(i) A statement by the State Attorney General (or the attorney 
for the State primacy agency if it has independent legal counsel) or the 
attorney representing the Indian tribe that certifies that the laws and 
regulations adopted by the State or tribal ordinances to carry out the 
program were duly adopted and are enforceable. State statutes and 
regulations cited by the State Attorney General and tribal ordinances 
cited by the attorney representing the Indian tribe shall be in the form 
of lawfully adopted State statutes and regulations or tribal ordinances 
at the time the certification is made and shall be fully effective by 
the time the program is approved by EPA. To qualify as ``independent 
legal counsel,'' the attorney signing the statement required by this 
section shall have full authority to independently represent the State 
primacy agency or Indian tribe in court on all matters pertaining to the 
State or tribal program.
    (ii) After EPA has received the documents required under paragraph 
(a) of this section, EPA may selectively require supplemental statements 
by the State Attorney General (or the attorney for the State primacy 
agency if it has independent legal counsel) or the attorney representing 
the Indian tribe. Each supplemental statement shall address all issues 
concerning the adequacy of State authorities to meet the requirements of 
Sec.  142.10 that have been identified by EPA after thorough examination 
as unresolved by the documents submitted under paragraph (a) of this 
section.
    (b)(1) The administrator shall act on an application submitted 
pursuant to Sec.  142.11 within 90 days after receiving such 
application, and shall promptly inform the State in writing of this 
action. If he denies the application, his written notification to the 
State shall include a statement of reasons for the denial.
    (2) A final determination by the Administrator that a State has met 
or has not met the requirements for primary enforcement responsibility 
shall take effect in accordance with the public notice requirements and 
related procedures under Sec.  142.13.
    (3) When the Administrator's determination becomes effective 
pursuant

[[Page 742]]

to Sec.  142.13, it shall continue in effect unless terminated pursuant 
to Sec.  142.17.

[41 FR 2918, Jan. 20, 1976, as amended at 54 FR 52138, Dec. 20, 1989; 60 
FR 33661, June 28, 1995; 63 FR 23367, Apr. 28, 1998]



Sec.  142.12  Revision of State programs.

    (a) General requirements. Either EPA or the primacy State may 
initiate actions that require the State to revise its approved State 
primacy program. To retain primary enforcement responsibility, States 
must adopt all new and revised national primary drinking water 
regulations promulgated in part 141 of this chapter and any other 
requirements specified in this part.
    (1) Whenever a State revises its approved primacy program to adopt 
new or revised Federal regulations, the State must submit a request to 
the Administrator for approval of the program revision, using the 
procedures described in paragraphs (b), (c), and (d) of this section. 
The Administrator shall approve or disapprove each State request for 
approval of a program revision based on the requirements of the Safe 
Drinking Water Act and of this part.
    (2) For all State program revisions not covered under Sec.  
142.12(a)(1), the review procedures outlined in Sec.  142.17(a) shall 
apply.
    (b) Timing of State requests for approval of program revisions to 
adopt new or revised Federal regulations. (1) Complete and final State 
requests for approval of program revisions to adopt new or revised EPA 
regulations must be submitted to the Administrator not later than 2 
years after promulgation of the new or revised EPA regulations, unless 
the State requests an extension and the Administrator has approved the 
request pursuant to paragraph (b)(2) of this section. If the State 
expects to submit a final State request for approval of a program 
revision to EPA more than 2 years after promulgation of the new or 
revised EPA regulations, the State shall request an extension of the 
deadline before the expiration of the 2-year period.
    (2) The final date for submission of a complete and final State 
request for a program revision may be extended by EPA for up to a two-
year period upon a written application by the State to the 
Administrator. In the extension application the State must demonstrate 
it is requesting the extension because it cannot meet the original 
deadline for reasons beyond its control despite a good faith effort to 
do so. The application must include a schedule for the submission of a 
final request by a certain time and provide sufficient information to 
demonstrate that the State:
    (i)(A) Currently lacks the legislative or regulatory authority to 
enforce the new or revised requirements, or
    (B) Currently lacks the program capability adequate to implement the 
new or revised requirements; or
    (C) Is requesting the extension to group two or more program 
revisions in a single legislative or regulatory action; and
    (ii) Is implementing the EPA requirements to be adopted by the State 
in its program revision pursuant to paragraph (b)(3) of this section 
within the scope of its current authority and capabilities.
    (3) To be granted an extension, the State must agree with EPA to 
meet certain requirements during the extension period, which may include 
the following types of activities as determined appropriate by the 
Administrator on a case-by-case basis:
    (i) Informing public water systems of the new EPA (and upcoming 
State) requirements and that EPA will be overseeing implementation of 
the requirements until the State, if eligible for interim primacy, 
submits a complete and final primacy revision request to EPA, or in all 
other cases, until EPA approves the State program revision;
    (ii) Collecting, storing and managing laboratory results, public 
notices, and other compliance and operation data required by the EPA 
regulations;
    (iii) Assisting EPA in the development of the technical aspects of 
enforcement actions and conducting informal follow-up on violations 
(telephone calls, letters, etc.);
    (iv) Providing technical assistance to public water systems;
    (v) Providing EPA with all information prescribed by Sec.  142.15 of 
this part on State reporting; and
    (vi) For States whose request for an extension is based on a current 
lack of

[[Page 743]]

program capability adequate to implement the new requirements, taking 
steps agreed to by EPA and the State during the extension period to 
remedy the deficiency.
    (c) Contents of a State request for approval of a program revision. 
(1) The State request for EPA approval of a program revision shall be 
concise and must include:
    (i) The documentation necessary (pursuant to Sec.  142.11(a)) to 
update the approved State primacy program, and identification of those 
elements of the approved State primacy program that have not changed 
because of the program revision. The documentation shall include a side-
by-side comparison of the Federal requirements and the corresponding 
State authorities, including citations to the specific statutes and 
administrative regulations or ordinances and, wherever appropriate, 
judicial decisions which demonstrate adequate authority to meet the 
requirements of Sec.  142.10 as they apply to the program revision.
    (ii) Any additional materials that are listed in Sec.  142.16 of 
this part for a specific EPA regulation, as appropriate; and
    (iii) For a complete and final State request only, unless one of the 
conditions listed in paragraph (c)(2) of this section are met, a 
statement by the State Attorney General (or the attorney for the State 
primacy agency if it has independent legal counsel) or the attorney 
representing the Indian tribe that certifies that the laws and 
regulations adopted by the State or tribal ordinances to carry out the 
program revision were duly adopted and are enforceable. State statutes 
and regulations cited by the State Attorney General and tribal 
ordinances cited by the attorney for the Indian tribe shall be in the 
form of lawfully adopted State statutes and regulations or tribal 
ordinances at the time the certification is made and shall be fully 
effective by the time the request for program revision is approved by 
EPA. To qualify as ``independent legal counsel,'' the attorney signing 
the statement required by this section shall have full authority to 
independently represent the State primacy agency or tribe in court on 
all matters pertaining to the State or tribal program.
    (2) An Attorney General's statement will be required as part of the 
State request for EPA approval of a program revision unless EPA 
specifically waives this requirement for a specific regulation at the 
time EPA promulgates the regulation, or by later written notice from the 
Administrator to the State.
    (3) After EPA has received the documents required under paragraph 
(c)(1) of this section, EPA may selectively require supplemental 
statements by the State Attorney General (or the attorney for the State 
primacy agency if it has independent legal counsel) or the attorney 
representing the Indian tribe. Each supplemental statement shall address 
all issues concerning the adequacy of State authorities to meet the 
requirements of Sec.  142.10 that have been identified by EPA after 
thorough examination as unresolved by the documents submitted under 
paragraph (c)(1) of this section.
    (d) Procedures for review of a State request for approval of a 
program revision--(1) Preliminary request. (i) The State may submit to 
the Administrator for his or her review a preliminary request for 
approval of each program revision, containing the information listed in 
paragraph (c)(1) of this section, in draft form. The preliminary request 
does not require an Attorney General's statement in draft form, but does 
require draft State statutory or regulatory changes and a side-by-side 
comparison of State authorities with EPA requirements to demonstrate 
that the State program revision meets EPA requirements under Sec.  
142.10 of this part. The preliminary request should be submitted to the 
Administrator as soon as practicable after the promulgation of the EPA 
regulations.
    (ii) The Administrator will review the preliminary request submitted 
in accordance with paragraph (d)(1)(i) of this section and make a 
tentative determination on the request. The Administrator will send the 
tentative determination and other comments or suggestions to the State 
for its use in developing the State's final request under paragraph 
(d)(2) of this section.
    (2) Final request. The State must submit a complete and final 
request for

[[Page 744]]

approval of a program revision to the Administrator for his or her 
review and approval. The request must contain the information listed in 
paragraph (c)(1) of this section in complete and final form, in 
accordance with any tentative determination EPA may have issued. 
Complete and final State requests for program revisions shall be 
submitted within two years of the promulgation of the new or revised EPA 
regulations, as specified in paragraph (b) of this section.
    (3) EPA's determination on a complete and final request. (i) The 
Administrator shall act on a State's request for approval of a program 
revision within 90 days after determining that the State request is 
complete and final and shall promptly notify the State of his/her 
determination.
    (ii) If the Administrator disapproves a final request for approval 
of a program revision, the Administrator will notify the State in 
writing. Such notification will include a statement of the reasons for 
disapproval.
    (iii) A final determination by the Administrator on a State's 
request for approval of a program revision shall take effect in 
accordance with the public notice requirements and related procedures 
under Sec.  142.13.
    (e) Interim primary enforcement authority. A State with an approved 
primacy program for each existing national primary drinking water 
regulation shall be considered to have interim primary enforcement 
authority with respect to each new or revised national drinking water 
regulation that it adopts beginning when the new or revised State 
regulation becomes effective or when the complete primacy revision 
application is submitted to the Administrator, whichever is later, and 
shall end when the Administrator approves or disapproves the State's 
revised primacy program.

[54 FR 52138, Dec. 20, 1989, as amended at 63 FR 23367, Apr. 28, 1998; 
66 FR 3780, Jan. 16, 2001]



Sec.  142.13  Public hearing.

    (a) The Administrator shall provide an opportunity for a public 
hearing before a final determination pursuant to Sec.  142.11 that the 
State meets or does not meet the requirements for obtaining primary 
enforcement responsibility, or a final determination pursuant to Sec.  
142.12(d)(3) to approve or disapprove a State request for approval of a 
program revision, or a final determination pursuant to Sec.  142.17 that 
a State no longer meets the requirements for primary enforcement 
responsibility.
    (b) The Administrator shall publish notice of any determination 
specified in paragraph (a) of this section in the Federal Register and 
in a newspaper or newspapers of general circulation in the State 
involved within 15 days after making such determination, with a 
statement of his reasons for the determination. Such notice shall inform 
interested persons that they may request a public hearing on the 
Administrator's determination. Such notice shall also indicate one or 
more locations in the State where information submitted by the State 
pursuant to Sec.  142.11 is available for inspection by the general 
public. A public hearing may be requested by any interested person other 
than a Federal agency. Frivolous or insubstantial requests for hearing 
may be denied by the Administrator.
    (c) Requests for hearing submitted pursuant to paragraph (b) of this 
section shall be submitted to the Administrator within 30 days after 
publication of notice of opportunity for hearing in the Federal 
Register. Such requests shall include the following information:
    (1) The name, address and telephone number of the individual, 
organization or other entity requesting a hearing.
    (2) A brief statement of the requesting person's interest in the 
Administrator's determination and of information that the requesting 
person intends to submit at such hearing.
    (3) The signature of the individual making the request; or, if the 
request is made on behalf of an organization or other entity, the 
signature of a responsible official of the organization or other entity.
    (d) The Administrator shall give notice in the Federal Register and 
in a newspaper or newspapers of general circulation in the State 
involved of any hearing to be held pursuant to a request submitted by an 
interested person or on his own motion. Notice of the hearing shall also 
be sent to the person

[[Page 745]]

requesting a hearing, if any, and to the State involved. Notice of the 
hearing shall include a statement of the purpose of the hearing, 
information regarding the time and location or locations for the hearing 
and the address and telephone number of an office at which interested 
persons may obtain further information concerning the hearing. At least 
one hearing location specified in the public notice shall be within the 
involved State. Notice of hearing shall be given not less than 15 days 
prior to the time scheduled for the hearing.
    (e) Hearings convened pursuant to paragraph (d) of this section 
shall be conducted before a hearing officer to be designated by the 
Administrator. The hearing shall be conducted by the hearing officer in 
an informal, orderly and expeditious manner. The hearing officer shall 
have authority to call witnesses, receive oral and written testimony and 
take such other action as may be necessary to assure the fair and 
efficient conduct of the hearing. Following the conclusion of the 
hearing, the hearing officer shall forward the record of the hearing to 
the Administrator.
    (f) After reviewing the record of the hearing, the Administrator 
shall issue an order affirming the determination referred to in 
paragraph (a) of this section or rescinding such determination. If the 
determination is affirmed, it shall become effective as of the date of 
the Administrator's order.
    (g) If no timely request for hearing is received and the 
Administrator does not determine to hold a hearing on his own motion, 
the Administrator's determination shall become effective 30 days after 
notice is issued pursuant to paragraph (b) of this section.
    (h) If a determination of the Administrator that a State no longer 
meets the requirements for primary enforcement responsibility becomes 
effective, the State may subsequently apply for a determination that it 
meets such requirements by submitting to the Administrator information 
demonstrating that it has remedied the deficiencies found by the 
Administrator without adversely sacrificing other aspects of its program 
required for primary enforcement responsibility.

[41 FR 2918, Jan. 20, 1976, as amended at 54 FR 52140, Dec. 20, 1989; 60 
FR 33661, June 28, 1995]



Sec.  142.14  Records kept by States.

    (a) Each State which has primary enforcement responsibility shall 
maintain records of tests, measurements, analyses, decisions, and 
determinations performed on each public water system to determine 
compliance with applicable provisions of State primary drinking water 
regulations.
    (1) Records of microbiological analyses shall be retained for not 
less than 1 year. Actual laboratory reports may be kept or data may be 
transferred to tabular summaries, provided that the information retained 
includes:
    (i) The analytical method used;
    (ii) The number of samples analyzed each month;
    (iii) The analytical results, set forth in a form that makes 
possible comparison with the limits specified in Sec. Sec.  141.63, 
141.71, and 141.72 of this chapter and with the limits specified in 
subpart Y of this chapter.
    (2) Records of microbiological analyses of repeat or special samples 
shall be retained for not less than one year in the form of actual 
laboratory reports or in an appropriate summary form.
    (3) Records of turbidity measurements must be kept for not less than 
one year. The information retained must be set forth in a form which 
makes possible comparison with the limits specified in Sec. Sec.  
141.71, 141.73, 141.173 and 141.175, 141.550-141.553 and 141.560-141.564 
of this chapter. Until June 29, 1993, for any public water system which 
is providing filtration treatment and until December 30, 1991, for any 
public water system not providing filtration treatment and not required 
by the State to provide filtration treatment, records kept must be set 
forth in a form which makes possible comparison with the limits 
contained in Sec.  141.13 of this chapter.
    (4)(i) Records of disinfectant residual measurements and other 
parameters necessary to document disinfection effectiveness in 
accordance with Sec. Sec.  141.72

[[Page 746]]

and 141.74 of this chapter and the reporting requirements of Sec. Sec.  
141.75, 141.175, and 141.570, of this chapter must be kept for not less 
than one year.
    (ii) Records of decisions made on a system-by-system and case-by-
case basis under provisions of part 141, subpart H, subpart P, or 
subpart T of this chapter, must be made in writing and kept by the 
State.
    (A) Records of decisions made under the following provisions shall 
be kept for 40 years (or until one year after the decision is reversed 
or revised) and a copy of the decision must be provided to the system:
    (1) Section 141.73(a)(1)--Any decision to allow a public water 
system using conventional filtration treatment or direct filtration to 
substitute a turbidity limit greater than 0.5 NTU;
    (2) Section 141.73(b)(1)--Any decision to allow a public water 
system using slow sand filtration to substitute a turbidity limit 
greater than 1 NTU;
    (3) Section 141.74(b)(2)--Any decision to allow an unfiltered public 
water system to use continuous turbidity monitoring;
    (4) Section 141.74(b)(6)(i)--Any decision to allow an unfiltered 
public water system to sample residual disinfectant concentration at 
alternate locations if it also has ground water source(s);
    (5) Section 141.74(c)(1)--Any decision to allow a public water 
system using filtration treatment to use continuous turbidity 
monitoring; or a public water system using slow sand filtration or 
filtration treatment other than conventional treatment, direct 
filtration or diatomaceous earth filtration to reduce turbidity sampling 
to once per day; or for systems serving 500 people or fewer to reduce 
turbidity sampling to once per day;
    (6) Section 141.74(c)(3)(i)--Any decision to allow a filtered public 
water system to sample disinfectant residual concentration at alternate 
locations if it also has ground water source(s);
    (7) Section 141.75(a)(2)(ix)--Any decision to allow reduced 
reporting by an unfiltered public water system;
    (8) Section 141.75(b)(2)(iv)--Any decision to allow reduced 
reporting by a filtered public water system; and
    (9) Section 141.76--Any decisions made to approve alternate recycle 
locations, require modifications to recycle return locations, or require 
modifications to recycle practices.
    (B) Records of decisions made under the following provisions shall 
be kept for one year after the decision is made:
    (1) Section 141.71(b)(1)(i)--Any decision that a violation of 
monthly CT compliance requirements was caused by circumstances that were 
unusual and unpredictable.
    (2) Section 141.71(b)(1)(iv)--Any decision that a violation of the 
disinfection effectiveness criteria was not caused by a deficiency in 
treatment of the source water;
    (3) Section 141.71(b)(5)--Any decision that a violation of the total 
coliform MCL was not caused by a deficiency in treatment of the source 
water;
    (4) Section 141.74(b)(1)--Any decision that total coliform 
monitoring otherwise required because the turbidity of the source water 
exceeds 1 NTU is not feasible, except that if such decision allows a 
system to avoid monitoring without receiving State approval in each 
instance, records of the decision shall be kept until one year after the 
decision is rescinded or revised.
    (C) Records of decisions made under the following provisions shall 
be kept for the specified period or 40 years, whichever is less.
    (1) Section 141.71(a)(2)(i)--Any decision that an event in which the 
source water turbidity which exceeded 5 NTU for an unfiltered public 
water system was unusual and unpredictable shall be kept for 10 years.
    (2) Section 141.71(b)(1)(iii)--Any decision by the State that 
failure to meet the disinfectant residual concentration requirements of 
Sec.  141.72(a)(3)(i) was caused by circumstances that were unusual and 
unpredictable, shall be kept unless filtration is installed. A copy of 
the decision must be provided to the system.
    (3) Section 141.71(b)(2)--Any decision that a public water system's 
watershed control program meets the requirements of this section shall 
be kept until the next decision is available and filed.
    (4) Section 141.70(c)--Any decision that an individual is a 
qualified operator for a public water system using a surface water 
source or a ground water

[[Page 747]]

source under the direct influence of surface water shall be maintained 
until the qualification is withdrawn. The State may keep this 
information in the form of a list which is updated periodically. If such 
qualified operators are classified by category, the decision shall 
include that classification.
    (5) Section 141.71(b)(3)--Any decision that a party other than the 
State is approved by the State to conduct on-site inspections shall be 
maintained until withdrawn. The State may keep this information in the 
form of a list which is updated periodically.
    (6) Section 141.71(b)(4)--Any decision that an unfiltered public 
water system has been identified as the source of a waterborne disease 
outbreak, and, if applicable, that it has been modified sufficiently to 
prevent another such occurrence shall be kept until filtration treatment 
is installed. A copy of the decision must be provided to the system.
    (7) Section 141.72--Any decision that certain interim disinfection 
requirements are necessary for an unfiltered public water system for 
which the State has determined that filtration is necessary, and a list 
of those requirements, shall be kept until filtration treatment is 
installed. A copy of the requirements must be provided to the system.
    (8) Section 141.72(a)(2)(ii)--Any decision that automatic shut-off 
of delivery of water to the distribution system of an unfiltered public 
water system would cause an unreasonable risk to health or interfere 
with fire protection shall be kept until rescinded.
    (9) Section 141.72(a)(4)(ii)--Any decision by the State, based on 
site-specific considerations, that an unfiltered system has no means for 
having a sample transported and analyzed for HPC by a certified 
laboratory under the requisite time and temperature conditions specified 
by Sec.  141.74(a)(3) and that the system is providing adequate 
disinfection in the distribution system, so that the disinfection 
requirements contained in Sec.  141.72(a)(4)(i) do not apply, and the 
basis for the decision, shall be kept until the decision is reversed or 
revised. A copy of the decision must be provided to the system.
    (10) Section 141.72(b)(3)(ii)--Any decision by the State, based on 
site-specific conditions, that a filtered system has no means for having 
a sample transported and analyzed for HPC by a certified laboratory 
under the requisite time and temperature conditions specified by Sec.  
141.74(a)(3) and that the system is providing adequate disinfection in 
the distribution system, so that the disinfection requirements contained 
in Sec.  141.72(b)(3)(i) do not apply, and the basis for the decision, 
shall be kept until the decision is reversed or revised. A copy of the 
decision must be provided to the system.
    (11) Section 141.73(d)--Any decision that a public water system, 
having demonstrated to the State that an alternative filtration 
technology, in combination with disinfection treatment, consistently 
achieves 99.9 percent removal and/or inactivation of Giardia lamblia 
cysts and 99.99 percent removal and/or inactivation of viruses, may use 
such alternative filtration technology, shall be kept until the decision 
is reversed or revised. A copy of the decision must be provided to the 
system.
    (12) Section 141.74(b), table 3.1--Any decision that a system using 
either preformed chloramines or chloramines formed by the addition of 
ammonia prior to the addition of chlorine has demonstrated that 99.99 
percent removal and/or inactivation of viruses has been achieved at 
particular CT values, and a list of those values, shall be kept until 
the decision is reversed or revised. A copy of the list of required 
values must be provided to the system.
    (13) Section 141.74(b)(3)(v)--Any decision that a system using a 
disinfectant other than chlorine may use CT99.9 values other 
than those in tables 2.1 or 3.1 and/or other operational parameters to 
determine if the minimum total inactivation rates required by Sec.  
141.72(a)(1) are being met, and what those values or parameters are, 
shall be kept until the decision is reversed or revised. A copy of the 
list of required values or parameters must be provided to the system.
    (14) Section 142.16(b)(2)(i)(B)--Any decision that a system using a 
ground water source is under the direct influence of surface water.

[[Page 748]]

    (iii) Records of any determination that a public water system 
supplied by a surface water source or a ground water source under the 
direct influence of surface water is not required to provide filtration 
treatment shall be kept for 40 years or until withdrawn, whichever is 
earlier. A copy of the determination must be provided to the system.
    (5) Records of each of the following decisions made pursuant to the 
total coliform provisions of part 141 shall be made in writing and 
retained by the State.
    (i) Records of the following decisions must be retained for 5 years.
    (A) Section 141.21(b)(1)--Any decision to waive the 24-hour time 
limit for collecting repeat samples after a total coliform-positive 
routine sample if the public water system has a logistical problem in 
collecting the repeat sample that is beyond the system's control, and 
what alternative time limit the system must meet.
    (B) Section 141.21(b)(5)--Any decision to allow a system to waive 
the requirement for five routine samples the month following a total 
coliform-positive sample. If the waiver decision is made as provided in 
Sec.  141.21(b)(5), the record of the decision must contain all the 
items listed in that paragraph.
    (C) Section 141.21(c)--Any decision to invalidate a total coliform-
positive sample. If the decision to invalidate a total coliform-positive 
sample as provided in Sec.  141.21(c)(1)(iii) is made, the record of the 
decision must contain all the items listed in that paragraph.
    (ii) Records of each of the following decisions must be retained in 
such a manner so that each system's current status may be determined.
    (A) Section 141.21(a)(2)--Any decision to reduce the total coliform 
monitoring frequency for a community water system serving 1,000 persons 
or fewer, that has no history of total coliform contamination in its 
current configuration and had a sanitary survey conducted within the 
past five years showing that the system is supplied solely by a 
protected groundwater source and is free of sanitary defects, to less 
than once per month, as provided in Sec.  141.21(a)(2); and what the 
reduced monitoring frequency is. A copy of the reduced monitoring 
frequency must be provided to the system.
    (B) Section 141.21(a)(3)(i)--Any decision to reduce the total 
coliform monitoring frequency for a non-community water system using 
only ground water and serving 1,000 persons or fewer to less than once 
per quarter, as provided in Sec.  141.21(a)(3)(i), and what the reduced 
monitoring frequency is. A copy of the reduced monitoring frequency must 
be provided to the system.
    (C) Section 141.21(a)(3)(ii)--Any decision to reduce the total 
coliform monitoring frequency for a non-community water system using 
only ground water and serving more than 1,000 persons during any month 
the system serves 1,000 persons or fewer, as provided in Sec.  
141.21(a)(3)(ii). A copy of the reduced monitoring frequency must be 
provided to the system.
    (D) Section 141.21(a)(5)--Any decision to waive the 24-hour limit 
for taking a total coliform sample for a public water system which uses 
surface water, or ground water under the direct influence of surface 
water, and which does not practice filtration in accordance with part 
141, subpart H, and which measures a source water turbidity level 
exceeding 1 NTU near the first service connection as provided in Sec.  
141.21(a)(5).
    (E) Section 141.21(d)(1)--Any decision that a non-community water 
system is using only protected and disinfected ground water and 
therefore may reduce the frequency of its sanitary survey to less than 
once every five years, as provided in Sec.  141.21(d), and what that 
frequency is. A copy of the reduced frequency must be provided to the 
system.
    (F) Section 141.21(d)(2)--A list of agents other than the State, if 
any, approved by the State to conduct sanitary surveys.
    (G) Section 141.21(e)(2)--Any decision to allow a public water 
system to forgo fecal coliform or E. coli testing on a total coliform-
positive sample if that system assumes that the total coliform-positive 
sample is fecal coliform-positive or E. coli- positive, as provided in 
Sec.  141.21(e)(2).
    (6) Records of analysis for other than microbiological contaminants 
(including total coliform, fecal coliform, and heterotrophic plate 
count), residual

[[Page 749]]

disinfectant concentration, other parameters necessary to determine 
disinfection effectiveness (including temperature and pH measurements), 
and turbidity shall be retained for not less than 12 years and shall 
include at least the following information:
    (i) Date and place of sampling.
    (ii) Date and results of analyses.
    (7) Any decisions made pursuant to the provisions of part 141, 
subpart P or subpart T of this chapter.
    (i) Records of systems consulting with the State concerning a 
modification to disinfection practice under Sec. Sec.  141.170(d), 
141.172(c), and 141.542 of this chapter, including the status of the 
consultation.
    (ii) Records of decisions that a system using alternative filtration 
technologies, as allowed under Sec. Sec.  141.173(b) and Sec.  141.552 
of this chapter, can consistently achieve a 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts, 99.99 percent removal and/or 
inactivation of viruses, and 99 percent removal of Cryptosporidium 
oocysts. The decisions must include State-set enforceable turbidity 
limits for each system. A copy of the decision must be kept until the 
decision is reversed or revised. The State must provide a copy of the 
decision to the system.
    (iii) Records of systems required to do filter self-assessment, CPE, 
or CCP under the requirements of Sec. Sec.  141.175 and 141.563 of this 
chapter.
    (8) Any decisions made pursuant to the provisions of 40 CFR part 
141, subparts U and V of this part.
    (i) IDSE monitoring plans, plus any modifications required by the 
State, must be kept until replaced by approved IDSE reports.
    (ii) IDSE reports and 40/30 certifications, plus any modifications 
required by the State, must be kept until replaced or revised in their 
entirety.
    (iii) Operational evaluations submitted by a system must be kept for 
10 years following submission.
    (9) Any decisions made pursuant to the provisions of part 141, 
subpart W of this chapter.
    (i) Results of source water E. coli and Cryptosporidium monitoring.
    (ii) The bin classification after the initial and after the second 
round of source water monitoring for each filtered system, as described 
in Sec.  141.710 of this chapter.
    (iii) Any change in treatment requirements for filtered systems due 
to watershed assessment during sanitary surveys, as described in Sec.  
141.711(d) of this chapter.
    (iv) The determination of whether the mean Cryptosporidium level is 
greater than 0.01 oocysts/L after the initial and after the second round 
of source water monitoring for each unfiltered system, as described in 
Sec.  141.712(a) of this chapter.
    (v) The treatment processes or control measures that systems use to 
meet their Cryptosporidium treatment requirements under Sec.  141.711 or 
Sec.  141.712 of this chapter.
    (vi) A list of systems required to cover or treat the effluent of an 
uncovered finished water storage facility, as specified in Sec.  141.714 
of this chapter.
    (10) Records of each of the following decisions made pursuant to the 
provisions of subpart Y of part 141 must be made in writing and retained 
by the State.
    (i) Records of the following decisions or activities must be 
retained for five years.
    (A) Sections 141.858(a), 141.853(c)(2), 141.856(c), and 141.857(c) 
of this chapter--Any case-by-case decision to waive the 24-hour time 
limit for collecting repeat samples after a total coliform-positive 
routine sample, or to extend the 24-hour limit for collection of samples 
following invalidation, or for an unfiltered subpart H system of this 
part to collect a total coliform sample following a turbidity 
measurement exceeding 1 NTU.
    (B) Sections 141.854(j) and 141.855(f) of this chapter--Any decision 
to allow a system to waive the requirement for three routine samples the 
month following a total coliform-positive sample. The record of the 
waiver decision must contain all the items listed in those sections.
    (C) Section 141.853(c) of this chapter--Any decision to invalidate a 
total coliform-positive sample. If the decision to invalidate a total 
coliform-positive sample as provided in Sec.  141.853(c)(1) of this 
chapter is made, the record of the

[[Page 750]]

decision must contain all the items listed in that section.
    (D) Section 141.859 of this chapter--Completed and approved subpart 
Y assessments, including reports from the system that corrective action 
has been completed as required by Sec.  141.861(a)(2) of this chapter.
    (ii) Records of each of the following decisions must be retained in 
such a manner so that each system's current status may be determined:
    (A) Section 141.854(e) of this chapter--Any decision to reduce the 
total coliform monitoring frequency for a non-community water system 
using only ground water and serving 1,000 or fewer people to less than 
once per quarter, as provided in Sec.  141.854(e) of this chapter, 
including what the reduced monitoring frequency is. A copy of the 
reduced monitoring frequency must be provided to the system.
    (B) Section 141.855(d) of this chapter--Any decision to reduce the 
total coliform monitoring frequency for a community water system serving 
1,000 or fewer people to less than once per month, as provided in Sec.  
141.855(d) of this chapter, including what the reduced monitoring 
frequency is. A copy of the reduced monitoring frequency must be 
provided to the system.
    (C) Section 141.857(d) of this chapter--Any decision to reduce the 
total coliform monitoring frequency for a non-community water system 
using only ground water and serving more than 1,000 persons during any 
month the system serves 1,000 or fewer people, as provided in Sec.  
141.857(d) of this chapter. A copy of the reduced monitoring frequency 
must be provided to the system.
    (D) Section 141.858(b)(2) of this chapter--Any decision to allow a 
system to forgo E. coli testing of a total coliform-positive sample if 
that system assumes that the total coliform-positive sample is E. coli-
positive.
    (b) Records required to be kept pursuant to paragraph (a) of this 
section must be in a form admissible as evidence in State enforcement 
proceedings.
    (c) Each State which has primary enforcement responsibility shall 
maintain current inventory information for every public water system in 
the State and shall retain inventory records of public water systems for 
not less than 12 years.
    (d) Each State which has primary enforcement responsibility shall 
retain, for not less than 12 years, files which shall include for each 
such public water system in the State:
    (1) Reports of sanitary surveys;
    (2) Records of any State approvals;
    (3) Records of any enforcement actions.
    (4) A record of the most recent vulnerability determination, 
including the monitoring results and other data supporting the 
determination, the State's findings based on the supporting data and any 
additional bases for such determination; except that it shall be kept in 
perpetuity or until a more current vulnerability determination has been 
issued.
    (5) A record of all current monitoring requirements and the most 
recent monitoring frequency decision pertaining to each contaminant, 
including the monitoring results and other data supporting the decision, 
the State's findings based on the supporting data and any additional 
bases for such decision; except that the record shall be kept in 
perpetuity or until a more recent monitoring frequency decision has been 
issued.
    (6) A record of the most recent asbestos repeat monitoring 
determination, including the monitoring results and other data 
supporting the determination, the State's findings based on the 
supporting data and any additional bases for the determination and the 
repeat monitoring frequency; except that these records shall be 
maintained in perpetuity or until a more current repeat monitoring 
determination has been issued.
    (7) Records of annual certifications received from systems pursuant 
to part 141, subpart K demonstrating the system's compliance with the 
treatment techniques for acrylamide and/or epichlorohydrin in Sec.  
14.111.
    (8) Records of the currently applicable or most recent State 
determinations, including all supporting information and an explanation 
of the technical basis for each decision, made under the following 
provisions of 40

[[Page 751]]

CFR, part 141, subpart I for the control of lead and copper:
    (i) Section 141.81(b)--for any water system deemed to be optimized 
under Sec.  141.81(b)(1) or (b)(3) of this chapter, any conditions 
imposed by the State on specific water systems to ensure the continued 
operation and maintenance of corrosion control treatment in place;
    (ii) Section 141.82(b)--decisions to require a water system to 
conduct corrosion control treatment studies;
    (iii) Section 141.82(d)--designations of optimal corrosion control 
treatment;
    (iv) Section 141.82(f)--designations of optimal water quality 
parameters;
    (v) Section 141.82(h)--decisions to modify a public water system's 
optimal corrosion control treatment or water quality parameters;
    (vi) Section 141.83(b)(2)--determinations of source water treatment;
    (vii) Section 141.83(b)(4)--designations of maximum permissible 
concentrations of lead and copper in source water;
    (viii) Section 141.84(e)--determinations establishing shorter lead 
service line service line replacement schedules under Sec.  141.84;
    (ix) Sections 141.81(b)(3)(iii), 141.86(d)(4)(vii), and 
141.86(g)(4)(iii)--determinations of additional monitoring requirements 
and/or other actions required to maintain optimal corrosion control by 
systems monitoring for lead and copper at the tap less frequently than 
once every six months that change treatment or add a new source of 
water;
    (x) Section 141.85--system-specific decisions regarding the content 
of written public education materials and/or the distribution of these 
materials;
    (xi) Section 141.86(b)(5)--system-specific determinations regarding 
use of non-first-draw samples at non-transient non-community water 
systems, and community water systems meeting the criteria of Sec.  
141.85(b)(7)(i) and (ii) of this chapter, that operate 24 hours a day;
    (xii) Section 141.86(c)--system-specific designations of sampling 
locations for systems subject to reduced monitoring;
    (xiii) Section 141.86(d)(iv)(A)--system-specific determinations 
pertaining to alternative sample collection periods for systems subject 
to reduced monitoring;
    (xiv) Section 141.86(g)--determinations of small system monitoring 
waivers, waiver recertifications, and waiver revocations;
    (xv) Section 141.87(c)(3)--determinations regarding representative 
entry point locations at ground water systems;
    (xvi) Section 141.90(e)(4)--system-specific determinations regarding 
the submission of information to demonstrate compliance with partial 
lead service line replacement requirements; and
    (xvii) Section 141.90(f)--system-specific decisions regarding the 
resubmission of detailed documentation demonstrating completion of 
public education requirements.
    (9) Records of reports and any other information submitted by PWSs 
under Sec.  141.90 of this chapter, including records of any 90th 
percentile values calculated by the State under Sec.  141.90(h) of this 
chapter.
    (10) Records of State activities, and the results thereof, to:
    (i) Verify compliance with State determinations issued under 
Sec. Sec.  141.82(f) of this chapter, 141.82(h) of this chapter, 
141.83(b)(2) of this chapter, and 141.83(b)(4) of this chapter;
    (ii) Verify compliance with the requirements related to partial lead 
service line replacement under Sec.  141.84(d) of this chapter and 
compliance with lead service line replacement schedules under Sec.  
141.84(e) of this chapter; and
    (iii) Invalidate tap water lead and copper samples under Sec.  
141.86(f) of this chapter.
    (11) Records of each system's currently applicable or most recently 
designated monitoring requirements. If, for the records identified in 
paragraphs (d)(8)(i) through (d)(8)(xvii) of this section, no change is 
made to State determinations during a 12-year retention period, the 
State shall retain the record until a new decision, determination, or 
designation has been issued.
    (12) Records of the currently applicable or most recent State 
determinations, including all supporting information and an explanation 
of the technical basis for each decision, made under the following 
provisions of 40

[[Page 752]]

CFR part 141, subpart L for the control of disinfectants and 
disinfection byproducts. These records must also include interim 
measures toward installation.
    (i) States must keep records of systems that are installing GAC or 
membrane technology in accordance with Sec.  141.64(b)(2) of this 
chapter. These records must include the date by which the system is 
required to have completed installation.
    (ii) States must keep records of systems that are required, by the 
State, to meet alternative minimum TOC removal requirements or for whom 
the State has determined that the source water is not amenable to 
enhanced coagulation in accordance with Sec.  141.135(b)(3) and (4) of 
this chapter, respectively. These records must include the alternative 
limits and rationale for establishing the alternative limits.
    (iii) States must keep records of subpart H systems using 
conventional treatment meeting any of the alternative compliance 
criteria in Sec.  141.135(a)(2) or (3) of this chapter.
    (iv) States must keep a register of qualified operators that have 
met the State requirements developed under Sec.  142.16(h)(2).
    (13) Records of systems with multiple wells considered to be one 
treatment plant in accordance with Sec.  141.132(a)(2) of this chapter 
and Sec.  142.16(h)(5).
    (14) Monitoring plans for subpart H systems serving more than 3,300 
persons in accordance with Sec.  141.132(f) of this chapter.
    (15) List of laboratories approved for analyses in accordance with 
Sec.  141.131(b) of this chapter.
    (16) List of systems required to monitor for disinfectants and 
disinfection byproducts in accordance with part 141, subpart L of this 
chapter. The list must indicate what disinfectants and DBPs, other than 
chlorine, TTHM, and HAA5, if any, are measured.
    (17) Records of the currently applicable or most recent State 
determination, including all supporting information and an explanation 
of the technical basis of each decision, made under the following 
provisions of 40 CFR part 141, subpart S and 40 CFR part 142.
    (i) Section 142.16(o)(2)(v). Records of written notices of 
significant deficiencies.
    (ii) Section 141.403(a)(5)(ii) of this chapter. Records of 
corrective action plans, schedule approvals, and State-specified interim 
measures.
    (iii) Section 142.16(o)(4). Records of confirmations under Sec.  
141.403(a) of this chapter that a significant deficiency has been 
corrected or the fecal contamination in the ground water source has been 
addressed.
    (iv) Section 141.402(a)(5) of this chapter. Records of State 
determinations and records of ground water system's documentation for 
not conducting triggered source water monitoring.
    (v) Section 141.402(d) of this chapter. Records of invalidations of 
fecal indicator-positive ground water source samples.
    (vi) Section 141.402(a)(2)(ii) of this chapter. Records of State 
approvals of source water monitoring plans.
    (vii) Section 142.16(o)(4)(ii). Records of notices of the minimum 
residual disinfection concentration (when using chemical disinfection) 
needed to achieve at least 4-log virus inactivation before or at the 
first customer.
    (viii) Sections 142.16(o)(4)(iv) and 142.16(o)(4)(v) Records of 
notices of the State-specified monitoring and compliance requirements 
(when using membrane filtration or alternative treatment) needed to 
achieve at least 4-log treatment of viruses (using inactivation, 
removal, or a State-approved combination of 4-log inactivation and 
removal) before or at the first customer.
    (ix) Sections 141.403(b)(1) and 141.403(b)(2) of this chapter. 
Records of written notices from the ground water system that it provides 
at least 4-log treatment of viruses (using inactivation, removal, or a 
State-approved combination of 4-log virus inactivation and removal) 
before or at the first customer for a ground water source.
    (x) Section 142.16(o)(4)(vi). Records of written determinations that 
the ground water system may discontinue 4-log treatment of viruses 
(using inactivation, removal, or a State-approved combination of 4-log 
inactivation and removal).

[[Page 753]]

    (e) Each State which has primary enforcement responsibility shall 
retain records pertaining to each variance and exemption granted by it 
for a period of not less than 5 years following the expiration of such 
variance or exemption.
    (f) Public notification records under subpart Q of part 141 of this 
chapter received from public water systems (including certifications of 
compliance and copies of public notices) and any state determinations 
establishing alternative public notification requirements for the water 
systems must be retained for three years.
    (g) Records required to be kept under this section shall be 
available to the Regional Administrator upon request. The records 
required to be kept under this section shall be maintained and made 
available for public inspection by the State, or, the State at its 
option may require suppliers of water to make available for public 
inspection those records maintained in accordance with Sec.  141.33.

[41 FR 2918, Jan. 20, 1976]

    Editorial Note: For Federal Register citations affecting Sec.  
142.14, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  142.15  Reports by States.

    Each State which has primary enforcement responsibility shall submit 
to the Administrator the following information:
    (a) Each State which has primary enforcement responsibility shall 
submit quarterly reports to the Administrator on a schedule and in a 
format prescribed by the Administrator, consisting of the following 
information:
    (1) New violations by public water systems in the State during the 
previous quarter of State regulations adopted to incorporate the 
requirements of national primary drinking water regulations, including 
violations of the public notification requirements under subpart Q of 
part 141 of this chapter;
    (2) New enforcement actions taken by the State during the previous 
quarter against public water systems with respect to State regulations 
adopted to incorporate the requirements of national primary drinking 
water regulations;
    (3) Notification of any new variance or exemption granted during the 
previous quarter. The notice shall include a statement of reasons for 
the granting of the variance or exemption, including documentation of 
the need for the variance or exemption and the finding that the granting 
of the variance or exemption will not result in an unreasonable risk to 
health. The State may use a single notification statement to report two 
or more similar variances or exemptions.
    (b) Each State which has primary enforcement responsibility shall 
submit annual reports to the Administrator on a schedule and in a format 
prescribed by the Administrator, consisting of the following 
information:
    (1) All additions or corrections to the State's inventory of public 
water systems;
    (2) A summary of the status of each variance and exemption currently 
in effect.
    (c) Special reports--(1) Surface Water Treatment Rule. (i)(A) A list 
identifying the name, PWS identification number and date of the 
determination for each public water system supplied by a surface water 
source or a ground water source under the direct influence of surface 
water, which the State has determined is not required to provide 
filtration treatment.
    (B) A list identifying the name and PWS identification number of 
each public water system supplied by a surface water source or ground 
water source under the direct influence of surface water, which the 
State has determined, based on an evaluation of site-specific 
considerations, has no means of having a sample transported and analyzed 
for HPC by a certified laboratory under the requisite time and 
temperature conditions specified in Sec.  141.74(a)(3) and is providing 
adequate disinfection in the distribution system, regardless of whether 
the system is in compliance with the criteria of Sec.  141.72 (a)(4)(i) 
or (b)(3)(i) of this chapter, as allowed by Sec.  141.72 (a)(4)(ii) and 
(b)(3)(ii). The list must include the effective date of each 
determination.

[[Page 754]]

    (ii) Notification within 60 days of the end of the calendar quarter 
of any determination that a public water system using a surface water 
source or a ground water source under the direct influence of surface 
water is not required to provide filtration treatment. The notification 
must include a statement describing the system's compliance with each 
requirement of the State's regulations that implement Sec.  141.71 and a 
summary of comments, if any, received from the public on the 
determination. A single notification may be used to report two or more 
such determinations.
    (2) Total coliforms. A list of public water systems which the State 
is allowing to monitor less frequently than once per month for community 
water systems or less frequently than once per quarter for non-community 
water systems as provided in Sec.  141.21(a), including the effective 
date of the reduced monitoring requirement for each system.
    (3) Total coliforms under subpart Y. A list of systems that the 
State is allowing to monitor less frequently than once per month for 
community water systems or less frequently than once per quarter for 
non-community water systems as provided in Sec. Sec.  141.855 and 
141.854 of this chapter, including the applicable date of the reduced 
monitoring requirement for each system.
    (4) States shall report quarterly, in a format and on a schedule 
prescribed by the Administrator, the following information related to 
each system's compliance with the treatment techniques for lead and 
copper under 40 CFR part 141, subpart I during the preceding calendar 
quarter. Specifically, States shall report as follows:
    (i) For any reports provided prior to May 15, 2000, States shall 
report the name and PWS identification number:
    (A) Each public water system which exceeded the lead and copper 
action levels and the date upon which the exceedance occurred;
    (B) Each public water system required to complete the corrosion 
control evaluation specified in Sec.  141.82(c) and the date the State 
received the results of the evaluations from each system;
    (C) Each public water system for which the State has designated 
optimal corrosion control treatment under Sec.  141.82(d), the date of 
the determination, and each system that completed installation of 
treatment as certified under Sec.  141.90(c)(3);
    (D) Each public water system for which the State has designated 
optimal water quality parameters under Sec.  141.82(f) and the date of 
the determination;
    (E) Each public water system which the State has required to install 
source water treatment under Sec.  141.83(b)(2), the date of the 
determination, and each system that completed installation of treatment 
as certified under Sec.  141.90(d)(2);
    (F) Each public water system for which the State has specified 
maximum permissible source water levels under Sec.  141.83(b)(4); and
    (G) Each public water system required to begin replacing lead 
service lines as specified in Sec.  141.84, each public water system for 
which the State has established a replacement schedule under Sec.  
141.84(f), and each system reporting compliance with its replacement 
schedule under Sec.  141.90(e)(2).
    (ii) For any reports provided after May 14, 2000 and before January 
14, 2002, States may report in accordance with either paragraph 
(c)(4)(i) or (c)(4)(iii) of this section.
    (iii) For all reports submitted on or after January 14, 2002, States 
shall report the PWS identification number of each public water system 
identified in paragraphs (c)(4)(iii)(A) through (F) of this section.
    (A) For each large and medium-size public water system, all 90th 
percentile lead levels calculated during each monitoring period 
specified in Sec.  141.86 of this chapter, and the first and last day of 
the monitoring period for which the 90th percentile lead level was 
calculated;
    (B) For each small public water system, the 90th percentile lead 
level calculated during each monitoring period in which the system 
exceeds the lead action level, and the first and last day of each 
monitoring period in which an exceedance occurred;
    (C) For each public water system (regardless of size), the 90th 
percentile

[[Page 755]]

copper level calculated during each monitoring period in which the 
system exceeds the copper action level, and the first and last day of 
each monitoring period in which an exceedance occurred;
    (D) For each public water system for which the State has designated 
optimal water quality parameters under Sec.  141.82(f) of this chapter, 
or which the State has deemed to have optimized corrosion control under 
Sec.  141.81(b)(1) or (b)(3) of this chapter, the date of the 
determination and the paragraph(s) under which the State made its 
determination;
    (E) For each public water system required to begin replacing lead 
service lines as specified in Sec.  141.84 of this chapter and the date 
each system must begin replacement; and
    (F) For each public water system that has implemented optimal 
corrosion control, completed applicable source water treatment 
requirements pursuant to Sec.  141.83 of this chapter and/or completed 
lead service line replacement requirements pursuant to Sec.  141.84 of 
this chapter, and the date of the State's determination that these 
requirements have been met. The date reported shall be the latest of the 
following events:
    (1) The date the State designates optimal water quality parameters 
under Sec.  141.82(f) of this chapter or deems the system to have 
optimized corrosion control pursuant to Sec.  141.81(b)(1) or (b)(3) of 
this chapter;
    (2) For systems triggered into source water treatment, the date the 
State designates maximum permissible source water levels under Sec.  
141.83(b)(4) of this chapter or determines pursuant to Sec.  
141.83(b)(2) of this chapter that source water treatment is not 
required; or
    (3) For systems triggered into lead service line replacement, the 
date the system completes lead service line replacement or becomes 
eligible to cease lead service line replacement pursuant to Sec.  
141.84(f) of this chapter.
    (5) Sanitary surveys. A list of subpart H systems that have had a 
sanitary survey completed during the previous year and an annual 
evaluation of the State's program for conducting sanitary surveys under 
Sec.  142.16(b)(3) of this chapter.
    (6) Subpart W. (i) The bin classification after the initial and 
after the second round of source water monitoring for each filtered 
system, as described in Sec.  141.710 of this chapter.
    (ii) Any change in treatment requirements for these systems due to 
watershed assessment during sanitary surveys, as described in Sec.  
141.711(d) of this chapter.
    (iii) The determination of whether the mean Cryptosporidium level is 
greater than 0.01 oocysts/L both after the initial and after the second 
round of source water monitoring for each unfiltered system, as 
described in Sec.  141.712(a) of this chapter.
    (7) Ground water rule--(i) Sanitary surveys. The month and year in 
which the most recent sanitary survey was completed or, for a State that 
uses a phased review process, the date the last element of the 
applicable eight elements was evaluated under Sec.  142.16(o)(2) for 
each ground water system.
    (ii) Corrective action requirements. For any corrective action under 
Sec.  141.403(a) of this chapter, the date the ground water system 
completed corrective action.
    (iii) Compliance monitoring. All ground water systems providing at 
least 4-log treatment of viruses (using inactivation, removal, or a 
State-approved combination of 4-log virus inactivation and removal) 
before or at the first customer for any ground water source(s).
    (d) The reports submitted pursuant to this section shall be made 
available by the State to the public for inspection at one or more 
locations within the State.

[41 FR 2918, Jan. 20, 1976]

    Editorial Note: For Federal Register citations affecting Sec.  
142.15, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  142.16  Special primacy requirements.

    (a) State public notification requirements. (1) Each State that has 
primary enforcement authority under this part must submit complete and 
final requests for approval of program revisions to adopt the 
requirements of subpart Q of part 141 of this chapter, using

[[Page 756]]

the procedures in Sec.  142.12(b) through (d). At its option, a State 
may, by rule, and after notice and comment, establish alternative public 
notification requirements with respect to the form and content of the 
public notice required under subpart Q of part 141 of this chapter. The 
alternative requirements must provide the same type and amount of 
information required under subpart Q and must meet the primacy 
requirements under Sec.  142.10.
    (2) As part of the revised primacy program, a State must also 
establish enforceable requirements and procedures when the State adds to 
or changes the requirements under:
    (i) Table 1 to 40 CFR 141.201(a)(Item (3)(v))--To require public 
water systems to give a public notice for violations or situations other 
than those listed in appendix A of subpart Q of part 141 of this 
chapter;
    (ii) 40 CFR 141.201(c)(2)--To allow public water systems, under the 
specific circumstances listed in Sec.  141.201(c)(2), to limit the 
distribution of the public notice to persons served by the portion of 
the distribution system that is out of compliance;
    (iii) Table 1 of 40 CFR 141.202(a) (Items (5), (6), and (9))--To 
require public water systems to give a Tier 1 public notice (rather than 
a Tier 2 or Tier 3 notice) for violations or situations listed in 
appendix A of subpart Q of part 141 of this chapter;
    (iv) 40 CFR 141.202(b)(3)--To require public water systems to comply 
with additional Tier 1 public notification requirements set by the State 
subsequent to the initial 24-hour Tier 1 notice, as a result of their 
consultation with the State required under Sec. Sec.  141.202(b)(2);
    (v) 40 CFR 141.202(c), 141.203(c) and 141.204(c)--To require a 
different form and manner of delivery for Tier 1, 2 and 3 public 
notices.
    (vi) Table 1 to 40 CFR 141.203(a) (Item (2))--To require the public 
water systems to provide a Tier 2 public notice (rather than Tier (3)) 
for monitoring or testing procedure violations specified by the State;
    (vii) 40 CFR 141.203(b)(1)--To grant public water systems an 
extension up to three months for distributing the Tier 2 public notice 
in appropriate circumstances (other than those specifically excluded in 
the rule);
    (viii) 40 CFR 141.203(b)(2)--To grant a different repeat notice 
frequency for the Tier 2 public notice in appropriate circumstances 
(other than those specifically excluded in the rule), but no less 
frequently than once per year;
    (ix) 40 CFR 141.203(b)(3)--To respond within 24 hours to a request 
for consultation by the public water system to determine whether a Tier 
1 (rather than a Tier 2) notice is required for a turbidity MCL 
violation under Sec.  141.13(b) or a SWTR/IESWTR TT violation due to a 
single exceedance of the maximum allowable turbidity limit;
    (x) 40 CFR 141.205(c)--To determine the specific multilingual 
requirement for a public water system, including defining ``large 
proportion of non-English-speaking consumers.''
    (b) Requirements for States to adopt 40 CFR part 141, subpart H 
Filtration and Disinfection. In addition to the general primacy 
requirements enumerated elsewhere in this part, including the 
requirement that State provisions are no less stringent than the federal 
requirements, an application for approval of a State program revision 
that adopts 40 CFR part 141, subpart H Filtration and Disinfection, must 
contain the information specified in this paragraph (b), except that 
States which require without exception all public water systems using a 
surface water source or a ground water source under the direct influence 
of surface water to provide filtration need not demonstrate that the 
State program has provisions that apply to systems which do not provide 
filtration treatment. However, such States must provide the text of the 
State statutes or regulations which specifies that all public water 
systems using a surface water source or a ground water source under the 
direct influence of surface water must provide filtration.
    (1) Enforceable requirements. (i) In addition to adopting criteria 
no less stringent than those specified in part 141, subpart H of this 
chapter, the State's application must include enforceable design and 
operating criteria

[[Page 757]]

for each filtration treatment technology allowed or a procedure for 
establishing design and operating conditions on a system-by-system basis 
(e.g., a permit system).
    (ii) States must have the appropriate rules or other authority to 
assure that PWSs respond in writing to significant deficiencies outlined 
in sanitary survey reports required under paragraph (b)(3) of this 
section no later than 45 days after receipt of the report, indicating 
how and on what schedule the system will address significant 
deficiencies noted in the survey.
    (iii) States must have the appropriate rules or other authority to 
assure that PWSs take necessary steps to address significant 
deficiencies identified in sanitary survey reports required under 
paragraph (b)(3) of this section, if such deficiencies are within the 
control of the PWS and its governing body.
    (2) State practices or procedures. (i) A State application for 
program revision approval must include a description of how the State 
will accomplish the following:
    (A) Section 141.70(c) (qualification of operators)--Qualify 
operators of systems using a surface water source or a ground water 
source under the direct influence of surface water.
    (B) Determine which systems using a ground water source are under 
the direct influence of surface water by June 29, 1994 for community 
water systems and by June 29, 1999 for non-community water systems.
    (C) Section 141.72(b)(1) (achieving required Giardia lamblia and 
virus removal in filtered systems)--Determine that the combined 
treatment process incorporating disinfection treatment and filtration 
treatment will achieve the required removal and/or inactivation of 
Giardia lamblia and viruses.
    (D) Section 141.74(a) (State approval of parties to conduct 
analyses)--approve parties to conduct pH, temperature, turbidity, and 
residual disinfectant concentration measurements.
    (E) Determine appropriate filtration treatment technology for source 
waters of various qualities.
    (ii) For a State which does not require all public water systems 
using a surface water source or ground water source under the direct 
influence of surface water to provide filtration treatment, a State 
application for program revision approval must include a description of 
how the State will accomplish the following:
    (A) Section 141.71(b)(2) (watershed control program)--Judge the 
adequacy of watershed control programs.
    (B) Section 141.71(b)(3) (approval of on-site inspectors)--Approve 
on-site inspectors other than State personnel and evaluate the results 
of on-site inspections.
    (iii) For a State which adopts any of the following discretionary 
elements of part 141 of this chapter, the application must describe how 
the State will:
    (A) Section 141.72 (interim disinfection requirements)--Determine 
interim disinfection requirements for unfiltered systems which the State 
has determined must filter which will be in effect until filtration is 
installed.
    (B) Section 141.72 (a)(4)(ii) and (b)(3)(ii) (determination of 
adequate disinfection in system without disinfectant residual)--
Determine that a system is unable to measure HPC but is still providing 
adequate disinfection in the distribution system, as allowed by Sec.  
141.72(a)(4)(ii) for systems which do not provide filtration treatment 
and Sec.  141.72(b)(3)(ii) for systems which do provide filtration 
treatment.
    (C) Section 141.73 (a)(1) and (b)(1) (alternative turbidity limit)--
Determine whether an alternative turbidity limit is appropriate and what 
the level should be as allowed by Sec.  141.73(a)(1) for a system using 
conventiona1 filtration treatment or direct filtration and by Sec.  
141.73(b)(1) for a system using slow sand filtration.
    (D) Section 141.73(d) (alternative filtration technologies)--
Determine that a public water system has demonstrated that an alternate 
filtration technology, in combination with disinfection treatment, 
achieves adequate removal and/or disinfection of Giardia lamblia and 
viruses.
    (E) Section 141.74(a)(5) (alternate analytical method for 
chlorine)--Approve DPD colorimetric test kits for free and combined 
chlorine measurement or approve calibration of automated methods by the 
Indigo Method for ozone determination.

[[Page 758]]

    (F) Section 141.74 (b)(2) and (c)(1) (approval of continuous 
turbidity monitoring)--Approve continuous turbidity monitoring, as 
allowed by Sec.  141.74(b)(2) for a public water system which does not 
provide filtration treatment and Sec.  141.74(c)(1) for a system which 
does provide filtration treatment.
    (G) Section 141.74 (b)(6)(i) and (c)(3)(i) (approval of alternate 
disinfectant residual concentration sampling plans)--Approve alternate 
disinfectant residual concentration sampling plans for systems which 
have a combined ground water and surface water or ground water and 
ground water under the direct influence of a surface water distribution 
system, as allowed by Sec.  141.74(b)(6)(i) for a public water system 
which does not provide filtration treatment and Sec.  141.74(c)(3)(i) 
for a public water system which does provide filtration treatment.
    (H) Section 141.74(c)(1) (reduction of turbidity monitoring)--Decide 
whether to allow reduction of turbidity monitoring for systems using 
slow sand filtration, an approved alternate filtration technology or 
serving 500 people or fewer.
    (I) Section 141.75 (a)(2)(ix) and (b)(2)(iv) (reduced reporting)--
Determine whether reduced reporting is appropriate, as allowed by Sec.  
141.75(a)(2)(ix) for a public water system which does not provide 
filtration treatment and Sec.  141.75(b)(2)(iv) for a public water 
system which does provide filtration treatment.
    (iv) For a State which does not require all public water systems 
using a surface water source or ground water source under the direct 
influence of surface water to provide filtration treatment and which 
uses any of the following discretionary provisions, the application must 
describe how the State will:
    (A) Section 141.71(a)(2)(i) (source water turbidity requirements)--
Determine that an exceedance of turbidity limits in source water was 
caused by circumstances that were unusual and unpredictable.
    (B) Section 141.71(b)(1)(i) (monthly CT compliance requirements)--
Determine whether failure to meet the requirements for monthly CT 
compliance in Sec.  141.72(a)(1) was caused by circumstances that were 
unusual and unpredictable.
    (C) Section 141.71(b)(1)(iii) (residual disinfectant concentration 
requirements)--Determine whether failure to meet the requirements for 
residual disinfectant concentration entering the distribution system in 
Sec.  141.72(a)(3)(i) was caused by circumstances that were unusual and 
unpredictable.
    (D) Section 141.71(b)(1)(iv) (distribution system disinfectant 
residual concentration requirements)--Determine whether failure to meet 
the requirements for distribution system residual disinfectant 
concentration in Sec.  141.72(a)(4) was related to a deficiency in 
treatment.
    (E) Section 141.71(b)(4) (system modification to prevent waterborne 
disease outbreak)--Determine that a system, after having been identified 
as the source of a waterborne disease outbreak, has been modified 
sufficiently to prevent another such occurrence.
    (F) Section 141.71(b)(5) (total coliform MCL)--Determine whether a 
total coliform MCL violation was caused by a deficiency in treatment.
    (G) Section 141.72(a)(1) (disinfection requirements)--Determine that 
different ozone, chloramine, or chlorine dioxide CT99.9 
values or conditions are adequate to achieve required disinfection.
    (H) Section 141.72(a)(2)(ii) (shut-off of water to distribution 
system)--Determine whether a shut-off of water to the distribution 
system when the disinfectant residual concentration entering the 
distribution system is less than 0.2 mg/1 will cause an unreasonable 
risk to health or interfere with fire protection.
    (I) Section 141.74(b)(1) (coliform monitoring)--Determine that 
coliform monitoring which otherwise might be required is not feasible 
for a system.
    (J) Section 141.74(b), table 3.1 (disinfection with chloramines)--
Determine the conditions to be met to insure 99.99 percent removal and/
or inactivation of viruses in systems which use either preformed 
chloramines or chloramines for which ammonia is added to the water 
before chlorine, as allowed by table 3.1.

[[Page 759]]

    (3) Sanitary survey. In addition to the general requirements for 
sanitary surveys contained in Sec.  142.10(b)(2), an application must 
describe how the State will implement a sanitary survey program that 
meets the requirements in paragraphs (b)(3)(i) through (v) of this 
section. For the purposes of this paragraph, ``sanitary survey'' means 
an onsite review of the water source (identifying sources of 
contamination using results of source water assessments where 
available), facilities, equipment, operation, maintenance, and 
monitoring compliance of a public water system to evaluate the adequacy 
of the system, its sources and operations and the distribution of safe 
drinking water.
    (i) The State must conduct sanitary surveys for all surface water 
systems (including groundwater under the influence) that address the 
eight sanitary survey components listed in paragraphs (b)(3)(i)(A) 
through (H) of this section no less frequently than every three years 
for community systems and no less frequently than every five years for 
noncommunity systems. The State may allow sanitary surveys conducted 
after December 1995 to serve as the first set of required sanitary 
surveys if the surveys address the eight sanitary survey components 
listed in paragraphs (b)(3)(i)(A) through (H) of this section.
    (A) Source.
    (B) Treatment.
    (C) Distribution system.
    (D) Finished water storage.
    (E) Pumps, pump facilities, and controls.
    (F) Monitoring and reporting and data verification.
    (G) System management and operation.
    (H) Operator compliance with State requirements.
    (ii) For community systems determined by the State to have 
outstanding performance based on prior sanitary surveys, subsequent 
sanitary surveys may be conducted no less than every five years. In its 
primacy application, the State must describe how it will decide whether 
a system has outstanding performance and is thus eligible for sanitary 
surveys at a reduced frequency.
    (iii) Components of a sanitary survey may be completed as part of a 
staged or phased state review process within the established frequency.
    (iv) When conducting sanitary surveys for systems required to comply 
with the disinfection profiling requirements in Sec.  141.172 of this 
chapter, the State must also review the disinfection profile as part of 
the sanitary survey.
    (v) In its primacy application, the State must describe how it will 
decide whether a deficiency identified during a sanitary survey is 
significant for the purposes of paragraph (b)(1)(ii) of this section.
    (c) Total coliform requirements. In addition to meeting the general 
primacy requirements of this part, an application for approval of a 
State program revision that adopts the requirements of the national 
primary drinking water regulation for total coliforms must contain the 
following information:
    (1) The application must describe the State's plan for determining 
whether sample siting plans are acceptable (including periodic reviews), 
as required by Sec.  141.21(a)(1).
    (2) The national primary drinking water regulation for total 
coliforms in part 141 gives States the option to impose lesser 
requirements in certain circumstances, which are listed below. If a 
State chooses to exercise any of these options, its application for 
approval of a program revision must include the information listed below 
(the State need only provide the information listed for those options it 
has chosen to use).
    (i) Section 141.21(a)(2) (Reduced monitoring requirements for 
community water systems serving 1,000 or fewer persons)--A description 
of how the State will determine whether it is appropriate to reduce the 
total coliform monitoring frequency for such systems using the criteria 
in Sec.  141.21(a)(2) and how it will determine the revised frequency.
    (ii) Section 141.21(a)(3)(i) (Reduced monitoring requirements for 
non-community water systems using ground water and serving 1,000 persons 
or fewer)--A description of how the State will determine whether it is 
appropriate to reduce the total coliform monitoring frequency for such 
systems

[[Page 760]]

using the criteria in Sec.  141.21(a)(3)(i) and how it will determine 
the revised frequency.
    (iii) Section 141.21(a)(3)(ii) (Reduced monitoring for non-community 
water systems using ground water and serving more than 1,000 persons)--A 
description of how the State will determine whether it is appropriate to 
reduce the total coliform monitoring frequency for non-community water 
systems using only ground water and serving more than 1,000 persons 
during any month the system serves 1,000 persons or fewer and how it 
will determine the revised frequency.
    (iv) Section 141.21(a)(5) (Waiver of time limit for sampling after a 
turbidity sampling result exceeds 1 NTU)--A description of how the State 
will determine whether it is appropriate to waive the 24-hour time 
limit.
    (v) Section 141.21(b)(1) (Waiver of time limit for repeat samples)--
A description of how the State will determine whether it is appropriate 
to waive the 24-hour time limit and how it will determine what the 
revised time limit will be.
    (vi) Section 141.21(b)(3) (Alternative repeat monitoring 
requirements for systems with a single service connection)--A 
description of how the State will determine whether it is appropriate to 
allow a system with a single service connection to use an alternative 
repeat monitoring scheme, as provided in Sec.  141.21(b)(3), and what 
the alternative requirements will be.
    (vii) Section 141.21(b)(5) (Waiver of requirement to take five 
routine samples the month after a system has a total coliform-positive 
sample)--A description of how the State will determine whether it is 
appropriate to waive the requirement for certain systems to collect five 
routine samples during the next month it serves water to the public, 
using the criteria in Sec.  141.21(b)(5).
    (viii) Section 141.21(c) (Invalidation of total coliform-positive 
samples)--A description of how the State will determine whether it is 
appropriate to invalidate a total coliform-positive sample, using the 
criteria in Sec.  141.21(c).
    (ix) Section 141.21(d) (Sanitary surveys)--A description of the 
State's criteria and procedures for approving agents other than State 
personnel to conduct sanitary surveys.
    (x) Section 141.21(e)(2) (Waiver of fecal coliform or E. coli 
testing on a total coliform-positive sample)--A description of how the 
State will determine whether it is appropriate to waive fecal coliform 
or E. coli testing on a total coliform-positive sample.
    (d) Requirements for States to adopt 40 CFR part 141, subpart I--
Control of Lead and Copper. An application for approval of a State 
program revision which adopts the requirements specified in 40 CFR part 
141, subpart I, must contain (in addition to the general primacy 
requirements enumerated elsewhere in this part, including the 
requirement that State regulations be at least as stringent as the 
federal requirements) a description of how the State will accomplish the 
following program requirements:
    (1) Section 141.82--State designation of optimal corrosion control.
    (i) Sections 141.82(d), 141.82(f), and 141.82(h)--Designating 
optimal corrosion control treatment methods, optimal water quality 
parameters, and modifications thereto.
    (ii) Section 141.82(g)--Designating an alternative approach for 
aggregating multiple measurements collected during the same day for a 
water quality parameter at a sampling location, if the State elects to 
adopt a formula other than the one specified in Sec.  141.82(g)(1) of 
this chapter.
    (2) Sections 141.83(b)(2) and 141.83(b)(4)--Designating source water 
treatment methods, maximum permissible source water levels for lead and 
copper and modifications thereto.
    (3) Section 141.90(e)--Verifying compliance with lead service line 
replacement schedules and completion of all partial lead service line 
replacement activities.
    (4) Section 141.86(d)(4)(iv)(A)--Designating an alternative period 
for sample collection for community water systems subject to reduced 
monitoring.
    (e) An application for approval of a State program revision which 
adopts the requirements specified in Sec. Sec.  141.11, 141.23, 141.24, 
141.32, 141.61, and 141.62 for a newly regulated contaminant must 
contain the following (in addition to

[[Page 761]]

the general primacy requirements enumerated elsewhere in this part, 
including the requirement that State regulations be at least as 
stringent as the Federal requirements):
    (1) If a State chooses to issue waivers from the monitoring 
requirements in Sec. Sec.  141.23 and 141.24, the State shall describe 
the procedures and criteria which it will use to review waiver 
applications and issue waiver determinations.
    (i) The procedures for each contaminant or class of contaminants 
shall include a description of:
    (A) The waiver application requirements;
    (B) The State review process for ``use'' waivers and for 
``susceptibility'' waivers; and
    (C) The State decision criteria, including the factors that will be 
considered in deciding to grant or deny waivers. The decision criteria 
must include the factors specified in Sec. Sec.  141.24(f)(8) and 
141.24(h)(6).
    (ii) The State must specify the monitoring data and other 
documentation required to demonstrate that the contaminant is eligible 
for a ``use'' and/or ``susceptibility'' waiver.
    (2) A monitoring plan for the initial monitoring period by which the 
State will assure all systems complete the required initial monitoring 
within the regulatory deadlines.
    Note: States may update their monitoring plan submitted under the 
Phase II Rule or simply note in their application that they will use the 
same monitoring plan for the Phase V Rule.
    (i) The initial monitoring plan must describe how systems will be 
scheduled during the initial monitoring period and demonstrate that the 
analytical workload on certified laboratories for each of the three 
years has been taken into account, to assure that the State's plan will 
result in a high degree of monitoring compliance and that as a result 
there is a high probability of compliance and will be updated as 
necessary.
    (ii) The State must demonstrate that the initial monitoring plan is 
enforceable under State law.
    (f) Consumer Confidence Report requirements. (1) Each State that has 
primary enforcement responsibility must adopt the requirements of 40 CFR 
part 141, subpart O no later than August 21, 2000. States must submit 
revised programs to EPA for approval using the procedures in Sec.  
142.12(b) through (d).
    (2) Each State that has primary enforcement responsibility must make 
reports submitted to the States in compliance with 40 CFR 141.155(c) 
available to the public upon request.
    (3) Each State that has primary enforcement responsibility must 
maintain a copy of the reports for a period of one year and the 
certifications obtained pursuant to 40 CFR 141.155(c) for a period of 5 
years.
    (4) Each State that has primary enforcement responsibility must 
report violations of this subpart in accordance with the requirements of 
Sec.  142.15(a)(1).
    (g) Requirements for States to adopt 40 CFR part 141, Subpart P--
Enhanced Filtration and Disinfection--Systems Serving 10,000 or More 
People. In addition to the general primacy requirements enumerated 
elsewhere in this part, including the requirement that State provisions 
are no less stringent than the Federal requirements, an application for 
approval of a State program revision that adopts 40 CFR part 141, 
Subpart P Enhanced Filtration and Disinfection--Systems Serving 10,000 
or More People, must contain the information specified in this 
paragraph:
    (1) Enforceable requirements. States must have the appropriate rules 
or other authority to require PWSs to conduct a Composite Correction 
Program (CCP) and to assure that PWSs implement any followup 
recommendations that result as part of the CCP. The CCP consists of two 
elements--a Comprehensive Performance Evaluation (CPE) and Comprehensive 
Technical Assistance (CTA). A CPE is a thorough review and analysis of a 
plant's performance-based capabilities and associated administrative, 
operation and maintenance practices. It is conducted to identify factors 
that may be adversely impacting a plant's capability to achieve 
compliance and emphasizes approaches that can be implemented without 
significant capital improvements. A CTA is the performance improvement 
phase that is implemented if the CPE results indicate improved 
performance potential. During

[[Page 762]]

the CTA phase, the system must identify and systematically address 
plant-specific factors. The CTA is a combination of utilizing CPE 
results as a basis for followup, implementing process control priority-
setting techniques and maintaining long-term involvement to 
systematically train staff and administrators.
    (2) State practices or procedures. (i) Section 141.172(a)(3) of this 
chapter--How the State will approve a more representative annual data 
set than the data set determined under Sec.  141.172 (a)(1) or (2) of 
this chapter for the purpose of determining applicability of the 
requirements of Sec.  141.172 of this chapter.
    (ii) Section 141.172(b)(5) of this chapter--How the State will 
approve a method to calculate the logs of inactivation for viruses for a 
system that uses either chloramines or ozone for primary disinfection.
    (iii) Section 141.172(c) of this chapter--How the State will consult 
with PWSs to evaluate modifications to disinfection practice.
    (iv) Section 141.173(b) of this chapter--For filtration technologies 
other than conventional filtration treatment, direct filtration, slow 
sand filtration, or diatomaceous earth filtration, how the State will 
determine that a public water system may use a filtration technology if 
the PWS demonstrates to the State, using pilot plant studies or other 
means, that the alternative filtration technology, in combination with 
disinfection treatment that meets the requirements of Sec.  141.172(b) 
of this chapter, consistently achieves 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts and 99.99 percent removal and/or 
inactivation of viruses, and 99 percent removal of Cryptosporidium 
oocysts. For a system that makes this demonstration, how the State will 
set turbidity performance requirements that the system must meet 95 
percent of the time and that the system may not exceed at any time at a 
level that consistently achieves 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts, 99.99 percent removal and/or 
inactivation of viruses, and 99 percent removal of Cryptosporidium 
oocysts.
    (h) Requirements for States to adopt 40 CFR part 141, subpart L. In 
addition to the general primacy requirements elsewhere in this part, 
including the requirement that State regulations be at least as 
stringent as federal requirements, an application for approval of a 
State program revision that adopts 40 CFR part 141, subpart L, must 
contain a description of how the State will accomplish the following 
program requirements:
    (1) Section 141.64(b)(2) of this chapter (interim treatment 
requirements). Determine any interim treatment requirements for those 
systems electing to install GAC or membrane filtration and granted 
additional time to comply with Sec.  141.64 of this chapter.
    (2) Section 141.130(c) of this chapter (qualification of operators). 
Qualify operators of public water systems subject to 40 CFR part 141, 
subpart L. Qualification requirements established for operators of 
systems subject to 40 CFR part 141, subpart H--Filtration and 
Disinfection may be used in whole or in part to establish operator 
qualification requirements for meeting 40 CFR part 141, subpart L 
requirements if the State determines that the 40 CFR part 141, subpart H 
requirements are appropriate and applicable for meeting subpart L 
requirements.
    (3) Section 141.131(c)(2) of this chapter (DPD colorimetric test 
kits). Approve DPD colorimetric test kits for free and total chlorine 
measurements. State approval granted under Sec.  141.74(a)(2) of this 
chapter for the use of DPD colorimetric test kits for free chlorine 
testing is acceptable for the use of DPD test kits in measuring free 
chlorine residuals as required in 40 CFR part 141, subpart L.
    (4) Sections 141.131(c)(3) and (d) of this chapter (State approval 
of parties to conduct analyses). Approve parties to conduct pH, bromide, 
alkalinity, and residual disinfectant concentration measurements. The 
State's process for approving parties performing water quality 
measurements for systems subject to 40 CFR part 141, subpart H 
requirements in paragraph (b)(2)(i)(D) of this section may be used for 
approving

[[Page 763]]

parties measuring water quality parameters for systems subject to 
subpart L requirements, if the State determines the process is 
appropriate and applicable.
    (5) Section 141.132(a)(2) of this chapter (multiple wells as a 
single source). Define the criteria to use to determine if multiple 
wells are being drawn from a single aquifer and therefore be considered 
a single source for compliance with monitoring requirements.
    (6) Approve alternate minimum TOC removal (Step 2) requirements, as 
allowed under the provisions of Sec.  141.135(b) of this chapter.
    (i) Requirements for States to adopt 40 CFR part 141, Sec.  141.76 
Recycle provisions. In addition to the general primacy requirements 
enumerated elsewhere in this part, including the requirement that the 
State provisions are no less stringent than the federal requirements, an 
application for approval of a State program revision that adopts 40 CFR 
part 141, Sec.  141.76 Recycle Provisions must contain the information 
specified in this paragraph:
    (1) State practices or procedures. (i) Section 141.76(d) of this 
chapter--States must have the proper rules and authority to use Sanitary 
Surveys, comprehensive performance evaluations (CPEs), other 
inspections, or other activities to evaluate recycle data maintained by 
systems under Sec.  141.76(d) of this chapter and require modifications 
to recycle practices.
    (ii) [Reserved]
    (2) [Reserved]
    (j) An application for approval of a State program revision which 
adopts the requirements specified in Sec. Sec.  141.11, 141.23, 141.24, 
141.32, 141.61 and 141.62 for an existing regulated contaminant must 
contain the following (in addition to the general primacy requirements 
enumerated elsewhere in this part, including the requirement that State 
regulations be at least as stringent as the federal requirements):
    (1) If a State chooses to issue waivers from the monitoring 
requirements in Sec. Sec.  141.23 and 141.24, the State shall describe 
the procedures and criteria, that it will use to review waiver 
applications and issue waiver determinations. The State shall provide 
the same information required in paragraph (e)(1)(i) and (ii) of this 
section. States may update their existing waiver criteria or use the 
requirements submitted under the National Primary Drinking Water 
Regulations for the inorganic and organic contaminants (i.e., Phase II/V 
rule) in 16(e) of this section. States may simply note in their 
application any revisions to existing waiver criteria or note that the 
same procedures to issue waivers will be used.
    (2) A monitoring plan by which the State will ensure all systems 
complete the required monitoring by the regulatory deadlines. States may 
update their existing monitoring plan or use the same monitoring plan 
submitted under the National Primary Drinking Water Regulations for the 
inorganic and organic contaminants (i.e., Phase II/V rule) in 16(e) of 
this section. States may simply note in their application any revisions 
to an existing monitoring plan or note that the same monitoring plan 
will be used. The State must demonstrate that the monitoring plan is 
enforceable under State law.
    (k) States establish the initial monitoring requirements for new 
systems and new sources. States must explain their initial monitoring 
schedules and how these monitoring schedules ensure that public water 
systems and sources comply with MCL's and monitoring requirements. 
States must also specify the time frame in which new systems will 
demonstrate compliance with the MCLs.
    (l) An application for approval of a State program revision for 
radionuclides which adopts the requirements specified in Sec.  
141.26(a)(2)(ii)(C) of this chapter must contain the following (in 
addition to the general primacy requirements enumerated in this part, 
including that State regulations be at least as stringent as the Federal 
requirements):
    (1) If a State chooses to use grandfathered data in the manner 
described in Sec.  141.26(a)(2)(ii)(C) of this chapter, then the State 
must describe the procedures and criteria which it will use to make 
these determinations (whether distribution system or entry point 
sampling points are used).
    (i) The decision criteria that the State will use to determine that 
data collected in the distribution system are

[[Page 764]]

representative of the drinking water supplied from each entry point to 
the distribution system. These determinations must consider:
    (A) All previous monitoring data.
    (B) The variation in reported activity levels.
    (C) Other factors affecting the representativeness of the data (e.g. 
geology).
    (ii) [Reserved]
    (2) A monitoring plan by which the State will assure all systems 
complete the required monitoring within the regulatory deadlines. States 
may update their existing monitoring plan or use the same monitoring 
plan submitted for the requirements in Sec.  142.16(e)(2) under the 
national primary drinking water regulations for the inorganic and 
organic contaminants (i.e. the phase II/V rules). States may note in 
their application any revision to an existing monitoring plan or note 
that the same monitoring plan will be used. The State must demonstrate 
that the monitoring plan is enforceable under State law.
    (m) Requirements for States to adopt 40 CFR part 141, subparts U and 
V. In addition to the general primacy requirements elsewhere in this 
part, including the requirements that State regulations be at least as 
stringent as federal requirements, an application for approval of a 
State program revision that adopts 40 CFR part 141, subparts U and V, 
must contain a description of how the State will implement a procedure 
for addressing modification of wholesale system and consecutive system 
monitoring on a case-by-case basis for part 141 subpart V outside the 
provisions of Sec.  141.29 of this chapter, if the State elects to use 
such an authority. The procedure must ensure that all systems have at 
least one compliance monitoring location.
    (n) Requirements for States to adopt 40 CFR part 141, subpart W. In 
addition to the general primacy requirements elsewhere in this part, 
including the requirements that State regulations be at least as 
stringent as Federal requirements, an application for approval of a 
State program revision that adopts 40 CFR part 141, subpart W, must 
contain a description of how the State will accomplish the following 
program requirements where allowed in State programs.
    (1) Approve an alternative to the E. coli levels that trigger 
Cryptosporidium monitoring by filtered systems serving fewer than 10,000 
people, as described in Sec.  141.701(a)(5).
    (2) Assess significant changes in the watershed and source water as 
part of the sanitary survey process and determine appropriate follow-up 
action for systems, as described in Sec.  141.711(d) of this chapter.
    (3) Approve watershed control programs for the 0.5-log treatment 
credit in the microbial toolbox, as described in Sec.  141.716(a) of 
this chapter.
    (4) Approve protocols for demonstration of performance treatment 
credits in the microbial toolbox, as allowed under Sec.  141.718(c) of 
this chapter.
    (5) Approve protocols for alternative ozone and chlorine dioxide CT 
values in the microbial toolbox, as allowed under Sec.  141.720(c) of 
this chapter.
    (6) Approve an alternative approach to UV reactor validation testing 
in the microbial toolbox, as allowed under Sec.  141.720(d)(2)(iii) of 
this chapter.
    (o) Requirements for States to adopt 40 CFR part 141, subpart S. In 
addition to the general primacy requirements specified elsewhere in this 
part, including the requirement that State regulations are no less 
stringent than the Federal requirements, an application for approval of 
a State program revision that adopts 40 CFR part 141, subpart S, must 
contain the information specified in this paragraph (o).
    (1) Legal authority. The application for primacy must demonstrate 
the State has:
    (i) The authority contained in statute or regulation to ensure that 
ground water systems conduct source water monitoring under Sec. Sec.  
141.402(a)(2), 141.402(a)(3) and 141.402(a)(4)(ii)(A) of this chapter.
    (ii) The authority contained in statute or regulation to ensure that 
ground water systems take the appropriate corrective actions including 
interim measures, if necessary, needed to address significant 
deficiencies.
    (iii) The authority contained in statute or regulation to ensure 
that ground water systems take the appropriate corrective actions, 
including interim

[[Page 765]]

measures if necessary, to address any source water fecal contamination 
identified during source water monitoring under Sec.  141.402 of this 
chapter.
    (iv) The authority contained in statute or regulation to ensure that 
ground water systems consult with the State regarding corrective 
action(s).
    (2) State practices or procedures for sanitary surveys. In addition 
to the general requirements for sanitary surveys contained in Sec.  
142.10(b)(2), a primacy application must describe how the State will 
implement a sanitary survey program that meets the requirements of 
paragraph (o)(2)(i) of this section. A ``sanitary survey,'' as conducted 
by the State, includes but is not limited to, an onsite review of the 
water source(s) (identifying sources of contamination by using results 
of source water assessments or other relevant information where 
available), facilities, equipment, operation, maintenance, and 
monitoring compliance of a public water system to evaluate the adequacy 
of the system, its sources and operations and the distribution of safe 
drinking water.
    (i) The State must conduct sanitary surveys that address the eight 
sanitary survey components listed in this section no less frequently 
than every three years for community water systems, except as provided 
in paragraph (o)(2)(iii) of this section, and every five years for non-
community water systems. The State may conduct more frequent sanitary 
surveys for any system. The initial sanitary survey for each community 
water system must be conducted by December 31, 2012, unless the system 
meets the requirements of paragraph (o)(2)(iii) of this section. The 
initial sanitary survey for each community water system that meets the 
requirements of paragraph (o)(2)(iii) of this section and for each non-
community water system must be conducted by December 31, 2014. The 
sanitary survey must include an evaluation of each of the following 
elements as applicable:
    (A) Source,
    (B) Treatment,
    (C) Distribution system,
    (D) Finished water storage,
    (E) Pumps, pump facilities, and controls,
    (F) Monitoring, reporting, and data verification,
    (G) System management and operation, and
    (H) Operator compliance with State requirements.
    (ii) The State may use a phased review process to meet the 
requirements of (o)(2)(i) of this section if all the applicable elements 
of paragraphs (o)(2)(i)(A) through (o)(2)(i)(H) of this section are 
evaluated within the required interval.
    (iii) The State may conduct sanitary surveys once every five years 
for community water systems if the system either provides at least 4-log 
treatment of viruses (using inactivation, removal, or a State-approved 
combination of 4-log inactivation and removal) before or at the first 
customer for all its ground water sources, or if it has an outstanding 
performance record, as determined by the State and documented in 
previous sanitary surveys and has no history of total coliform MCL or 
monitoring violations under Sec.  141.21 of this chapter since the last 
sanitary survey. In its primacy application, the State must describe how 
it will determine whether a community water system has an outstanding 
performance record.
    (iv) The State must define and describe in its primacy application 
at least one specific significant deficiency in each of the eight 
sanitary survey elements in paragraphs (o)(2)(i)(A) through (o)(2)(i)(H) 
of this section. Significant deficiencies include, but are not limited 
to, defects in design, operation, or maintenance, or a failure or 
malfunction of the sources, treatment, storage, or distribution system 
that the State determines to be causing, or have potential for causing, 
the introduction of contamination into the water delivered to consumers.
    (v) As a condition of primacy, the State must provide ground water 
systems with written notice describing any significant deficiencies no 
later than 30 days after the State identifies the significant 
deficiency. The notice may specify corrective actions and deadlines for 
completion of corrective actions. The State may provide the written 
notice at the time of the sanitary survey.
    (3) State practices or procedures for source water microbial 
monitoring. The

[[Page 766]]

State's primacy application must include a description of the following:
    (i) The criteria the State will use under Sec. Sec.  
141.402(a)(2)(i) and 141.402(d)(2) of this chapter for extending the 24-
hour time limit for a system to collect a ground water source sample to 
comply with the source water monitoring requirements.
    (ii) The criteria the State will use under Sec. Sec.  
141.402(a)(5)(i) and 141.402(a)(5)(ii) of this chapter to determine 
whether the cause of the total coliform-positive sample taken under 
Sec.  141.21(a) of this chapter is directly related to the distribution 
system.
    (iii) The criteria the State will use for determining whether to 
invalidate a fecal indicator-positive ground water source sample under 
Sec.  141.402(d)(1)(ii) of this chapter.
    (iv) The criteria the State will use to allow source water microbial 
monitoring at a location after treatment under Sec.  141.402(e)(1) of 
this chapter.
    (4) State practices or procedures for treatment technique 
requirements. As a condition of primacy, the State must verify that 
significant deficiencies or source water fecal contamination have been 
addressed. The State must verify within 30 days after the ground water 
system has reported to the State that it has completed corrective 
action. The State must verify either through written confirmation from 
the ground water system or a site visit by the State. Written notice 
from the ground water system under Sec.  141.405(a)(2) of this chapter 
may serve as this verification. The State's primacy application must 
include the following:
    (i) The process the State will use to determine that a ground water 
system achieves at least a 4-log treatment of viruses (using 
inactivation, removal, or a combination of inactivation and removal) 
before or at the first customer for a ground water source for systems 
that are not subject to the source water monitoring requirements of 
Sec.  141.402(a) of this chapter because the ground water system has 
informed the State that it provides at least 4-log treatment of viruses.
    (ii) The process the State will use to determine the minimum 
residual disinfectant concentration the system must provide prior to the 
first customer for systems using chemical disinfection.
    (iii) The State-approved alternative technologies that ground water 
systems may use alone or in combination with other approved technologies 
to achieve at least 4-log treatment of viruses (using inactivation, 
removal, or a State-approved combination of 4-log inactivation and 
removal) before or at the first customer for a ground water source.
    (iv) The monitoring and compliance requirements the State will 
require for ground water systems treating to at least 4-log treatment of 
viruses (using inactivation, removal, or a State-approved combination of 
inactivation and removal) before or at the first customer for State-
approved alternative treatment technologies.
    (v) The monitoring, compliance and membrane integrity testing 
requirements the State will require to demonstrate virus removal for 
ground water systems using membrane filtration technologies.
    (vi) The criteria, including public health-based considerations and 
incorporating on-site investigations and source water monitoring results 
the State will use to determine if a ground water system may discontinue 
4-log treatment of viruses (using inactivation, removal, or a State-
approved combination of inactivation and removal) before or at the first 
customer.
    (p) Requirements for States to adopt 40 CFR part 141, Subpart T--
Enhanced Filtration and Disinfection--Systems Serving Fewer Than 10,000 
People. In addition to the general primacy requirements enumerated 
elsewhere in this part, including the requirement that State provisions 
are no less stringent than the Federal requirements, an application for 
approval of a State program revision that adopts 40 CFR part 141, 
Subpart T--Enhanced Filtration and Disinfection--Systems Serving Fewer 
than 10,000 People, must contain the information specified in this 
paragraph:
    (1) Enforceable requirements. States must have rules or other 
authority to require systems to participate in a Comprehensive Technical 
Assistance (CTA) activity, the performance improvement phase of the 
Composite Correction Program (CCP). The State

[[Page 767]]

must determine whether a CTA must be conducted based on results of a CPE 
which indicate the potential for improved performance, and a finding by 
the State that the system is able to receive and implement technical 
assistance provided through the CTA. A CPE is a thorough review and 
analysis of a system's performance-based capabilities and associated 
administrative, operation and maintenance practices. It is conducted to 
identify factors that may be adversely impacting a plant's capability to 
achieve compliance. During the CTA phase, the system must identify and 
systematically address factors limiting performance. The CTA is a 
combination of utilizing CPE results as a basis for follow-up, 
implementing process control priority-setting techniques and maintaining 
long-term involvement to systematically train staff and administrators.
    (2) State practices or procedures. (i) Section 141.530-141.536--How 
the State will approve a more representative data set for optional TTHM 
and HAA5 monitoring and profiling.
    (ii) Section 141.535 of this chapter--How the State will approve a 
method to calculate the logs of inactivation for viruses for a system 
that uses either chloramines, ozone, or chlorine dioxide for primary 
disinfection.
    (iii) Section 141.542 of this chapter--How the State will consult 
with the system and approve significant changes to disinfection 
practices.
    (iv) Section 141.552 of this chapter--For filtration technologies 
other than conventional filtration treatment, direct filtration, slow 
sand filtration, or diatomaceous earth filtration, how the State will 
determine that a public water system may use a filtration technology if 
the PWS demonstrates to the State, using pilot plant studies or other 
means, that the alternative filtration technology, in combination with 
disinfection treatment that meets the requirements of Sec.  141.72(b) of 
this chapter, consistently achieves 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts and 99.99 percent removal and/or 
inactivation of viruses, and 99 percent removal of Cryptosporidium 
oocysts. For a system that makes this demonstration, how the State will 
set turbidity performance requirements that the system must meet 95 
percent of the time and that the system may not exceed at any time at a 
level that consistently achieves 99.9 percent removal and/or 
inactivation of Giardia lamblia cysts, 99.99 percent removal and/or 
inactivation of viruses, and 99 percent removal of Cryptosporidium 
oocysts.
    (q) Requirements for States to adopt 40 CFR part 141 subpart Y--
Revised Total Coliform Rule. In addition to the general primacy 
requirements elsewhere in this part, including the requirements that 
State regulations be at least as stringent as federal requirements, an 
application for approval of a State program revision that adopts 40 CFR 
part 141, subpart Y, must contain the information specified in this 
paragraph (q).
    (1) In their application to EPA for approval to implement the 
federal requirements, the primacy application must indicate what 
baseline and reduced monitoring provisions of 40 CFR part 141, subpart Y 
the State will adopt and must describe how they will implement 40 CFR 
part 141, subpart Y in these areas so that EPA can be assured that 
implementation plans meet the minimum requirements of the rule.
    (2) The State's application for primacy for subpart Y must include a 
written description for each provision included in paragraphs (q)(2)(i) 
through (ix) of this section.
    (i) Sample Siting Plans--The frequency and process used to review 
and revise sample siting plans in accordance with 40 CFR part 141, 
subpart Y to determine adequacy.
    (ii) Reduced Monitoring Criteria--An indication of whether the State 
will adopt the reduced monitoring provisions of 40 CFR part 141, subpart 
Y. If the State adopts the reduced monitoring provisions, it must 
describe the specific types or categories of water systems that will be 
covered by reduced monitoring and whether the State will use all or a 
reduced set of the criteria specified in Sec. Sec.  141.854(h)(2) and 
141.855(d)(1)(iii) of this chapter. For each of the reduced monitoring 
criteria, the State must describe how the criterion will be evaluated to 
determine when systems qualify.

[[Page 768]]

    (iii) Assessments and Corrective Actions--The process for 
implementing the new assessment and corrective action phase of the rule, 
including the elements in paragraphs (q)(2)(iii)(A) through (D) of this 
section.
    (A) Elements of Level 1 and Level 2 assessments. This must include 
an explanation of how the State will ensure that Level 2 assessments 
provide a more detailed examination of the system (including the 
system's monitoring and operational practices) than do Level 1 
assessments through the use of more comprehensive investigation and 
review of available information, additional internal and external 
resources, and other relevant practices.
    (B) Examples of sanitary defects.
    (C) Examples of assessment forms or formats.
    (D) Methods that systems may use to consult with the State on 
appropriate corrective actions.
    (iv) Invalidation of routine and repeat samples collected under 40 
CFR part 141, subpart Y--The criteria and process for invalidating total 
coliform and E. coli-positive samples under 40 CFR part 141, subpart Y. 
This description must include criteria to determine if a sample was 
improperly processed by the laboratory, reflects a domestic or other 
non-distribution system plumbing problem or reflects circumstances or 
conditions that do not reflect water quality in the distribution system.
    (v) Approval of individuals allowed to conduct Level 2 assessments 
under 40 CFR part 141, subpart Y--The criteria and process for approval 
of individuals allowed to conduct Level 2 assessments under 40 CFR part 
141, subpart Y.
    (vi) Special monitoring evaluation--The procedure for performing 
special monitoring evaluations during sanitary surveys for ground water 
systems serving 1,000 or fewer people to determine whether systems are 
on an appropriate monitoring schedule.
    (vii) Seasonal systems--How the State will identify seasonal 
systems, how the State will determine when systems on less than monthly 
monitoring must monitor, and what start-up provisions seasonal system 
must meet under 40 CFR part 141, subpart Y.
    (viii) Additional criteria for reduced monitoring--How the State 
will require systems on reduced monitoring to demonstrate:
    (A) Continuous disinfection entering the distribution system and a 
residual in the distribution system.
    (B) Cross connection control.
    (C) Other enhancements to water system barriers.
    (ix) Criteria for extending the 24-hour period for collecting repeat 
samples.--Under Sec. Sec.  141.858(a) and 141.853(c)(2) of this chapter, 
criteria for systems to use in lieu of case-by-case decisions to waive 
the 24-hour time limit for collecting repeat samples after a total 
coliform-positive routine sample, or to extend the 24-hour limit for 
collection of samples following invalidation. If the State elects to use 
only case-by-case waivers, the State does not need to develop and submit 
criteria.

[54 FR 15188, Apr. 17, 1989]

    Editorial Note: For Federal Register citations affecting Sec.  
142.16, see the List of CFR Sections Affected, which appears in the 
Finding Aids section of the printed volume and at www.fdsys.gov.



Sec.  142.17  Review of State programs and procedures for withdrawal 
of approved primacy programs.

    (a)(1) At least annually the Administrator shall review, with 
respect to each State determined to have primary enforcement 
responsibility, the compliance of the State with the requirements set 
forth in 40 CFR part 142, subpart B, and the approved State primacy 
program. At the time of this review, the State shall notify the 
Administrator of any State-initiated program changes (i.e., changes 
other than those to adopt new or revised EPA regulations), and of any 
transfer of all or part of its program from the approved State agency to 
any other State agency.
    (2) When, on the basis of the Administrator's review or other 
available information, the Administrator determines that a State no 
longer meets the requirements set forth in 40 CFR part 142, subpart B, 
the Administrator shall initiate proceedings to withdraw primacy 
approval. Among the factors the Administrator intends to consider as 
relevant to this determination are the following, where appropriate: 
whether

[[Page 769]]

the State has requested and has been granted, or is awaiting EPA's 
decision on, an extension under Sec.  142.12(b)(2) of the deadlines for 
meeting those requirements; and whether the State is taking corrective 
actions that may have been required by the Administrator. The 
Administrator shall notify the State in writing that EPA is initiating 
primacy withdrawal proceedings and shall summarize in the notice the 
information available that indicates that the State no longer meets such 
requirements.
    (3) The State notified pursuant to paragraph (a)(2) of this section 
may, within 30 days of receiving the Administrator's notice, submit to 
the Administrator evidence demonstrating that the State continues to 
meet the requirements for primary enforcement responsibility.
    (4) After reviewing the submission of the State, if any, made 
pursuant to paragraph (a)(3) of this section, the Administrator shall 
make a final determination either that the State no longer meets the 
requirements of 40 CFR part 142, subpart B, or that the State continues 
to meet those requirements, and shall notify the State of his or her 
determination. Any final determination that the State no longer meets 
the requirements of 40 CFR part 142, subpart B, shall not become 
effective except as provided in Sec.  142.13.
    (b) If a State which has primary enforcement responsibility decides 
to relinquish that authority, it may do so by notifying the 
Administrator in writing of the State's decision at least 90 days before 
the effective date of the decision.

[54 FR 52140, Dec. 20, 1989, as amended at 60 FR 33661, June 28, 1995]



Sec.  142.18  EPA review of State monitoring determinations.

    (a) A Regional Administrator may annul a State monitoring 
determination for the types of determinations identified in Sec. Sec.  
141.23(b), 141.23(c), 141.24(f), 141.24(h), and 141.40(n) in accordance 
with the procedures in paragraph (b) of this section.
    (b) When information available to a Regional Administrator, such as 
the results of an annual review, indicate a State determination fails to 
apply the standards of the approved State program, he may propose to 
annul the State monitoring determination by sending the State and the 
affected PWS a draft Rescission Order. The draft order shall:
    (1) Identify the PWS, the State determination, and the provisions at 
issue;
    (2) Explain why the State determination is not in compliance with 
the State program and must be changed; and
    (3) Describe the actions and terms of operation the PWS will be 
required to implement.
    (c) The State and PWS shall have 60 days to comment on the draft 
Rescission Order.
    (d) The Regional Administrator may not issue a Rescission Order to 
impose conditions less stringent than those imposed by the State.
    (e) The Regional Administrator shall also provide an opportunity for 
comment upon the draft Rescission Order, by
    (1) Publishing a notice in a newspaper in general circulation in 
communities served by the affected system; and
    (2) Providing 30 days for public comment on the draft order.
    (f) The State shall demonstrate that the determination is 
reasonable, based on its approved State program.
    (g) The Regional Administrator shall decide within 120 days after 
issuance of the draft Rescission Order to:
    (1) Issue the Rescission Order as drafted;
    (2) Issue a modified Rescission Order; or
    (3) Cancel the Rescission Order.
    (h) The Regional Administrator shall set forth the reasons for his 
decision, including a responsiveness summary addressing significant 
comments from the State, the PWS and the public.
    (i) The Regional Administrator shall send a notice of his final 
decision to the State, the PWS and all parties who commented upon the 
draft Rescission Order.
    (j) The Rescission Order shall remain in effect until cancelled by 
the Regional Administrator. The Regional Administrator may cancel a 
Rescission

[[Page 770]]

Order at any time, so long as he notifies those who commented on the 
draft order.
    (k) The Regional Administrator may not delegate the signature 
authority for a final Rescission Order or the cancellation of an order.
    (l) Violation of the actions, or terms of operation, required by a 
Rescission Order is a violation of the Safe Drinking Water Act.

[56 FR 3595, Jan. 30, 1991]



Sec.  142.19  EPA review of State implementation of national primary 
drinking water regulations for lead and copper.

    (a) Pursuant to the procedures in this section, the Regional 
Administrator may review state determinations establishing corrosion 
control or source water treatment requirements for lead or copper and 
may issue an order establishing federal treatment requirements for a 
public water system pursuant to Sec.  141.82 (d) and (f) and Sec.  
141.83(b) (2) and (4) where the Regional Administrator finds that:
    (1) A State has failed to issue a treatment determination by the 
applicable deadline;
    (2) A State has abused its discretion in making corrosion control or 
source water treatment determinations in a substantial number of cases 
or in cases affecting a substantial population, or
    (3) The technical aspects of State's determination would be 
indefensible in an expected federal enforcement action taken against a 
system.
    (b) If the Regional Administrator determines that review of state 
determination(s) under this section may be appropriate, he shall request 
the State to forward to EPA the state determination and all information 
that was considered by the State in making its determination, including 
public comments, if any, within 60 days of the Regional Adminstrator's 
request.
    (c) Proposed review of state determinations:
    (1) Where the Regional Administrator finds that review of a state 
determination under paragraph (a) of this section is appropriate, he 
shall issue a proposed review order which shall:
    (i) Identify the public water system(s) affected, the State 
determination being reviewed and the provisions of state and/or federal 
law at issue;
    (ii) Identify the determination that the State failed to carry out 
by the applicable deadline, or identify the particular provisions of the 
State determination which, in the Regional Administrator's judgment, 
fail to carry out properly applicable treatment requirements, and 
explain the basis for the Regional Administrator's conclusion;
    (iii) Identify the treatment requirements which the Regional 
Administrator proposes to apply to the affected system(s), and explain 
the basis for the proposed requirements;
    (iv) Request public comment on the proposed order and the supporting 
record.
    (2) The Regional Administrator shall provide notice of the proposed 
review order by:
    (i) Mailing the proposed order to the affected public water 
system(s), the state agency whose order is being reviewed, and any other 
parties of interest known to the Regional Administrator; and
    (ii) Publishing a copy of the proposed order in a newspaper of 
general circulation in the affected communities.
    (3) The Regional Administrator shall make available for public 
inspection during the comment period the record supporting the proposed 
order, which shall include all of the information submitted by the State 
to EPA under paragraph (b) of this section, all other studies, 
monitoring data and other information considered by the Agency in 
developing the proposed order.
    (d) Final review order:
    (1) Based upon review of all information obtained regarding the 
proposed review order, including public comments, the Regional 
Administrator shall issue a final review order within 120 days after 
issuance of the proposed order which affirms, modifies, or withdraws the 
proposed order. The Regional Administrator may extend the time period 
for issuing the final order for good cause. If the final order modifies 
or withdraws the proposed order, the final order shall explain the 
reasons supporting the change.
    (2) The record of the final order shall consist of the record 
supporting the

[[Page 771]]

proposed order, all public comments, all other information considered by 
the Regional Administrator in issuing the final order and a document 
responding to all significant public comments submitted on the proposed 
order. If new points are raised or new material supplied during the 
public comment period, the Regional Administrator may support the 
responses on those matters by adding new materials to the record. The 
record shall be complete when the final order is issued.
    (3) Notice of the final order shall be provided by mailing the final 
order to the affected system(s), the State, and all parties who 
commented on the proposed order.
    (4) Upon issuance of the final order, its terms constitute 
requirements of the national primary drinking water regulation for lead 
and/or copper until such time as the Regional Administrator issues a new 
order (which may include recision of the previous order) pursuant to the 
procedures in this section. Such requirements shall supersede any 
inconsistent treatment requirements established by the State pursuant to 
the national primary drinking water regulations for lead and copper.
    (5) The Regional Administrator may not issue a final order to impose 
conditions less stringent than those imposed by the State.
    (e) The Regional Administrator may not delegate authority to sign 
the final order under this section.
    (f) Final action of the Regional Administrator under paragraph (d) 
of this section shall constitute action of the Administrator for 
purposes of 42 U.S.C. Sec.  300j-7(a)(2).

[56 FR 26563, June 7, 1991]



        Subpart C_Review of State-Issued Variances and Exemptions



Sec.  142.20  State-issued variances and exemptions under Section 1415(a) 
and Section 1416 of the Act.

    (a) States with primary enforcement responsibility may issue 
variances to public water systems (other than small system variances) 
from the requirements of primary drinking water regulations under 
conditions and in a manner which are not less stringent than the 
requirements under Section 1415(a) of the Act. In States that do not 
have primary enforcement responsibility, variances may be granted by the 
Administrator pursuant to Subpart E of this part.
    (1) A State must document all findings that are required under 
Section 1415(a) of the Act.
    (2) If a State prescribes a schedule pursuant to section 1415(a) of 
the Act requiring compliance with a contaminant level for which the 
variance is granted later than five years from the date of issuance of 
the variance the State must--
    (i) Document its rationale for the extended compliance schedule;
    (ii) Discuss the rationale for the extended compliance schedule in 
the required public notice and opportunity for public hearing; and
    (iii) Provide the shortest practicable time schedule feasible under 
the circumstances.
    (b) States with primary enforcement responsibility may issue 
exemptions from the requirements of primary drinking water regulations 
under conditions and in a manner which are not less stringent than the 
requirements under Section 1416 of the Act. In States that do not have 
primary enforcement responsibility, exemptions may be granted by the 
Administrator pursuant to Subpart F of this part.
    (1) A State must document all findings that are required under 
Section 1416 of the Act:
    (i) Before finding that management and restructuring changes cannot 
be made, a State must consider the following measures, and the 
availability of State Revolving Loan Fund assistance, or any other 
Federal or State program, that is reasonably likely to be available 
within the period of the exemption to implement these measures:
    (A) Consideration of rate increases, accounting changes, the 
appointment of a State-certified operator under the State's Operator 
Certification program, contractual agreements for joint operation with 
one or more public water systems;

[[Page 772]]

    (B) Activities consistent with the State's Capacity Development 
Strategy to help the public water system acquire and maintain technical, 
financial, and managerial capacity to come into compliance with the Act; 
and
    (C) Ownership changes, physical consolidation with another public 
water system, or other feasible and appropriate means of consolidation 
which would result in compliance with the Act;
    (ii) The State must consider the availability of an alternative 
source of water, including the feasibility of partnerships with 
neighboring public water systems, as identified by the public water 
system or by the State consistent with the Capacity Development 
Strategy.
    (2) In the case of a public water system serving a population of not 
more than 3,300 persons and which needs financial assistance for the 
necessary improvements under the initial compliance schedule, an 
exemption granted by the State under section 1416(b)(2)(B)(i) or (ii) of 
the Act may be renewed for one or more additional 2-year periods, but 
not to exceed a total of 6 additional years, only if the State 
establishes that the public water system is taking all practicable steps 
to meet the requirements of Section 1416(b)(2)(B) of the Act and the 
established compliance schedule to achieve full compliance with the 
contaminant level or treatment technique for which the exemption was 
granted. A State must document its findings in granting an extension 
under this paragraph.

[63 FR 43847, Aug. 14, 1998]



Sec.  142.21  State consideration of a variance or exemption request.

    A State with primary enforcement responsibility shall act on any 
variance or exemption request submitted to it, within 90 days of receipt 
of the request.



Sec.  142.22  Review of State variances, exemptions and schedules.

    (a) Not later than 18 months after the effective date of the interim 
national primary drinking water regulations the Administrator shall 
complete a comprehensive review of the variances and exemptions granted 
(and schedules prescribed pursuant thereto) by the States with primary 
enforcement responsibility during the one-year period beginning on such 
effective date. The Administrator shall conduct such subsequent reviews 
of exemptions and schedules as he deems necessary to carry out the 
purposes of this title, but at least one review shall be completed 
within each 3-year period following the completion of the first review 
under this paragraph.
    (b) Notice of a proposed review shall be published in the Federal 
Register. Such notice shall (1) provide information respecting the 
location of data and other information respecting the variances and 
exemptions to be reviewed (including data and other information 
concerning new scientific matters bearing on such variances and 
exemptions), and (2) advise of the opportunity to submit comments on the 
variances and exemptions reviewed and on the need for continuing them. 
Upon completion of any such review, the Administrator shall publish in 
the Federal Register the results of his review, together with findings 
responsive to any comments submitted in connection with such review.



Sec.  142.23  Notice to State.

    (a) If the Administrator finds that a State has, in a substantial 
number of instances, abused its discretion in granting variances or 
exemptions under section 1415(a) or section 1416(a) of the Act or failed 
to prescribe schedules in accordance with section 1415(a) or section 
1416(b) of the Act, he shall notify the State of his findings. Such 
notice shall:
    (1) Identify each public water system for which the finding was 
made;
    (2) Specify the reasons for the finding; and
    (3) As appropriate, propose revocation of specific variances or 
exemptions, or propose revised schedules for specific public water 
systems.
    (b) The Administrator shall also notify the State of a public 
hearing to be held on the provisions of the notice required by paragraph 
(a) of this section. Such notice shall specify the time and

[[Page 773]]

location for the hearing. If, upon notification of a finding by the 
Administrator, the State takes adequate corrective action, the 
Administrator shall rescind his notice to the State of a public hearing, 
provided that the Administrator is notified of the corrective action 
prior to the hearing.
    (c) The Administrator shall publish notice of the public hearing in 
the Federal Register and in a newspaper or newspapers of general 
circulation in the involved State including a summary of the findings 
made pursuant to paragraph (a) of this section, a statement of the time 
and location for the hearing, and the address and telephone number of an 
office at which interested persons may obtain further information 
concerning the hearing.
    (d) Hearings convened pursuant to paragraphs (b) and (c) of this 
section shall be conducted before a hearing officer to be designated by 
the Administrator. The hearing shall be conducted by the hearing officer 
in an informal, orderly and expeditious manner. The hearing officer 
shall have authority to call witnesses, receive oral and written 
testimony and take such other action as may be necessary to assure the 
fair and efficient conduct of the hearing. Following the conclusion of 
the hearing, the hearing officer shall forward the record of the hearing 
to the Administrator.
    (e) Within 180 days after the date notice is given pursuant to 
paragraph (b) of this section, the Administrator shall:
    (1) Rescind the finding for which the notice was given and promptly 
notify the State of such rescission, or
    (2) Promulgate with any modifications as appropriate such revocation 
and revised schedules proposed in such notice and promptly notify the 
State of such action.
    (f) A revocation or revised schedule shall take effect 90 days after 
the State is notified under paragraph (e)(2) of this section.



Sec.  142.24  Administrator's rescission.

    If, upon notification of a finding by the Administrator under Sec.  
142.23, the State takes adequate corrective action before the effective 
date of the revocation or revised schedule, the Administrator shall 
rescind the application of his finding to that variance, exemption or 
schedule.



                      Subpart D_Federal Enforcement



Sec.  142.30  Failure by State to assure enforcement.

    (a) The Administrator shall notify a State and the appropriate 
supplier of water whenever he finds during a period in which the State 
has primary enforcement responsibility for public water systems that a 
public water system within such State is not in compliance with any 
primary drinking water regulation contained in part 141 of this chapter 
or with any schedule or other requirements imposed pursuant to a 
variance or exemption granted under section 1415 or 1416 of the Act: 
Provided, That the State will be deemed to have been notified of a 
violation referred to in a report submitted by the State.
    (b) The Administrator shall provide advice and technical assistance 
to such State and public water system as may be appropriate to bring the 
system into compliance by the earliest feasible time.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987]



Sec.  142.31  [Reserved]



Sec.  142.32  Petition for public hearing.

    (a) If the Administrator makes a finding of noncompliance pursuant 
to Sec.  142.30 with respect to a public water system in a State which 
has primary enforcement responsibility, the Administrator may, for the 
purpose of assisting that State in carrying out such responsibility and 
upon the petition of such State or public water system or persons served 
by such system, hold, after appropriate notice, public hearings for the 
purpose of gathering information as described in Sec.  142.33.
    (b) A petition for a public hearing pursuant to paragraph (a) of 
this section shall be filed with the Administrator and shall include the 
following information:
    (1) The name, address and telephone number of the individual or 
other entity requesting a hearing.
    (2) If the petition is filed by a person other than the State or 
public water

[[Page 774]]

system, a statement that the person is served by the system.
    (3) A brief statement of information that the requesting person 
intends to submit at the requested hearing.
    (4) The signature of the individual submitting the petition; or, if 
the petition is filed on behalf of a State, public water system or other 
entity, the signature of a responsible official of the State or other 
entity.



Sec.  142.33  Public hearing.

    (a) If the Administrator grants the petition for public hearing, he 
shall give appropriate public notice of such hearing. Such notice shall 
be by publication in the Federal Register and in a newspaper of general 
circulation or by other appropriate communications media covering the 
area served by such public water system.
    (b) A hearing officer designated by the Administrator shall gather 
during the public hearing information from technical or other experts, 
Federal, State, or other public officials, representatives of the public 
water system, persons served by the system, and other interested persons 
on:
    (1) The ways in which the system can within the earliest feasible 
time be brought into compliance, and
    (2) The means for the maximum feasible protection of the public 
health during any period in which such system is not in compliance.
    (c) On the basis of the hearing and other available information the 
Administrator shall issue recommendations which shall be sent to the 
State and public water system and shall be made available to the public 
and communications media.



Sec.  142.34  Entry and inspection of public water systems.

    (a) Any supplier of water or other person subject to a national 
primary drinking water regulation shall, at any time, allow the 
Administrator, or a designated representative of the Administrator, upon 
presenting appropriate credentials and a written notice of inspection, 
to enter any establishment, facility or other property of such supplier 
or other person to determine whether such supplier or other person has 
acted or is acting in compliance with the requirements of the Act or 
subchapter D of this chapter. Such inspection may include inspection, at 
reasonable times, of records, files, papers, processes, controls and 
facilities, or testing of any feature of a public water system, 
including its raw water source.
    (b) Prior to entry into any establishment, facility or other 
property within a State which has primary enforcement responsibility, 
the Administrator shall notify, in writing, the State agency charged 
with responsibility for safe drinking water of his intention to make 
such entry and shall include in his notification a statement of reasons 
for such entry. The Administrator shall, upon a showing by the State 
agency that such an entry will be detrimental to the administration of 
the State's program of primary enforcement responsibility, take such 
showing into consideration in determining whether to make such entry. 
The Administrator shall in any event offer the State agency the 
opportunity of having a representative accompany the Administrator or 
his representative on such entry.
    (c) No State agency which receives notice under paragraph (b) of 
this section may use the information contained in the notice to inform 
the person whose property is proposed to be entered of the proposed 
entry; if a State so uses such information, notice to the agency under 
paragraph (b) of this section is not required for subsequent inspections 
of public water systems until such time as the Administrator determines 
that the agency has provided him satisfactory assurances that it will no 
longer so use information contained in a notice received under paragraph 
(b) of this section.



Subpart E_Variances Issued by the Administrator Under Section 1415(a) of 
                                 the Act



Sec.  142.40  Requirements for a variance.

    (a) The Administrator may grant one or more variances to any public 
water system within a State that does not have primary enforcement 
responsibility from any requirement respecting a maximum contaminant 
level of an

[[Page 775]]

applicable national primary drinking water regulation upon a finding 
that:
    (1) Because of characteristics of the raw water sources which are 
reasonably available to the system, the system cannot meet the 
requirements respecting the maximum contaminant levels of such drinking 
water regulations despite application of the best technology, treatment 
techniques, or other means, which the Administrator finds are generally 
available (taking costs into consideration); and
    (2) The granting of a variance will not result in an unreasonable 
risk to the health of persons served by the system.
    (b) The Administrator may grant one or more variances to any public 
water system within a State that does not have primary enforcement 
responsibility from any requirement of a specified treatment technique 
of an applicable national primary drinking water regulation upon a 
finding that the public water system applying for the variance has 
demonstrated that such treatment technique is not necessary to protect 
the health of persons because of the nature of the raw water source of 
such system.



Sec.  142.41  Variance request.

    A supplier of water may request the granting of a variance pursuant 
to this subpart for a public water system within a State that does not 
have primary enforcement responsibility by submitting a request for a 
variance in writing to the Administrator. Suppliers of water may submit 
a joint request for variances when they seek similar variances under 
similar circumstances. Any written request for a variance or variances 
shall include the following information:
    (a) The nature and duration of variance requested.
    (b) Relevant analytical results of water quality sampling of the 
system, including results of relevant tests conducted pursuant to the 
requirements of the national primary drinking water regulations.
    (c) For any request made under Sec.  142.40(a):
    (1) Explanation in full and evidence of the best available treatment 
technology and techniques.
    (2) Economic and legal factors relevant to ability to comply.
    (3) Analytical results of raw water quality relevant to the variance 
request.
    (4) A proposed compliance schedule, including the date each step 
toward compliance will be achieved. Such schedule shall include as a 
minimum the following dates:
    (i) Date by which arrangement for alternative raw water source or 
improvement of existing raw water source will be completed.
    (ii) Date of initiation of the connection of the alternative raw 
water source or improvement of existing raw water source.
    (iii) Date by which final compliance is to be achieved.
    (5) A plan for the provision of safe drinking water in the case of 
an excessive rise in the contaminant level for which the variance is 
requested.
    (6) A plan for additional interim control measures during the 
effective period of variance.
    (d) For any request made under Sec.  142.40(b), a statement that the 
system will perform monitoring and other reasonable requirements 
prescribed by the Administrator as a condition to the variance.
    (e) Other information, if any, believed to be pertinent by the 
applicant.
    (f) Such other information as the Administrator may require.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987]



Sec.  142.42  Consideration of a variance request.

    (a) The Administrator shall act on any variance request submitted 
pursuant to Sec.  142.41 within 90 days of receipt of the request.
    (b) In his consideration of whether the public water system is 
unable to comply with a contaminant level required by the national 
primary drinking water regulations because of the nature of the raw 
water source, the Administrator shall consider such factors as the 
following:
    (1) The availability and effectiveness of treatment methods for the 
contaminant for which the variance is requested.

[[Page 776]]

    (2) Cost and other economic considerations such as implementing 
treatment, improving the quality of the source water or using an 
alternate source.
    (c) A variance may be issued to a public water system on the 
condition that the public water system install the best technology, 
treatment techniques, or other means, which the Administrator finds are 
available (taking costs into consideration) and based upon an evaluation 
satisfactory to the Administrator that indicates that alternative 
sources of water are not reasonably available to the public water 
system.
    (d) In his consideration of whether a public water system should be 
granted a variance to a required treatment technique because such 
treatment is unnecessary to protect the public health, the Administrator 
shall consider such factors as the following:
    (1) Quality of the water source including water quality data and 
pertinent sources of pollution.
    (2) Source protection measures employed by the public water system.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987; 63 
FR 43847, Aug. 14, 1998]



Sec.  142.43  Disposition of a variance request.

    (a) If the Administrator decides to deny the application for a 
variance, he shall notify the applicant of his intention to issue a 
denial. Such notice shall include a statement of reasons for the 
proposed denial, and shall offer the applicant an opportunity to 
present, within 30 days of receipt of the notice, additional information 
or argument to the Administrator. The Administrator shall make a final 
determination on the request within 30 days after receiving any such 
additional information or argument. If no additional information or 
argument is submitted by the applicant the application shall be denied.
    (b) If the Administrator proposes to grant a variance request 
submitted pursuant to Sec.  142.41, he shall notify the applicant of his 
decision in writing. Such notice shall identify the variance, the 
facility covered, and shall specify the period of time for which the 
variance will be effective.
    (1) For the type of variance specified in Sec.  142.40(a) such 
notice shall provide that the variance will be terminated when the 
system comes into compliance with the applicable regulation, and may be 
terminated upon a finding by the Administrator that the system has 
failed to comply with any requirements of a final schedule issued 
pursuant to Sec.  142.44.
    (2) For the type of variance specified in Sec.  142.40(b) such 
notice shall provide that the variance may be terminated at any time 
upon a finding that the nature of the raw water source is such that the 
specified treatment technique for which the variance was granted is 
necessary to protect the health of persons or upon a finding that the 
public water system has failed to comply with monitoring and other 
requirements prescribed by the Administrator as a condition to the 
granting of the variance.
    (c) For a variance specified in Sec.  142.40(a)(1) the Administrator 
shall propose a schedule for:
    (1) Compliance (including increments of progress) by the public 
water system with each contaminant level requirement covered by the 
variance; and,
    (2) Implementation by the public water system of such additional 
control measures as the Administrator may require for each contaminant 
covered by the variance.
    (d) The proposed schedule for compliance shall specify dates by 
which steps towards compliance are to be taken, including at the 
minimum, where applicable:
    (1) Date by which arrangement for an alternative raw water source or 
improvement of existing raw water source will be completed.
    (2) Date of initiation of the connection for the alternative raw 
water source or improvement of the existing raw water source.
    (3) Date by which final compliance is to be achieved.
    (e) The proposed schedule may, if the public water system has no 
access to an alternative raw water source, and can effect or anticipate 
no adequate improvement of the existing raw water

[[Page 777]]

source, specify an indefinite time period for compliance until a new and 
effective treatment technology is developed at which time a new 
compliance schedule shall be prescribed by the Administrator.
    (f) The proposed schedule for implementation of additional interim 
control measures during the period of variance shall specify interim 
treatment techniques, methods and equipment, and dates by which steps 
toward meeting the additional interim control measures are to be met.
    (g) The schedule shall be prescribed by the Administrator at the 
time of granting of the variance, subsequent to provision of opportunity 
for hearing pursuant to Sec.  142.44.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987]



Sec.  142.44  Public hearings on variances and schedules.

    (a) Before a variance and schedule proposed by the Administrator 
pursuant to Sec.  142.43 may take effect, the Administrator shall 
provide notice and opportunity for public hearing on the variance and 
schedule. A notice given pursuant to the preceding sentence may cover 
the granting of more than one variance and a hearing held pursuant to 
such notice shall include each of the variances covered by the notice.
    (b) Public notice of an opportunity for hearing on a variance and 
schedule shall be circulated in a manner designed to inform interested 
and potentially interested persons of the proposed variance and 
schedule, and shall include at least the following:
    (1) Posting of a notice in the principal post office of each 
municipality or area served by the public water system, and publishing 
of a notice in a newspaper or newspapers of general circulation in the 
area served by the public water system; and
    (2) Mailing of a notice to the agency of the State in which the 
system is located which is responsible for the State's water supply 
program, and to other appropriate State or local agencies at the 
Administrator's discretion.
    (3) Such notice shall include a summary of the proposed variance and 
schedule and shall inform interested persons that they may request a 
public hearing on the proposed variance and schedule.
    (c) Requests for hearing may be submitted by any interested person 
other than a Federal agency. Frivolous or insubstantial requests for 
hearing may be denied by the Administrator. Requests must be submitted 
to the Administrator within 30 days after issuance of the public notices 
provided for in paragraph (b) of this section. Such requests shall 
include the following information:
    (1) The name, address and telephone number of the individual, 
organization or other entity requesting a hearing;
    (2) A brief statement of the interest of the person making the 
request in the proposed variance and schedule, and of information that 
the requester intends to submit at such hearing;
    (3) The signature of the individual making the request, or, if the 
request is made on behalf of an organization or other entity, the 
signature of a responsible official of the organization or other entity.
    (d) The Administrator shall give notice in the manner set forth in 
paragraph (b) of this section of any hearing to be held pursuant to a 
request submitted by an interested person or on his own motion. Notice 
of the hearing shall also be sent to the persons requesting the hearing, 
if any. Notice of the hearing shall include a statement of the purpose 
of the hearing, information regarding the time and location for the 
hearing, and the address and telephone number of an office at which 
interested persons may obtain further information concerning the 
hearing. At least one hearing location specified in the public notice 
shall be within the involved State. Notice of hearing shall be given not 
less than 15 days prior to the time scheduled for the hearing.
    (e) A hearing convened pursuant to paragraph (d) of this section 
shall be conducted before a hearing officer to be designated by the 
Administrator. The hearing shall be conducted by the hearing officer in 
an informal, orderly and expeditious manner. The hearing officer shall 
have authority to call witnesses, receive oral and written testimony and 
take such other action as may be necessary to assure the fair and

[[Page 778]]

efficient conduct of the hearing. Following the conclusion of the 
hearing, the hearing officer shall forward the record of the hearing to 
the Administrator.
    (f) The variance and schedule shall become effective 30 days after 
notice of opportunity for hearing is given pursuant to paragraph (b) of 
this section if no timely request for hearing is submitted and the 
Administrator does not determine to hold a public hearing on his own 
motion.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987]



Sec.  142.45  Action after hearing.

    Within 30 days after the termination of the public hearing held 
pursuant to Sec.  142.44, the Administrator shall, taking into 
consideration information obtained during such hearing and relevant 
information, confirm, revise or rescind the proposed variance and 
schedule.

[52 FR 20675, June 2, 1987]



Sec.  142.46  Alternative treatment techniques.

    The Administrator may grant a variance from any treatment technique 
requirement of a national primary drinking water regulation to a 
supplier of water, whether or not the public water system for which the 
variance is requested is located in a State which has primary 
enforcement responsibility, upon a showing from any person that an 
alternative treatment technique not included in such requirement is at 
least as efficient in lowering the level of the contaminant with respect 
to which such requirements was prescribed. A variance under this 
paragraph shall be conditioned on the use of the alternative treatment 
technique which is the basis of the variance.



            Subpart F_Exemptions Issued by the Administrator



Sec.  142.50  Requirements for an exemption.

    (a) The Administrator may exempt any public water system within a 
State that does not have primary enforcement responsibility from any 
requirement regarding a maximum contaminant level or any treatment 
technique requirement, or from both, of an applicable national primary 
drinking water regulation upon a finding that--
    (1) Due to compelling factors (which may include economic factors, 
including qualification of the public water system as a system serving a 
disadvantaged community pursuant to section 1452(d) of the Act), the 
public water system is unable to comply with such contaminant level or 
treatment technique requirement or to implement measures to develop an 
alternative source of water supply;
    (2) The public water system was in operation on the effective date 
of such contaminant level or treatment technique requirement, or for a 
public water system that was not in operation by that date, no 
reasonable alternative source of drinking water is available to such new 
public water system;
    (3) The granting of the exemption will not result in an unreasonable 
risk to health; and
    (4) Management or restructuring changes (or both), as provided in 
Sec.  142.20(b)(1)(i), cannot reasonably be made that will result in 
compliance with the applicable national primary drinking water 
regulation or, if compliance cannot be achieved, improve the quality of 
the drinking water.
    (b) No exemption shall be granted unless the public water system 
establishes that the public water system is taking all practicable steps 
to meet the standard; and
    (1) The public water system cannot meet the standard without capital 
improvements which cannot be completed prior to the date established 
pursuant to Section 1412(b)(10) of the Act;
    (2) In the case of a public water system which needs financial 
assistance for the necessary improvements, the public water system has 
entered into an agreement to obtain such financial assistance or 
assistance pursuant to Section 1452 of the Act, or any other Federal or 
State program that is reasonably likely to be available within the 
period of the exemption; or
    (3) The public water system has entered into an enforceable 
agreement to become a part of a regional public water system.

[[Page 779]]

    (c) A public water system may not receive an exemption under this 
subpart if the public water system was granted a variance under Section 
1415(e) of the Act.

[63 FR 43847, Aug. 14, 1998]



Sec.  142.51  Exemption request.

    A supplier of water may request the granting of an exemption 
pursuant to this subpart for a public water system within a State that 
does not have primary enforcement responsibility by submitting a request 
for exemption in writing to the Administrator. Suppliers of water may 
submit a joint request for exemptions when they seek similar exemptions 
under similar circumstances. Any written request for an exemption or 
exemptions shall include the following information:
    (a) The nature and duration of exemption requested.
    (b) Relevant analytical results of water quality sampling of the 
system, including results of relevant tests conducted pursuant to the 
requirements of the national primary drinking water regulations.
    (c) Explanation of the compelling factors such as time or economic 
factors which prevent such system from achieving compliance.
    (d) Other information, if any, believed by the applicant to be 
pertinent to the application.
    (e) A proposed compliance schedule, including the date when each 
step toward compliance will be achieved.
    (f) Such other information as the Administrator may require.



Sec.  142.52  Consideration of an exemption request.

    (a) The Administrator shall act on any exemption request submitted 
pursuant to Sec.  142.51 within 90 days of receipt of the request.
    (b) In his consideration of whether the public water system is 
unable to comply due to compelling factors, the Administrator shall 
consider such factors as the following:
    (1) Construction, installation, or modification of the treatment 
equipment or systems.
    (2) The time needed to put into operation a new treatment facility 
to replace an existing system which is not in compliance.
    (3) Economic feasibility of compliance.



Sec.  142.53  Disposition of an exemption request.

    (a) If the Administrator decides to deny the application for an 
exemption, he shall notify the applicant of his intention to issue a 
denial. Such notice shall include a statement of reasons for the 
proposed denial, and shall offer the applicant an opportunity to 
present, within 30 days of receipt of the notice, additional information 
or argument to the Administrator. The Administrator shall make a final 
determination on the request within 30 days after receiving any such 
additional information or argument. If no additional information or 
argument is submitted by the applicant, the application shall be denied.
    (b) If the Administrator grants an exemption request submitted 
pursuant to Sec.  142.51, he shall notify the applicant of his decision 
in writing. Such notice shall identify the facility covered, and shall 
specify the termination date of the exemption. Such notice shall provide 
that the exemption will be terminated when the system comes into 
compliance with the applicable regulation, and may be terminated upon a 
finding by the Administrator that the system has failed to comply with 
any requirements of a final schedule issued pursuant to Sec.  142.55.
    (c) The Administrator shall propose a schedule for:
    (1) Compliance (including increments of progress or measures to 
develop an alternative source of water supply) by the public water 
system with each contaminant level requirement or treatment technique 
requirement with respect to which the exemption was granted; and
    (2) Implementation by the public water system of such control 
measures as the Administrator may require for each contaminant covered 
by the exemption.
    (d) The schedule shall be prescribed by the Administrator at the 
time the exemption is granted, subsequent to

[[Page 780]]

provision of opportunity for hearing pursuant to Sec.  142.54.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987; 63 
FR 43848, Aug. 14, 1998]



Sec.  142.54  Public hearings on exemption schedules.

    (a) Before a schedule proposed by the Administrator pursuant to 
Sec.  142.53 may take effect, the Administrator shall provide notice and 
opportunity for public hearing on the schedule. A notice given pursuant 
to the preceding sentence may cover the proposal of more than one such 
schedule and a hearing held pursuant to such notice shall include each 
of the schedules covered by the notice.
    (b) Public notice of an opportunity for hearing on an exemption 
schedule shall be circulated in a manner designed to inform interested 
and potentially interested persons of the proposed schedule, and shall 
include at least the following:
    (1) Posting of a notice in the principal post office of each 
municipality or area served by the public water system, and publishing 
of a notice in a newspaper or newspapers of general circulation in the 
area served by the public water system.
    (2) Mailing of a notice to the agency of the State in which the 
system is located which is responsible for the State's water supply 
program and to other appropriate State or local agencies at the 
Administrator's discretion.
    (3) Such notices shall include a summary of the proposed schedule 
and shall inform interested persons that they may request a public 
hearing on the proposed schedule.
    (c) Requests for hearing may be submitted by any interested person 
other than a Federal agency. Frivolous or insubstantial requests for 
hearing may be denied by the Administrator. Requests must be submitted 
to the Administrator within 30 days after issuance of the public notices 
provided for in paragraph (b) of this section. Such requests shall 
include the following information:
    (1) The name, address and telephone number of the individual, 
organization or other entity requesting a hearing;
    (2) A brief statement of the interest of the person making the 
request in the proposed schedule and of information that the requesting 
person intends to submit at such hearing; and
    (3) The signature of the individual making the request, or, if the 
request is made on behalf of an organization or other entity, the 
signature of a responsible official of the organization or other entity.
    (d) The Administrator shall give notice in the manner set forth in 
paragraph (b) of this section of any hearing to be held pursuant to a 
request submitted by an interested person or on his own motion. Notice 
of the hearing shall also be sent to the person requesting the hearing, 
if any. Notice of the hearing shall include a statement of the purpose 
of the hearing, information regarding the time and location of the 
hearing, and the address and telephone number of an office at which 
interested persons may obtain further information concerning the 
hearing. At least one hearing location specified in the public notice 
shall be within the involved State. Notice of the hearing shall be given 
not less than 15 days prior to the time scheduled for the hearing.
    (e) A hearing convened pursuant to paragraph (d) of this section 
shall be conducted before a hearing officer to be designated by the 
Administrator. The hearing shall be conducted by the hearing officer in 
an informal, orderly and expeditious manner. The hearing officer shall 
have authority to call witnesses, receive oral and written testimony and 
take such action as may be necessary to assure the fair and efficient 
conduct of the hearing. Following the conclusion of the hearing, the 
hearing officer shall forward the record of the hearing to the 
Administrator.

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987]



Sec.  142.55  Final schedule.

    (a) Within 30 days after the termination of the public hearing 
pursuant to Sec.  142.54, the Administrator shall, taking into 
consideration information obtained during such hearing, revise the 
proposed schedule as necessary and

[[Page 781]]

prescribe the final schedule for compliance and interim measures for the 
public water system granted an exemption under Sec.  142.52.
    (b) Such schedule must require compliance with each contaminant 
level and treatment technique requirement with respect to which the 
exemption was granted as expeditiously as practicable but not later than 
3 years after the otherwise applicable compliance date established in 
section 1412(b)(10) of the Act.
    (c) [Reserved]

[41 FR 2918, Jan. 20, 1976, as amended at 52 FR 20675, June 2, 1987; 63 
FR 43848, Aug. 14, 1998]



Sec.  142.56  Extension of date for compliance.

    In the case of a public water system which serves a population of 
not more than 3,300 persons and which needs financial assistance for the 
necessary improvements, an exemption granted under Sec.  142.50(b) (1) 
or (2) may be renewed for one or more additional 2-year periods, but not 
to exceed a total of 6 additional years, if the public water system 
establishes that the public water system is taking all practicable steps 
to meet the requirements of section 1416(b)(2)(B) of the Act and the 
established compliance schedule.

[63 FR 43848, Aug. 14, 1998]



Sec.  142.57  Bottled water, point-of-use, and point-of-entry devices.

    (a) A State may require a public water system to use bottled water, 
point-of-use devices, or point-of-entry devices as a condition of 
granting an exemption from the requirements of Sec. Sec.  141.61 (a) and 
(c), and 141.62 of this chapter.
    (b) Public water systems using bottled water as a condition of 
obtaining an exemption from the requirements of Sec. Sec.  141.61 (a) 
and (c) and 141.62(b) must meet the requirements in Sec.  142.62(g).
    (c) Public water systems that use point-of-use or point-of-entry 
devices as a condition for receiving an exemption must meet the 
requirements in Sec.  141.62(h).

[56 FR 3596, Jan. 30, 1991, as amended at 56 FR 30280, July 1, 1991]



  Subpart G_Identification of Best Technology, Treatment Techniques or 
                     Other Means Generally Available



Sec.  142.60  Variances from the maximum contaminant level 
for total trihalomethanes.

    (a) The Administrator, pursuant to section 1415(a)(1)(A) of the Act, 
hereby identifies the following as the best technology, treatment 
techiques or other means generally available for achieving compliance 
with the maximum contaminant level for total trihalomethanes (Sec.  
141.12(c)):
    (1) Use of chloramines as an alternate or supplemental disinfectant 
or oxidant.
    (2) Use of chlorine dioxide as an alternate or supplemental 
disinfectant or oxidant.
    (3) Improved existing clarification for THM precursor reduction.
    (4) Moving the point of chlorination to reduce TTHM formation and, 
where necessary, substituting for the use of chlorine as a pre-oxidant 
chloramines, chlorine dioxide or potassium permanganate.
    (5) Use of powdered activated carbon for THM precursor or TTHM 
reduction seasonally or intermittently at dosages not to exceed 10 mg/L 
on an annual average basis.
    (b) The Administrator in a state that does not have primary 
enforcement responsibility or a state with primary enforcement 
responsibility (primacy state) that issues variances shall require a 
community water system to install and/or use any treatment method 
identified in Sec.  142.60(a) as a condition for granting a variance 
unless the Administrator or primacy state determines that such treatment 
method identified in Sec.  142.60(a) is not available and effective for 
TTHM control for the system. A treatment method shall not be considered 
to be ``available and effective'' for an individual system if the 
treatment method would not be technically appropriate and technically 
feasible for that system or would only result in a marginal reduction in 
TTHM for the system. If, upon application by a system for a variance, 
the Administrator or primacy state that issues variances determines that 
none

[[Page 782]]

of the treatment methods identified in Sec.  142.60(a) is available and 
effective for the system, that system shall be entitled to a variance 
under the provisions of section 1415(a)(1)(A) of the Act. The 
Administrator's or primacy state's determination as to the availability 
and effectiveness of such treatment methods shall be based upon studies 
by the system and other relevant information. If a system submits 
information intending to demonstrate that a treatment method is not 
available and effective for TTHM control for that system, the 
Administrator or primacy state shall make a finding whether this 
information supports a decision that such treatment method is not 
available and effective for that system before requiring installation 
and/or use of such treatment method.
    (c) Pursuant to Sec.  142.43 (c) through (g) or corresponding state 
regulations, the Administrator or primacy state that issues variances 
shall issue a schedule of compliance that may require the system being 
granted the variance to examine the following treatment methods (1) to 
determine the probability that any of these methods will significantly 
reduce the level of TTHM for that system, and (2) if such probability 
exists, to determine whether any of these methods are technically 
feasible and economically reasonable, and that the TTHM reductions 
obtained will be commensurate with the costs incurred with the 
installation and use of such treatment methods for that system:

    Introduction of off-line water storage for THM precursor reduction.
    Aeration for TTHM reduction, where geographically and 
environmentally appropriate.
    Introduction of clarification where not currently practiced.
    Consideration of alternative sources of raw water.
    Use of ozone as an alternate or supplemental disinfectant or 
oxidant.

    (d) If the Administrator or primacy state that issues variances 
determines that a treatment method identified in Sec.  142.60(c) is 
technically feasible, economically reasonable and will achieve TTHM 
reductions commensurate with the costs incurred with the installation 
and/or use of such treatment method for the system, the Administrator or 
primacy state shall require the system to install and/or use that 
treatment method in connection with a compliance schedule issued under 
the provisions of section 1415(a)(1)(A) of the Act. The Administrator's 
or primacy state's determination shall be based upon studies by the 
system and other relevant information. In no event shall the 
Administrator require a system to install and/or use a treatment method 
not described in Sec.  142.60 (a) or (c) to obtain or maintain a 
variance from the TTHM Rule or in connection with any variance 
compliance schedule.

[48 FR 8414, Feb. 28, 1983]



Sec.  142.61  Variances from the maximum contaminant level for fluoride.

    (a) The Administrator, pursuant to section 1415(a)(1)(A) of the Act, 
hereby identifies the following as the best technology, treatment 
techniques or other means generally available for achieving compliance 
with the Maximum Contaminant Level for fluoride.
    (1) Activated alumina absorption, centrally applied
    (2) Reverse osmosis, centrally applied
    (b) The Administrator in a state that does not have primary 
enforcement responsibility or a state with primary enforcement 
responsibility (primacy state) that issues variances shall require a 
community water system to install and/or use any treatment method 
identified in Sec.  142.61(a) as a condition for granting a variance 
unless the Administrator or the primacy state determines that such 
treatment method identified in Sec.  142.61(a) as a condition for 
granting a variance is not available and effective for fluoride control 
for the system. A treatment method shall not be considered to be 
``available and effective'' for an individual system if the treatment 
method would not be technically appropriate and technically feasible for 
that system. If, upon application by a system for a variance, the 
Administrator or primacy state that issues variances determines that 
none of the treatment methods identified in Sec.  142.61(a) are 
available and effective for the system, that system shall be entitled to 
a variance under the provisions of section

[[Page 783]]

1415(a)(1)(A) of the Act. The Administrator's or primacy state's 
determination as to the availability and effectiveness of such treatment 
methods shall be based upon studies by the system and other relevant 
information. If a system submits information to demonstrate that a 
treatment method is not available and effective for fluoride control for 
that system, the Administrator or primacy state shall make a finding 
whether this information supports a decision that such treatment method 
is not available and effective for that system before requiring 
installation and/or use of such treatment method.
    (c) Pursuant to Sec.  142.43 (c)-(g) or corresponding state 
regulations, the Administrator or primacy state that issues variances 
shall issue a schedule of compliance that may require the system being 
granted the variance to examine the following treatment methods (1) to 
determine the probability that any of these methods will significantly 
reduce the level of fluoride for that system, and (2) if such 
probability exists, to determine whether any of these methods are 
technically feasible and economically reasonable, and that the fluoride 
reductions obtained will be commensurate with the costs incurred with 
the installation and use of such treatment methods for that system:
    (1) Modification of lime softening;
    (2) Alum coagulation;
    (3) Electrodialysis;
    (4) Anion exchange resins;
    (5) Well field management;
    (6) Alternate source;
    (7) Regionalization.
    (d) If the Administrator or primary state that issues variances 
determines that a treatment method identified in Sec.  142.61(c) or 
other treatment method is technically feasible, economically reasonable, 
and will achieve fluoride reductions commensurate with the costs 
incurred with the installation and/or use of such treatment method for 
the system, the Administrator or primacy state shall require the system 
to install and/or use that treatment method in connection with a 
compliance schedule issued under the provisions of section 1415(a)(1)(A) 
of the Act. The Administrator's or primacy state's determination shall 
be based upon studies by the system and other relevant information.

[51 FR 11411, Apr. 2, 1986]



Sec.  142.62  Variances and exemptions from the maximum contaminant levels 
for organic and inorganic chemicals.

    (a) The Administrator, pursuant to section 1415(a)(1)(A) of the Act 
hereby identifies the technologies listed in paragraphs (a)(1) through 
(a)(54) of this section as the best technology, treatment techniques, or 
other means available for achieving compliance with the maximum 
contaminant levels for organic chemicals listed in Sec.  141.61 (a) and 
(c):

----------------------------------------------------------------------------------------------------------------
                                                              Best available technologies
             Contaminant             ---------------------------------------------------------------------------
                                               PTA \1\                  GAC \2\                   OX \3\
----------------------------------------------------------------------------------------------------------------
(1) Benzene.........................  X                         X
(2) Carbon tetrachloride............  X                         X
(3) 1,2-Dichloroethane..............  X                         X
(4) Trichloroethylene...............  X                         X
(5) para-Dichlorobenzene............  X                         X
(6) 1,1-Dichloroethylene............  X                         X
(7) 1,1,1-Trichloroethane...........  X                         X
(8) Vinyl chloride..................  X
(9) cis-1,2-Dichloroethylene........  X                         X
(10) 1,2-Dichloropropane............  X                         X
(11) Ethylbenzene...................  X                         X
(12) Monochlorobenzene..............  X                         X
(13) o-Dichlorobenzene..............  X                         X
(14) Styrene........................  X                         X
(15) Tetrachloroethylene............  X                         X
(16) Toluene........................  X                         X
(17) trans-1,2-Dichloroethylene.....  X                         X
(18) Xylense (total)................  X                         X
(19) Alachlor.......................  ........................  X
(20) Aldicarb.......................  ........................  X
(21) Aldicarb sulfoxide.............  ........................  X
(22) Aldicarb sulfone...............  ........................  X

[[Page 784]]

 
(23) Atrazine.......................  ........................  X
(24) Carbofuran.....................  ........................  X
(25) Chlordane......................  ........................  X
(26) Dibromochloropropane...........  X                         X
(27) 2,4-D..........................  ........................  X
(28) Ethylene dibromide.............  X                         X
(29) Heptachlor.....................  ........................  X
(30) Heptachlor epoxide.............  ........................  X
(31) Lindane........................  ........................  X
(32) Methoxychlor...................  ........................  X
(33) PCBs...........................  ........................  X
(34) Pentachlorophenol..............  ........................  X
(35) Toxaphene......................  ........................  X
(36) 2,4,5-TP.......................  ........................  X
(37) Benzo[a]pyrene.................  ........................  X
(38) Dalapon........................  ........................  X
(39) Dichloromethane................  X
(40) Di(2-ethylhexyl)adipate........  X                         X
(41) Di(2-ethylhexyl)phthalate......  ........................  X
(42) Dinoseb........................  ........................  X
(43) Diquat.........................  ........................  X
(44) Endothall......................  ........................  X
(45) Endrin.........................  ........................  X
(46) Glyphosate.....................  ........................  .......................  X
(47) Hexachlorobenzene..............  ........................  X
(48) Hexachlorocyclopentadiene......  X                         X
(49) Oxamyl (Vydate)................  ........................  X
(50) Picloram.......................  ........................  X
(51) Simazine.......................  ........................  X
(52) 1,2,4-Trichlorobenzene.........  X                         X
(53) 1,1,2-Trichloroethane..........  X                         X
(54) 2,3,7,8-TCDD (Dioxin)..........  ........................  X
----------------------------------------------------------------------------------------------------------------
\1\ Packed Tower Aeration
\2\ Granular Activated Carbon
\3\ Oxidation (Chlorination or Ozonation)

    (b) The Administrator, pursuant to section 1415(a)(1)(A) of the Act, 
hereby identifies the following as the best technology, treatment 
techniques, or other means available for achieving compliance with the 
maximum contaminant levels for the inorganic chemicals listed in Sec.  
141.62:

         BAT for Inorganic Compounds Listed in Sec.   141.62(b)
------------------------------------------------------------------------
                      Chemical name                           BAT(s)
------------------------------------------------------------------------
Antimony................................................             2,7
Arsenic \4\.............................................    \5\ 1, 2, 5,
                                                             6, 7, 9, 12
Asbestos................................................           2,3,8
Barium..................................................         5,6,7,9
Beryllium...............................................       1,2,5,6,7
Cadmium.................................................         2,5,6,7
Chromium................................................     2,5,6 \2\,7
Cyanide.................................................          5,7,10
Mercury.................................................       2 \1\,4,6
                                                               \1\,7 \1\
Nickel..................................................           5,6,7
Nitrite.................................................           5,7,9
Nitrate.................................................             5,7
Selenium................................................   1,2 \3\,6,7,9
Thallium................................................             1,5
------------------------------------------------------------------------
\1\ BAT only if influent Hg concentrations <=10[micro]g/1.
\2\ BAT for Chromium III only.
\3\ BAT for Selenium IV only.
\4\ BATs for Arsenic V. Pre-oxidation may be required to convert Arsenic
  III to Arsenic V.
\5\ To obtain high removals, iron to arsenic ratio must be at least
  20:1.

                          Key to BATS in Table

1 = Activated Alumina
2 = Coagulation/Filtration (not BAT for systems <500 service 
connections)
3 = Direct and Diatomite Filtration
4 = Granular Activated Carbon
5 = Ion Exchange
6 = Lime Softening (not BAT for systems <500 service connections)
7 = Reverse Osmosis
8 = Corrosion Control
9 = Electrodialysis
10 = Chlorine
11 = Ultraviolet
12 = Oxidation/Filtration

    (c) A State shall require community water systems and non-transient, 
non-community water systems to install and/or use any treatment method 
identified in Sec.  142.62 (a) and (b) as a condition for granting a 
variance except as provided in paragraph (d) of this section. If, after 
the system's installation

[[Page 785]]

of the treatment method, the system cannot meet the MCL, that system 
shall be eligible for a variance under the provisions of section 
1415(a)(1)(A) of the Act.
    (d) If a system can demonstrate through comprehensive engineering 
assessments, which may include pilot plant studies, that the treament 
methods identified in Sec.  142.62 (a) and (b) would only achieve a de 
minimis reduction in contaminants, the State may issue a schedule of 
compliance that requires the system being granted the variance to 
examine other treatment methods as a condition of obtaining the 
variance.
    (e) If the State determines that a treatment method identified in 
paragraph (d) of this section is technically feasible, the Administrator 
or primacy State may require the system to install and/or use that 
treatment method in connection with a compliance schedule issued under 
the provisions of section 1415(a)(1)(A) of the Act. The State's 
determination shall be based upon studies by the system and other 
relevant information.
    (f) The State may require a public water system to use bottled 
water, point-of-use devices, point-of-entry devices or other means as a 
condition of granting a variance or an exemption from the requirements 
of Sec. Sec.  141.61 (a) and (c) and 141.62, to avoid an unreasonable 
risk to health. The State may require a public water system to use 
bottled water and point-of-use devices or other means, but not point-of-
entry devices, as a condition for granting an exemption from corrosion 
control treatment requirements for lead and copper in Sec. Sec.  141.81 
and 141.82 to avoid an unreasonable risk to health. The State may 
require a public water system to use point-of-entry devices as a 
condition for granting an exemption from the source water and lead 
service line replacement requirements for lead and copper under 
Sec. Sec.  141.83 or 141.84 to avoid an unreasonable risk to health.
    (g) Public water systems that use bottled water as a condition for 
receiving a variance or an exemption from the requirements of Sec. Sec.  
141.61 (a) and (c) and 141.62, or an exemption from the requirements of 
Sec. Sec.  141.81-141.84 must meet the requirements specified in either 
paragraph (g)(1) or (g)(2) and paragraph (g)(3) of this section:
    (1) The Administrator or primacy State must require and approve a 
monitoring program for bottled water. The public water system must 
develop and put in place a monitoring program that provides reasonable 
assurances that the bottled water meets all MCLs. The public water 
system must monitor a representative sample of the bottled water for all 
contaminants regulated under Sec. Sec.  141.61 (a) and (c) and 141.62 
during the first three-month period that it supplies the bottled water 
to the public, and annually thereafter. Results of the monitoring 
program shall be provided to the State annually.
    (2) The public water system must receive a certification from the 
bottled water company that the bottled water supplied has been taken 
from an ``approved source'' as defined in 21 CFR 129.3(a); the bottled 
water company has conducted monitoring in accordance with 21 CFR 
129.80(g) (1) through (3); and the bottled water does not exceed any 
MCLs or quality limits as set out in 21 CFR 165.110, part 110, and part 
129. The public water system shall provide the certification to the 
State the first quarter after it supplies bottled water and annually 
thereafter. At the State's option a public water system may satisfy the 
requirements of this subsection if an approved monitoring program is 
already in place in another State.
    (3) The public water system is fully responsible for the provision 
of sufficient quantities of bottled water to every person supplied by 
the public water system via door-to-door bottled water delivery.
    (h) Public water systems that use point-of-use or point-of-entry 
devices as a condition for obtaining a variance or an exemption from 
NPDWRs must meet the following requirements:
    (1) It is the responsibility of the public water system to operate 
and maintain the point-of-use and/or point-of-entry treatment system.
    (2) Before point-of-use or point-of-entry devices are installed, the 
public water system must obtain the approval of a monitoring plan which 
ensures

[[Page 786]]

that the devices provide health protection equivalent to that provided 
by central water treatment.
    (3) The public water system must apply effective technology under a 
State-approved plan. The microbiological safety of the water must be 
maintained at all times.
    (4) The State must require adequate certification of performance, 
field testing, and, if not included in the certification process, a 
rigorous engineering design review of the point-of-use and/or point-of-
entry devices.
    (5) The design and application of the point-of-use and/or point-of-
entry devices must consider the potential for increasing concentrations 
of heterotrophic bacteria in water treated with activated carbon. It may 
be necessary to use frequent backwashing, post-contactor disinfection, 
and Heterotrophic Plate Count monitoring to ensure that the 
microbiological safety of the water is not compromised.
    (6) The State must be assured that buildings connected to the system 
have sufficient point-of-use or point-of-entry devices that are properly 
installed, maintained, and monitored such that all consumers will be 
protected.
    (7) In requiring the use of a point-of-entry device as a condition 
for granting an exemption from the treatment requirements for lead and 
copper under Sec. Sec.  141.83 or 141.84, the State must be assured that 
use of the device will not cause increased corrosion of lead and copper 
bearing materials located between the device and the tap that could 
increase contaminant levels at the tap.

[56 FR 3596, Jan. 30, 1991, as amended at 56 FR 26563, June 7, 1991; 57 
FR 31848, July 17, 1992; 59 FR 33864, June 30, 1994; 59 FR 34325, July 
1, 1994; 66FR 7066, Jan. 22, 2001; 69 FR 38857, June 29, 2004]



Sec.  142.63  Variances and exemptions from the maximum contaminant level 
for total coliforms.

    (a) No variances or exemptions from the maximum contaminant level in 
Sec.  141.63 of this chapter are permitted.
    (b) EPA has stayed this section as it relates to the total coliform 
MCL of Sec.  141.63(a) of this chapter for systems that demonstrate to 
the State that the violation of the total coliform MCL is due to a 
persistent growth of total coliforms in the distribution system rather 
than fecal or pathogenic contamination, a treatment lapse or deficiency, 
or a problem in the operation or maintenance of the distribution system. 
This stay is applicable until March 31, 2016, at which time the total 
coliform MCL is no longer applicable.

[54 FR 27568, June 29, 1989, as amended at 56 FR 1557, Jan. 15, 1991; 78 
FR 10365, Feb. 13, 2013]



Sec.  142.64  Variances and exemptions from the requirements of part 141, 
subpart H--Filtration and Disinfection.

    (a) No variances from the requirements in part 141, subpart H are 
permitted.
    (b) No exemptions from the requirements in Sec.  141.72 (a)(3) and 
(b)(2) to provide disinfection are permitted.

[54 FR 27540, June 29, 1989]



Sec.  142.65  Variances and exemptions from the maximum contaminant levels 
for radionuclides.

    (a)(1) Variances and exemptions from the maximum contaminant levels 
for combined radium-226 and radium-228, uranium, gross alpha particle 
activity (excluding Radon and Uranium), and beta particle and photon 
radioactivity.
    (i) The Administrator, pursuant to section 1415(a)(1)(A) of the Act, 
hereby identifies the following as the best available technology, 
treatment techniques, or other means available for achieving compliance 
with the maximum contaminant levels for the radionuclides listed in 
Sec.  141.66(b), (c), (d), and (e) of this chapter, for the purposes of 
issuing variances and exemptions, as shown in Table A to this paragraph.

         Table A--BAT for Radionuclides Listed in Sec.   141.66
------------------------------------------------------------------------
                Contaminant                              BAT
------------------------------------------------------------------------
Combined radium-226 and radium-228........  Ion exchange, reverse
                                             osmosis, lime softening.
Uranium...................................  Ion exchange, reverse
                                             osmosis, lime softening,
                                             coagulation/filtration.
Gross alpha particle activity (excluding    Reverse osmosis.
 radon and uranium).
Beta particle and photon radioactivity....  Ion exchange, reverse
                                             osmosis.
------------------------------------------------------------------------


[[Page 787]]

    (ii) In addition, the Administrator hereby identifies the following 
as the best available technology, treatment techniques, or other means 
available for achieving compliance with the maximum contaminant levels 
for the radionuclides listed in Sec.  141.66(b), (c), (d), and (e) of 
this chapter, for the purposes of issuing variances and exemptions to 
small drinking water systems, defined here as those serving 10,000 
persons or fewer, as shown in Table C to this paragraph.

         Table B--List of Small Systems Compliance Technologies for Radionuclides and Limitations to Use
----------------------------------------------------------------------------------------------------------------
                                           Limitations
            Unit technologies                 (see          Operator skill level      Raw water quality range &
                                           footnotes)           required \1\              considerations \1\
----------------------------------------------------------------------------------------------------------------
1. Ion exchange (IE)....................        (\a\)   Intermediate...............  All ground waters.
2. Point of use (POU \2\ ) IE...........        (\b\)   Basic......................  All ground waters.
3. Reverse osmosis (RO).................        (\c\)   Advanced...................  Surface waters usually
                                                                                      require pre-filtration.
4. POU \2\ RO...........................        (\b\)   Basic......................  Surface waters usually
                                                                                      require pre-filtration.
5. Lime softening.......................        (\d\)   Advanced...................  All waters.
6. Green sand filtration................        (\e\)   Basic.
7. Co-precipitation with barium sulfate.        (\f\)   Intermediate to Advanced...  Ground waters with suitable
                                                                                      water quality.
8. Electrodialysis/electrodialysis        ............  Basic to Intermediate......  All ground waters.
 reversal.
9. Pre-formed hydrous manganese oxide           (\g\)   Intermediate...............  All ground waters.
 filtration.
10. Activated alumina...................  (\a\), (\h\)  Advanced...................  All ground waters;
                                                                                      competing anion
                                                                                      concentrations may affect
                                                                                      regeneration frequency.
11. Enhanced coagulation/filtration.....        (\i\)   Advanced...................  Can treat a wide range of
                                                                                      water qualities.
----------------------------------------------------------------------------------------------------------------
\1\ National Research Council (NRC). Safe Water from Every Tap: Improving Water Service to Small Communities.
  National Academy Press. Washington, D.C. 1997.
\2\ A POU, or ``point-of-use'' technology is a treatment device installed at a single tap used for the purpose
  of reducing contaminants in drinking water at that one tap. POU devices are typically installed at the kitchen
  tap. See the April 21, 2000 NODA for more details.
 
Limitations Footnotes: Technologies for Radionuclides:
\a\ The regeneration solution contains high concentrations of the contaminant ions. Disposal options should be
  carefully considered before choosing this technology.
\b\ When POU devices are used for compliance, programs for long-term operation, maintenance, and monitoring must
  be provided by water utility to ensure proper performance.
\c\ Reject water disposal options should be carefully considered before choosing this technology. See other RO
  limitations described in the SWTR compliance technologies table.
\d\ The combination of variable source water quality and the complexity of the water chemistry involved may make
  this technology too complex for small surface water systems.
\e\ Removal efficiencies can vary depending on water quality.
\f\ This technology may be very limited in application to small systems. Since the process requires static
  mixing, detention basins, and filtration, it is most applicable to systems with sufficiently high sulfate
  levels that already have a suitable filtration treatment train in place.
\g\ This technology is most applicable to small systems that already have filtration in place.
\h\ Handling of chemicals required during regeneration and pH adjustment may be too difficult for small systems
  without an adequately trained operator.
\i\ Assumes modification to a coagulation/filtration process already in place.


          Table C--BAT for Small Community Water Systems for the Radionuclides Listed in Sec.   141.66
----------------------------------------------------------------------------------------------------------------
                                           Compliance technologies \1\ for system size categories (population
                                                                        served)
             Contaminant              --------------------------------------------------------------------------
                                                25-500                 501-3,300               3,300-10,000
----------------------------------------------------------------------------------------------------------------
Combined radium-226 and radium-228...  1, 2, 3, 4, 5, 6, 7, 8,  1, 2, 3, 4, 5, 6, 7, 8,  1, 2, 3, 4, 5, 6, 7, 8,
                                        9.                       9.                       9.
Gross alpha particle activity........  3, 4...................  3, 4...................  3, 4.
Beta particle activity and photon      1, 2, 3, 4.............  1, 2, 3, 4.............  1, 2, 3, 4.
 activity.
Uranium..............................  1, 2, 4, 10, 11........  1, 2, 3, 4, 5, 10, 11..  1, 2, 3, 4, 5, 10, 11.
----------------------------------------------------------------------------------------------------------------
\1\ Note: Numbers correspond to those technologies found listed in the table B to this paragraph.

    (2) A State shall require community water systems to install and/or 
use any treatment technology identified in Table A to this section, or 
in the case of small water systems (those serving 10,000 persons or 
fewer), Table B and

[[Page 788]]

Table C of this section, as a condition for granting a variance except 
as provided in paragraph (a)(3) of this section. If, after the system's 
installation of the treatment technology, the system cannot meet the 
MCL, that system shall be eligible for a variance under the provisions 
of section 1415(a)(1)(A) of the Act.
    (3) If a community water system can demonstrate through 
comprehensive engineering assessments, which may include pilot plant 
studies, that the treatment technologies identified in this section 
would only achieve a de minimus reduction in the contaminant level, the 
State may issue a schedule of compliance that requires the system being 
granted the variance to examine other treatment technologies as a 
condition of obtaining the variance.
    (4) If the State determines that a treatment technology identified 
under paragraph (a)(3) of this section is technically feasible, the 
Administrator or primacy State may require the system to install and/or 
use that treatment technology in connection with a compliance schedule 
issued under the provisions of section 1415(a)(1)(A) of the Act. The 
State's determination shall be based upon studies by the system and 
other relevant information.
    (5) The State may require a community water system to use bottled 
water, point-of-use devices, point-of-entry devices or other means as a 
condition of granting a variance or an exemption from the requirements 
of Sec.  141.66 of this chapter, to avoid an unreasonable risk to 
health.
    (6) Community water systems that use bottled water as a condition 
for receiving a variance or an exemption from the requirements of Sec.  
141.66 of this chapter must meet the requirements specified in either 
Sec.  142.62(g)(1) or Sec.  142.62(g)(2) and (g)(3).
    (7) Community water systems that use point-of-use or point-of-entry 
devices as a condition for obtaining a variance or an exemption from the 
radionuclides NPDWRs must meet the conditions in Sec.  142.62(h)(1) 
through (h)(6).
    (b) [Reserved]

[65 FR 76751, Dec. 7, 2000]



                         Subpart H_Indian Tribes

    Source: 53 FR 37411, Sept. 26, 1988, unless otherwise noted.



Sec.  142.72  Requirements for Tribal eligibility.

    The Administrator is authorized to treat an Indian tribe as eligible 
to apply for primary enforcement for the Public Water System Program and 
the authority to waive the mailing requirements of Sec.  141.155(a) if 
it meets the following criteria:
    (a) The Indian Tribe is recognized by the Secretary of the Interior.
    (b) The Indian Tribe has a tribal governing body which is currently 
``carrying out substantial governmental duties and powers'' over a 
defined area, (i.e., is currently performing governmental functions to 
promote the health, safety, and welfare of the affected population 
within a defined geographic area).
    (c) The Indian Tribe demonstrates that the functions to be performed 
in regulating the public water systems that the applicant intends to 
regulate are within the area of the Indian Tribal government's 
jurisdiction.
    (d) The Indian Tribe is reasonably expected to be capable, in the 
Administrator's judgment, of administering (in a manner consistent with 
the terms and purposes of the Act and all applicable regulations) an 
effective Public Water System program.

[53 FR 37411, Sept. 26, 1988, as amended at 59 FR 64344, Dec. 14, 1994; 
63 FR 44535, Aug. 19, 1998]



Sec.  142.76  Request by an Indian Tribe for a determination of eligibility.

    An Indian Tribe may apply to the Administrator for a determination 
that it meets the criteria of section 1451 of the Act. The application 
shall be concise and describe how the Indian Tribe will meet each of the 
requirements of Sec.  142.72. The application shall consist of the 
following information:
    (a) A statement that the Tribe is recognized by the Secretary of the 
Interior.
    (b) A descriptive statement demonstrating that the Tribal governing 
body is currently carrying out substantial governmental duties and 
powers

[[Page 789]]

over a defined area. The statement should:
    (1) Describe the form of the Tribal government;
    (2) Describe the types of governmental functions currently performed 
by the Tribal governing body such as, but not limited to, the exercise 
of police powers affecting (or relating to) the health, safety, and 
welfare of the affected population; taxation; and the exercise of the 
power of eminent domain; and
    (3) Identify the sources of the Tribal government's authority to 
carry out the governmental functions currently being performed.
    (c) A map or legal description of the area over which the Indian 
Tribe asserts jurisdiction; a statement by the Tribal Attorney General 
(or equivalent official) which describes the basis for the Tribe's 
jurisdictional assertion (including the nature or subject matter of the 
asserted jurisdiction); a copy of those documents such as Tribal 
constitutions, by-laws, charters, executive orders, codes, ordinances, 
and/or resolutions which the Tribe believes are relevant to its 
assertions regarding jurisdiction; and a description of the locations of 
the public water systems the Tribe proposes to regulate.
    (d) A narrative statement describing the capability of the Indian 
Tribe to administer an effective Public Water System program. The 
narrative statement should include:
    (1) A description of the Indian Tribe's previous management 
experience which may include, the administration of programs and 
services authorized by the Indian Self-Determination and Education 
Assistance Act (25 U.S.C. 450 et seq.), the Indian Mineral Development 
Act (25 U.S.C. 2101 et seq.), or the Indian Sanitation Facilities 
Construction Activity Act (42 U.S.C. 2004a).
    (2) A list of existing environmental or public health programs 
administered by the Tribal governing body and a copy of related Tribal 
laws, regulations and policies.
    (3) A description of the Indian Tribe's accounting and procurement 
systems.
    (4) A description of the entity (or entities) which exercise the 
executive, legislative, and judicial functions of the Tribal government.
    (5) A description of the existing, or proposed, agency of the Indian 
Tribe which will assume primary enforcement responsibility, including a 
description of the relationship between owners/operators of the public 
water systems and the agency.
    (6) A description of the technical and administrative capabilities 
of the staff to administer and manage an effective Public Water System 
Program or a plan which proposes how the Tribe will acquire additional 
administrative and/or technical expertise. The plan must address how the 
Tribe will obtain the funds to acquire the additional administrative and 
technical expertise.
    (e) The Administrator may, in his discretion, request further 
documentation necessary to support a Tribe's eligibility.
    (f) If the Administrator has previously determined that a Tribe has 
met the prerequisites that make it eligible to assume a role similar to 
that of a state as provided by statute under the Safe Drinking Water 
Act, the Clean Water Act, or the Clean Air Act, then that Tribe need 
provide only that information unique to the Public Water System program 
(paragraphs (c), (d)(5) and (6) of this section).

[53 FR 37411, Sept. 26, 1988, as amended at 59 FR 64344, Dec. 14, 1994]



Sec.  142.78  Procedure for processing an Indian Tribe's application.

    (a) The Administrator shall process a completed application of an 
Indian Tribe in a timely manner. He shall promptly notify the Indian 
Tribe of receipt of the application.
    (b) A tribe that meets the requirements of Sec.  141.72 of this 
chapter is eligible to apply for development grants and primacy 
enforcement responsibility for a Public Water System Program and 
associated funding under section 1443(a) of the Act and for primary 
enforcement responsibility for public water systems under section 1413 
of the Act and for the authority to waive the mailing requirement of 
Sec.  141.155(a) of this chapter.

[53 FR 37411 Sept. 26, 1988, as amended at 59 FR 64345, Dec. 14, 1994; 
63 FR 71376, Dec. 28, 1998]

[[Page 790]]



   Subpart I_Administrator's Review of State Decisions that Implement 
               Criteria Under Which Filtration Is Required

    Source: 54 FR 27540, June 29, 1989, unless otherwise noted.



Sec.  142.80  Review procedures.

    (a) The Administrator may initiate a comprehensive review of the 
decisions made by States with primary enforcement responsibility to 
determine, in accordance with Sec.  141.71 of this chapter, if public 
water systems using surface water sources must provide filtration 
treatment. The Administrator shall complete this review within one year 
of its initiation and shall schedule subsequent reviews as (s)he deems 
necessary.
    (b) EPA shall publish notice of a proposed review in the Federal 
Register. Such notice must:
    (1) Provide information regarding the location of data and other 
information pertaining to the review to be conducted and other 
information including new scientific matter bearing on the application 
of the criteria for avoiding filtration; and
    (2) Advise the public of the opportunity to submit comments.
    (c) Upon completion of any such review, the Administrator shall 
notify each State affected by the results of the review and shall make 
the results available to the public.



Sec.  142.81  Notice to the State.

    (a) If the Administrator finds through periodic review or other 
available information that a State (1) has abused its discretion in 
applying the criteria for avoiding filtration under Sec.  141.71 of this 
chapter in determining that a system does not have to provide filtration 
treatment, or (2) has failed to prescribe compliance schedules for those 
systems which must provide filtration in accordance with section 
1412(b)(7)(C)(ii) of the Act, (s)he shall notify the State of these 
findings. Such notice shall:
    (1) Identify each public water system for which the Administrator 
finds the State has abused its discretion;
    (2) Specify the reasons for the finding;
    (3) As appropriate, propose that the criteria of Sec.  141.71 of 
this chapter be applied properly to determine the need for a public 
water system to provide filtration treatment or propose a revised 
schedule for compliance by the public water system with the filtration 
treatment requirements;
    (b) The Administrator shall also notify the State that a public 
hearing is to be held on the provisions of the notice required by 
paragraph (a) of this section. Such notice shall specify the time and 
location of the hearing. If, upon notification of a finding by the 
Administrator that the State has abused its discretion under Sec.  
141.71 of this chapter, the State takes corrective action satisfactory 
to the Administrator, the Administrator may rescind the notice to the 
State of a public hearing.
    (c) The Administrator shall publish notice of the public hearing in 
the Federal Register and in a newspaper of general circulation in the 
involved State, including a summary of the findings made pursuant to 
paragraph (a) of this section, a statement of the time and location for 
the hearing, and the address and telephone number of an office at which 
interested persons may obtain further information concerning the 
hearing.
    (d) Hearings convened pursuant to paragraphs (b) and (c) of this 
section shall be conducted before a hearing officer to be designated by 
the Administrator. The hearing shall be conducted by the hearing officer 
in an informal, orderly, and expeditious manner. The hearing officer 
shall have the authority to call witnesses, receive oral and written 
testimony, and take such other action as may be necessary to ensure the 
fair and efficient conduct of the hearing. Following the conclusion of 
the hearing, the hearing officer may make a recommendation to the 
Administrator based on the testimony presented at the hearing and shall 
forward any such recommendation and the record of the hearing to the 
Administrator.
    (e) Within 180 days after the date notice is given pursuant to 
paragraph (b) of this section, the Administrator shall:

[[Page 791]]

    (1) Rescind the notice to the State of a public hearing if the State 
takes corrective action satisfactory to the Administrator; or
    (2) Rescind the finding for which the notice was given and promptly 
notify the State of such rescission; or
    (3) Uphold the finding for which the notice was given. In this 
event, the Administrator shall revoke the State's decision that 
filtration was not required or revoke the compliance schedule approved 
by the State, and promulgate, as appropriate, with any appropriate 
modifications, a revised filtration decision or compliance schedule and 
promptly notify the State of such action.
    (f) Revocation of a State's filtration decision or compliance 
schedule and/or promulgation of a revised filtration decision or 
compliance schedule shall take effect 90 days after the State is 
notified under paragraph (e)(3) of this section.

Subpart J [Reserved]



                  Subpart K_Variances for Small System

    Source: 63 FR 43848, Aug. 14, 1998, unless otherwise noted.

                           General Provisions



Sec.  142.301  What is a small system variance?

    Section 1415(e) of the Act authorizes the issuance of variances from 
the requirement to comply with a maximum contaminant level or treatment 
technique to systems serving fewer than 10,000 persons. The purpose of 
this subpart is to provide the procedures and criteria for obtaining 
these variances. The regulations in this subpart shall take effect on 
September 14, 1998.



Sec.  142.302  Who can issue a small system variance?

    A small system variance under this subpart may only be issued by 
either:
    (a) A State that is exercising primary enforcement responsibility 
under Subpart B for public water systems under the State's jurisdiction; 
or
    (b) The Administrator, for a public water system in a State which 
does not have primary enforcement responsibility.



Sec.  142.303  Which size public water systems can receive a small 
system variance?

    (a) A State exercising primary enforcement responsibility for public 
water systems (or the Administrator for other systems) may grant a small 
system variance to public water systems serving 3,300 or fewer persons.
    (b) With the approval of the Administrator pursuant to Sec.  
142.312, a State exercising primary enforcement responsibility for 
public water systems may grant a small system variance to public water 
systems serving more than 3,300 persons but fewer than 10,000 persons.
    (c) In determining the number of persons served by the public water 
system, the State or Administrator must include persons served by 
consecutive systems. A small system variance granted to a public water 
system would also apply to any consecutive system served by it.



Sec.  142.304  For which of the regulatory requirements is a small system 
variance available?

    (a) A small system variance is not available under this subpart for 
a national primary drinking water regulation for a microbial contaminant 
(including a bacterium, virus, or other organism) or an indicator or 
treatment technique for a microbial contaminant.
    (b) A small system variance under this subpart is otherwise only 
available for compliance with a requirement specifying a maximum 
contaminant level or treatment technique for a contaminant with respect 
to which;
    (1) a national primary drinking water regulation was promulgated on 
or after January 1, 1986; and
    (2) the Administrator has published a small system variance 
technology pursuant to Section 1412(b)(15) of the Act.

    Note to paragraph (b)(1): Small system variances are not available 
for public water systems above the pre-1986 maximum contaminant level 
even if subsequently revised. If the Agency revises a pre-1986 maximum 
contaminant level and makes it more stringent, then a variance would be 
available for that contaminant, but only up to the pre-1986 maximum 
contaminant level.

[[Page 792]]



Sec.  142.305  When can a small system variance be granted by a State?

    No small system variance can be granted by a State until the later 
of the following:
    (a) 90 days after the State proposes to grant the small system 
variance;
    (b) If a State is proposing to grant a small system variance to a 
public water system serving 3,300 or fewer persons and the Administrator 
objects to the small system variance, the date on which the State makes 
the recommended modifications or responds in writing to each objection; 
or
    (c) If a State is proposing to grant a small system variance to a 
public water system serving a population more than 3,300 and fewer than 
10,000 persons, the date the Administrator approves the small system 
variance. The Administrator must approve or disapprove the variance 
within 90 days after it is submitted to the Administrator for review.

               Review of Small System Variance Application



Sec.  142.306  What are the responsibilities of the public water system, 
State and the Administrator in ensuring that sufficient information 
is available and for evaluation of a small system variance application?

    (a) A public water system requesting a small system variance must 
provide accurate and correct information to the State or the 
Administrator to issue a small system variance in accordance with this 
subpart. A State may assist a public water system in compiling 
information required for the State or the Administrator to issue a small 
system variance in accordance with this subpart.
    (b) Based upon an application for a small system variance and other 
information, and before a small system variance may be proposed under 
this subpart, the State or the Administrator must find and document the 
following:
    (1) The public water system is eligible for a small system variance 
pursuant to Sec. Sec.  142.303 (i.e., the system serves a population of 
fewer than 10,000 persons) and 142.304 (i.e., the contaminant for which 
the small system variance is sought is not excluded from variance 
eligibility);
    (2) The public water system cannot afford to comply, in accordance 
with the affordability criteria established by the State (or by the 
Administrator in States which do not have primary enforcement 
responsibility), with the national primary drinking water regulation for 
which a small system variance is sought, including by:
    (i) Treatment;
    (ii) Alternative sources of water supply;
    (iii) Restructuring or consolidation changes, including ownership 
change and/or physical consolidation with another public water system; 
or
    (iv) Obtaining financial assistance pursuant to Section 1452 of the 
Act or any other Federal or State program;
    (3) The public water system meets the source water quality 
requirements for installing the small system variance technology 
developed pursuant to guidance published under section 1412(b)(15) of 
the Act;
    (4) The public water system is financially and technically capable 
of installing, operating and maintaining the applicable small system 
variance technology; and
    (5) The terms and conditions of the small system variance, as 
developed through compliance with Sec.  142.307, ensure adequate 
protection of human health, considering the following:
    (i) The quality of the source water for the public water system; and
    (ii) Removal efficiencies and expected useful life of the small 
system variance technology.



Sec.  142.307  What terms and conditions must be included in a small 
system variance?

    (a) A State or the Administrator must clearly specify enforceable 
terms and conditions of a small system variance.
    (b) The terms and conditions of a small system variance issued under 
this subpart must include, at a minimum, the following requirements:
    (1) Proper and effective installation, operation and maintenance of 
the applicable small system variance technology in accordance with 
guidance

[[Page 793]]

published by the Administrator pursuant to section 1412(b)(15) of the 
Act, taking into consideration any relevant source water characteristics 
and any other site-specific conditions that may affect proper and 
effective operation and maintenance of the technology;
    (2) Monitoring requirements, for the contaminant for which a small 
system variance is sought, as specified in 40 CFR part 141; and
    (3) Any other terms or conditions that are necessary to ensure 
adequate protection of public health, which may include:
    (i) Public education requirements; and
    (ii) Source water protection requirements.
    (c) The State or the Administrator must establish a schedule for the 
public water system to comply with the terms and conditions of the small 
system variance which must include, at a minimum, the following 
requirements:
    (1) Increments of progress, such as milestone dates for the public 
water system to apply for financial assistance and begin capital 
improvements;
    (2) Quarterly reporting to the State or Administrator of the public 
water system's compliance with the terms and conditions of the small 
system variance;
    (3) Schedule for the State or the Administrator to review the small 
system variance under paragraph (d) of this section; and
    (4) Compliance with the terms and conditions of the small system 
variance as soon as practicable but not later than 3 years after the 
date on which the small system variance is granted. The Administrator or 
State may allow up to 2 additional years if the Administrator or State 
determines that additional time is necessary for the public water system 
to:
    (i) Complete necessary capital improvements to comply with the small 
system variance technology, secure an alternative source of water, or 
restructure or consolidate; or
    (ii) Obtain financial assistance provided pursuant to section 1452 
of the Act or any other Federal or State program.
    (d) The State or the Administrator must review each small system 
variance granted not less often than every 5 years after the compliance 
date established in the small system variance to determine whether the 
public water system continues to meet the eligibility criteria and 
remains eligible for the small system variance and is complying with the 
terms and conditions of the small system variance. If the public water 
system would no longer be eligible for a small system variance, the 
State or the Administrator must determine whether continuing the 
variance is in the public interest. If the State or the Administrator 
finds that continuing the variance is not in the public interest, the 
variance must be withdrawn.

                          Public Participation



Sec.  142.308  What public notice is required before a State 
or the Administrator proposes to issue a small system variance?

    (a) At least fifteen (15) days before the date of proposal, and at 
least thirty (30) days prior to a public meeting to discuss the proposed 
small system variance, the State, Administrator, or public water system 
as directed by the State or Administrator, must provide notice to all 
persons served by the public water system. For billed customers, 
identified in paragraph (a)(1) of this section, this notice must include 
the information listed in paragraph (c) of this section. For other 
persons regularly served by the system, identified in paragraph (a)(2) 
of this section, the notice shall include the information identified in 
paragraph (d) of this section. Notice must be provided to all persons 
served by:
    (1) Direct mail or other home delivery to billed customers or other 
service connections, and
    (2) Any other method reasonably calculated to notify, in a brief and 
concise manner, other persons regularly served by the system. Such 
methods may include publication in a local newspaper, posting in public 
places or delivery to community organizations.
    (b) At the time of proposal, the State must publish a notice in the 
State equivalent to the Federal Register or a newspaper or newspapers of 
wide circulation in the State, or, in the case of the Administrator, in 
the Federal

[[Page 794]]

Register. This notice shall include the information listed in paragraph 
(c) of this section.
    (c) The notice in paragraphs (a)(1) and (b) of this section must 
include, at a minimum, the following:
    (1) Identification of the contaminant[s] for which a small system 
variance is sought;
    (2) A brief statement of the health effects associated with the 
contaminant[s] for which a small system variance is sought using 
language in appendix C of part 141 subpart O of this chapter;
    (3) The address and telephone number at which interested persons may 
obtain further information concerning the contaminant and the small 
system variance;
    (4) A brief summary, in easily understandable terms, of the terms 
and conditions of the small system variance;
    (5) A description of the consumer petition process under Sec.  
142.310 and information on contacting the EPA Regional Office;
    (6) a brief statement announcing the public meeting required under 
Sec.  142.309(a), including a statement of the purpose of the meeting, 
information regarding the time and location for the meeting, and the 
address and telephone number at which interested persons may obtain 
further information concerning the meeting; and
    (7) In communities with a large proportion of non-English-speaking 
residents, as determined by the primacy agency, information in the 
appropriate language regarding the content and importance of the notice.
    (d) The notice in paragraph (a)(2) of this section must provide 
sufficient information to alert readers to the proposed variance and 
direct them where to receive additional information.
    (e) At its option, the State or the Administrator may choose to 
issue separate notices or additional notices related to the proposed 
small system variance, provided that the requirements in paragraphs (a) 
through (d) of this section are satisfied.
    (f) Prior to promulgating the final variance, the State or the 
Administrator must respond in writing to all significant public comments 
received relating to the small system variance. Response to public 
comment and any other documentation supporting the issuance of a 
variance must be made available to the public after final promulgation.



Sec.  142.309  What are the public meeting requirements associated 
with the proposal of a small system variance?

    (a) A State or the Administrator must provide for at least one (1) 
public meeting on the small system variance no later than 15 days after 
the small system variance is proposed.
    (b) At the time of the public meeting, the State or Administrator 
must prepare and make publicly available, in addition to the information 
listed in Sec.  142.308(c), either:
    (1) The proposed small system variance, if the public meeting occurs 
after proposal of the small system variance; or
    (2) A draft of the proposed small system variance, if the public 
meeting occurs prior to proposal of the proposed small system variance.
    (c) Notice of the public meeting must be provided in the manner 
required under Sec.  142.308 at least 30 days in advance of the public 
meeting. This notice must be provided by the State, the Administrator, 
or the public water system as directed by the State or Administrator.



Sec.  142.310  How can a person served by the public water system obtain 
EPA review of a State proposed small system variance?

    (a) Any person served by the public water system may petition the 
Administrator to object to the granting of a small system variance 
within 30 days after a State proposes to grant a small system variance 
for a public water system.
    (b) The Administrator must respond to a petition filed by any person 
served by the public water system and determine whether to object to the 
small system variance under Sec.  142.311, no later than 60 days after 
the receipt of the petition.

[[Page 795]]

            EPA Review And Approval of Small System Variances



Sec.  142.311  What procedures allow the Administrator to object to a proposed 
small system variance or overturn a granted small system variance for a public 
water system serving 3,300 or fewer persons?

    (a) At the time a State proposes to grant a small system variance 
under this subpart, the State must submit to the Administrator the 
proposed small system variance and all supporting information, including 
any written public comments received prior to proposal.
    (b) The Administrator may review and object to any proposed small 
system variance within 90 days of receipt of the proposed small system 
variance. The Administrator must notify the State in writing of each 
basis for the objection and propose a modification to the small system 
variance to resolve the concerns of the Administrator. The State must 
make the recommended modification, respond in writing to each objection, 
or withdraw the proposal to grant the small system variance.
    (c) If the State issues the small system variance without resolving 
the concerns of the Administrator, the Administrator may overturn the 
State decision to grant the variance if the Administrator determines 
that the State decision does not comply with the Act or this rule.



Sec.  142.312  What EPA action is necessary when a State proposes to grant 
a small system variance to a public water system serving a population 
of more than 3,300 and fewer than 10,000 persons?

    (a) At the time a State proposes to grant a small system variance to 
a public water system serving a population of more than 3,300 and fewer 
than 10,000 persons, the State must submit the proposed small system 
variance and all supporting information, including public comments 
received prior to proposal, to the Administrator.
    (b) The Administrator must approve or disapprove the small system 
variance within 90 days of receipt of the proposed small system variance 
and supporting information. The Administrator must approve the small 
system variance if it meets each requirement within the Act and this 
rule.
    (c) If the Administrator disapproves the small system variance, the 
Administrator must notify the State in writing of the reasons for 
disapproval and the small system variance does not become effective. The 
State may resubmit the small system variance for review and approval 
with modifications to address the objections stated by the 
Administrator.



Sec.  142.313  How will the Administrator review a State's program 
under this subpart?

    (a) The Administrator must periodically review each State program 
under this subpart to determine whether small system variances granted 
by the State comply with the requirements of the Act, this rule and the 
affordability criteria developed by the State.
    (b) If the Administrator determines that small system variances 
granted by a State are not in compliance with the requirements of the 
Act, this rule or the affordability criteria developed by the State, the 
Administrator shall notify the State in writing of the deficiencies and 
make public the determinations.
    (c) The Administrator's review will be based in part on quarterly 
reports prepared by the States pursuant to Sec.  142.15(a)(1) relating 
to violations of increments of progress or other violated terms or 
conditions of small system variances.



PART 143_NATIONAL SECONDARY DRINKING WATER REGULATIONS--Table of Contents



Sec.
143.1 Purpose.
143.2 Definitions.
143.3 Secondary maximum contaminant levels.
143.4 Monitoring.

    Authority: 42 U.S.C. 300f et seq.

    Source: 44 FR 42198, July 19, 1979, unless otherwise noted.



Sec.  143.1  Purpose.

    This part establishes National Secondary Drinking Water Regulations 
pursuant to section 1412 of the Safe

[[Page 796]]

Drinking Water Act, as amended (42 U.S.C. 300g-1). These regulations 
control contaminants in drinking water that primarily affect the 
aesthetic qualities relating to the public acceptance of drinking water. 
At considerably higher concentrations of these contaminants, health 
implications may also exist as well as aesthetic degradation. The 
regulations are not Federally enforceable but are intended as guidelines 
for the States.



Sec.  143.2  Definitions.

    (a) Act means the Safe Drinking Water Act as amended (42 U.S.C. 300f 
et seq.).
    (b) Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    (c) Public water system means a system for the provision to the 
public of piped water for human consumption, if such a system has at 
least fifteen service connections or regularly serves an average of at 
least twenty-five individuals daily at least 60 days out of the year. 
Such term includes (1) any collection, treatment, storage, and 
distribution facilities under control of the operator of such system and 
used primarily in connection with such system, and (2) any collection or 
pretreatment storage facilities not under such control which are used 
primarily in connection with such system. A public water system is 
either a ``community water system'' or a ``non-community water system.''
    (d) State means the agency of the State or Tribal government which 
has jurisdiction over public water systems. During any period when a 
State does not have responsibi1ity pursuant to section 1443 of the Act, 
the term ``State'' means the Regional Administrator, U.S. Environmental 
Protection Agency.
    (e) Supplier of water means any person who owns or operates a public 
water system.
    (f) Secondary maximum contaminant levels means SMCLs which apply to 
public water systems and which, in the judgement of the Administrator, 
are requisite to protect the public welfare. The SMCL means the maximum 
permissible level of a contaminant in water which is delivered to the 
free flowing outlet of the ultimate user of public water system. 
Contamimants added to the water under circumstances controlled by the 
user, except those resulting from corrosion of piping and plumbing 
caused by water quality, are excluded from this definition.

[44 FR 42198, July 19, 1979, as amended at 53 FR 37412, Sept. 26, 1988]



Sec.  143.3  Secondary maximum contaminant levels.

    The secondary maximum contaminant levels for public water systems 
are as follows:

------------------------------------------------------------------------
                Contaminant                             Level
------------------------------------------------------------------------
Aluminum..................................  0.05 to 0.2 mg/l.
Chloride..................................  250 mg/l.
Color.....................................  15 color units.
Copper....................................  1.0 mg/l.
Corrosivity...............................  Non-corrosive.
Fluoride..................................  2.0 mg/l.
Foaming agents............................  0.5 mg/l.
Iron......................................  0.3 mg/l.
Manganese.................................  0.05 mg/l.
Odor......................................  3 threshold odor number.
pH........................................  6.5-8.5.
Silver....................................  0.1 mg/l.
Sulfate...................................  250 mg/l.
Total dissolved solids (TDS)..............  500 mg/l.
Zinc......................................  5 mg/l.
------------------------------------------------------------------------


These levels represent reasonable goals for drinking water quality. The 
States may establish higher or lower levels which may be appropriate 
dependent upon local conditions such as unavailability of alternate 
source waters or other compelling factors, provided that public health 
and welfare are not adversely affected.

[44 FR 42198, July 19, 1979, as amended at 51 FR 11412, Apr. 2, 1986; 56 
FR 3597, Jan. 30, 1991]



Sec.  143.4  Monitoring.

    (a) It is recommended that the parameters in these regulations 
should be monitored at intervals no less frequent than the monitoring 
performed for inorganic chemical contaminants listed in the National 
Interim Primary Drinking Water Regulations as applicable to community 
water systems. More frequent monitoring would be appropriate for 
specific parameters such as pH, color, odor or others under certain 
circumstances as directed by the State.
    (b) Measurement of pH, copper and fluoride to determine compliance 
under

[[Page 797]]

Sec.  143.3 may be conducted with one of the methods in Sec.  
141.23(k)(1). Analyses of aluminum, chloride, foaming agents, iron, 
manganese, odor, silver, sulfate, total dissolved solids (TDS) and zinc 
to determine compliance under Sec.  143.3 may be conducted with the 
methods in the following table or alternative methods listed in appendix 
A to subpart C of part 141. Criteria for analyzing aluminum, copper, 
iron, manganese, silver and zinc samples with digestion or directly 
without digestion, and other analytical test procedures are contained in 
Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 
1994. This document is available from the National Service Center for 
Environmental Publications (NSCEP), P.O. Box 42419, Cincinnati, OH 
45242-0419 or http://www.epa.gov/nscep/.

[[Page 798]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                     SM \4\ 18th and
           Contaminant               EPA           ASTM \3\              19th ed.         SM \4\ 20th ed.       SM \7\ Online             Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aluminum.....................  200.7 \2\  ....................  3120 B.............  3120 B.............  3120 B-99.........
                                  200.8 \2\  ....................  3113 B.............  ...................  3113 B-99.........
                                  200.9 \2\  ....................  3111 D.............  ...................  3111 D-99.........
2. Chloride.....................      300.0  D4327-97, 03........  4110 B.............  4110 B.............  4110 B-00.........
                                       \1\,
                                  300.1 \6\
                                                                   4500-Cl	 D.........  4500-Cl	 D.........  4500-Cl	 D-97.....
                                             D512-89 (Reapproved   4500-Cl	 B.........  4500-Cl	 B.........  4500-Cl	 B-97.....
                                              1999) B.
                                                                                                                                 D6508, Rev. 2 \8\
3. Color........................  .........  ....................  2120 B.............  2120 B.............  2120 B-01.........
4. Foaming Agents...............  .........  ....................  5540 C.............  5540 C.............  5540 C-00.........
5. Iron.........................  200.7 \2\  ....................  3120 B.............  3120 B.............  3120 B-99.........
                                  200.9 \2\  ....................  3111 B.............  ...................  3111 B-99.........
                                             ....................  3113 B.............  ...................  3113 B-99.........
6. Manganese....................  200.7 \2\  ....................  3120 B.............  3120 B.............  3120 B-99.........
                                  200.8 \2\  ....................  3111 B.............  ...................  3111 B-99.........
                                  200.9 \2\  ....................  3113 B.............  ...................  3113 B-99.........
7. Odor.........................             ....................  2150 B.............  2150 B.............  2150 B-97.........
8. Silver.......................  200.7 \2\  ....................  3120 B.............  3120 B.............  3120 B-99.          I-3720-85 \5\
                                  200.8 \2\  ....................  3111 B.............  ...................  3111 B-99.........
                                  200.9 \2\  ....................  3113 B.............  ...................  3113 B-99.........
9. Sulfate......................      300.0  D4327-97, 03........  4110 B.............  4110 B.............  4110 B-00.........
                                       \1\,
                                  300.1 \6\
                                  375.2 \1\  ....................  4500-SO4 \2\	 F....  4500-SO4 \2\	 F....
                                                                   4500-SO4 \2\	 C, D.  4500-SO4 \2\	 C, D.
                                             D516-90, 02.........  4500-SO4 \2\	 E....  4500-SO4 \2\	 E....
                                                                                                                                 D6508, Rev. 2 \8\
10. Total Dissolved Solids......             ....................  2540 C.............  2540 C.............  2540 C-97.........
11. Zinc........................  200.7 \2\  ....................  3120 B.............  3120 B.............  3120 B-99.........
                                  200.8 \2\  ....................  3111 B.............  ...................  3111 B-99.........
--------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents was approved by
  the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources
  listed below. Information regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be
  inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., Room 3334, Washington, DC (Telephone: 202-566-2426); or at the
  National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://
  www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
\1\ ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93-100, August 1993. Available at NTIS, PB94-120821.
\2\ ``Methods for the Determination of Metals in Environmental Samples--Supplement I,'' EPA/600/R-94-111, May 1994. Available at NTIS, PB 95-125472.
\3\ Annual Book of ASTM Standards, 1994, 1996, 1999, or 2004, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the
  method may be used. Copies may be obtained from the ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
\4\ Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American Public
  Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except
  that the versions of 3111 B, 3111 D, and 3113 B in the 20th edition may not be used.
\5\ Method I-3720-85, Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd ed., 1989. Available from
  Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.

[[Page 799]]

 
\6\ ``Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,'' Vol. 1, EPA 815R-00-014, August 2000. Available at NTIS,
  PB2000-106981.
\7\ Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods
  Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used.
\8\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and
  Chromate Electrolyte,'' available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.


[44 FR 42198, July 19, 1979, as amended at 53 FR 5147, Feb. 19, 1988; 56 
FR 30281, July 1, 1991; 59 FR 62470, Dec. 5, 1994; 64 FR 67466, Dec. 1, 
1999; 67 FR 65252, Oct. 23, 2002; 69 FR 18803, Apr. 9, 2004; 72 FR 
11248, Mar. 12, 2007; 74 FR 30959, June 29, 2009]

[[Page 800]]



PART 144_UNDERGROUND INJECTION CONTROL PROGRAM--Table of Contents



                      Subpart A_General Provisions

Sec.
144.1 Purpose and scope of part 144.
144.2 Promulgation of Class II programs for Indian lands.
144.3 Definitions.
144.4 Considerations under Federal law.
144.5 Confidentiality of information.
144.6 Classification of wells.
144.7 Identification of underground sources of drinking water and 
          exempted aquifers.
144.8 Noncompliance and program reporting by the Director.

                 Subpart B_General Program Requirements

144.11 Prohibition of unauthorized injection.
144.12 Prohibition of movement of fluid into underground sources of 
          drinking water.
144.13 Prohibition of Class IV wells.
144.14 Requirements for wells injecting hazardous waste.
144.15 Prohibition of non-experimental Class V wells for geologic 
          sequestration.
144.16 Waiver of requirement by Director.
144.17 Records.
144.18 Requirements for Class VI wells.
144.19 Transitioning from Class II to Class VI.

        Subpart C_Authorization of Underground Injection by Rule

144.21 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells.
144.22 Existing Class II enhanced recovery and hydrocarbon storage 
          wells.
144.23 Class IV wells.
144.24 Class V wells.
144.25 Requiring a permit.
144.26 Inventory requirements.
144.27 Requiring other information.
144.28 Requirements for Class I, II, and III wells authorized by rule.

                    Subpart D_Authorization by Permit

144.31 Application for a permit; authorization by permit.
144.32 Signatories to permit applications and reports.
144.33 Area permits.
144.34 Emergency permits.
144.35 Effect of a permit.
144.36 Duration of permits.
144.37 Continuation of expiring permits.
144.38 Transfer of permits.
144.39 Modification or revocation and reissuance of permits.
144.40 Termination of permits.
144.41 Minor modifications of permits.

                       Subpart E_Permit Conditions

144.51 Conditions applicable to all permits.
144.52 Establishing permit conditions.
144.53 Schedule of compliance.
144.54 Requirements for recording and reporting of monitoring results.
144.55 Corrective action.

 Subpart F_Financial Responsibility: Class I Hazardous Waste Injection 
                                  Wells

144.60 Applicability.
144.61 Definitions of terms as used in this subpart.
144.62 Cost estimate for plugging and abandonment.
144.63 Financial assurance for plugging and abandonment.
144.64 Incapacity of owners or operators, guarantors, or financial 
          institutions.
144.65 Use of State-required mechanisms.
144.66 State assumption of responsibility.
144.70 Wording of the instruments.

  Subpart G_Requirements for Owners and Operators of Class V Injection 
                                  Wells

144.79 General.

                  Definition of Class V Injection Wells

144.80 What is a Class V injection well?
144.81 Does this subpart apply to me?

              Requirements for All Class V Injection Wells

144.82 What must I do to protect underground sources of drinking water?
144.83 Do I need to notify anyone about my Class V injection well?
144.84 Do I need to get a permit?

 Additional Requirements for Class V Large-Capacity Cesspools and Motor 
                      Vehicle Waste Disposal Wells

144.85 Do these additional requirements apply to me?
144.86 What are the definitions I need to know?
144.87 How does the identification of ground water protection areas and 
          other sensitive areas affect me?
144.88 What are the additional requirements?
144.89 How do I close my Class V injection well?

    Authority: Safe Drinking Water Act, 42 U.S.C. 300f et seq.; Resource 
Conservation and Recovery Act, 42 U.S.C. 6901 et seq.

    Source: 48 FR 14189, Apr. 1, 1983, unless otherwise noted.

[[Page 801]]



                      Subpart A_General Provisions



Sec.  144.1  Purpose and scope of part 144.

    (a) Contents of part 144. The regulations in this part set forth 
requirements for the Underground Injection Control (UIC) program 
promulgated under Part C of the Safe Drinking Water Act (SDWA) (Pub. L. 
93-523, as amended; 42 U.S.C. 300f et seq.) and, to the extent that they 
deal with hazardous waste, the Resource Conservation and Recovery Act 
(RCRA) (Pub. L. 94-580 as amended; 42 U.S.C. 6901 et seq.).
    (b) Applicability. (1) The regulations in this part establish 
minimum requirements for UIC programs. To the extent set forth in part 
145, each State must meet these requirements in order to obtain primary 
enforcement authority for the UIC program in that State.
    (2) In addition to serving as minimum requirements for UIC programs, 
the regulations in this part constitute a part of the UIC program for 
States listed in part 147 to be administered directly by EPA.
    (c) The information requirements located in the following sections 
have been cleared by the Office of Management and Budget: Sections 
144.11, 144.28(c)(d)(i), 144.31, 14.33, 144.51(j)(m) (n), 144.52(a), 
144.54, 144.55, 144.15, 144.23, 144.26, 144.27, 144.28(i)(k), 144.51(o), 
146.52. The OMB clearance number is 2040-0042.
    (d) Authority. (1) Section 1421 of SDWA requires the Administrator 
to promulgate regulations establishing minimum requirements for 
effective UIC programs.
    (2) Section 1422 of SDWA requires the Administrator to list in the 
Federal Register ``each State for which in his judgment a State 
underground injection control program may be necessary to assure that 
underground injection will not endanger drinking water sources'' and to 
establish by regulation a program for EPA administration of UIC programs 
in the absence of an approved State program in a listed State.
    (3) Section 1423 of SDWA provides procedures for EPA enforcement of 
UIC requirements.
    (4) Section 1431 authorizes the Administrator to take action to 
protect the health of persons when a contaminant which is present in or 
may enter a public water system or underground source of drinking water 
may present an imminent and substantial endangerment to the health of 
persons.
    (5) Section 1445 of SDWA authorizes the promulgation of regulations 
for such recordkeeping, reporting, and monitoring requirements ``as the 
Administrator may reasonably require * * * to assist him in establishing 
regulations under this title,'' and a ``right of entry and inspection to 
determine compliance with this title, including for this purpose, 
inspection, at reasonable time, or records, files, papers, processes, 
controls, and facilities * * *.''
    (6) Section 1450 of SDWA authorizes the Administrator ``to prescribe 
such regulations as are necessary or appropriate to carry out his 
functions'' under SDWA.
    (e) Overview of the UIC program. An UIC program is necessary in any 
State listed by EPA under section 1422 of the SDWA. Because all States 
have been listed, the SDWA requires all States to submit an UIC program 
within 270 days after July 24, 1980, the effective date of 40 CFR part 
146, which was the final element of the UIC minimum requirements to be 
originally promulgated, unless the Administrator grants an extension, 
which can be for a period not to exceed an additional 270 days. If a 
State fails to submit an approvable program, EPA will establish a 
program for that State. Once a program is established, SDWA provides 
that all underground injections in listed States are unlawful and 
subject to penalties unless authorized by a permit or a rule. This part 
sets forth the requirements governing all UIC programs, authorizations 
by permit or rule and prohibits certain types of injection. The 
technical regulations governing these authorizations appear in 40 CFR 
part 146.
    (f) Structure of the UIC program--(1) Part 144. This part sets forth 
the permitting and other program requirements that must be met by UIC 
Programs, whether run by a State or by EPA. It is divided into the 
following subparts:
    (i) Subpart A describes general elements of the program, including 
definitions and classifications.

[[Page 802]]

    (ii) Subpart B sets forth the general program requirements, 
including the performance standards applicable to all injection 
activities, basic elements that all UIC programs must contain, and 
provisions for waiving permit of rule requirements under certain 
circumstances.
    (iii) Subpart C sets forth requirements for wells authorized by 
rule.
    (iv) Subpart D sets forth permitting procedures.
    (v) Subpart E sets forth specific conditions, or types of 
conditions, that must at a minimum be included in all permits.
    (vi) Subpart F sets forth the financial responsibility requirements 
for owners and operators of all existing and new Class I hazardous waste 
injection wells.
    (vii) Subpart G of this part sets forth requirements for owners and 
operators of Class V injection wells.
    (viii) Subpart H of part 146 sets forth requirements for owners or 
operators of Class VI injection wells.
    (2) Part 145. While part 144 sets forth minimum requirements for all 
UIC Programs, these requirements are specifically identified as elements 
of a State application for primacy to administer an UIC Program in part 
145. Part 145 also sets forth the necessary elements of a State 
submission and the procedural requirements for approval of State 
programs.
    (3) Part 124. The public participation requirements that must be met 
by UIC Programs, whether administered by the State or by EPA, are set 
forth in part 124. EPA must comply with all part 124 requirements; State 
administered programs must comply with part 124 as required by part 145. 
These requirements carry out the purposes of the public participation 
requirement of 40 CFR part 25 (Public Participation), and supersede the 
requirements of that part as they apply to the UIC Program.
    (4) Part 146. This part sets forth the technical criteria and 
standards that must be met in permits and authorizations by rule as 
required by part 144.
    (g) Scope of the permit or rule requirement. The UIC permit program 
regulates underground injection by six classes of wells (see definition 
of ``well injection,'' Sec.  144.3). The six classes of wells are set 
forth in Sec.  144.6. All owners or operators of these injection wells 
must be authorized either by permit or rule by the Director. In carrying 
out the mandate of the SDWA, this subpart provides that no injection 
shall be authorized by permit or rule if it results in the movement of 
fluid containing any contaminant into underground sources of drinking 
water (USDWs--see Sec.  144.3 for definition), if the presence of that 
contaminant may cause a violation of any primary drinking water 
regulation under 40 CFR part 141 or may adversely affect the health of 
persons (Sec.  144.12). Existing Class IV wells which inject hazardous 
waste directly into an underground source of drinking water are to be 
eliminated over a period of six months and new such Class IV wells are 
to be prohibited (Sec.  144.13). For Class V wells, if remedial action 
appears necessary, a permit may be required (Sec.  144.25) or the 
Director must require remedial action or closure by order (Sec.  
144.6(c)). During UIC program development, the Director may identify 
aquifers and portions of aquifers which are actual or potential sources 
of drinking water. This will provide an aid to the Director in carrying 
out his or her duty to protect all USDWs. An aquifer is a USDW if it 
fits the definition under Sec.  144.3, even if it has not been 
``identified.'' The Director may also designate ``exempted aquifers'' 
using the criteria in 40 CFR 146.4 of this chapter. Such aquifers are 
those which would otherwise qualify as ``underground sources of drinking 
water'' to be protected, but which have no real potential to be used as 
drinking water sources. Therefore, they are not USDWs. No aquifer is an 
exempted aquifer until it has been affirmatively designated under the 
procedures at Sec.  144.7. Aquifers which do not fit the definition of 
``underground source of drinking water'' are not ``exempted aquifers.'' 
They are simply not subject to the special protection afforded USDWs. 
During initial Class VI program development, the Director shall not 
expand the areal extent of an existing Class II enhanced oil recovery or 
enhanced gas recovery aquifer exemption for Class VI injection wells and 
EPA shall not approve a program that applies for aquifer exemption 
expansions of Class II-Class VI exemptions as

[[Page 803]]

part of the program description. All Class II to Class VI aquifer 
exemption expansions previously issued by EPA must be incorporated into 
the Class VI program descriptions pursuant to requirements at Sec.  
145.23(f)(9).
    (1) Specific inclusions. The following wells are included among 
those types of injection activities which are covered by the UIC 
regulations. (This list is not intended to be exclusive but is for 
clarification only.)
    (i) Any injection well located on a drilling platform inside the 
State's territorial waters.
    (ii) Any dug hole or well that is deeper than its largest surface 
dimension, where the principal function of the hole is emplacement of 
fluids.
    (iii) Any well used by generators of hazardous waste, or by owners 
or operators of hazardous waste management facilities, to dispose of 
fluids containing hazardous waste. This includes the disposal of 
hazardous waste into what would otherwise be septic systems and 
cesspools, regardless of their capacity.
    (iv) Any septic tank, cesspool, or other well used by a multiple 
dwelling, community, or Regional system for the injection of wastes.
    (2) Specific exclusions. The following are not covered by these 
regulations:
    (i) Injection wells located on a drilling platform or other site 
that is beyond the State's territorial waters.
    (ii) Individual or single family residential waste disposal systems 
such as domestic cesspools or septic systems.
    (iii) Non-residential cesspools, septic systems or similar waste 
disposal systems if such systems (A) Are used solely for the disposal of 
sanitary waste, and (B) have the capacity to serve fewer than 20 persons 
a day.
    (iv) Injection wells used for injection of hydrocarbons which are of 
pipeline quality and are gases at standard temperature and pressure for 
the purpose of storage.
    (v) Any dug hole, drilled hole, or bored shaft which is not used for 
the subsurface emplacement of fluids.
    (3) The prohibition applicable to Class IV wells under Sec.  144.13 
does not apply to injections of hazardous wastes into aquifers or 
portions thereof which have been exempted pursuant to Sec.  146.04.
    (h) Interim Status under RCRA for Class I Hazardous Waste Injection 
Wells. The minimum national standards which define acceptable injection 
of hazardous waste during the period of interim status under RCRA are 
set out in the applicable provisions of this part, parts 146 and 147, 
and Sec.  265.430 of this chapter. The issuance of a UIC permit does not 
automatically terminate RCRA interim status. A Class I well's interim 
status does, however, automatically terminate upon issuance to that well 
of a RCRA permit, or upon the well's receiving a RCRA permit-by-rule 
under Sec.  270.60(b) of this chapter. Thus, until a Class I well 
injecting hazardous waste receives a RCRA permit or RCRA permit-by-rule, 
the well's interim status requirements are the applicable requirements 
imposed pursuant to this part and parts 146, 147, and 265 of this 
chapter, including any requirements imposed in the UIC permit.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20181, May 11, 1984; 52 
FR 20676, June 2, 1987; 52 FR 45797, Dec. 1, 1987; 53 FR 28147, July 26, 
1988; 64 FR 68565, Dec. 7, 1999; 67 FR 39592, June 7, 2002; 75 FR 77286, 
Dec. 10, 2010]



Sec.  144.2  Promulgation of Class II programs for Indian lands.

    Notwithstanding the requirements of this part or parts 124 and 146 
of this chapter, the Administrator may promulgate an alternate UIC 
Program for Class II wells on any Indian reservation or Indian lands. In 
promulgating such a program the Administrator shall consider the 
following factors:
    (a) The interest and preferences of the tribal government having 
responsibility for the given reservation or Indian lands;
    (b) The consistency between the alternate program and any program in 
effect in an adjoining jurisdiction; and
    (c) Such other factors as are necessary and appropriate to carry out 
the Safe Drinking Water Act.



Sec.  144.3  Definitions.

    Terms not defined in this section have the meaning given by the 
appropriate Act. When a defined term appears in a definition, the 
defined term

[[Page 804]]

is sometimes placed within quotation marks as an aid to readers.
    Administrator means the Administrator of the United States 
Environmental Protection Agency, or an authorized representative.
    Application means the EPA standard national forms for applying for a 
permit, including any additions, revisions or modifications to the 
forms; or forms approved by EPA for use in approved States, including 
any approved modifications or revisions.
    Appropriate Act and regulations means the Solid Waste Disposal Act, 
as amended by the Resource Conservation and Recovery Act (RCRA); or Safe 
Drinking Water Act (SDWA), whichever is applicable; and applicable 
regulations promulgated under those statutes.
    Approved State Program means a UIC program administered by the State 
or Indian Tribe that has been approved by EPA according to SDWA sections 
1422 and/or 1425.
    Aquifer means a geological ``formation,'' group of formations, or 
part of a formation that is capable of yielding a significant amount of 
water to a well or spring.
    Area of review means the area surrounding an injection well 
described according to the criteria set forth in Sec.  146.06 or in the 
case of an area permit, the project area plus a circumscribing area the 
width of which is either \1/4\ of a mile or a number calculated 
according to the criteria set forth in Sec.  146.06.
    Cesspool means a ``drywell'' that receives untreated sanitary waste 
containing human excreta, and which sometimes has an open bottom and/or 
perforated sides.
    Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    Director means the Regional Administrator, the State director or the 
Tribal director as the context requires, or an authorized 
representative. When there is no approved State or Tribal program, and 
there is an EPA administered program, ``Director'' means the Regional 
Administrator. When there is an approved State or Tribal program, 
``Director'' normally means the State or Tribal director. In some 
circumstances, however, EPA retains the authority to take certain 
actions even when there is an approved State or Tribal program. In such 
cases, the term ``Director'' means the Regional Administrator and not 
the State or Tribal director.
    Draft permit means a document prepared under Sec.  124.6 indicating 
the Director's tentative decision to issue or deny, modify, revoke and 
reissue, terminate, or reissue a ``permit.'' A notice of intent to 
terminate a permit, and a notice of intent to deny a permit, as 
discussed in Sec.  124.5 are types of ``draft permits.'' A denial of a 
request for modification, revocation and reissuance, or termination, as 
discussed in Sec.  124.5 is not a ``draft permit.''
    Drilling mud means a heavy suspension used in drilling an 
``injection well,'' introduced down the drill pipe and through the drill 
bit.
    Drywell means a well, other than an improved sinkhole or subsurface 
fluid distribution system, completed above the water table so that its 
bottom and sides are typically dry except when receiving fluids.
    Eligible Indian Tribe is a Tribe that meets the statutory 
requirements established at 42 U.S.C. 300j-11(b)(1).
    Emergency permit means a UIC ``permit'' issued in accordance with 
Sec.  144.34.
    Environmental Protection Agency (``EPA'') means the United States 
Environmental Protection Agency.
    EPA means the United States ``Environmental Protection Agency.''
    Exempted aquifer means an ``aquifer'' or its portion that meets the 
criteria in the definition of ``underground source of drinking water'' 
but which has been exempted according to the procedures in Sec.  144.7.
    Existing injection well means an ``injection well'' other than a 
``new injection well.''
    Facility or activity means any UIC ``injection well,'' or an other 
facility or activity that is subject to regulation under the UIC 
program.
    Fluid means any material or substance which flows or moves whether 
in a semisolid, liquid, sludge, gas, or any other form or state.
    Formation means a body of consolidated or unconsolidated rock 
characterized by a degree of lithologic homogeneity which is 
prevailingly, but not

[[Page 805]]

necessarily, tabular and is mappable on the earth's surface or traceable 
in the subsurface.
    Formation fluid means ``fluid'' present in a ``formation'' under 
natural conditions as opposed to introduced fluids, such as ``drilling 
mud.''
    Generator means any person, by site location, whose act or process 
produces hazardous waste identified or listed in 40 CFR part 261.
    Geologic sequestration means the long-term containment of a gaseous, 
liquid, or supercritical carbon dioxide stream in subsurface geologic 
formations. This term does not apply to carbon dioxide capture or 
transport.
    Ground water means water below the land surface in a zone of 
saturation.
    Hazardous waste means a hazardous waste as defined in 40 CFR 261.3.
    Hazardous waste management facility (``HWM facility'') means all 
contiguous land, and structures, other appurtenances, and improvements 
on the land used for treating, storing, or disposing of hazardous waste. 
A facility may consist of several treatment, storage, or disposal 
operational units (for example, one or more landfills, surface 
impoundments, or combination of them).
    HWM facility means ``Hazardous Waste Management facility''
    Improved sinkhole means a naturally occurring karst depression or 
other natural crevice found in volcanic terrain and other geologic 
settings which have been modified by man for the purpose of directing 
and emplacing fluids into the subsurface.
    Indian lands means ``Indian country'' as defined in 18 U.S.C. 1151. 
That section defines Indian country as:
    (a) All land within the limits of any Indian reservation under the 
jurisdiction of the United States government, notwithstanding the 
issuance of any patent, and, including rights-of-way running through the 
reservation;
    (b) All dependent Indian communities within the borders of the 
United States whether within the original or subsequently acquired 
territory thereof, and whether within or without the limits of a State; 
and
    (c) All Indian allotments, the Indian titles to which have not been 
extinguished, including rights-of-way running through the same.
    Indian Tribe means any Indian Tribe having a Federally recognized 
governing body carrying out substantial governmental duties and powers 
over a defined area.
    Injection well means a ``well'' into which ``fluids'' are being 
injected.
    Injection zone means a geological ``formation'' group of formations, 
or part of a formation receiving fluids through a ``well.''
    Interstate Agency means an agency of two or more States established 
by or under an agreement or compact approved by the Congress, or any 
other agency of two or more States or Indian Tribes having substantial 
powers or duties pertaining to the control of pollution as determined 
and approved by the Administrator under the ``appropriate Act and 
regulations.''
    Major facility means any UIC ``facility or activity'' classified as 
such by the Regional Administrator, or, in the case of approved State 
programs, the Regional Administrator in conjunction with the State 
Director.
    Manifest means the shipping document originated and signed by the 
``generator'' which contains the information required by subpart B of 40 
CFR part 262.
    New injection wells means an ``injection well'' which began 
injection after a UIC program for the State applicable to the well is 
approved or prescribed.
    Owner or operator means the owner or operator of any ``facility or 
activity'' subject to regulation under the UIC program.
    Permit means an authorization, license, or equivalent control 
document issued by EPA or an approved State to implement the 
requirements of this part, parts 145, 146 and 124. ``Permit'' includes 
an area permit (Sec.  144.33) and an emergency permit (Sec.  144.34). 
Permit does not include UIC authorization by rule (Sec.  144.21), or any 
permit which has not yet been the subject of final agency action, such 
as a ``draft permit.''
    Person means an individual, association, partnership, corporation, 
municipality, State, Federal, or Tribal agency, or an agency or employee 
thereof.
    Plugging means the act or process of stopping the flow of water, oil 
or gas

[[Page 806]]

into or out of a formation through a borehole or well penetrating that 
formation.
    Point of injection means the last accessible sampling point prior to 
waste fluids being released into the subsurface environment through a 
Class V injection well. For example, the point of injection of a Class V 
septic system might be the distribution box--the last accessible 
sampling point before the waste fluids drain into the underlying soils. 
For a dry well, it is likely to be the well bore itself.
    Project means a group of wells in a single operation.
    Radioactive Waste means any waste which contains radioactive 
material in concentrations which exceed those listed in 10 CFR part 20, 
appendix B, table II, column 2.
    RCRA means the Solid Waste Disposal Act as amended by the Resource 
Conservation and Recovery Act of 1976 (Pub. L. 94-580, as amended by 
Pub. L. 95-609, Pub. L. 96-510, 42 U.S.C. 6901 et seq.).
    Regional Administrator means the Regional Administrator of the 
appropriate Regional Office of the Environmental Protection Agency or 
the authorized representative of the Regional Administrator.
    Sanitary waste means liquid or solid wastes originating solely from 
humans and human activities, such as wastes collected from toilets, 
showers, wash basins, sinks used for cleaning domestic areas, sinks used 
for food preparation, clothes washing operations, and sinks or washing 
machines where food and beverage serving dishes, glasses, and utensils 
are cleaned. Sources of these wastes may include single or multiple 
residences, hotels and motels, restaurants, bunkhouses, schools, ranger 
stations, crew quarters, guard stations, campgrounds, picnic grounds, 
day-use recreation areas, other commercial facilities, and industrial 
facilities provided the waste is not mixed with industrial waste.
    Schedule of compliance means a schedule of remedial measures 
included in a ``permit,'' including an enforceable sequence of interim 
requirements (for example, actions, operations, or milestone events) 
leading to compliance with the ``appropriate Act and regulations.''
    SDWA means the Safe Drinking Water Act (Pub. L. 93-523, as amended; 
42 U.S.C. 300f et seq.).
    Septic system means a ``well'' that is used to emplace sanitary 
waste below the surface and is typically comprised of a septic tank and 
subsurface fluid distribution system or disposal system.
    Site means the land or water area where any ``facility or activity'' 
is physically located or conducted, including adjacent land used in 
connection with the facility or activity.
    State means any of the 50 States, the District of Columbia, Guam, 
the Commonwealth of Puerto Rico, the Virgin Islands, American Samoa, the 
Trust Territory of the Pacific Islands, the Commonwealth of the Northern 
Mariana Islands, or an Indian Tribe treated as a State.
    State Director means the chief administrative officer of any State, 
interstate, or Tribal agency operating an ``approved program,'' or the 
delegated representative of the State director. If the responsibility is 
divided among two or more States, interstate, or Tribal agencies, 
``State Director'' means the chief administrative officer of the State, 
interstate, or Tribal agency authorized to perform the particular 
procedure or function to which reference is made.
    State/EPA agreement means an agreement between the Regional 
Administrator and the State which coordinates EPA and State activities, 
responsibilities and programs.
    Stratum (plural strata) means a single sedimentary bed or layer, 
regardless of thickness, that consists of generally the same kind of 
rock material.
    Subsurface fluid distribution system means an assemblage of 
perforated pipes, drain tiles, or other similar mechanisms intended to 
distribute fluids below the surface of the ground.
    Total dissolved solids means the total dissolved (filterable) solids 
as determined by use of the method specified in 40 CFR part 136.
    Transferee means the owner or operator receiving ownership and/or 
operational control of the well.

[[Page 807]]

    Transferor means the owner or operator transferring ownership and/or 
operational control of the well.
    UIC means the Underground Injection Control program under Part C of 
the Safe Drinking Water Act, including an ``approved State program.''
    Underground injection means a ``well injection.''
    Underground source of drinking water (USDW) means an aquifer or its 
portion:
    (a)(1) Which supplies any public water system; or
    (2) Which contains a sufficient quantity of ground water to supply a 
public water system; and
    (i) Currently supplies drinking water for human consumption; or
    (ii) Contains fewer than 10,000 mg/l total dissolved solids; and
    (b) Which is not an exempted aquifer.
    USDW means ``underground source of drinking water.''
    Well means: A bored, drilled, or driven shaft whose depth is greater 
than the largest surface dimension; or, a dug hole whose depth is 
greater than the largest surface dimension; or, an improved sinkhole; 
or, a subsurface fluid distribution system.
    Well injection means the subsurface emplacement of fluids through a 
well.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 45305, Nov. 15, 1984; 52 
FR 20676, June 2, 1987; 53 FR 37412, Sept. 26, 1988; 58 FR 63895, Dec. 
3, 1993; 59 FR 64345, Dec. 14, 1994; 64 FR 68565, Dec. 7, 1999; 75 FR 
77287, Dec. 10, 2010]



Sec.  144.4  Considerations under Federal law.

    The following is a list of Federal laws that may apply to the 
issuance of permits under these rules. When any of these laws is 
applicable, its procedures must be followed. When the applicable law 
requires consideration or adoption of particular permit conditions or 
requires the denial of a permit, those requirements also must be 
followed.
    (a) The Wild and Scenic Rivers Act, 16 U.S.C. 1273 et seq. Section 7 
of the Act prohibits the Regional Administrator from assisting by 
license or otherwise the construction of any water resources project 
that would have a direct, adverse effect on the values for which a 
national wild and scenic river was established.
    (b) The National Historic Preservation Act of 1966, 16 U.S.C. 470 et 
seq. Section 106 of the Act and implementing regulations (36 CFR part 
800) require the Regional Administrator, before issuing a license, to 
adopt measures when feasible to mitigate potential adverse effects of 
the licensed activity and properties listed or eligible for listing in 
the National Register of Historic Places. The Act's requirements are to 
be implemented in cooperation with State Historic Preservation Officers 
and upon notice to, and when appropriate, in consultation with the 
Advisory Council on Historic Preservation.
    (c) The Endangered Species Act, 16 U.S.C. 1531 et seq. Section 7 of 
the Act and implementing regulations (50 CFR part 402) require the 
Regional Administrator to ensure, in consultation with the Secretary of 
the Interior or Commerce, that any action authorized by EPA is not 
likely to jeopardize the continued existence of any endangered or 
threatened species or adversely affect its critical habitat.
    (d) The Coastal Zone Management Act, 16 U.S.C. 1451 et seq. Section 
307(c) of the Act and implementing regulations (15 CFR part 930) 
prohibit EPA from issuing a permit for an activity affecting land or 
water use in the coastal zone until the applicant certifies that the 
proposed activity complies with the State Coastal Zone Management 
program, and the State or its designated agency concurs with the 
certification (or the Secretary of Commerce overrides the States 
nonconcurrence).
    (e) The Fish and Wildlife Coordination Act, 16 U.S.C. 661 et seq., 
requires the Regional Administrator, before issuing a permit proposing 
or authorizing the impoundment (with certain exemptions), diversion, or 
other control or modification of any body of water, consult with the 
appropriate State agency exercising jurisdiction over wildlife resources 
to conserve these resources.
    (f) Executive orders. [Reserved]

(Clean Water Act (33 U.S.C. 1251 et seq.), Safe Drinking Water Act (42 
U.S.C. 300f et seq.), Clean Air Act (42 U.S.C. 7401 et seq.), Resource 
Conservation and Recovery Act (42 U.S.C. 6901 et seq.))

[48 FR 14189, Apr. 1, 1983, as amended at 48 FR 39621, Sept. 1, 1983]

[[Page 808]]



Sec.  144.5  Confidentiality of information.

    (a) In accordance with 40 CFR part 2, any information submitted to 
EPA pursuant to these regulations may be claimed as confidential by the 
submitter. Any such claim must be asserted at the time of submission in 
the manner prescribed on the application form or instructions or, in the 
case of other submissions, by stamping the words ``confidential business 
information'' on each page containing such information. If no claim is 
made at the time of submission, EPA may make the information available 
to the public without further notice. If a claim is asserted, the 
information will be treated in accordance with the procedures in 40 CFR 
part 2 (Public Information).
    (b) Claims of confidentiality for the following information will be 
denied:
    (1) The name and address of any permit applicant or permittee;
    (2) Information which deals with the existence, absence, or level of 
contaminants in drinking water.



Sec.  144.6  Classification of wells.

    Injection wells are classified as follows:
    (a) Class I. (1) Wells used by generators of hazardous waste or 
owners or operators of hazardous waste management facilities to inject 
hazardous waste beneath the lowermost formation containing, within one-
quarter mile of the well bore, an underground source of drinking water.
    (2) Other industrial and municipal disposal wells which inject 
fluids beneath the lowermost formation containing, within one quarter 
mile of the well bore, an underground source of drinking water.
    (3) Radioactive waste disposal wells which inject fluids below the 
lowermost formation containing an underground source of drinking water 
within one quarter mile of the well bore.
    (b) Class II. Wells which inject fluids:
    (1) Which are brought to the surface in connection with natural gas 
storage operations, or conventional oil or natural gas production and 
may be commingled with waste waters from gas plants which are an 
intergral part of production operations, unless those waters are 
classified as a hazardous waste at the time of injection.
    (2) For enhanced recovery of oil or natural gas; and
    (3) For storage of hydrocarbons which are liquid at standard 
temperature and pressure.
    (c) Class III. Wells which inject for extraction of minerals 
including:
    (1) Mining of sulfur by the Frasch process;
    (2) In situ production of uranium or other metals; this category 
includes only in-situ production from ore bodies which have not been 
conventionally mined. Solution mining of conventional mines such as 
stopes leaching is included in Class V.
    (3) Solution mining of salts or potash.
    (d) Class IV. (1) Wells used by generators of hazardous waste or of 
radioactive waste, by owners or operators of hazardous waste management 
facilities, or by owners or operators of radioactive waste disposal 
sites to dispose of hazardous waste or radioactive waste into a 
formation which within one-quarter (\1/4\) mile of the well contains an 
underground source of drinking water.
    (2) Wells used by generators of hazardous waste or of radioactive 
waste, by owners or operators of hazardous waste management facilities, 
or by owners or operators of radioactive waste disposal sites to dispose 
of hazardous waste or radioactive waste above a formation which within 
one-quarter (\1/4\) mile of the well contains an underground source of 
drinking water.
    (3) Wells used by generators of hazardous waste or owners or 
operators of hazardous waste management facilities to dispose of 
hazardous waste, which cannot be classified under paragraph (a)(1) or 
(d) (1) and (2) of this section (e.g., wells used to dispose of 
hazardous waste into or above a formation which contains an aquifer 
which has been exempted pursuant to Sec.  146.04).
    (e) Class V. Injection wells not included in Class I, II, III, IV, 
or VI. Specific types of Class V injection wells are described in Sec.  
144.81.
    (f) Class VI. Wells that are not experimental in nature that are 
used for geologic sequestration of carbon dioxide

[[Page 809]]

beneath the lowermost formation containing a USDW; or, wells used for 
geologic sequestration of carbon dioxide that have been granted a waiver 
of the injection depth requirements pursuant to requirements at Sec.  
146.95 of this chapter; or, wells used for geologic sequestration of 
carbon dioxide that have received an expansion to the areal extent of an 
existing Class II enhanced oil recovery or enhanced gas recovery aquifer 
exemption pursuant to Sec. Sec.  146.4 of this chapter and 144.7(d).

[48 FR 14189, Apr. 1, 1983, as amended at 52 FR 20676, June 2, 1987; 64 
FR 68565, Dec. 7, 1999; 75 FR 77287, Dec. 10, 2010]



Sec.  144.7  Identification of underground sources of drinking water 
and exempted aquifers.

    (a) The Director may identify (by narrative description, 
illustrations, maps, or other means) and shall protect as underground 
sources of drinking water, all aquifers and parts of aquifers which meet 
the definition of ``underground source of drinking water'' in Sec.  
144.3, except to the extent there is an applicable aquifer exemption 
under paragraph (b) of this section or an expansion to the areal extent 
of an existing Class II enhanced oil recovery or enhanced gas recovery 
aquifer exemption for the exclusive purpose of Class VI injection for 
geologic sequestration under paragraph (d) of this section. Other than 
EPA approved aquifer exemption expansions that meet the criteria set 
forth in Sec.  146.4(d) of this chapter, new aquifer exemptions shall 
not be issued for Class VI injection wells. Even if an aquifer has not 
been specifically identified by the Director, it is an underground 
source of drinking water if it meets the definition in Sec.  144.3.
    (b)(1) The Director may identify (by narrative description, 
illustrations, maps, or other means) and describe in geographic and/or 
geometric terms (such as vertical and lateral limits and gradient) which 
are clear and definite, all aquifers or parts thereof which the Director 
proposes to designate as exempted aquifers using the criteria in Sec.  
146.4 of this chapter.
    (2) No designation of an exempted aquifer submitted as part of a UIC 
program shall be final until approved by the Administrator as part of a 
UIC program. No designation of an expansion to the areal extent of a 
Class II enhanced oil recovery or enhanced gas recovery aquifer 
exemption for the exclusive purpose of Class VI injection for geologic 
sequestration shall be final until approved by the Administrator as a 
revision to the applicable Federal UIC program under part 147 or as a 
substantial revision of an approved State UIC program in accordance with 
Sec.  145.32 of this chapter.
    (3) Subsequent to program approval or promulgation, the Director 
may, after notice and opportunity for a public hearing, identify 
additional exempted aquifers. For approved State programs exemption of 
aquifers identifed (i) under Sec.  146.04(b) shall be treated as a 
program revision under Sec.  145.32; (ii) under Sec.  146.04(c) shall 
become final if the State Director submits the exemption in writing to 
the Administrator and the Administrator has not disapproved the 
designation within 45 days. Any disapproval by the Administrator shall 
state the reasons and shall constitute final Agency action for purposes 
of judicial review.
    (c)(1) For Class III wells, the Director shall require an applicant 
for a permit which necessitates an aquifer exemption under Sec.  
146.04(b)(1) to furnish the data necessary to demonstrate that the 
aquifer is expected to be mineral or hydrocarbon producing. Information 
contained in the mining plan for the proposed project, such as a map and 
general description of the mining zone, general information on the 
mineralogy and geochemistry of the mining zone, analysis of the 
amenability of the mining zone to the proposed mining method, and a 
time-table of planned development of the mining zone shall be considered 
by the Director in addition to the information required by Sec.  
144.31(g).
    (2) For Class II wells, a demonstration of commercial producibility 
shall be made as follows:
    (i) For a Class II well to be used for enhanced oil recovery 
processes in a field or project containing aquifers from which 
hydrocarbons were previously produced, commercial producibility shall be 
presumed by the Director upon a demonstration by the

[[Page 810]]

applicant of historical production having occurred in the project area 
or field.
    (ii) For Class II wells not located in a field or project containing 
aquifers from which hydrocarbons were previously produced, information 
such as logs, core data, formation description, formation depth, 
formation thickness and formation parameters such as permeability and 
porosity shall be considered by the Director, to the extent such 
information is available.
    (d) Expansion to the areal extent of existing Class II aquifer 
exemptions for Class VI wells. Owners or operators of Class II enhanced 
oil recovery or enhanced gas recovery wells may request that the 
Director approve an expansion to the areal extent of an aquifer 
exemption already in place for a Class II enhanced oil recovery or 
enhanced gas recovery well for the exclusive purpose of Class VI 
injection for geologic sequestration. Such requests must be treated as a 
revision to the applicable Federal UIC program under part 147 or as a 
substantial program revision to an approved State UIC program under 
Sec.  145.32 of this chapter and will not be final until approved by 
EPA.
    (1) The owner or operator of a Class II enhanced oil recovery or 
enhanced gas recovery well that requests an expansion of the areal 
extent of an existing aquifer exemption for the exclusive purpose of 
Class VI injection for geologic sequestration must define (by narrative 
description, illustrations, maps, or other means) and describe in 
geographic and/or geometric terms (such as vertical and lateral limits 
and gradient) that are clear and definite, all aquifers or parts thereof 
that are requested to be designated as exempted using the criteria in 
Sec.  146.4 of this chapter.
    (2) In evaluating a request to expand the areal extent of an aquifer 
exemption of a Class II enhanced oil recovery or enhanced gas recovery 
well for the purpose of Class VI injection, the Director must determine 
that the request meets the criteria for exemptions in Sec.  146.4. In 
making the determination, the Director shall consider:
    (i) Current and potential future use of the USDWs to be exempted as 
drinking water resources;
    (ii) The predicted extent of the injected carbon dioxide plume, and 
any mobilized fluids that may result in degradation of water quality, 
over the lifetime of the GS project, as informed by computational 
modeling performed pursuant to Sec.  146.84(c)(1), in order to ensure 
that the proposed injection operation will not at any time endanger 
USDWs including non-exempted portions of the injection formation;
    (iii) Whether the areal extent of the expanded aquifer exemption is 
of sufficient size to account for any possible revisions to the 
computational model during reevaluation of the area of review, pursuant 
to Sec.  146.84(e); and
    (iv) Any information submitted to support a waiver request made by 
the owner or operator under Sec.  146.95, if appropriate.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77287, Dec. 10, 2010]



Sec.  144.8  Noncompliance and program reporting by the Director.

    The Director shall prepare quarterly and annual reports as detailed 
below. When the State is the permit-issuing authority, the State 
Director shall submit any reports required under this section to the 
Regional Administrator. When EPA is the permit-issuing authority, the 
Regional Administrator shall submit any report required under this 
section to EPA Headquarters.
    (a) Quarterly reports. The Director shall submit quarterly narrative 
reports for major facilities as follows:
    (1) Format. The report shall use the following format:
    (i) Provide an alphabetized list of permittees. When two or more 
permittees have the same name, the lowest permit number shall be entered 
first.
    (ii) For each entry on the list, include the following information 
in the following order:
    (A) Name, location, and permit number of the noncomplying 
permittees.
    (B) A brief description and date of each instance of noncompliance 
for that permittee. Instances of noncompliance may include one or more 
the kinds set forth in paragraph (a)(2) of this section. When a 
permittee has noncompliance of more than one kind, combine the 
information into a single entry for each such permittee.

[[Page 811]]

    (C) The date(s) and a brief description of the action(s) taken by 
the Director to ensure compliance.
    (D) Status of the instance(s) of noncompliance with the date of the 
review of the status or the date of resolution.
    (E) Any details which tend to explain or mitigate the instance(s) of 
noncompliance.
    (2) Instances of noncompliance to be reported. Any instances of 
noncompliance within the following categories shall be reported in 
successive reports until the noncompliance is reported as resolved. Once 
noncompliance is reported as resolved it need not appear in subsequent 
reports.
    (i) Failure to complete construction elements. When the permittee 
has failed to complete, by the date specified in the permit, an element 
of a compliance schedule involving either planning for construction or a 
construction step (for example, begin construction, attain operation 
level); and the permittee has not returned to compliance by 
accomplishing the required elements of the schedule within 30 days from 
the date a compliance schedule report is due under the permit.
    (ii) Modifications to schedules of compliance. When a schedule of 
compliance in the permit has been modified under Sec. Sec.  144.39 or 
144.41 because of the permittee's noncompliance.
    (iii) Failure to complete or provide compliance schedule or 
monitoring reports. When the permittee has failed to complete or provide 
a report required in a permit compliance schedule (for example, progress 
report or notice of noncompliance or compliance) or a monitoring report; 
and the permittee has not submitted the complete report within 30 days 
from the date it is due under the permit for compliance schedules, or 
from the date specified in the permit for monitoring reports.
    (iv) Deficient reports. When the required reports provided by the 
permittee are so deficient as to cause misunderstanding by the Director 
and thus impede the review of the status of compliance.
    (v) Noncompliance with other permit requirements. Noncompliance 
shall be reported in the following circumstances:
    (A) Whenever the permittee has violated a permit requirement (other 
than reported under paragraph (a)(2) (i) or (ii) of this section), and 
has not returned to compliance within 45 days from the date reporting of 
noncompliance was due under the permit; or
    (B) When the Director determines that a pattern of noncompliance 
exists for a major facility permittee over the most recent four 
consecutive reporting periods. This pattern includes any violation of 
the same requirement in two consecutive reporting periods, and any 
violation of one or more requirements in each of four consecutive 
reporting periods; or
    (C) When the Director determines significant permit noncompliance or 
other significant event has occurred, such as a migration of fluids into 
a USDW.
    (vi) All other. Statistical information shall be reported quarterly 
on all other instances of noncompliance by major facilities with permit 
requirements not otherwise reported under paragraph (a) of this section.
    (b) Annual reports--(1) Annual noncompliance report. Statistical 
reports shall be submitted by the Director on nonmajor UIC permittees 
indicating the total number reviewed, the number of noncomplying 
nonmajor permittees, the number of enforcement actions, and number of 
permit modifications extending compliance deadlines. The statistical 
information shall be organized to follow the types of noncompliance 
listed in paragraph (a) of this section.
    (2) For State-administered UIC Programs only. In addition to the 
annual noncompliance report, the State Director shall:
    (i) Submit each year a program report to the Administrator (in a 
manner and form prescribed by the Administrator) consisting of:
    (A) A detailed description of the State's implementation of its 
program;
    (B) Suggested changes, if any to the program description (see Sec.  
145.23(f)) which are necessary to reflect more accurately the State's 
progress in issuing permits;
    (C) An updated inventory of active underground injection operations 
in the State.
    (ii) In addition to complying with the requirements of paragraph 
(b)(2)(i) of

[[Page 812]]

this section, the Director shall provide the Administrator, on February 
28th and August 31st of each of the first two years of program 
operation, the information required in 40 CFR 146.15, 146.25, and 
146.35.
    (iii) All Class VI program reports shall be consistent with 
reporting requirements set forth in Sec.  146.91 of this chapter.
    (c) Schedule. (1) For all quarterly reports. On the last working day 
of May, August, November, and February, the State Director shall submit 
to the Regional Administrator information concerning noncompliance with 
permit requirements by major facilities in the State in accordance with 
the following schedule. The Regional Administrator shall prepare and 
submit information for EPA-issued permits to EPA Headquarters in 
accordance with the same schedule.

    Quarters Covered by Reports on Noncompliance by Major Facilities
                    [Date for completion of reports]
January, February, and March...............................   \1\ May 31
April, May, and June.......................................  \1\ Aug. 31
July, August, and September................................  \1\ Nov. 30
October, November, and December............................  \1\ Feb. 28
 
\1\ Reports must be made available to the public for inspection and
  copying on this date.

    (2) For all annual reports. The period for annual reports shall be 
for the calendar year ending December 31, with reports completed and 
available to the public no more than 60 days later.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77287, Dec. 10, 2010]



                 Subpart B_General Program Requirements



Sec.  144.11  Prohibition of unauthorized injection.

    Any underground injection, except into a well authorized by rule or 
except as authorized by permit issued under the UIC program, is 
prohibited. The construction of any well required to have a permit is 
prohibited until the permit has been issued.

[48 FR 14189, Apr. 1, 1983, as amended at 58 FR 63895, Dec. 3, 1993]



Sec.  144.12  Prohibition of movement of fluid into underground sources 
of drinking water.

    (a) No owner or operator shall construct, operate, maintain, 
convert, plug, abandon, or conduct any other injection activity in a 
manner that allows the movement of fluid containing any contaminant into 
underground sources of drinking water, if the presence of that 
contaminant may cause a violation of any primary drinking water 
regulation under 40 CFR part 142 or may otherwise adversely affect the 
health of persons. The applicant for a permit shall have the burden of 
showing that the requirements of this paragraph are met.
    (b) For Class I, II, III, and VI wells, if any water quality 
monitoring of an underground source of drinking water indicates the 
movement of any contaminant into the underground source of drinking 
water, except as authorized under part 146, the Director shall prescribe 
such additional requirements for construction, corrective action, 
operation, monitoring, or reporting (including closure of the injection 
well) as are necessary to prevent such movement. In the case of wells 
authorized by permit, these additional requirements shall be imposed by 
modifying the permit in accordance with Sec.  144.39, or the permit may 
be terminated under Sec.  144.40 if cause exists, or appropriate 
enforcement action may be taken if the permit has been violated. In the 
case of wells authorized by rule, see Sec. Sec.  144.21 through 144.24. 
For EPA administered programs, such enforcement action shall be taken in 
accordance with appropriate sections of the SDWA.
    (c) For Class V wells, if at any time the Director learns that a 
Class V well may cause a violation of primary drinking water regulations 
under 40 CFR part 142, he or she shall:
    (1) Require the injector to obtain an individual permit;
    (2) Order the injector to take such actions (including, where 
required, closure of the injection well) as may be necessary to prevent 
the violation. For EPA administered programs, such orders shall be 
issued in accordance with the appropriate provisions of the SDWA; or
    (3) Take enforcement action.

[[Page 813]]

    (d) Whenever the Director learns that a Class V well may be 
otherwise adversely affecting the health of persons, he or she may 
prescribe such actions as may be necessary to prevent the adverse 
effect, including any action authorized under paragraph (c) of this 
section.
    (e) Notwithstanding any other provision of this section, the 
Director may take emergency action upon receipt of information that a 
contaminant which is present in or likely to enter a public water system 
or underground source of drinking water may present an imminent and 
substantial endangerment to the health of persons. If the Director is an 
EPA official, he must first determine that the appropriate State and 
local authorities have not taken appropriate action to protect the 
health of such persons, before taking emergency action.

[48 FR 14189, Apr. 1, 1983, as amended at 52 FR 20676, June 2, 1987; 75 
FR 77288, Dec. 10, 2010]



Sec.  144.13  Prohibition of Class IV wells.

    (a) The following are prohibited, except as provided in paragraph 
(c) of this section:
    (1) The construction of any Class IV well.
    (2) The operation or maintenance of any Class IV well not in 
operation prior to July 18, 1980.
    (3) The operation or maintenance of any Class IV well that was in 
operation prior to July 18, 1980, after six months following the 
effective date of a UIC program approved or promulgated for the state.
    (4) Any increase in the amount of hazardous waste or change in the 
type of hazardous waste injected into a Class IV well.
    (b) The owner or operator of a Class IV well shall comply with the 
requirements of Sec.  144.14, and with the requirements of Sec.  144.23 
regarding closure of Class IV wells.
    (c) Wells used to inject contaminated ground water that has been 
treated and is being reinjected into the same formation from which it 
was drawn are not prohibited by this section if such injection is 
approved by EPA, or a State, pursuant to provisions for cleanup of 
releases under the Comprehensive Environmental Response, Compensation, 
and Liability Act of 1980 (CERCLA), 42 U.S.C. 9601-9657, or pursuant to 
requirements and provisions under the Resource Conservation and Recovery 
Act (RCRA), 42 U.S.C. 6901 through 6987.
    (d) Clarification. The following wells are not prohibited by this 
action:
    (1) Wells used to inject hazardous waste into aquifers or portions 
thereof that have been exempted pursuant to Sec.  146.4, if the exempted 
aquifer into which waste is injected underlies the lowermost formation 
containing a USDW. Such wells are Class I wells as specified in Sec.  
144.6(a)(1), and the owner or operator must comply with the requirements 
applicable to Class I wells.
    (2) Wells used to inject hazardous waste where no USDW exists within 
one quarter mile of the well bore in any underground formation, provided 
that the Director determines that such injection is into a formation 
sufficiently isolated to ensure that injected fluids do not migrate from 
the injection zone. Such wells are Class I wells as specified in Sec.  
144.6(a)(1), and the owner or operator must comply with the requirements 
applicable to Class I wells.

[49 FR 20181, May 11, 1984, as amended at 67 FR 39593, June 7, 2002]



Sec.  144.14  Requirements for wells injecting hazardous waste.

    (a) Applicability. The regulations in this section apply to all 
generators of hazardous waste, and to the owners or operators of all 
hazardous waste management facilities, using any class of well to inject 
hazardous wastes accompanied by a manifest. (See also Sec.  144.13.)
    (b) Authorization. The owner or operator of any well that is used to 
inject hazardous waste required to be accompanied by a manifest or 
delivery document shall apply for authorization to inject as specified 
in Sec.  144.31 within 6 months after the approval or promulgation of 
the State UIC program.
    (c) Requirements. In addition to complying with the applicable 
requirements of this part and 40 CFR part 146, the owner or operator of 
each facility meeting the requirements of paragraph (b) of this section, 
shall comply with the following:

[[Page 814]]

    (1) Notification. The owner or operator shall comply with the 
notification requirements of section 3010 of Public Law 94-580.
    (2) Identification number. The owner or operator shall comply with 
the requirements of 40 CFR 264.11.
    (3) Manifest system. The owner or operator shall comply with the 
applicable recordkeeping and reporting requirements for manifested 
wastes in 40 CFR 264.71.
    (4) Manifest discrepancies. The owner or operator shall comply with 
40 CFR 264.72.
    (5) Operating record. The owner or operator shall comply with 40 CFR 
264.73(a), (b)(1), and (b)(2).
    (6) Annual report. The owner or operator shall comply with 40 CFR 
264.75.
    (7) Unmanifested waste report. The owner or operator shall comply 
with 40 CFR 264.75.
    (8) Personnel training. The owner or operator shall comply with the 
applicable personnel training requirements of 40 CFR 264.16.
    (9) Certification of closure. When abandonment is completed, the 
owner or operator must submit to the Director certification by the owner 
or operator and certification by an independent registered professional 
engineer that the facility has been closed in accordance with the 
specifications in Sec.  144.52(a)(6).
    (d) Additional requirements for Class IV wells. [Reserved]



Sec.  144.15  Prohibition of non-experimental Class V wells 
for geologic sequestration.

    The construction, operation or maintenance of any non-experimental 
Class V geologic sequestration well is prohibited.

[75 FR 77288, Dec. 10, 2010]



Sec.  144.16  Waiver of requirement by Director.

    (a) When injection does not occur into, through or above an 
underground source of drinking water, the Director may authorize a well 
or project with less stringent requirements for area of review, 
construction, mechanical integrity, operation, monitoring, and reporting 
than required in 40 CFR part 146 or Sec.  144.52 to the extent that the 
reduction in requirements will not result in an increased risk of 
movement of fluids into an underground source of drinking water.
    (b) When injection occurs through or above an underground source of 
drinking water, but the radius of endangering influence when computed 
under Sec.  146.06(a) is smaller or equal to the radius of the well, the 
Director may authorize a well or project with less stringent 
requirements for operation, monitoring, and reporting than required in 
40 CFR part 146 or Sec.  144.52 to the extent that the reduction in 
requirements will not result in an increased risk of movement of fluids 
into an underground source of drinking water.
    (c) When reducing requirements under paragraph (a) or (b) of this 
section, the Director shall prepare a fact sheet under Sec.  124.8 
explaining the reasons for the action.



Sec.  144.17  Records.

    The Director or the Administrator may require, by written notice on 
a selective well-by-well basis, an owner or operator of an injection 
well to establish and maintain records, make reports, conduct 
monitoring, and provide other information as is deemed necessary to 
determine whether the owner or operator has acted or is acting in 
compliance with Part C of the SDWA or its implementing regulations.

[58 FR 63895, Dec. 3, 1993]



Sec.  144.18  Requirements for Class VI wells.

    Owners or operators of Class VI wells must obtain a permit. Class VI 
wells cannot be authorized by rule to inject carbon dioxide.

[75 FR 77288, Dec. 10, 2010]



Sec.  144.19  Transitioning from Class II to Class VI.

    (a) Owners or operators that are injecting carbon dioxide for the 
primary purpose of long-term storage into an oil and gas reservoir must 
apply for and obtain a Class VI geologic sequestration permit when there 
is an increased risk to USDWs compared to Class II operations. In 
determining if there is an increased risk to USDWs,

[[Page 815]]

the owner or operator must consider the factors specified in Sec.  
144.19(b).
    (b) The Director shall determine when there is an increased risk to 
USDWs compared to Class II operations and a Class VI permit is required. 
In order to make this determination the Director must consider the 
following:
    (1) Increase in reservoir pressure within the injection zone(s);
    (2) Increase in carbon dioxide injection rates;
    (3) Decrease in reservoir production rates;
    (4) Distance between the injection zone(s) and USDWs;
    (5) Suitability of the Class II area of review delineation;
    (6) Quality of abandoned well plugs within the area of review;
    (7) The owner's or operator's plan for recovery of carbon dioxide at 
the cessation of injection;
    (8) The source and properties of injected carbon dioxide; and
    (9) Any additional site-specific factors as determined by the 
Director.

[75 FR 77288, Dec. 10, 2010]



        Subpart C_Authorization of Underground Injection by Rule



Sec.  144.21  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells.

    (a) An existing Class I, II (except enhanced recovery and 
hydrocarbon storage) and III injection well is authorized by rule if the 
owner or operator injects into the existing well within one year after 
the date at which a UIC program authorized under the SDWA becomes 
effective for the first time or inventories the well pursuant to the 
requirements of Sec.  144.26. An owner or operator of a well which is 
authorized by rule pursuant to this section shall rework, operate, 
maintain, convert, plug, abandon or inject into the well in compliance 
with applicable regulations.
    (b) Duration of well authorization by rule. Well authorization under 
this section expires upon the effective date of a permit issued pursuant 
to Sec. Sec.  144.25, 144.31, 144.33 or 144.34; after plugging and 
abandonment in accordance with an approved plugging and abandonment plan 
pursuant to Sec. Sec.  144.28(c) and 146.10, and upon submission of a 
plugging and abandonment report pursuant to Sec.  144.28(k); or upon 
conversion in compliance with Sec.  144.28(j).
    (c) Prohibitions on injection. An owner or operator of a well 
authorized by rule pursuant to this section is prohibited from injecting 
into the well:
    (1) Upon the effective date of an applicable permit denial;
    (2) Upon failure to submit a permit application in a timely manner 
pursuant to Sec. Sec.  144.25 or 144.31;
    (3) Upon failure to submit inventory information in a timely manner 
pursuant to Sec.  144.26;
    (4) Upon failure to comply with a request for information in a 
timely manner pursuant to Sec.  144.27;
    (5) Upon failure to provide alternative financial assurance pursuant 
to Sec.  144.28(d)(7);
    (6) Forty-eight hours after receipt of a determination by the 
Director pursuant to Sec.  144.28(f)(3) that the well lacks mechanical 
integrity, unless the Director requires immediate cessation;
    (7) Upon receipt of notification from the Director pursuant to Sec.  
144.28(l) that the transferee has not demonstrated financial 
responsibility pursuant to Sec.  144.28(d);
    (8) For Class I and III wells:
    (i) In States with approved programs, five years after the effective 
date of the UIC program unless a timely and complete permit application 
is pending the Director's decision; or
    (ii) In States with programs administered by EPA, one year after the 
effective date of the UIC program unless a timely and complete permit 
application is pending the Director's decision; or
    (9) For Class II wells (except enhanced recovery and hydrocarbon 
storage), five years after the effective date of the UIC program unless 
a timely and complete permit application is pending the Director's 
decision.
    (d) Class II and III wells in existing fields or projects. 
Notwithstanding the prohibition in Sec.  144.11, this section authorizes 
Class II and Class III wells or projects in existing fields or projects 
to continue normal operations until permitted, including construction, 
operation, and plugging and abandonment of wells as part of the 
operation, provided the owner or operator maintains

[[Page 816]]

compliance with all applicable requirements.
    (e) Requirements. The owner or operator of a well authorized under 
this section shall comply with the applicable requirements of Sec.  
144.28 and part 147 of this chapter no later than one year after 
authorization.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20181, May 11, 1984; 58 
FR 63895, Dec. 3, 1993]



Sec.  144.22  Existing Class II enhanced recovery and hydrocarbon 
storage wells.

    (a) An existing Class II enhanced recovery or hydrocarbon storage 
injection well is authorized by rule for the life of the well or 
project, if the owner or operator injects into the existing well within 
one year after the date which a UIC program authorized under the SDWA 
becomes effective for the first time or inventories the well pursuant to 
the requirements of Sec.  144.26. An owner or operator of a well which 
is authorized by rule pursuant to this section shall rework, operate, 
maintain, convert, plug, abandon or inject into the well in compliance 
with applicable regulations.
    (b) Duration of well authorization by rule. Well authorization under 
this section expires upon the effective date of a permit issued pursuant 
to Sec.  144.19, Sec.  144.25, Sec.  144.31, Sec.  144.33 or Sec.  
144.34; after plugging and abandonment in accordance with an approved 
plugging and abandonment plan pursuant to Sec. Sec.  144.28(c) and 
146.10 of this chapter; and upon submission of a plugging and 
abandonment report pursuant to Sec.  144.28(k); or upon conversion in 
compliance with Sec.  144.28(j).
    (c) Prohibitions on injection. An owner or operator of a well 
authorized by rule pursuant to this section is prohibited from injecting 
into the well:
    (1) Upon the effective date of an applicable permit denial;
    (2) Upon failure to submit a permit application in a timely manner 
pursuant to Sec.  144.25 or Sec.  144.31;
    (3) Upon failure to submit inventory information in a timely manner 
pursuant to Sec.  144.26;
    (4) Upon failure to comply with a request for information in a 
timely manner pursuant to Sec.  144.27;
    (5) Upon failure to provide alternative financial assurance pursuant 
to Sec.  144.28(d)(7);
    (6) Forty-eight hours after receipt of a determination by the 
Director pursuant to Sec.  144.28(f)(3) that the well lacks mechanical 
integrity, unless the Director requires immediate cessation; or
    (7) Upon receipt of notification from the Director pursuant to Sec.  
144.28(l) that the transferee has not demonstrated financial 
responsibility pursuant to Sec.  144.28(d).
    (d) Requirements. The owner or operator of a well authorized under 
this section shall comply with the applicable requirements of Sec.  
144.28 and part 147 of this chapter. Such owner or operator shall comply 
with the casing and cementing requirements no later than 3 years and 
other requirements no later than 1 year after authorization.

[49 FR 20181, May 11, 1984, as amended at 58 FR 63896, Dec. 3, 1993; 75 
FR 77288, Dec. 10, 2010]



Sec.  144.23  Class IV wells.

    (a) Injection into existing Class IV wells is authorized for up to 
six months after approval or promulgation of the UIC Program. Such wells 
are subject to the requirements of Sec. Sec.  144.13 and 144.14(c).
    (b) Closure. For EPA administered programs only,
    (1) Prior to abandoning any Class IV well, the owner or operator 
shall plug or otherwise close the well in a manner acceptable to the 
Regional Administrator.
    (2) [Reserved]
    (3) The owner or operator of a Class IV well must notify the 
Regional Administrator of intent to abandon the well at least thirty 
days prior to abandonment.
    (c) Notwithstanding the requirements of paragraphs (a) and (b) of 
this section, injection wells used to inject contaminated ground water 
that has been treated and is being injected into the same formation from 
which it was drawn are authorized by rule for the life of the well if 
such subsurface emplacement of fluids is approved by EPA, or a State, 
pursuant to provisions for cleanup of releases under the Comprehensive 
Environmental Response, Compensation, and Liability Act of

[[Page 817]]

1980 (CERCLA), 42 U.S.C. 9601-9675, or pursuant to requirements and 
provisions under the Resource Conservation and Recovery Act (RCRA), 42 
U.S.C. 6901-6992k.

[49 FR 20181, May 11, 1984, as amended at 60 FR 33932, June 29, 1995; 64 
FR 68566, Dec. 7, 1999]



Sec.  144.24  Class V wells.

    (a) A Class V injection well is authorized by rule, subject to the 
conditions in Sec.  144.84
    (b) Duration of well authorization by rule. Well authorization under 
this section expires upon the effective date of a permit issued pursuant 
to Sec. Sec.  144.25, 144.31, 144.33 or 144.34, or upon proper closure 
of the well.
    (c) Prohibition of injection. An owner or operator of a well which 
is authorized by rule pursuant to this section is prohibited from 
injecting into the well:
    (1) Upon the effective date of an applicable permit denial;
    (2) Upon failure to submit a permit application in a timely manner 
pursuant to Sec. Sec.  144.25 or 144.31;
    (3) Upon failure to submit inventory information in a timely manner 
pursuant to Sec.  144.26; or
    (4) Upon failure to comply with a request for information in a 
timely manner pursuant to Sec.  144.27.

[58 FR 63896, Dec. 3, 1993, as amended at 64 FR 68566, Dec. 7, 1999]



Sec.  144.25  Requiring a permit.

    (a) The Director may require the owner or operator of any Class I, 
II, III or V injection well which is authorized by rule under this 
subpart to apply for and obtain an individual or area UIC permit. Cases 
where individual or area UIC permits may be required include:
    (1) The injection well is not in compliance with any requirement of 
the rule;
    Note: Any underground injection which violates any authorization by 
rule is subject to appropriate enforcement action.
    (2) The injection well is not or no longer is within the category of 
wells and types of well operations authorized in the rule;
    (3) The protection of USDWs requires that the injection operation be 
regulated by requirements, such as for corrective action, monitoring and 
reporting, or operation, which are not contained in the rule.
    (4) When the injection well is a Class I, II (except existing 
enhanced recovery and hydrocarbon storage) or III well, in accordance 
with a schedule established by the Director pursuant to Sec.  144.31(c).
    (b) For EPA-administered programs, the Regional Administrator may 
require an owner or operator of any well which is authorized by rule 
under this subpart to apply for an individual or area UIC permit under 
this paragraph only if the owner or operator has been notified in 
writing that a permit application is required. The owner or operator of 
a well which is authorized by rule under this subpart is prohibited from 
injecting into the well upon the effective date of permit denial, or 
upon failure by the owner or operator to submit an application in a 
timely manner as specified in the notice. The notice shall include: a 
brief statement of the reasons for requiring a permit; an application 
form; a statement setting a time for the owner or operator to file the 
application; and a statement of the consequences of denial or issuance 
of the permit, or failure to submit an application, as described in this 
paragraph.
    (c) An owner or operator of a well authorized by rule may request to 
be excluded from the coverage of this subpart by applying for an 
individual or area UIC permit. The owner or operator shall submit an 
application under Sec.  144.31 with reasons supporting the request, to 
the Director. The Director may grant any such requests.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20182, May 11, 1984; 58 
FR 63896, Dec. 3, 1993]



Sec.  144.26  Inventory requirements.

    The owner or operator of an injection well which is authorized by 
rule under this subpart shall submit inventory information to the 
Director. Such an owner or operator is prohibited from injecting into 
the well upon failure to submit inventory information for the well 
within the time frame specified in paragraph (d) of this section.
    (a) Contents. As part of the inventory, the Director shall require 
and the owner/operator shall provide at least the following information:

[[Page 818]]

    (1) Facility name and location;
    (2) Name and address of legal contact;
    (3) Ownership of facility;
    (4) Nature and type of injection wells; and
    (5) Operating status of injection wells.
    Note: This information is requested on national form ``Inventory of 
Injection Wells,'' OMB No. 158-R0170.

    (b) Additional contents. For EPA administered programs only, the 
owner or operator of a well listed in paragraph (b)(1) of this section 
shall provide the information listed in paragraph (b)(2) of this 
section.
    (1) This section applies to the following wells:
    (i) Class II enhanced recovery wells;
    (ii) Class IV wells;
    (iii) The following Class V wells:
    (A) Sand or other backfill wells [Sec.  146.5(e)(8)];
    (B) Radioactive waste disposal wells that are not Class I wells (40 
CFR 146.5 (e)(11))
    (C) Geothermal energy recovery wells [Sec.  146.5(e)(12)];
    (D) Brine return flow wells [Sec.  146.5(e)(14)];
    (E) Wells used in experimental technologies [Sec.  146.5(e)(15)];
    (F) Municipal and industrial disposal wells other than Class I; and
    (G) Any other Class V wells at the discretion of the Regional 
Administrator.
    (2) The owner or operator of a well listed in paragraph (b)(1) shall 
provide a listing of all wells owned or operated setting forth the 
following information for each well. (A single description of wells at a 
single facility with substantially the same characteristics is 
acceptable).
    (i) For Class II only, the field name(s);
    (ii) Location of each well or project given by Township, Range, 
Section, and Quarter-Section, or by latitude and longitude to the 
nearest second, according to the conventional practice in the State;
    (iii) Date of completion of each well;
    (iv) Identification and depth of the formation(s) into which each 
well is injecting;
    (v) Total depth of each well;
    (vi) Casing and cementing record, tubing size, and depth of packer;
    (vii) Nature of the injected fluids;
    (viii) Average and maximum injection pressure at the wellhead;
    (ix) Average and maximum injection rate; and
    (x) Date of the last mechanical integrity test, if any.
    (c) Notice. Upon approval of the UIC Program in a State, the 
Director shall notify owners or operators of injection wells of their 
duty to submit inventory information. The method of notification 
selected by the Director must assure that the owners or operators will 
be made aware of the inventory requirement.
    (d) Deadlines. (1) The owner or operator of an injection well shall 
submit inventory information no later than one year after the date of 
approval or effective date of the UIC program for the State. The 
Director need not require inventory information from any facility with 
interim status under RCRA.
    (2) For EPA administered programs the information need not be 
submitted if a complete permit application is submitted within one year 
of the effective data of the UIC program. The owner or operator of Class 
IV well shall submit inventory information no later than 60 days after 
the effective date of the program.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20182, May 11, 1984; 58 
FR 63896, Dec. 3, 1993; 64 FR 68566, Dec. 7, 1999; 67 FR 39593, June 7, 
2002]



Sec.  144.27  Requiring other information.

    (a) For EPA administered programs only, in addition to the inventory 
requirements of Sec.  144.26, the Regional Administrator may require the 
owner or operator of any well authorized by rule under this subpart to 
submit information as deemed necessary by the Regional Administrator to 
determine whether a well may be endangering an underground source of 
drinking water in violation of Sec.  144.12 of this part.
    (b) Such information requirements may include, but are not limited 
to:
    (1) Performance of ground-water monitoring and the periodic 
submission of reports of such monitoring;

[[Page 819]]

    (2) An analysis of injected fluids, including periodic submission of 
such analyses; and
    (3) A description of the geologic strata through and into which 
injection is taking place.
    (c) Any request for information under this section shall be made in 
writing, and include a brief statement of the reasons for requiring the 
information. An owner or operator shall submit the information within 
the time period(s) provided in the notice.
    (d) An owner or operator of an injection well authorized by rule 
under this subpart is prohibited from injecting into the well upon 
failure of the owner or operator to comply with a request for 
information within the time period(s) specified by the Director pursuant 
to paragraph (c) of this section. An owner or operator of a well 
prohibited from injection under this section shall not resume injection 
except under a permit issued pursuant to Sec. Sec.  144.25, 144.31, 
144.33 or 144.34.

[49 FR 20182, May 11, 1984, as amended at 58 FR 63896, Dec. 3, 1993]



Sec.  144.28  Requirements for Class I, II, and III wells authorized by rule.

    The following requirements apply to the owner or operator of a Class 
I, II or III well authorized by rule under this subpart, as provided by 
Sec. Sec.  144.21(e) and 144.22(d).
    (a) The owner or operator shall comply with all applicable 
requirements of this subpart and subpart B of this part. Any 
noncompliance with these requirements constitutes a violation of the 
Safe Drinking Water Act and is grounds for enforcement action, except 
that the owner or operator need not comply with these requirements to 
the extent and for the duration such noncompliance is authorized by an 
emergency permit under Sec.  144.34.
    (b) Twenty-four hour reporting. The owner or operator shall report 
any noncompliance which may endanger health or the environment, 
including:
    (1) Any monitoring or other information which indicates that any 
contaminant may cause an endangerment to a USDW; or
    (2) Any noncompliance or malfunction of the injection system which 
may cause fluid migration into or between USDWs.

Any information shall be provided orally within 24 hours from the time 
the owner or operator becomes aware of the circumstances. A written 
submission shall also be provided within five days of the time the owner 
or operator becomes aware of the circumstances. The written submission 
shall contain a description of the noncompliance and its cause, the 
period of noncompliance, including exact dates and times, and if the 
noncompliance has not been corrected, the anticipated time it is 
expected to continue; and steps taken or planned to reduce, eliminate, 
and prevent recurrence of the noncompliance.
    (c) Plugging and abandonment plan. (1) The owner or operator shall 
prepare, maintain, and comply with a plan for plugging and abandonment 
of the well or project that meets the requirements of Sec.  146.10 of 
this chapter and is acceptable to the Director. For purposes of this 
paragraph, temporary intermittent cessation of injection operations is 
not abandonment.
    (2) For EPA administered programs:
    (i) The owner or operator shall submit the plan, on a form provided 
by the Regional Administrator, no later than one year after the 
effective date of the UIC program in the state.
    (ii) The owner or operator shall submit any proposed significant 
revision to the method of plugging reflected in the plan no later than 
the notice of plugging required by Sec.  144.28(j)(2) (i.e., 45 days 
prior to plugging unless shorter notice is approved).
    (iii) The plan shall include the following information:
    (A) The nature and quantity and material to be used in plugging;
    (B) The location and extent (by depth) of the plugs;
    (C) Any proposed test or measurement to be made;
    (D) The amount, size, and location (by depth) of casing to be left 
in the well;
    (E) The method and location where casing is to be parted; and
    (F) [Reserved]
    (G) The estimated cost of plugging the well.
    (iv) After a cessation of operations of two years the owner or 
operator shall

[[Page 820]]

plug and abandon the well in accordance with the plan unless he:
    (A) Provides notice to the Regional Administrator;
    (B) Describe actions or procedures, satisfactory to the Regional 
Administrator, that the owner or operator will take to ensure that the 
well will not endanger USDWs during the period of temporary abandonment. 
These actions and procedures shall include compliance with the technical 
requirements applicable to active injection wells unless waived by the 
Regional Administrator.
    (v) The owner or operator of any well that has been temporarily 
abandoned [ceased operations for more than two years and has met the 
requirements of paragraphs (c)(2) (A) and (B) of this section] shall 
notify the Regional Administrator prior to resuming operation of the 
well.
    (d) Financial responsibility. (1) The owner, operator and/or, for 
EPA-administered programs, the transferor of a Class I, II or III well, 
is required to demonstrate and maintain financial responsibility and 
resources to close, plug and abandon the underground injection operation 
in a manner prescribed by the Director until:
    (i) The well has been plugged and abandoned in accordance with an 
approved plugging and abandonment plan pursuant to Sec. Sec.  144.28(c) 
and 146.10 and submission of a plugging and abandonment report has been 
made pursuant to Sec.  144.28(k);
    (ii) The well has been converted in compliance with the requirements 
of Sec.  144.28(j); or
    (iii) For EPA-administered programs, the transferor has received 
notice from the Director that the transferee has demonstrated financial 
responsibility for the well. The owner or operator shall show evidence 
of such financial responsibility to the Director by the submission of a 
surety bond, or other adequate assurance, such as a financial statement.
    (2) For EPA-administered programs, the owner or operator shall 
submit such evidence no later than one year after the effective date of 
the UIC program in the State. Where the ownership or operational control 
of the well is transferred more than one year after the effective date 
of the UIC program, the transferee shall submit such evidence no later 
than the date specified in the notice required pursuant to Sec.  
144.28(l)(2).
    (3) For EPA administered programs the Regional Administrator may 
require the owner or operator to submit a revised demonstration of 
financial responsibility if the Regional Administrator has reason to 
believe that the original demonstration is no longer adequate to cover 
the cost of closing, plugging and abandoning the well.
    (4) For EPA administered programs the owner or operator of a well 
injecting hazardous waste must comply with the financial responsibility 
requirements of subpart F of this part.
    (5) For EPA-administered programs, an owner or operator must notify 
the Regional Administrator by certified mail of the commencement of any 
voluntary or involuntary proceeding under Title 11 (Bankruptcy) of the 
United States Code which names the owner or operator as debtor, within 
10 business days after the commencement of the proceeding. Any party 
acting as guarantor for the owner or operator for the purpose of 
financial responsibility must so notify the Regional Administrator, if 
the guarantor is named as debtor in any such proceeding.
    (6) In the event of commencement of a proceeding specified in 
paragraph (d)(5) of this section, an owner or operator who has furnished 
a financial statement for the purpose of demonstrating financial 
responsibility under this section shall be deemed to be in violation of 
this paragraph until an alternative financial assurance demonstration 
acceptable to the Regional Administrator is provided either by the owner 
or operator or by its trustee in bankruptcy, receiver, or other 
authorized party. All parties shall be prohibited from injecting into 
the well until such alternate financial assurance is provided.
    (e) Casing and cementing requirements. For enhanced recovery and 
hydrocarbon storage wells:
    (1) The owner or operator shall case and cement the well to prevent 
movement of fluids into or between underground sources of drinking 
water. In determining and specifying casing and

[[Page 821]]

cementing requirements, the following factors shall be considered:
    (i) Depth to the injection zone;
    (ii) Depth to the bottom of all USDWs; and
    (iii) Estimated maximum and average injection pressures.
    (2) In addition, in determining and specifying casing and cementing 
requirements the Director may consider information on:
    (i) Nature of formation fluids;
    (ii) Lithology of injection and confining zones;
    (iii) External pressure, internal pressure, and axial loading;
    (iv) Hole size;
    (v) Size and grade of all casing strings; and
    (vi) Class of cement.
    (3) The requirements in paragraphs (e) (1) and (2) of this section 
need not apply if:
    (i) Regulatory controls for casing and cementing existed at the time 
of drilling of the well and the well is in compliance with those 
controls; and
    (ii) Well injection will not result in the movement of fluids into 
an underground source of drinking water so as to create a significant 
risk to the health of persons.
    (4) When a State did not have regulatory controls for casing and 
cementing prior to the time of the submission of the State program to 
the Administrator, the Director need not apply the casing and cementing 
requirements in paragraph (e)(1) of this section if he submits as a part 
of his application for primacy, an appropriate plan for casing and 
cementing of existing, newly converted, and newly drilled wells in 
existing fields, and the Administrator approves the plan.
    (f) Operating requirements. (1) Injection between the outermost 
casing protecting underground sources of drinking water and the well 
bore is prohibited.
    (2) The owner or operator of a Class I, II or III injection well 
authorized by rule shall establish and maintain mechanical integrity as 
defined in Sec.  146.8 of this chapter until the well is properly 
plugged in accordance with an approved plugging and abandonment plan 
pursuant to Sec. Sec.  144.28(c) and 146.10, and a plugging and 
abandonment report pursuant to Sec.  144.28(k) is submitted, or until 
the well is converted in compliance with Sec.  144.28(j). For EPA-
administered programs, the Regional Administrator may require by written 
notice that the owner or operator comply with a schedule describing when 
mechanical integrity demonstrations shall be made.
    (3) When the Director determines that a Class I (non-hazardous), II 
or III injection well lacks mechanical integrity pursuant to Sec.  146.8 
of this chapter, the Director shall give written notice of his 
determination to the owner or operator. Unless the Director requires 
immediate cessation, the owner or operator shall cease injection into 
the well within 48 hours of receipt of the Director's determination. The 
Director may allow plugging of the well in accordance with the 
requirements of Sec.  146.10 of this chapter, or require the owner or 
operator to perform such additional construction, operation, monitoring, 
reporting and corrective action as is necessary to prevent the movement 
of fluid into or between USDWs caused by the lack of mechanical 
integrity. The owner or operator may resume injection upon receipt of 
written notification from the Director that the owner or operator has 
demonstrated mechanical integrity pursuant to Sec.  146.8 of this 
chapter.
    (4) The Director may allow the owner or operator of a well which 
lacks mechanical integrity pursuant to Sec.  146.8(a)(1) of this chapter 
to continue or resume injection if the owner or operator has made a 
satisfactory demonstration that there is no movement of fluid into or 
between USDWs.
    (5) For Class I wells, unless an alternative to a packer has been 
approved under Sec.  146.12(c) of this chapter, the owner or operator 
shall fill the annulus between the tubing and the long string of casings 
with a fluid approved by the Director and maintain a pressure, also 
approved by the Director, on the annulus. For EPA administered programs, 
the owner or operator of a Class I well completed with tubing and packer 
shall fill the annulus between tubing and casing with a noncorrosive 
fluid and maintain a positive pressure on the annulus. For other Class I 
wells, the owner or operator shall insure that the

[[Page 822]]

alternative completion method will reliably provide a comparable level 
of protection to underground sources of drinking water.
    (6) Injection pressure.
    (i) For Class I and III wells:
    (A) Except during stimulation, the owner or operator shall not 
exceed an injection pressure at the wellhead which shall be calculated 
so as to assure that the pressure during injection does not initiate new 
fractures or propagate existing fractures in the injection zone; and
    (B) The owner or operator shall not inject at a pressure which will 
initiate fractures in the confining zone or cause the movement of 
injection or formation fluids into an underground source of drinking 
water.
    (ii) For Class II wells:
    (A) The owner or operator shall not exceed a maximum injection 
pressure at the wellhead which shall be calculated so as to assure that 
the pressure during injection does not initiate new fractures of 
propagate existing fractures in the confining zone adjacent to the 
USDWs; and
    (B) The owner or operator shall not inject at a pressure which will 
cause the movement of injection or formation fluids into an underground 
source of drinking water.
    (g) Monitoring requirements. The owner or operator shall perform the 
monitoring as described in this paragraph. For EPA administered 
programs, monitoring of the nature of the injected fluids shall comply 
with applicable analytical methods cited and described in table I of 40 
CFR 136.3 or in appendix III of 40 CFR part 261 or by other methods that 
have been approved by the Regional Administrator.
    (1) The owner or operator of a Class I well shall:
    (i) Analyze the nature of the injected fluids with sufficient 
frequency to yield data representative of their characteristics;
    (ii) Install and use continuous recording devices to monitor 
injection pressure, flow rate and volume, and the pressure on the 
annulus between the tubing and the long string of casing;
    (iii) Install and use monitoring wells within the area of review if 
required by the Director, to monitor any migration of fluids into and 
pressure in the underground sources of drinking water. The type, number 
and location of the wells, the parameters to be measured, and the 
frequency of monitoring must be approved by the Director.
    (2) For Class II wells:
    (i) The owner or operator shall monitor the nature of the injected 
fluids with sufficient frequency to yield data representative of their 
characteristics. For EPA administered programs, this frequency shall be 
at least once within the first year of the authorization and thereafter 
when changes are made to the fluid.
    (ii) The owner or operator shall observe the injection pressure, 
flow rate, and cumulative volume at least with the following 
frequencies:
    (A) Weekly for produced fluid disposal operations;
    (B) Monthly for enhanced recovery operations;
    (C) Daily during the injection of liquid hydrocarbons and injection 
for withdrawal of stored hydrocarbons; and
    (D) Daily during the injection phase of cyclic steam operations.
    (iii) The owner or operator shall record one observation of 
injection pressure, flow rate and cumulative volume at reasonable 
intervals no greater than thirty days.
    (iv) For enhanced recovery and hydrocarbon storage wells:
    (A) The owner or operator shall demonstrate mechanical integrity 
pursuant to Sec.  146.8 of this chapter at least once every five years 
during the life of the injection well.
    (B) For EPA administered programs, the Regional Administrator by 
written notice may require the owner or operator to comply with a 
schedule describing when such demonstrations shall be made.
    (C) For EPA administered programs, the owner or operator of any well 
required to be tested for mechanical integrity shall notify the Regional 
Administrator at least 30 days prior to any required mechanical 
integrity test. The Regional Administrator may allow a shorter 
notification period if it would be sufficient to enable EPA to witness 
the mechanical integrity testing if it chose. Notification may be in the 
form of a yearly or quarterly schedule of

[[Page 823]]

planned mechanical integrity tests, or it may be on an individual basis.
    (v) The owner or operator of a hydrocarbon storage or enhanced 
recovery wells may monitor them by manifold monitoring on a field or 
project basis rather than on an individual well basis if such facilities 
consist of more than one injection well, operate with a common manifold, 
and provided the owner or operator demonstrates to the Director that 
manifold monitoring is comparable to individual well monitoring.
    (3)(i) For Class III wells the owner or operator shall provide to 
the Director a qualitative analysis and ranges in concentrations of all 
constituents of injected fluids at least once within the first year of 
authorization and thereafter whenever the injection fluid is modified to 
the extent that the initial data are incorrect or incomplete. The owner 
or operator may request Federal confidentiality as specified in 40 CFR 
part 2. If the information is proprietary the owner or operator may in 
lieu of the ranges in concentrations choose to submit maximum 
concentrations which shall not be exceeded. In such a case the owner or 
operator shall retain records of the undisclosed concentrations and 
provide them upon request to the Regional Administrator as part of any 
enforcement investigation; and
    (ii) Monitor injection pressure and either flow rate or volume semi-
monthly, or meter and record daily injected and produced fluid volumes 
as appropriate;
    (iii) Monitor the fluid level in the injection zone semi-monthly, 
where appropriate;
    (iv) All Class III wells may be monitored on a field or project 
basis rather than an individual well basis by manifold monitoring. 
Manifold monitoring may be used in cases of facilities consisting of 
more than one injection well, operating with a common manifold. Separate 
monitoring systems for each well are not required provided the owner or 
operator demonstrates to the Director that manifold monitoring is 
comparable to individual well monitoring.
    (h) Reporting requirements. The owner or operator shall submit 
reports to the Director as follows:
    (1) For Class I wells, quarterly reports on:
    (i) The physical, chemical, and other relevant characteristics of 
the injection fluids;
    (ii) Monthly average, maximum, and minimum values for injection 
pressure, flow rate and volume, and annular pressure;
    (iii) The results from ground-water monitoring wells prescribed in 
paragraph (g)(1)(iii) of this section;
    (iv) The results of any test of the injection well conducted by the 
owner or operator during the reported quarter if required by the 
Director; and
    (v) Any well work over performed during the reported quarter.
    (2) For Class II wells:
    (i) An annual report to the Director summarizing the results of all 
monitoring, as required in paragraph (g)(2) of this section. Such 
summary shall include monthly records of injected fluids, and any major 
changes in characteristics or sources of injected fluids. Previously 
submitted information may be included by reference.
    (ii) The owner or operator of hydrocarbon storage and enhanced 
recovery projects may report on a field or project basis rather than on 
an individual well basis where manifold monitoring is used.
    (3) For Class III wells:
    (i) Quarterly reporting on all monitoring, as required in paragraph 
(g)(3) of this section;
    (ii) Quarterly reporting of the results of any periodic tests 
required by the Director that are performed during the reported quarter;
    (iii) Monitoring may be reported on a project or field basis rather 
than an individual well basis where manifold monitoring is used.
    (i) Retention of records. The owner or operator shall retain records 
of all monitoring information, including the following:
    (1) Calibration and maintenance records and all original strip chart 
recordings for continuous monitoring instrumentation, and copies of all 
reports required by this section, for a period of at least three years 
from the date of the sample, measurement, or report. This period may be 
extended by request of the Director at any time; and

[[Page 824]]

    (2) The nature and composition of all injected fluids until three 
years after the completion of any plugging and abandonment procedures 
specified under Sec.  144.52(l)(6). The Director may require the owner 
or operator to deliver the records to the Director at the conclusion of 
the retention period. For EPA administered programs, the owner or 
operator shall continue to retain the records after the three year 
retention period unless he delivers the records to the Regional 
Administrator or obtains written approval from the Regional 
Administrator to discard the records.
    (j) Notice of abandonment. (1) The owner or operator shall notify 
the Director, according to a time period required by the Director, 
before conversion or abandonment of the well.
    (2) For EPA-administered programs, the owner or operator shall 
notify the Regional Administrator at least 45 days before plugging and 
abandonment. The Regional Administrator, at his discretion, may allow a 
shorter notice period.
    (k) Plugging and abandonment report. For EPA-administered programs, 
within 60 days after plugging a well or at the time of the next 
quarterly report (whichever is less) the owner or operator shall submit 
a report to the Regional Administrator. If the quarterly report is due 
less than 15 days before completion of plugging, then the report shall 
be submitted within 60 days. The report shall be certified as accurate 
by the person who performed the plugging operation. Such report shall 
consist of either:
    (1) A statement that the well was plugged in accordance with the 
plan previously submitted to the Regional Administrator; or
    (2) Where actual plugging differed from the plan previously 
submitted, an updated version of the plan, on the form supplied by the 
Regional Administrator, specifying the different procedures used.
    (l) Change of ownership or operational control. For EPA-administered 
programs:
    (1) The transferor of a Class I, II or III well authorized by rule 
shall notify the Regional Administrator of a transfer of ownership or 
operational control of the well at least 30 days in advance of the 
proposed transfer.
    (2) The notice shall include a written agreement between the 
transferor and the transferee containing a specific date for transfer of 
ownership or operational control of the well; and a specific date when 
the financial responsibility demonstration of Sec.  144.28(d) will be 
met by the transferee.
    (3) The transferee is authorized to inject unless he receives 
notification from the Director that the transferee has not demonstrated 
financial responsibility pursuant to Sec.  144.28(d).
    (m) Requirements for Class I hazardous waste wells. The owner or 
operator of any Class I well injecting hazardous waste shall comply with 
Sec.  144.14(c). In addition, for EPA-administered programs the owner or 
operator shall properly dispose of, or decontaminate by removing all 
hazardous waste residues, all injection well equipment.

[49 FR 20182, May 11, 1984, as amended at 58 FR 63897, Dec. 3, 1993]



                    Subpart D_Authorization by Permit



Sec.  144.31  Application for a permit; authorization by permit.

    (a) Permit application. Unless an underground injection well is 
authorized by rule under subpart C of this part, all injection 
activities including construction of an injection well are prohibited 
until the owner or operator is authorized by permit. An owner or 
operator of a well currently authorized by rule must apply for a permit 
under this section unless well authorization by rule was for the life of 
the well or project. Authorization by rule for a well or project for 
which a permit application has been submitted terminates for the well or 
project upon the effective date of the permit. Procedures for 
applications, issuance and administration of emergency permits are found 
exclusively in Sec.  144.34. A RCRA permit applying the standards of 
part 264, subpart C of this chapter will constitute a UIC permit for 
hazardous waste injection wells for which the technical standards in 
part 146 of this chapter are not generally appropriate.

[[Page 825]]

    (b) Who applies? When a facility or activity is owned by one person 
but is operated by another person, it is the operator's duty to obtain a 
permit.
    (c) Time to apply. Any person who performs or proposes an 
underground injection for which a permit is or will be required shall 
submit an application to the Director in accordance with the UIC program 
as follows:
    (1) For existing wells, as expeditiously as practicable and in 
accordance with the schedule in any program description under Sec.  
145.23(f) or (for EPA administered programs) on a schedule established 
by the Regional Administrator, but no later than 4 years from the 
approval or promulgation of the UIC program, or as required under Sec.  
144.14(b) for wells injecting hazardous waste. For EPA administered 
programs the owner or operator of Class I or III wells shall submit a 
complete permit application no later than 1 year after the effective 
date of the program.
    (2) For new injection wells, except new wells in projects authorized 
under Sec.  144.21(d) or authorized by an existing area permit under 
Sec.  144.33(c), a reasonable time before construction is expected to 
begin.
    (d) Completeness. The Director shall not issue a permit before 
receiving a complete application for a permit except for emergency 
permits. An application for a permit is complete when the Director 
receives an application form and any supplemental information which are 
completed to his or her satisfaction. The completeness of any 
application for a permit shall be judged independently of the status of 
any other permit application or permit for the same facility or 
activity. For EPA-administered programs, an application which is 
reviewed under Sec.  124.3 is complete when the Director receives either 
a complete application or the information listed in a notice of 
deficiency.
    (e) Information requirements. All applicants for Class I, II, III, 
and V permits shall provide the following information to the Director, 
using the application form provided by the Director. Applicants for 
Class VI permits shall follow the criteria provided in Sec.  146.82 of 
this chapter.
    (1) The activities conducted by the applicant which require it to 
obtain permits under RCRA, UIC, the National Pollution Discharge 
Elimination system (NPDES) program under the Clean Water Act, or the 
Prevention of Significant Deterioration (PSD) program under the Clean 
Air Act.
    (2) Name, mailing address, and location of the facility for which 
the application is submitted.
    (3) Up to four SIC codes which best reflect the principal products 
or services provided by the facility.
    (4) The operator's name, address, telephone number, ownership 
status, and status as Federal, State, private, public, or other entity.
    (5) Whether the facility is located on Indian lands.
    (6) A listing of all permits or construction approvals received or 
applied for under any of the following programs:
    (i) Hazardous Waste Management program under RCRA.
    (ii) UIC program under SDWA.
    (iii) NPDES program under CWA.
    (iv) Prevention of Significant Deterioration (PSD) program under the 
Clean Air Act.
    (v) Nonattainment program under the Clean Air Act.
    (vi) National Emission Standards for Hazardous Pollutants (NESHAPS) 
preconstruction approval under the Clean Air Act.
    (vii) Ocean dumping permits under the Marine Protection Research and 
Sanctuaries Act.
    (viii) Dredge and fill permits under section 404 of CWA.
    (ix) Other relevant environmental permits, including State permits.
    (7) A topographic map (or other map if a topographic map is 
unavailable) extending one mile beyond the property boundaries of the 
source depicting the facility and each of its intake and discharge 
structures; each of its hazardous waste treatment, storage, or disposal 
facilities; each well where fluids from the facility are injected 
underground; and those wells, springs, and other surface water bodies, 
and drinking water wells listed in public records or otherwise known to 
the applicant within a quarter mile of the facility property boundary.
    (8) A brief description of the nature of the business.

[[Page 826]]

    (9) For EPA-administered programs, the applicant shall identify and 
submit on a list with the permit application the names and addresses of 
all owners of record of land within one-quarter mile of the facility 
boundary. This requirement may be waived by the Regional Administrator 
where the site is located in a populous area and the Regional 
Administrator determines that the requirement would be impracticable.
    (10) A plugging and abandonment plan that meets the requirements of 
Sec.  146.10 of this chapter and is acceptable to the Director.
    (f) Recordkeeping. Applicants shall keep records of all data used to 
complete permit applications and any supplemental information submitted 
under Sec.  144.31 for a period of at least 3 years from the date the 
application is signed.
    (g) Information Requirements for Class I Hazardous Waste Injection 
Wells Permits. (1) The following information is required for each active 
Class I hazardous waste injection well at a facility seeking a UIC 
permit:
    (i) Dates well was operated.
    (ii) Specification of all wastes which have been injected in the 
well, if available.
    (2) The owner or operator of any facility containing one or more 
active hazardous waste injection wells must submit all available 
information pertaining to any release of hazardous waste or constituents 
from any active hazardous waste injection well at the facility.
    (3) The owner or operator of any facility containing one or more 
active Class I hazardous waste injection wells must conduct such 
preliminary site investigations as are necessary to determine whether a 
release is occurring, has occurred, or is likely to have occurred.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20185, May 11, 1984; 52 
FR 45797, Dec. 1, 1987; 52 FR 46963, Dec. 10, 1987; 58 FR 63897, Dec. 3, 
1993; 75 FR 77288, Dec. 10, 2010]



Sec.  144.32  Signatories to permit applications and reports.

    (a) Applications. All permit applications, except those submitted 
for Class II wells (see paragraph (b) of this section), shall be signed 
as follows:
    (1) For a corporation: by a responsible corporate officer. For the 
purpose of this section, a responsible corporate officer means; (i) A 
president, secretary, treasurer, or vice president of the corporation in 
charge of a principal business function, or any other person who 
performs similar policy- or decisionmaking functions for the 
corporation, or (ii) the manager of one or more manufacturing, 
production, or operating facilities employing more than 250 persons or 
having gross annual sales or expenditures exceeding $25 million (in 
second-quarter 1980 dollars), if authority to sign documents has been 
assigned or delegated to the manager in accordance with corporate 
procedures.

    Note: EPA does not require specific assignments or delegations of 
authority to responsible corporate officers identified in Sec.  
144.32(a)(1)(i). The Agency will presume that these responsible 
corporate officers have the requisite authority to sign permit 
applications unless the corporation has notified the Director to the 
contrary. Corporate procedures governing authority to sign permit 
applications may provide for assignment or delegation to applicable 
corporate positions under Sec.  144.32(a)(1)(ii) rather than to specific 
individuals.

    (2) For a partnership or sole proprietorship: by a general partner 
or the proprietor, respectively; or
    (3) For a municipality, State, Federal, or other public agency: by 
either a principal executive officer or ranking elected official. For 
purposes of this section, a principal executive officer of a Federal 
agency includes: (i) The chief executive officer of the agency, or (ii) 
a senior executive officer having responsibility for the overall 
operations of a principal geographic unit of the agency (e.g., Regional 
Administrators of EPA).
    (b) Reports. All reports required by permits, other information 
requested by the Director, and all permit applications submitted for 
Class II wells under Sec.  144.31 shall be signed by a person described 
in paragraph (a) of this section, or by a duly authorized representative 
of that person. A person is a duly authorized representative only if:
    (1) The authorization is made in writing by a person described in 
paragraph (a) of this section;

[[Page 827]]

    (2) The authorization specifies either an individual or a position 
having responsibility for the overall operation of the regulated 
facility or activity, such as the position of plant manager, operator of 
a well or a well field, superintendent, or position of equivalent 
responsibility. (A duly authorized representative may thus be either a 
named individual or any individual occupying a named position); and
    (3) The written authorization is submitted to the Director.
    (c) Changes to authorization. If an authorization under paragraph 
(b) of this section is no longer accurate because a different individual 
or position has responsibility for the overall operation of the 
facility, a new authorization satisfying the requirements of paragraph 
(b) of this section must be submitted to the Director prior to or 
together with any reports, information, or applications to be signed by 
an authorized representative.
    (d) Certification. Any person signing a document under paragraph (a) 
or (b) of this section shall make the following certification:

    I certify under penalty of law that this document and all 
attachments were prepared under my direction or supervision in 
accordance with a system designed to assure that qualified personnel 
properly gather and evaluate the information submitted. Based on my 
inquiry of the person or persons who manage the system, or those persons 
directly responsible for gathering the information, the information 
submitted is, to the best of my knowledge and belief, true, accurate, 
and complete. I am aware that there are significant penalties for 
submitting false information, including the possibility of fine and 
imprisonment for knowing violations.

(Clean Water Act (33 U.S.C. 1251 et seq.), Safe Drinking Water Act (42 
U.S.C. 300f et seq.), Clean Air Act (42 U.S.C. 7401 et seq.), Resource 
Conservation and Recovery Act (42 U.S.C. 6901 et seq.)

[48 FR 14189, Apr. 1, 1983, as amended at 48 FR 39621, Sept. 1, 1983]



Sec.  144.33  Area permits.

    (a) The Director may issue a permit on an area basis, rather than 
for each well individually, provided that the permit is for injection 
wells:
    (1) Described and identified by location in permit application(s) if 
they are existing wells, except that the Director may accept a single 
description of wells with substantially the same characteristics;
    (2) Within the same well field, facility site, reservoir, project, 
or similar unit in the same State;
    (3) Operated by a single owner or operator; and
    (4) Used to inject other than hazardous waste; and
    (5) Other than Class VI wells.
    (b) Area permits shall specify:
    (1) The area within which underground injections are authorized, and
    (2) The requirements for construction, monitoring, reporting, 
operation, and abandonment, for all wells authorized by the permit.
    (c) The area permit may authorize the permittee to construct and 
operate, convert, or plug and abandon wells within the permit area 
provided:
    (1) The permittee notifies the Director at such time as the permit 
requires;
    (2) The additional well satisfies the criteria in paragraph (a) of 
this section and meets the requirements specified in the permit under 
paragraph (b) of this section; and
    (3) The cumulative effects of drilling and operation of additional 
injection wells are considered by the Director during evaluation of the 
area permit application and are acceptable to the Director.
    (d) If the Director determines that any well constructed pursuant to 
paragraph (c) of this section does not satisfy any of the requirements 
of paragraphs (c) (1) and (2) of this section the Director may modify 
the permit under Sec.  144.39, terminate under Sec.  144.40, or take 
enforcement action. If the Director determines that cumulative effects 
are unacceptable, the permit may be modified under Sec.  144.39.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77288, Dec. 10, 2010]



Sec.  144.34  Emergency permits.

    (a) Coverage. Notwithstanding any other provision of this part or 
part 124, the Director may temporarily permit a specific underground 
injection if:
    (1) An imminent and substantial endangerment to the health of 
persons will result unless a temporary emergency permit is granted; or

[[Page 828]]

    (2) A substantial and irretrievable loss of oil or gas resources 
will occur unless a temporary emergency permit is granted to a Class II 
well; and
    (i) Timely application for a permit could not practicably have been 
made; and
    (ii) The injection will not result in the movement of fluids into 
underground sources of drinking water; or
    (3) A substantial delay in production of oil or gas resources will 
occur unless a temporary emergency permit is granted to a new Class II 
well and the temporary authorization will not result in the movement of 
fluids into an underground source of drinking water.
    (b) Requirements for issuance. (1) Any temporary permit under 
paragraph (a)(1) of this section shall be for no longer term than 
required to prevent the hazard.
    (2) Any temporary permit under paragraph (a)(2) of this section 
shall be for no longer than 90 days, except that if a permit application 
has been submitted prior to the expiration of the 90-day period, the 
Director may extend the temporary permit until final action on the 
application.
    (3) Any temporary permit under paragraph (a)(3) of this section 
shall be issued only after a complete permit application has been 
submitted and shall be effective until final action on the application.
    (4) Notice of any temporary permit under this paragraph shall be 
published in accordance with Sec.  124.11 within 10 days of the issuance 
of the permit.
    (5) The temporary permit under this section may be either oral or 
written. If oral, it must be followed within 5 calendar days by a 
written temporary emergency permit.
    (6) The Director shall condition the temporary permit in any manner 
he or she determines is necessary to ensure that the injection will not 
result in the movement of fluids into an underground source of drinking 
water.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20185, May 11, 1984]



Sec.  144.35  Effect of a permit.

    (a) Except for Class II and III wells, compliance with a permit 
during its term constitutes compliance, for purposes of enforcement, 
with Part C of the SDWA. However, a permit may be modified, revoked and 
reissued, or terminated during its term for cause as set forth in 
Sec. Sec.  144.39 and 144.40.
    (b) The issuance of a permit does not convey any property rights of 
any sort, or any exclusive privilege.
    (c) The issuance of a permit does not authorize any injury to 
persons or property or invasion of other private rights, or any 
infringement of State or local law or regulations.



Sec.  144.36  Duration of permits.

    (a) Permits for Class I and V wells shall be effective for a fixed 
term not to exceed 10 years. UIC permits for Class II and III wells 
shall be issued for a period up to the operating life of the facility. 
UIC permits for Class VI wells shall be issued for the operating life of 
the facility and the post-injection site care period. The Director shall 
review each issued Class II, III, and VI well UIC permit at least once 
every 5 years to determine whether it should be modified, revoked and 
reissued, terminated or a minor modification made as provided in Sec.  
144.39, Sec.  144.40, or Sec.  144.41.
    (b) Except as provided in Sec.  144.37, the term of a permit shall 
not be extended by modification beyond the maximum duration specified in 
this section.
    (c) The Director may issue any permit for a duration that is less 
than the full allowable term under this section.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77288, Dec. 10, 2010]



Sec.  144.37  Continuation of expiring permits.

    (a) EPA permits. When EPA is the permit-issuing authority, the 
conditions of an expired permit continue in force under 5 U.S.C. 558(c) 
until the effective date of a new permit if:
    (1) The permittee has submitted a timely application which is a 
complete application for a new permit; and
    (2) The Regional Administrator, through no fault of the permittee 
does not issue a new permit with an effective date on or before the 
expiration date of the previous permit (for example, when issuance is 
impracticable due to time or resource constraints).
    (b) Effect. Permits continued under this section remain fully 
effective and enforceable.

[[Page 829]]

    (c) Enforcement. When the permittee is not in compliance with the 
conditions of the expiring or expired permit the Regional Administrator 
may choose to do any or all of the following:
    (1) Initiate enforcement action based upon the permit which has been 
continued;
    (2) Issue a notice of intent to deny the new permit. If the permit 
is denied, the owner or operator would then be required to cease the 
activities authorized by the continued permit or be subject to 
enforcement action for operating without a permit;
    (3) Issue a new permit under part 124 with appropriate conditions; 
or
    (4) Take other actions authorized by these regulations.
    (d) State continuation. An EPA issued permit does not continue in 
force beyond its time expiration date under Federal law if at that time 
a State is the permitting authority. A State authorized to administer 
the UIC program may continue either EPA or State-issued permits until 
the effective date of the new permits, if State law allows. Otherwise, 
the facility or activity is operating without a permit from the time of 
expiration of the old permit to the effective date of the State-issued 
new permit.



Sec.  144.38  Transfer of permits.

    (a) Transfers by modification. Except as provided in paragraph (b) 
of this section, a permit may be transferred by the permittee to a new 
owner or operator only if the permit has been modified or revoked and 
reissued (under Sec.  144.39(b)(2)), or a minor modification made (under 
Sec.  144.41(d)), to identify the new permittee and incorporate such 
other requirements as may be necessary under the Safe Drinking Water 
Act.
    (b) Automatic transfers. As an alternative to transfers under 
paragraph (a) of this section, any UIC permit for a well not injecting 
hazardous waste or injecting carbon dioxide for geologic sequestration 
may be automatically transferred to a new permittee if:
    (1) The current permittee notifies the Director at least 30 days in 
advance of the proposed transfer date referred to in paragraph (b)(2) of 
this section;
    (2) The notice includes a written agreement between the existing and 
new permittees containing a specific date for transfer or permit 
responsibility, coverage, and liability between them, and the notice 
demonstrates that the financial responsibility requirements of Sec.  
144.52(a)(7) will be met by the new permittee; and
    (3) The Director does not notify the existing permittee and the 
proposed new permittee of his or her intent to modify or revoke and 
reissue the permit. A modification under this paragraph may also be a 
minor modification under Sec.  144.41. If this notice is not received, 
the transfer is effective on the date specified in the agreement 
mentioned in paragraph (b)(2) of this section.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77288, Dec. 10, 2010]



Sec.  144.39  Modification or revocation and reissuance of permits.

    When the Director receives any information (for example, inspects 
the facility, receives information submitted by the permittee as 
required in the permit (see Sec.  144.51 of this chapter), receives a 
request for modification or revocation and reissuance under Sec.  124.5, 
or conducts a review of the permit file) he or she may determine whether 
or not one or more of the causes listed in paragraphs (a) and (b) of 
this section for modification or revocation and reissuance or both 
exist. If cause exists, the Director may modify or revoke and reissue 
the permit accordingly, subject to the limitations of paragraph (c) of 
this section, and may request an updated application if necessary. When 
a permit is modified, only the conditions subject to modification are 
reopened. If a permit is revoked and reissued, the entire permit is 
reopened and subject to revision and the permit is reissued for a new 
term. See Sec.  124.5(c)(2) of this chapter. If cause does not exist 
under this section or Sec.  144.41 of this chapter, the Director shall 
not modify or revoke and reissue the permit. If a permit modification 
satisfies the criteria in Sec.  144.41 for ``minor modifications'' the 
permit may be modified without a draft permit or

[[Page 830]]

public review. Otherwise, a draft permit must be prepared and other 
procedures in part 124 must be followed.
    (a) Causes for modification. The following are causes for 
modification. For Class I hazardous waste injection wells, Class II, 
Class III or Class VI wells the following may be causes for revocation 
and reissuance as well as modification; and for all other wells the 
following may be cause for revocation or reissuance as well as 
modification when the permittee requests or agrees.
    (1) Alterations. There are material and substantial alterations or 
additions to the permitted facility or activity which occurred after 
permit issuance which justify the application of permit conditions that 
are different or absent in the existing permit.
    (2) Information. The Director has received information. Permits 
other than for Class II and III wells may be modified during their terms 
for this cause only if the information was not available at the time of 
permit issuance (other than revised regulations, guidance, or test 
methods) and would have justified the application of different permit 
conditions at the time of issuance. For UIC area permits (Sec.  144.33), 
this cause shall include any information indicating that cumulative 
effects on the environment are unacceptable.
    (3) New regulations. The standards or regulations on which the 
permit was based have been changed by promulgation of new or amended 
standards or regulations or by judicial decision after the permit was 
issued. Permits other than for Class I hazardous waste injection wells, 
Class II, Class III or Class VI wells may be modified during their 
permit terms for this cause only as follows:
    (i) For promulgation of amended standards or regulations, when:
    (A) The permit condition requested to be modified was based on a 
promulgated part 146 regulation; and
    (B) EPA has revised, withdrawn, or modified that portion of the 
regulation on which the permit condition was based, and
    (C) A permittee requests modification in accordance with Sec.  124.5 
within ninety (90) days after Federal Register notice of the action on 
which the request is based.
    (ii) For judicial decisions, a court of competent jurisdiction has 
remanded and stayed EPA promulgated regulations if the remand and stay 
concern that portion of the regulations on which the permit condition 
was based and a request is filed by the permittee in accordance with 
Sec.  124.5 within ninety (90) days of judicial remand.
    (4) Compliance schedules. The Director determines good cause exists 
for modification of a compliance schedule, such as an act of God, 
strike, flood, or materials shortage or other events over which the 
permittee has little or no control and for which there is no reasonably 
available remedy. See also Sec.  144.41(c) (minor modifications).
    (5) Basis for modification of Class VI permits. Additionally, for 
Class VI wells, whenever the Director determines that permit changes are 
necessary based on:
    (i) Area of review reevaluations under Sec.  146.84(e)(1) of this 
chapter;
    (ii) Any amendments to the testing and monitoring plan under Sec.  
146.90(j) of this chapter;
    (iii) Any amendments to the injection well plugging plan under Sec.  
146.92(c) of this chapter;
    (iv) Any amendments to the post-injection site care and site closure 
plan under Sec.  146.93(a)(3) of this chapter;
    (v) Any amendments to the emergency and remedial response plan under 
Sec.  146.94(d) of this chapter; or
    (vi) A review of monitoring and/or testing results conducted in 
accordance with permit requirements.
    (b) Causes for modification or revocation and reissuance. The 
following are causes to modify or, alternatively, revoke and reissue a 
permit:
    (1) Cause exists for termination under Sec.  144.40, and the 
Director determines that modification or revocation and reissuance is 
appropriate.
    (2) The Director has received notification (as required in the 
permit, see Sec.  144.41(d)) of a proposed transfer of the permit. A 
permit also may be modified to reflect a transfer after the effective 
date of an automatic transfer (Sec.  144.38(b)) but will not be revoked 
and reissued after the effective date of the

[[Page 831]]

transfer except upon the request of the new permittee.
    (3) A determination that the waste being injected is a hazardous 
waste as defined in Sec.  261.3 either because the definition has been 
revised, or because a previous determination has been changed.
    (c) Facility siting. Suitability of the facility location will not 
be considered at the time of permit modification or revocation and 
reissuance unless new information or standards indicate that a threat to 
human health or the environment exists which was unknown at the time of 
permit issuance.

[48 FR 14189, Apr. 1, 1983, as amended at 53 FR 28147, July 26, 1988; 75 
FR 77288, Dec. 10, 2010]



Sec.  144.40  Termination of permits.

    (a) The Director may terminate a permit during its term, or deny a 
permit renewal application for the following causes:
    (1) Noncompliance by the permittee with any condition of the permit;
    (2) The permittee's failure in the application or during the permit 
issuance process to disclose fully all relevant facts, or the 
permittee's misrepresentation of any relevant facts at any time; or
    (3) A determination that the permitted activity endangers human 
health or the environment and can only be regulated to acceptable levels 
by permit modification or termination;
    (b) The Director shall follow the applicable procedures in part 124 
in terminating any permit under this section.



Sec.  144.41  Minor modifications of permits.

    Upon the consent of the permittee, the Director may modify a permit 
to make the corrections or allowances for changes in the permitted 
activity listed in this section, without following the procedures of 
part 124. Any permit modification not processed as a minor modification 
under this section must be made for cause and with part 124 draft permit 
and public notice as required in Sec.  144.39. Minor modifications may 
only:
    (a) Correct typographical errors;
    (b) Require more frequent monitoring or reporting by the permittee;
    (c) Change an interim compliance date in a schedule of compliance, 
provided the new date is not more than 120 days after the date specified 
in the existing permit and does not interfere with attainment of the 
final compliance date requirement; or
    (d) Allow for a change in ownership or operational control of a 
facility where the Director determines that no other change in the 
permit is necessary, provided that a written agreement containing a 
specific date for transfer of permit responsibility, coverage, and 
liability between the current and new permittees has been submitted to 
the Director.
    (e) Change quantities or types of fluids injected which are within 
the capacity of the facility as permitted and, in the judgment of the 
Director, would not interfere with the operation of the facility or its 
ability to meet conditions described in the permit and would not change 
its classification.
    (f) Change construction requirements approved by the Director 
pursuant to Sec.  144.52(a)(1) (establishing UIC permit conditions), 
provided that any such alteration shall comply with the requirements of 
this part and part 146.
    (g) Amend a plugging and abandonment plan which has been updated 
under Sec.  144.52(a)(6).
    (h) Amend a Class VI injection well testing and monitoring plan, 
plugging plan, post-injection site care and site closure plan, or 
emergency and remedial response plan where the modifications merely 
clarify or correct the plan, as determined by the Director.

[48 FR 14189, Apr. 1, 1983, as amended at 75 FR 77289, Dec. 10, 2010]



                       Subpart E_Permit Conditions



Sec.  144.51  Conditions applicable to all permits.

    The following conditions apply to all UIC permits. All conditions 
applicable to all permits shall be incorporated into the permits either 
expressly or by reference. If incorporated by reference, a specific 
citation to these regulations (or the corresponding approved State 
regulations) must be given in the permit.

[[Page 832]]

    (a) Duty to comply. The permittee must comply with all conditions of 
this permit. Any permit noncompliance constitutes a violation of the 
Safe Drinking Water Act and is grounds for enforcement action; for 
permit termination, revocation and reissuance, or modification; or for 
denial of a permit renewal application; except that the permittee need 
not comply with the provisions of this permit to the extent and for the 
duration such noncompliance is authorized in an emergency permit under 
Sec.  144.34.
    (b) Duty to reapply. If the permittee wishes to continue an activity 
regulated by this permit after the expiration date of this permit, the 
permittee must apply for and obtain a new permit.
    (c) Need to halt or reduce activity not a defense. It shall not be a 
defense for a permittee in an enforcement action that it would have been 
necessary to halt or reduce the permitted activity in order to maintain 
compliance with the conditions of this permit.
    (d) Duty to mitigate. The permittee shall take all reasonable steps 
to minimize or correct any adverse impact on the environment resulting 
from noncompliance with this permit.
    (e) Proper operation and maintenance. The permittee shall at all 
times properly operate and maintain all facilities and systems of 
treatment and control (and related appurtenances) which are installed or 
used by the permittee to achieve compliance with the conditions of this 
permit. Proper operation and maintenance includes effective performance, 
adequate funding, adequate operator staffing and training, and adequate 
laboratory and process controls, including appropriate quality assurance 
procedures. This provision requires the operation of back-up or 
auxiliary facilities or similar systems only when necessary to achieve 
compliance with the conditions of the permit.
    (f) Permit actions. This permit may be modified, revoked and 
reissued, or terminated for cause. The filing of a request by the 
permittee for a permit modification, revocation and reissuance, or 
termination, or a notification of planned changes or anticipated 
noncompliance, does not stay any permit condition.
    (g) Property rights. This permit does not convey any property rights 
of any sort, or any exclusive privilege.
    (h) Duty to provide information. The permittee shall furnish to the 
Director, within a time specified, any information which the Director 
may request to determine whether cause exists for modifying, revoking 
and reissuing, or terminating this permit, or to determine compliance 
with this permit. The permittee shall also furnish to the Director, upon 
request, copies of records required to be kept by this permit.
    (i) Inspection and entry. The permittee shall allow the Director, or 
an authorized representative, upon the presentation of credentials and 
other documents as may be required by law, to:
    (1) Enter upon the permittee's premises where a regulated facility 
or activity is located or conducted, or where records must be kept under 
the conditions of this permit;
    (2) Have access to and copy, at reasonable times, any records that 
must be kept under the conditions of this permit;
    (3) Inspect at reasonable times any facilities, equipment (including 
monitoring and control equipment), practices, or operations regulated or 
required under this permit; and
    (4) Sample or monitor at reasonable times, for the purposes of 
assuring permit compliance or as otherwise authorized by the SDWA, any 
substances or parameters at any location.
    (j) Monitoring and records. (1) Samples and measurements taken for 
the purpose of monitoring shall be representative of the monitored 
activity.
    (2) The permittee shall retain records of all monitoring 
information, including the following:
    (i) Calibration and maintenance records and all original strip chart 
recordings for continuous monitoring instrumentation, copies of all 
reports required by this permit, and records of all data used to 
complete the application for this permit, for a period of at least 3 
years from the date of the sample, measurement, report, or application. 
This period may be extended by request of the Director at any time; and

[[Page 833]]

    (ii) The nature and composition of all injected fluids until three 
years after the completion of any plugging and abandonment procedures 
specified under Sec.  144.52(a)(6), or under part 146 subpart G as 
appropriate. The Director may require the owner or operator to deliver 
the records to the Director at the conclusion of the retention period. 
For EPA administered programs, the owner or operator shall continue to 
retain the records after the three year retention period unless he 
delivers the records to the Regional Administrator or obtains written 
approval from the Regional Administrator to discard the records.
    (3) Records of monitoring information shall include:
    (i) The date, exact place, and time of sampling or measurements;
    (ii) The individual(s) who performed the sampling or measurements;
    (iii) The date(s) analyses were performed;
    (iv) The individual(s) who performed the analyses;
    (v) The analytical techniques or methods used; and
    (vi) The results of such analyses.
    (4) Owners or operators of Class VI wells shall retain records as 
specified in subpart H of part 146, including Sec. Sec.  146.84(g), 
146.91(f), 146.92(d), 146.93(f), and 146.93(h) of this chapter.
    (k) Signatory requirement. All applications, reports, or information 
submitted to the Administrator shall be signed and certified. (See Sec.  
144.32.)
    (l) Reporting requirements--(1) Planned changes. The permittee shall 
give notice to the Director as soon as possible of any planned physical 
alterations or additions to the permitted facility.
    (2) Anticipated noncompliance. The permittee shall give advance 
notice to the Director of any planned changes in the permitted facility 
or activity which may result in noncompliance with permit requirements.
    (3) Transfers. This permit is not transferable to any person except 
after notice to the Director. The Director may require modification or 
revocation and reissuance of the permit to change the name of the 
permittee and incorporate such other requirements as may be necessary 
under the Safe Drinking Water Act. (See Sec.  144.38; in some cases, 
modification or revocation and reissuance is mandatory.)
    (4) Monitoring reports. Monitoring results shall be reported at the 
intervals specified elsewhere in this permit.
    (5) Compliance schedules. Reports of compliance or noncompliance 
with, or any progress reports on, interim and final requirements 
contained in any compliance schedule of this permit shall be submitted 
no later than 30 days following each schedule date.
    (6) Twenty-four hour reporting. The permittee shall report any 
noncompliance which may endanger health or the environment, including:
    (i) Any monitoring or other information which indicates that any 
contaminant may cause an endangerment to a USDW; or
    (ii) Any noncompliance with a permit condition or malfunction of the 
injection system which may cause fluid migration into or between USDWs.

Any information shall be provided orally within 24 hours from the time 
the permittee becomes aware of the circumstances. A written submission 
shall also be provided within 5 days of the time the permittee becomes 
aware of the circumstances. The written submission shall contain a 
description of the noncompliance and its cause, the period of 
noncompliance, including exact dates and times, and if the noncompliance 
has not been corrected, the anticipated time it is expected to continue; 
and steps taken or planned to reduce, eliminate, and prevent 
reoccurrence of the noncompliance.
    (7) Other noncompliance. The permittee shall report all instances of 
noncompliance not reported under paragraphs (l) (4), (5), and (6) of 
this section, at the time monitoring reports are submitted. The reports 
shall contain the information listed in paragraph (l)(6) of this 
section.
    (8) Other information. Where the permittee becomes aware that it 
failed to submit any relevant facts in a permit application, or 
submitted incorrect information in a permit application or in any report 
to the Director, it shall promptly submit such facts or information.
    (m) Requirements prior to commencing injection. Except for all new 
wells authorized by an area permit under

[[Page 834]]

Sec.  144.33(c), a new injection well may not commence injection until 
construction is complete, and
    (1) The permittee has submitted notice of completion of construction 
to the Director; and
    (2)(i) The Director has inspected or otherwise reviewed the new 
injection well and finds it is in compliance with the conditions of the 
permit; or
    (ii) The permittee has not received notice form the Director of his 
or her intent to inspect or otherwise review the new injection well 
within 13 days of the date of the notice in paragraph (m)(1) of this 
section, in which case prior inspection or review is waived and the 
permittee may commence injection. The Director shall include in his 
notice a reasonable time period in which he shall inspect the well.
    (n) The permittee shall notify the Director at such times as the 
permit requires before conversion or abandonment of the well or in the 
case of area permits before closure of the project.
    (o) A Class I, II or III permit shall include and a Class V permit 
may include conditions which meet the applicable requirements of Sec.  
146.10 of this chapter to ensure that plugging and abandonment of the 
well will not allow the movement of fluids into or between USDWs. Where 
the plan meets the requirements of Sec.  146.10 of this chapter, the 
Director shall incorporate the plan into the permit as a permit 
condition. Where the Director's review of an application indicates that 
the permittee's plan is inadequate, the Director may require the 
applicant to revise the plan, prescribe conditions meeting the 
requirements of this paragraph, or deny the permit. A Class VI permit 
shall include conditions which meet the requirements set forth in Sec.  
146.92 of this chapter. Where the plan meets the requirements of Sec.  
146.92 of this chapter, the Director shall incorporate it into the 
permit as a permit condition. For purposes of this paragraph, temporary 
or intermittent cessation of injection operations is not abandonment.
    (p) Plugging and abandonment report. For EPA-administered programs, 
within 60 days after plugging a well or at the time of the next 
quarterly report (whichever is less) the owner or operator shall submit 
a report to the Regional Administrator. If the quarterly report is due 
less than 15 days before completion of plugging, then the report shall 
be submitted within 60 days. The report shall be certified as accurate 
by the person who performed the plugging operation. Such report shall 
consist of either:
    (1) A statement that the well was plugged in accordance with the 
plan previously submitted to the Regional Administrator; or
    (2) Where actual plugging differed from the plan previously 
submitted, and updated version of the plan on the form supplied by the 
regional administrator, specifying the differences.
    (q) Duty to establish and maintain mechanical integrity. (1) The 
owner or operator of a Class I, II, III or VI well permitted under this 
part shall establish mechanical integrity prior to commencing injection 
or on a schedule determined by the Director. Thereafter the owner or 
operator of Class I, II, and III wells must maintain mechanical 
integrity as defined in Sec.  146.8 of this chapter and the owner or 
operator of Class VI wells must maintain mechanical integrity as defined 
in Sec.  146.89 of this chapter. For EPA-administered programs, the 
Regional Administrator may require by written notice that the owner or 
operator comply with a schedule describing when mechanical integrity 
demonstrations shall be made.
    (2) When the Director determines that a Class I, II, III or VI well 
lacks mechanical integrity pursuant to Sec.  146.8 or Sec.  146.89 of 
this chapter for Class VI of this chapter, he/she shall give written 
notice of his/her determination to the owner or operator. Unless the 
Director requires immediate cessation, the owner or operator shall cease 
injection into the well within 48 hours of receipt of the Director's 
determination. The Director may allow plugging of the well pursuant to 
the requirements of Sec.  146.10 of this chapter or require the 
permittee to perform such additional construction, operation, 
monitoring, reporting and corrective action as is necessary to prevent 
the movement of fluid into or between USDWs caused by the lack of 
mechanical integrity. The owner or operator may resume injection upon 
written notification from the Director that the owner or operator

[[Page 835]]

has demonstrated mechanical integrity pursuant to Sec.  146.8 of this 
chapter.
    (3) The Director may allow the owner or operator of a well which 
lacks mechanical integrity pursuant to Sec.  146.8(a)(1) of this chapter 
to continue or resume injection, if the owner or operator has made a 
satisfactory demonstration that there is no movement of fluid into or 
between USDWs.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20185, May 11, 1984; 53 
FR 28147, July 26, 1988; 58 FR 63898, Dec. 3, 1993; 75 FR 77289, Dec. 
10, 2010]



Sec.  144.52  Establishing permit conditions.

    (a) In addition to conditions required in Sec.  144.51, the Director 
shall establish conditions, as required on a case-by-case basis under 
Sec.  144.36 (duration of permits), Sec.  144.53(a) (schedules of 
compliance), Sec.  144.54 (monitoring), and for EPA permits only Sec.  
144.53(b) (alternate schedules of compliance), and Sec.  144.4 
(considerations under Federal law). Permits for owners or operators of 
hazardous waste injection wells shall include conditions meeting the 
requirements of Sec.  144.14 (requirements for wells injecting hazardous 
waste), paragraphs (a)(7) and (a)(9) of this section, and subpart G of 
part 146. Permits for owners or operators of Class VI injection wells 
shall include conditions meeting the requirements of subpart H of part 
146. Permits for other wells shall contain the following requirements, 
when applicable.
    (1) Construction requirements as set forth in part 146. Existing 
wells shall achieve compliance with such requirements according to a 
compliance schedule established as a permit condition. The owner or 
operator of a proposed new injection well shall submit plans for 
testing, drilling, and construction as part of the permit application. 
Except as authorized by an area permit, no constuction may commence 
until a permit has been issued containing construction requirements (see 
Sec.  144.11). New wells shall be in compliance with these requirements 
prior to commencing injection operations. Changes in construction plans 
during construction may be approved by the Administrator as minor 
modifications (Sec.  144.41). No such changes may be physically 
incorporated into construction of the well prior to approval of the 
modification by the Director.
    (2) Corrective action as set forth in Sec. Sec.  144.55, 146.7, and 
146.84 of this chapter.
    (3) Operation requirements as set forth in 40 CFR part 146; the 
permit shall establish any maximum injection volumes and/or pressures 
necessary to assure that fractures are not initiated in the confining 
zone, that injected fluids do not migrate into any underground source of 
drinking water, that formation fluids are not displaced into any 
underground source of drinking water, and to assure compliance with the 
part 146 operating requirements.
    (4) Requirements for wells managing hazardous waste, as set forth in 
Sec.  144.14.
    (5) Monitoring and reporting requirements as set forth in 40 CFR 
part 146. The permittee shall be required to identify types of tests and 
methods used to generate the monitoring data. For EPA administered 
programs, monitoring of the nature of injected fluids shall comply with 
applicable analytical methods cited and described in table I of 40 CFR 
136.3 or in appendix III of 40 CFR part 261 or in certain circumstances 
by other methods that have been approved by the Regional Administrator.
    (6) After a cessation of operations of two years the owner or 
operator shall plug and abandon the well in accordance with the plan 
unless he:
    (i) Provides notice to the Regional Administrator;
    (ii) Describes actions or procedures, satisfactory to the Regional 
Administrator, that the owner or operator will take to ensure that the 
well will not endanger USDWs during the period of temporary abandonment. 
These actions and procedures shall include compliance with the technical 
requirements applicable to active injection wells unless waived by the 
Regional Administrator.
    (7) Financial responsibility. (i) The permittee, including the 
transferor of a permit, is required to demonstrate and maintain 
financial responsibility and resources to close, plug, and abandon the 
underground injection operation in a manner prescribed by the Director 
until:

[[Page 836]]

    (A) The well has been plugged and abandoned in accordance with an 
approved plugging and abandonment plan pursuant to Sec. Sec.  144.51(o), 
146.10, and 146.92 of this chapter, and submitted a plugging and 
abandonment report pursuant to Sec.  144.51(p); or
    (B) The well has been converted in compliance with the requirements 
of Sec.  144.51(n); or
    (C) The transferor of a permit has received notice from the Director 
that the owner or operator receiving transfer of the permit, the new 
permittee, has demonstrated financial responsibility for the well.
    (ii) The permittee shall show evidence of such financial 
responsibility to the Director by the submission of a surety bond, or 
other adequate assurance, such as a financial statement or other 
materials acceptable to the Director. For EPA administered programs, the 
Regional Administrator may on a periodic basis require the holder of a 
lifetime permit to submit an estimate of the resources needed to plug 
and abandon the well revised to reflect inflation of such costs, and a 
revised demonstration of financial responsibility, if necessary. The 
owner or operator of a well injecting hazardous waste must comply with 
the financial responsibility requirements of subpart F of this part. For 
Class VI wells, the permittee shall show evidence of such financial 
responsibility to the Director by the submission of a qualifying 
instrument (see Sec.  146.85(a) of this chapter), such as a financial 
statement or other materials acceptable to the Director. The owner or 
operator of a Class VI well must comply with the financial 
responsibility requirements set forth in Sec.  146.85 of this chapter.
    (8) Mechanical integrity. A permit for any Class I, II, III or VI 
well or injection project which lacks mechanical integrity shall 
include, and for any Class V well may include, a condition prohibiting 
injection operations until the permittee shows to the satisfaction of 
the Director under Sec.  146.8, or Sec.  146.89 of this chapter for 
Class VI, that the well has mechanical integrity.
    (9) Additional conditions. The Director shall impose on a case-by-
case basis such additional conditions as are necessary to prevent the 
migration of fluids into underground sources of drinking water.
    (b)(1) In addition to conditions required in all permits the 
Director shall establish conditions in permits as required on a case-by-
case basis, to provide for and assure compliance with all applicable 
requirements of the SDWA and parts 144, 145, 146 and 124.
    (2) For a State issued permit, an applicable requirement is a State 
statutory or regulatory requirement which takes effect prior to final 
administrative disposition of the permit. For a permit issued by EPA, an 
applicable requirement is a statutory or regulatory requirement 
(including any interim final regulation) which takes effect prior to the 
issuance of the permit. Section 124.14 (reopening of comment period) 
provides a means for reopening EPA permit proceedings at the discretion 
of the Director where new requirements become effective during the 
permitting process and are of sufficient magnitude to make additional 
proceedings desirable. For State and EPA administered programs, an 
applicable requirement is also any requirement which takes effect prior 
to the modification or revocation and reissuance of a permit, to the 
extent allowed in Sec.  144.39.
    (3) New or reissued permits, and to the extent allowed under Sec.  
144.39 modified or revoked and reissued permits, shall incorporate each 
of the applicable requirements referenced in Sec.  144.52.
    (c) Incorporation. All permit conditions shall be incorporated 
either expressly or by reference. If incorporated by reference, a 
specific citation to the applicable regulations or requirements must be 
given in the permit.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20185, May 11, 1984; 53 
FR 28147, July 26, 1988; 58 FR 63898; Dec. 3, 1993; 65 FR 30913, May 15, 
2000; 75 FR 77289, Dec. 10, 2010]



Sec.  144.53  Schedule of compliance.

    (a) General. The permit may, when appropriate, specify a schedule of 
compliance leading to compliance with the SDWA and parts 144, 145, 146, 
and 124.
    (1) Time for compliance. Any schedules of compliance shall require 
compliance as soon as possible, and in no case later than 3 years after 
the effective date of the permit.

[[Page 837]]

    (2) Interim dates. Except as provided in paragraph (b)(1)(ii) of 
this section, if a permit establishes a schedule of compliance which 
exceeds 1 year from the date of permit issuance, the schedule shall set 
forth interim requirements and the dates for their achievement.
    (i) The time between interim dates shall not exceed 1 year.
    (ii) If the time necessary for completion of any interim requirement 
is more than 1 year and is not readily divisible into stages for 
completion, the permit shall specify interim dates for the submission of 
reports of progress toward completion of the interim requirements and 
indicate a projected completion date.
    (3) Reporting. The permit shall be written to require that if 
paragraph (a)(1) of this section is applicable, progress reports be 
submitted no later than 30 days following each interim date and the 
final date of compliance.
    (b) Alternative schedules of compliance. A permit applicant or 
permittee may cease conducting regulated activities (by plugging and 
abandonment) rather than continue to operate and meet permit 
requirements as follows:
    (1) If the permittee decides to cease conducting regulated 
activities at a given time within the term of a permit which has already 
been issued:
    (i) The permit may be modified to contain a new or additional 
schedule leading to timely cessation of activities; or
    (ii) The permittee shall cease conducting permitted activities 
before noncompliance with any interim or final compliance schedule 
requirement already specified in the permit.
    (2) If the decision to cease conducting regulated activities is made 
before issuance of a permit whose term will include the termination 
date, the permit shall contain a schedule leading to termination which 
will ensure timely compliance with applicable requirements.
    (3) If the permittee is undecided whether to cease conducting 
regulated activities, the Director may issue or modify a permit to 
contain two schedules as follows:
    (i) Both schedules shall contain an identical interim deadline 
requiring a final decision on whether to cease conducting regulated 
activities no later than a date which ensures sufficient time to comply 
with applicable requirements in a timely manner if the decision is to 
continue conducting regulated activities;
    (ii) One schedule shall lead to timely compliance with applicable 
requirements;
    (iii) The second schedule shall lead to cessation of regulated 
activities by a date which will ensure timely compliance with applicable 
requirements;
    (iv) Each permit containing two schedules shall include a 
requirement that after the permittee has made a final decision under 
paragraph (b)(3)(i) of this section it shall follow the schedule leading 
to compliance if the decision is to continue conducting regulated 
activities, and follow the schedule leading to termination if the 
decision is to cease conducting regulated activities.
    (4) The applicant's or permittee's decision to cease conducting 
regulated activities shall be evidenced by a firm public commitment 
satisfactory to the Director, such as a resolution of the board of 
directors of a corporation.



Sec.  144.54  Requirements for recording and reporting of monitoring results.

    All permits shall specify:
    (a) Requirements concerning the proper use, maintenance, and 
installation, when appropriate, of monitoring equipment or methods 
(including biological monitoring methods when appropriate);
    (b) Required monitoring including type, intervals, and frequency 
sufficient to yield data which are representative of the monitored 
activity including when appropriate, continuous monitoring;
    (c) Applicable reporting requirements based upon the impact of the 
regulated activity and as specified in part 146. Reporting shall be no 
less frequent than specified in the above regulations.



Sec.  144.55  Corrective action.

    (a) Coverage. Applicants for Class I, II, (other than existing), or 
III injection well permits shall identify the location of all known 
wells within the injection well's area of review which penetrate the 
injection zone, or in the case

[[Page 838]]

of Class II wells operating over the fracture pressure of the injection 
formation, all known wells within the area of review penetrating 
formations affected by the increase in pressure. For such wells which 
are improperly sealed, completed, or abandoned, the applicant shall also 
submit a plan consisting of such steps or modifications as are necessary 
to prevent movement of fluid into underground sources of drinking water 
(``corrective action''). Where the plan is adequate, the Director shall 
incorporate it into the permit as a condition. Where the Director's 
review of an application indicates that the permittee's plan is 
inadequate (based on the factors in Sec.  146.07), the Director shall 
require the applicant to revise the plan, prescribe a plan for 
corrective action as a condition of the permit under paragraph (b) of 
this section, or deny the application. The Director may disregard the 
provisions of Sec.  146.06 (Area of Review) and Sec.  146.07 (Corrective 
Action) when reviewing an application to permit an existing Class II 
well.
    (b) Requirements--(1) Existing injection wells. Any permit issued 
for an existing injection well (other than Class II) requiring 
corrective action shall include a compliance schedule requiring any 
corrective action accepted or prescribed under paragraph (a) of this 
section to be completed as soon as possible.
    (2) New injection wells. No owner or operator of a new injection 
well may begin injection until all required corrective action has been 
taken.
    (3) Injection pressure limitation. The Director may require as a 
permit condition that injection pressure be so limited that pressure in 
the injection zone does not exceed hydrostatic pressure at the site of 
any improperly completed or abandoned well within the area of review. 
This pressure limitation shall satisfy the corrective action 
requirement. Alternatively, such injection pressure limitation can be 
part of a compliance schedule and last until all other required 
corrective action has been taken.
    (4) Class III wells only. When setting corrective action 
requirements the Director shall consider the overall effect of the 
project on the hydraulic gradient in potentially affected USDWs, and the 
corresponding changes in potentiometric surface(s) and flow direction(s) 
rather than the discrete effect of each well. If a decision is made that 
corrective action is not necessary based on the determinations above, 
the monitoring program required in Sec.  146.33(b) shall be designed to 
verify the validity of such determinations.



 Subpart F_Financial Responsibility: Class I Hazardous Waste Injection 
                                  Wells

    Source: 49 FR 20186, May 11, 1984, unless otherwise noted.



Sec.  144.60  Applicability.

    (a) The requirements of Sec. Sec.  144.62, 144.63, and 144.70 apply 
to owners and operators of all existing and new Class I Hazardous waste 
injection wells, except as provided otherwise in this section.



Sec.  144.61  Definitions of terms as used in this subpart.

    (a) Plugging and abandonment plan means the plan for plugging and 
abandonment prepared in accordance with the requirements of Sec. Sec.  
144.28 and 144.51.
    (b) Current plugging cost estimate means the most recent of the 
estimates prepared in accordance with Sec.  144.62 (a), (b) and (c).
    (c) Parent corporation means a corporation which directly owns at 
least 50 percent of the voting stock of the corporation which is the 
injection well owner or operator; the latter corporation is deemed a 
subsidiary of the parent corporation.
    (d) The following terms are used in the specifications for the 
financial test for plugging and abandonment. The definitions are 
intended to represent the common meanings of the terms as they are 
generally used by the business community.
    Assets means all existing and all probable future economic benefits 
obtained or controlled by a particular entity.
    Current assets means cash or other assets or resources commonly 
identified as those which are reasonably expected

[[Page 839]]

to be realized in cash or sold or consumed during the normal operating 
cycle of the business.
    Current liabilities means obligations whose liquidation is 
reasonably expected to require the use of existing resources properly 
classifiable as current assets or the creation of other current 
liabilities.
    Independently audited refers to an audit performed by an independent 
certified public accountant in accordance with generally accepted 
auditing standards.
    Liabilities means probable future sacrifices of economic benefits 
arising from present obligations to transfer assets or provide services 
to other entities in the future as a result of past transactions or 
events.
    Net working capital means current assets minus current liabilities.
    Net worth means total assets minus total liabilities and is 
equivalent to owner's equity.
    Tangible net worth means the tangible assets that remain after 
deducting liabilities; such assets would not include intangibles such as 
goodwill and rights to patents or royalties.



Sec.  144.62  Cost estimate for plugging and abandonment.

    (a) The owner or operator must prepare a written estimate, in 
current dollars, of the cost of plugging the injection well in 
accordance with the plugging and abandonment plan as specified in 
Sec. Sec.  144.28 and 144.51. The plugging and abandonment cost estimate 
must equal the cost of plugging and abandonment at the point in the 
facility's operating life when the extent and manner of its operation 
would making plugging and abandonment the most expensive, as indicated 
by its plugging and abandonment plan.
    (b) The owner or operator must adjust the plugging and abandonment 
cost estimate for inflation within 30 days after each anniversary of the 
date on which the first plugging and abandonment cost estimate was 
prepared. The adjustment must be made as specified in paragraphs (b) (1) 
and (2) of this section, using an inflation factor derived from the 
annual Oil and Gas Field Equipment Cost Index. The inflation factor is 
the result of dividing the latest published annual Index by the Index 
for the previous year.
    (1) The first adjustment is made by multiplying the plugging and 
abandonment cost estimate by the inflation factor. The result is the 
adjusted plugging and abandonment cost estimate.
    (2) Subsequent adjustments are made by multiplying the latest 
adjusted plugging and abandonment cost estimate by the latest inflation 
factor.
    (c) The owner or operator must revise the plugging and abandonment 
cost estimate whenever a change in the plugging and abandonment plan 
increases the cost of plugging and abandonment. The revised plugging and 
abandonment cost estimate must be adjusted for inflation as specified in 
Sec.  144.62(b).
    (d) The owner or operator must keep the following at the facility 
during the operating life of the facility: the latest plugging and 
abandonment cost estimate prepared in accordance with Sec.  144.62 (a) 
and (c) and, when this estimate has been adjusted in accordance with 
Sec.  144.62(b), the latest adjusted plugging and abandonment cost 
estimate.



Sec.  144.63  Financial assurance for plugging and abandonment.

    An owner or operator of each facility must establish financial 
assurance for the plugging and abandonment of each existing and new 
Class I hazardous waste injection well. He must choose from the options 
as specified in paragraphs (a) through (f) of this section.
    (a) Plugging and abandonment trust fund. (1) An owner or operator 
may satisfy the requirements of this section by establishing a plugging 
and abandonment trust fund which conforms to the requirements of this 
paragraph and submitting an originally signed duplicate of the trust 
agreement to the Regional Administrator. An owner or operator of a Class 
I well injecting hazardous waste must submit the originally signed 
duplicate of the trust agreement to the Regional Administrator with the 
permit application or for approval to operate under rule. The trustee 
must be an entity which has the authority to act as a trustee and whose 
trust operations are regulated and examined by a Federal or State 
agency.

[[Page 840]]

    (2) The wording of the trust agreement must be identical to the 
wording specified in Sec.  144.70(a)(1), and the trust agreement must be 
accompanied by a formal certification of acknowledgment (for example, 
see Sec.  144.70(a)(2)). Schedule A of the trust agreement must be 
updated within 60 days after a change in the amount of the current 
plugging and abandonment cost estimate covered by the agreement.
    (3) Payments into the trust fund must be made annually by the owner 
or operator over the term of the initial permit or over the remaining 
operating life of the injection well as estimated in the plugging and 
abandonment plan, whichever period is shorter; this period is hereafter 
referred to as the ``pay-in period.'' The payments into the plugging and 
abandonment trust fund must be made as follows:
    (i) For a new well, the first payment must be made before the 
initial injection of hazardous waste. A receipt from the trustee for 
this payment must be submitted by the owner or operator to the Regional 
Administrator before this initial injection of hazardous waste. The 
first payment must be at least equal to the current plugging and 
abandonment cost estimate, except as provided in Sec.  144.70(g), 
divided by the number of years in the pay-in period. Subsequent payments 
must be made no later than 30 days after each anniversary date of the 
first payment. The amount of each subsequent payment must be determined 
by this formula:
[GRAPHIC] [TIFF OMITTED] TC15NO91.138

where PE is the current plugging and abandonment cost estimate, CV is 
          the current value of the trust fund, and Y is the number of 
          years remaining in the pay-in period.

    (ii) If an owner or operator establishes a trust fund as specified 
in Sec.  144.63(a) of this chapter, and the value of that trust fund is 
less than the current plugging and abandonment cost estimate when a 
permit is awarded for the injection well, the amount of the current 
plugging and abandonment cost estimate still to be paid into the trust 
fund must be paid in over the pay-in period as defined in paragraph 
(a)(3) of this section. Payments must continue to be made no later than 
30 days after each anniversary date of the first payment made pursuant 
to part 144 of this chapter. The amount of each payment must be 
determined by this formula:
[GRAPHIC] [TIFF OMITTED] TC15NO91.139

where PE is the current plugging and abandonment cost estimate, CV is 
          the current value of the trust fund, and Y is the number of 
          years remaining in the pay-in period.

    (4) The owner or operator may accelerate payments into the trust 
fund or he may deposit the full amount of the current plugging and 
abandonment cost estimate at the time the fund is established. However, 
he must maintain the value of the fund at no less than the value that 
the fund would have if annual payments were made as specified in 
paragraph (a)(3) of this section.
    (5) If the owner or operator establishes a plugging and abandonment 
trust fund after having used one or more alternate mechanisms specified 
in this section or in Sec.  144.63 of this chapter, his first payment 
must be in at least the amount that the fund would contain if the trust 
fund were established initially and annual payments made according to 
specifications of this paragraph.
    (6) After the pay-in period is completed, whenever the current 
plugging and abandonment cost estimate changes, the owner or operator 
must compare the new estimate with the trustee's most recent annual 
valuation of the trust fund. If the value of the fund is less than the 
amount of the new estimate, the owner or operator, within 60 days after 
the change in the cost estimate, must either deposit an amount into the 
fund so that its value after this deposit at least equals the amount of 
the current plugging and abandonment cost estimate, or obtain other 
financial assurance as specified in this section to cover the 
difference.
    (7) If the value of the trust fund is greater than the total amount 
of the current plugging and abandonment cost estimate, the owner or 
operator may submit a written request to the Regional Administrator for 
release of

[[Page 841]]

the amount in excess of the current plugging and abandonment cost 
estimate.
    (8) If an owner or operator substitutes other financial assurance as 
specified in this section for all or part of the trust fund, he may 
submit a written request to the Regional Administrator for release of 
the amount in excess of the current plugging and abandonment cost 
estimate covered by the trust fund.
    (9) Within 60 days after receiving a request from the owner or 
operator for release of funds as specified in paragraph (a) (7) or (8) 
of this section, the Regional Administrator will instruct the trustee to 
release to the owner or operator such funds as the Regional 
Administrator specifies in writing.
    (10) After beginning final plugging and abandonment, an owner or 
operator or any other person authorized to perform plugging and 
abandonment may request reimbursement for plugging and abandonment 
expenditures by submitting itemized bills to the Regional Administrator. 
Within 60 days after receiving bills for plugging and abandonment 
activities, the Regional Administrator will determine whether the 
plugging and abandonment expenditures are in accordance with the 
plugging and abandonment plan or otherwise justified, and if so, he will 
instruct the trustee to make reimbursement in such amounts as the 
Regional Administrator specifies in writing. If the Regional 
Administrator has reason to believe that the cost of plugging and 
abandonment will be significantly greater than the value of the trust 
fund, he may withhold reimbursement of such amounts as he deems prudent 
until he determines, in accordance with Sec.  144.63(i), that the owner 
or operator is no longer required to maintain financial assurance for 
plugging and abandonment.
    (11) The Regional Administrator will agree to termination of the 
trust when:
    (i) An owner or operator substitutes alternate financial assurance 
as specified in this section; or
    (ii) The Regional Administrator releases the owner or operator from 
the requirements of this section in accordance with Sec.  144.63(i).
    (b) Surety bond guaranteeing payment into a plugging and abandonment 
trust fund. (1) An owner or operator must satisfy the requirements of 
this section by obtaining a surety bond which conforms to the 
requirements of this paragraph and submitting the bond to the Regional 
Administrator with the application for a permit or for approval to 
operate under rule. The bond must be effective before the initial 
injection of hazardous waste. The surety company issuing the trust must, 
at a minimum, be among those listed as acceptable sureties on Federal 
bonds in Circular 570 of the U.S. Department of the Treasury.
    (2) The wording of the surety bond must be identical to the wording 
in Sec.  144.70(b).
    (3) The owner or operator who uses a surety bond to satisfy the 
requirements of this section must also establish a standby trust fund. 
Under the terms of the bond, all payments made thereunder will be 
deposited by the surety directly into the standby trust fund in 
accordance with instructions from the Regional Administrator. This 
standby trust fund must meet the requirements specified in Sec.  
144.63(a), except that:
    (i) An originally signed duplicate of the trust agreement must be 
submitted to the Regional Administrator with the surety bond; and
    (ii) Until the standby trust fund is funded pursuant to the 
requirements of this section, the following are not required by these 
requirements:
    (A) Payments into the trust fund as specified in Sec.  144.63(a);
    (B) Updating of Schedule A of the trust agreement [see Sec.  
144.70(a)] to show current plugging and abandonment cost estimates;
    (C) Annual valuations as required by the trust agreement; and
    (D) Notices of nonpayment as required by the trust agreement.
    (4) The bond must guarantee that the owner or operator will:
    (i) Fund the standby trust fund in an amount equal to the penal sum 
of the bond before beginning of plugging and abandonment of the 
injection well; or
    (ii) Fund the standby trust fund in an amount equal to the penal sum 
within 15 days after an order to begin plugging

[[Page 842]]

and abandonment is issued by the Regional Administrator or a U.S. 
district court or other court of competent jurisdiction; or
    (iii) Provide alternate financial assurance as specified in this 
section, and obtain the Regional Administrator's written approval of the 
assurance provided, within 90 days after receipt by both the owner or 
operator and the Regional Administrator of a notice of cancellation of 
the bond from the surety.
    (5) Under the terms of the bond, the surety will become liable on 
the bond obligation when the owner or operator fails to perform as 
guaranteed by the bond.
    (6) The penal sum of the bond must be in amount at least equal to 
the current plugging and abandonment cost estimate, except as provided 
in Sec.  144.63(g).
    (7) Whenever the current plugging and abandonment cost estimate 
increases to an amount greater than the penal sum, the owner or 
operator, within 60 days after the increase, must either cause the penal 
sum to be increased to an amount at least equal to the current plugging 
and abandonment cost estimate and submit evidence of such increase to 
the Regional Administrator, or obtain other financial assurance as 
specified in this section to cover the increase. Whenever the current 
plugging and abandonment cost estimate decreases, the penal sum may be 
reduced to the amount of the current plugging and abandonment cost 
estimate following written approval by the Regional Administrator.
    (8) Under the terms of the bond, the surety may cancel the bond by 
sending notice of cancellation by certified mail to the owner or 
operator and to the Regional Administrator. Cancellation may not occur, 
however, during 120 days beginning on the date of the receipt of the 
notice of cancellation by both owner or operator and the Regional 
Administrator as evidenced by the returned receipts.
    (9) The owner or operator may cancel the bond if the Regional 
Administrator has given prior written consent based on his receipt of 
evidence of alternate financial assurance as specified in this section.
    (c) Surety bond guaranteeing performance of plugging and 
abandonment. (1) An owner or operator may satisfy the requirements of 
this section by obtaining a surety bond which conforms to the 
requirements of this paragraph and submitting the bond to the Regional 
Administrator. An owner or operator of a new facility must submit the 
bond to the Regional Administrator with the permit application or for 
approval to operate under rule. The bond must be effective before 
injection of hazardous waste is started. The surety company issuing the 
bond must, at a minimum, be among those listed as acceptable sureties on 
Federal bonds in Circular 570 of the U.S. Department of the Treasury.
    (2) The wording of the surety bond must be identical to the wording 
specified in Sec.  144.70(c).
    (3) The owner or operator who uses a surety bond to satisfy the 
requirements of this section must also establish a standby trust fund. 
Under the terms of the bond, all payments made thereunder will be 
deposited by the surety directly into the standby trust fund in 
accordance with instructions from the Regional Administrator. The 
standby trust must meet the requirements specified in Sec.  144.63(a), 
except that:
    (i) An original signed duplicate of the trust agreement must be 
submitted to the Regional Administrator with the surety bond; and
    (ii) Unless the standby trust fund is funded pursuant to the 
requirements of this section, the following are not required by these 
regulations:
    (A) Payments into the trust fund as specified in Sec.  144.63(a);
    (B) Updating of Schedule A of the trust agreement [see Sec.  
144.70(a)] to show current plugging and abandonment cost estimates;
    (C) Annual valuations as required by the trust agreement; and
    (D) Notices of nonpayment as required by the trust agreement.
    (4) The bond must guarantee that the owner or operator will:
    (i) Perform plugging and abandonment in accordance with the plugging 
and abandonment plan and other requirements of the permit for the 
injection well whenever required to do so; or

[[Page 843]]

    (ii) Provide alternate financial assurance as specified in this 
section, and obtain the Regional Administrator's written approval of the 
assurance provided, within 90 days after receipt by both the owner or 
operator and the Regional Administrator of a notice of cancellation of 
the bond from the surety.
    (5) Under the terms of the bond, the surety will become liable on 
the bond obligation when the owner or operator fails to perform as 
guaranteed by the bond. Following a determination that the owner or 
operator has failed to perform plugging and abandonment in accordance 
with the plugging and abandonment plan and other permit requirements 
when required to do so, under terms of the bond the surety will perform 
plugging and abandonment as guaranteed by the bond or will deposit the 
amount of the penal sum into the standby trust fund.
    (6) The penal sum of the bond must be in an amount at least equal to 
the current plugging and abandonment cost estimate.
    (7) Whenever the current plugging and abandonment cost estimate 
increases to an amount greater than the penal sum, the owner or 
operator, within 60 days after the increase, must either cause the penal 
sum to be increased to an amount at least equal to the current plugging 
and abandonment cost estimate and submit evidence of such increase to 
the Regional Administrator, or obtain other financial assurance as 
specified in this section. Whenever the plugging and abandonment cost 
estimate decreases, the penal sum may be reduced to the amount of the 
current plugging and abandonment cost estimate following written 
approval by the Regional Administrator.
    (8) Under the terms of the bond, the surety may cancel the bond by 
sending notice of cancellation by certified mail to the owner or 
operator and to the Regional Administrator. Cancellation may not occur, 
however, during the 120 days beginning on the date of receipt of the 
notice of cancellation by both the owner or operator and the Regional 
Administrator, as evidenced by the return receipts.
    (9) The owner or operator may cancel the bond if the Regional 
Administrator has given prior written consent. The Regional 
Administrator will provide such written consent when:
    (i) An owner or operator substitute alternate financial assurance as 
specified in this section; or
    (ii) The Regional Administrator releases the owner or operator from 
the requirements of this section in accordance with Sec.  144.63(i).
    (10) The surety will not be liable for deficiencies in the 
performance of plugging and abandonment by the owner or operator after 
the Regional Administrator releases the owner or operator from the 
requirements of this section in accordance with Sec.  144.63(i).
    (d) Plugging and abandonment letter of credit. (1) An owner or 
operator may satisfy the requirements of this section by obtaining an 
irrevocable standby letter of credit which conforms to the requirements 
of this paragraph and submitting the letter to the Regional 
Administrator. An owner or operator of an injection well must submit the 
letter of credit to the Regional Administrator during submission of the 
permit application or for approval to operate under rule. The letter of 
credit must be effective before initial injection of hazardous waste. 
The issuing institution must be an entity which has the authority to 
issue letters of credit and whose letter-of-credit operations are 
regulated and examined by a Federal or State agency.
    (2) The wording of the letter of credit must be identical to the 
wording specified in Sec.  144.70(d).
    (3) An owner or operator who uses a letter of credit to satisfy the 
requirements of this section must also establish a standby trust fund. 
Under the terms of the letter of credit, all amounts paid pursuant to a 
draft by the Regional Administrator will be deposited by the issuing 
institution directly into the standby trust fund in accordance with 
instructions from the Regional Administrator. This standby trust fund 
must meet the requirements of the trust fund specified in Sec.  
144.63(a), except that:
    (i) An originally signed duplicate of the trust agreement must be 
submitted to the Regional Administrator with the letter of credit; and

[[Page 844]]

    (ii) Unless the standby trust fund is funded pursuant to the 
requirements of this section, the following are not required by these 
regulations:
    (A) Payments into the trust fund as specified in Sec.  144.63(a);
    (B) Updating of Schedule A of the trust agreement (see Sec.  
144.70(a)) to show current plugging and abandonment cost estimates;
    (C) Annual valuations as required by the trust agreement; and
    (D) Notices of nonpayment as required by the trust agreement.
    (4) The letter of credit must be accompanied by a letter from the 
owner or operator referring to the letter of credit by number, issuing 
institution, and date, and providing the following information: the EPA 
Identification Number, name, and address of the facility, and the amount 
of funds assured for plugging and abandonment of the well by the letter 
of credit.
    (5) The letter of credit must be irrevocable and issued for a period 
of at least 1 year. The letter of credit must provide that the 
expiration date will be automatically extended for a period of at least 
1 year unless, at least 120 days before the current expiration date, the 
issuing institution notifies both the owner or operator and the Regional 
Administrator by certified mail of a decision not to extend the 
expiration date. Under the terms of the letter of credit, the 120 days 
will begin on the date when both the owner or operator and the Regional 
Administrator have received the notice, as evidenced by the return 
receipts.
    (6) The letter of credit must be issued in an amount at least equal 
to the current plugging and abandonment cost estimate, except as 
provided in Sec.  144.63(g).
    (7) Whenever the current plugging and abandonment cost estimate 
increases to an amount greater than the amount of the credit, the owner 
or operator, within 60 days after the increase, must either cause the 
amount of the credit to be increased so that it at least equals the 
current plugging and abandonment cost estimate and submit evidence of 
such increase to the Regional Administrator, or obtain other financial 
assurance as specified in this section to cover the increase. Whenever 
the current plugging and abandonment cost estimate decreases, the amount 
of the credit may be reduced to the amount of the current plugging and 
abandonment cost estimate following written approval by the Regional 
Administrator.
    (8) Following a determination that the owner or operator has failed 
to perform final plugging and abandonment in accordance with the 
plugging and abandonment plan and other permit requirements when 
required to do so, the Regional Administrator may draw on the letter of 
credit.
    (9) If the owner or operator does not establish alternate financial 
assurance as specified in this section and obtain written approval of 
such alternate assurance from the Regional Administrator within 90 days 
after receipt by both the owner or operator and the Regional 
Administrator of a notice from the issuing institution that it has 
decided not to extend the letter of credit beyond the current expiration 
date, the Regional Administrator will draw on the letter of credit. The 
Regional Administrator may delay the drawing if the issuing institution 
grants an extension of the term of the credit. During the last 30 days 
of any such extension the Regional Administrator will draw on the letter 
of credit if the owner or operator has failed to provide alternate 
financial assurance as specified in this section and obtain written 
approval of such assurance from the Regional Administrator.
    (10) The Regional Administrator will return the letter of credit to 
the issuing institution for termination when:
    (i) An owner or operator substitutes alternate financial assurance 
as specified in this section; or
    (ii) The Regional Administrator releases the owner or operator from 
the requirements of this section in accordance with Sec.  144.63(i).
    (e) Plugging and abandonment insurance. (1) An owner or operator may 
satisfy the requirements of this section by obtaining plugging and 
abandonment insurance which conforms to the requirements of this 
paragraph and submitting a certificate of such insurance to the Regional 
Administrator. An owner or operator of a new injection

[[Page 845]]

well must submit the certificate of insurance to the Regional 
Administrator with the permit application or for approval operate under 
rule. The insurance must be effective before injection starts. At a 
minimum, the insurer must be licensed to transact the business of 
insurance, or eligible to provide insurance as an excess or surplus 
lines insurer, in one or more States.
    (2) The wording of the certificate of insurance must be identical to 
the wording specified in Sec.  144.70(e).
    (3) The plugging and abandonment insurance policy must be issued for 
a face amount at least equal to the current plugging and abandonment 
estimate, except as provided in Sec.  144.63(g). The term ``face 
amount'' means the total amount the insurer is obligated to pay under 
the policy. Actual payments by the insurer will not change the face 
amount, although the insurers future liability will be lowered by the 
amount of the payments.
    (4) The plugging and abandonment insurance policy must guarantee 
that funds will be available whenever final plugging and abandonment 
occurs. The policy must also guarantee that once plugging and 
abandonment begins, the issurer will be responsible for paying out 
funds, up to an amount equal to the face amount of the policy, upon the 
direction of the Regional Administrator, to such party or parties as the 
Regional Administrator specifies.
    (5) After beginning plugging and abandonment, an owner or operator 
or any other person authorized to perform plugging and abandonment may 
request reimbursement for plugging and abandonment expenditures by 
submitting itemized bills to the Regional Administrator. Within 60 days 
after receiving bills for plugging and abandonment activities, the 
Regional Administrator will determine whether the plugging and 
abandonment expenditures are in accordance with the plugging and 
abandonment plan or otherwise justified, and if so, he will instruct the 
insurer to make reimbursement in such amounts as the Regional 
Administrator specifies in writing. If the Regional Administrator has 
reason to believe that the cost of plugging and abandonment will be 
significantly greater than the face amount of the policy, he may 
withhold reimbursement of such amounts as he deems prudent until he 
determines, in accordance with Sec.  144.63(i), that the owner or 
operator is no longer required to maintain financial assurance for 
plugging and abandonment of the injection well.
    (6) The owner or operator must maintain the policy in full force and 
effect until the Regional Administrator consents to termination of the 
policy by the owner or operator as specified in paragraph (e)(10) of 
this section. Failure to pay the premium, without substitution of 
alternate financial assurance as specified in this section, will 
constitute a significant violation of these regulations, warranting such 
remedy as the Regional Administrator deems necessary. Such violation 
will be deemed to begin upon receipt by the Regional Administrator of a 
notice of future cancellation, termination, or failure to renew due to 
nonpayment of the premium, rather than upon the date of expiration.
    (7) Each policy must contain provisions allowing assignment to a 
successor owner or operator. Such assignment may be conditional upon 
consent of the insurer, provided such consent is not unreasonably 
refused.
    (8) The policy must provide that the insurer may not cancel, 
terminate, or fail to renew the policy except for failure to pay the 
premium. The automatic renewal of the policy must, at a minimum, provide 
the insured with the option of renewal at the face amount of the 
expiring policy. If there is a failure to pay the premium, the insurer 
may elect to cancel, terminate, or fail to renew the policy by sending 
notice by certified mail to the owner or operator and the Regional 
Administrator. Cancellation, termination, or failure to renew may not 
occur, however, during 120 days beginning with the date of receipt of 
the notice by both the Regional Administrator and the owner or operator, 
as evidenced by the return of receipts. Cancellation, termination, or 
failure to renew may not occur and the policy will remain in full force 
and effect in the event that on or before the date of expiration:
    (i) The Regional Administrator deems the injection well abandoned; 
or

[[Page 846]]

    (ii) The permit is terminated or revoked or a new permit is denied; 
or
    (iii) Plugging and abandonment is ordered by the Regional 
Administrator or a U.S. district court or other court of competent 
jurisdiction; or
    (iv) The owner or operator is named as debtor in a voluntary or 
involuntary proceeding under title 11 (Bankruptcy), U.S. Code; or
    (v) The premium due is paid.
    (9) Whenever the current plugging and abandonment cost estimate 
increases to an amount greater than the face amount of the policy, the 
owner or operator, within 60 days after the increase, must either cause 
the face amount to be increased to an amount at least equal to the 
current plugging and abandonment estimate and submit evidence of such 
increase to the Regional Administrator, or obtain other financial 
assurance as specified in this section to cover the increase. Whenever 
the current plugging and abandonment cost estimate decreases, the face 
amount may be reduced to the amount of the current plugging and 
abandonment cost estimate following written approval by the Regional 
Administrator.
    (10) The Regional Administrator will give written consent to the 
owner or operator that he may terminate the insurance policy when:
    (i) An owner or operator substitutes alternate financial assurance 
as specified in this section; or
    (ii) The Regional Administrator releases the owner or operator from 
the requirements of this section in accordance with Sec.  144.63(i).
    (f) Financial test and corporate guarantee for plugging and 
abandonment. (1) An owner or operator may satisfy the requirements of 
this section by demonstrating that he passes a financial test as 
specified in this paragraph. To pass this test the owner or operator 
must meet the criteria of either paragraph (f)(1)(i) or (f)(1)(ii) of 
this section:
    (i) The owner or operator must have:
    (A) Two of the following three ratios: A ratio of total liabilities 
to net worth less than 2.0; a ratio of the sum of net income plus 
depreciation, depletion, and amortization to total liabilities greater 
than 0.1; and a ratio of current assets to current liabilities greater 
than 1.5; and
    (B) Net working capital and tangible net worth each at least six 
times the sum of the current plugging and abandonment cost estimate; and
    (C) Tangible net worth of at least $10 million; and
    (D) Assets in the United States amounting to at least 90 percent of 
his total assets or at least six times the sum of the current plugging 
and abandonment cost estimate.
    (ii) The owner or operator must have:
    (A) A current rating for his most recent bond issuance of AAA, AA, A 
or BBB as issued by Standard and Poor's or Aaa, Aa, A, or Baa as issued 
by Moody's; and
    (B) Tangible net worth at least six times the sum of the current 
plugging and abandonment cost estimate; and
    (C) Tangible net worth of at least $10 million; and
    (D) Assets located in the United States amounting to at least 90 
percent of his total assets or at least six times the sum of the current 
plugging and abandonment cost estimates.
    (2) The phrase ``current plugging and abandonment cost estimate'' as 
used in paragraph (f)(1) of this section refers to the cost estimate 
required to be shown in paragraphs 1 through 4 of the letter from the 
owner's or operator's chief financial officer Sec.  144.70(f).
    (3) To demonstrate that he meets this test, the owner or operator 
must submit the following items to the Regional Administrator:
    (i) A letter signed by the owner's or operator's chief financial 
officer and worded as specified in Sec.  144.70(f); and
    (ii) A copy of the independent certified public accountant's report 
on examination of the owner's or operator's financial statements for the 
latest completed fiscal year; and
    (iii) A special report from the owner's or operator's independent 
certified public accountant to the owner or operator stating that:
    (A) He has compared the data which the letter from the chief 
financial officer specifies as having been derived from the 
independently audited, year-end financial statements for the latest 
fiscal year with the amounts in such financial statements; and

[[Page 847]]

    (B) In connection with that procedure, no matters came to his 
attention which caused him to believe that the specified data should be 
adjusted.
    (4) An owner or operator of a new injection well must submit the 
items specified in paragraph (f)(3) of this section to the Regional 
Administrator within 90 days after the close of each succeeding fiscal 
year. This information must consist of all three items specified in 
paragraph (f)(3) of this section.
    (5) After the initial submission of items specified in paragraph 
(f)(3) of this section, the owner or operator must send updated 
information to the Regional Administrator within 90 days after the close 
of each succeeding fiscal year. This information must consist of all 
three items specified in paragraph (f)(3) of this section.
    (6) If the owner or operator no longer meets the requirements of 
paragraph (f)(1) of this section, he must send notice to the Regional 
Administrator of intent to establish alternate financial assurance as 
specified in this section. The notice must be sent by certified mail 
within 90 days after the end of the fiscal year for which the year-end 
financial data show that the owner or operator no longer meets the 
requirements. The owner or operator must provide the alternate financial 
assurance within 120 days after the end of such fiscal year.
    (7) The Regional Administrator may, based on a reasonable belief 
that the owner or operator may no longer meet the requirements of 
paragraph (f)(1) of this section, require reports of financial condition 
at any time from the owner or operator in addition to those specified in 
paragraph (f)(3) of this section. If the Regional Administrator finds, 
on the basis of such reports or other information, that the owner or 
operator no longer meets the requirements of paragraph (f)(1) of this 
section, the owner or operator must provide alternate financial 
assurance as specified in this section within 30 days after notification 
of such a finding.
    (8) The Regional Administrator may disallow use of this test on the 
basis of qualifications in the opinion expressed by the independent 
certified public accountant in his report on examination of the owner's 
or operator's financial statements [see paragraph (f)(3)(ii) of this 
section]. An adverse opinion or disclaimer of opinion will be cause for 
disallowance. The Regional Administrator will evaluate other 
qualifications on an individual basis. The owner or operator must 
provide alternate financial assurance as specified in this section 
within 30 days after notification of the disallowance.
    (9) The owner or operator is no longer required to submit the items 
specified in paragraph (f)(3) of this section when:
    (i) An owner or operator substitutes alternate financial assurance 
as specified in this section; or
    (ii) The Regional Administrator releases the owner or operator from 
the requirements of this section in accordance with Sec.  144.63(i).
    (10) An owner or operator may meet the requirements of this section 
by obtaining a written guarantee, hereafter referred to as ``corporate 
guarantee.'' The guarantee must be the parent corporation of the owner 
or operator. The guarantee must meet the requirements for owners or 
operators in paragraphs (f)(1) through (f)(8) of this section and must 
comply with the terms of the corporate guarantee. The wording of the 
corporate guarantee must be identical to the wording specified in Sec.  
144.70(h). The corporate guarantee must accompany the items sent to the 
Regional Administrator as specified in paragraph (f)(3) of this section. 
The terms of the corporate guarantee must provide that:
    (i) If the owner or operator fails to perform plugging and 
abandonment of the injection well covered by the corporate guarantee in 
accordance with the plugging and abandonment plan and other permit 
requirements whenever required to do so, the guarantee will do so or 
establish a trust fund as specified in Sec.  144.63(a) in the name of 
the owner or operator.
    (ii) The corporate guarantee will remain in force unless the 
guarantor sends notice of cancellation by certified mail to the owner or 
operator and the Regional Administrator, as evidenced by the return 
receipts. Cancellation may not occur, however, during the 120 days 
beginning on the date of receipt of the notice of cancellation

[[Page 848]]

by both the owner or operator and the Regional Administrator, as 
evidenced by the return receipts.
    (iii) If the owner or operator fails to provide alternate financial 
assurance as specified in this section and obtain the written approval 
of such alternate assurance from the Regional Administrator within 90 
days after receipt by both the owner or operator and the Regional 
Administrator of a notice of cancellation of the corporate guarantee 
from the guarantor, the guarantor will provide such alternative 
financial assurance in the name of the owner or operator.
    (g) Use of multiple financial mechanisms. An owner or operator may 
satisfy the requirements of this section by establishing more than one 
financial mechanism per injection well. These mechanisms are limited to 
trust funds, surety bonds, guaranteeing payment into a trust fund, 
letters of credit, and insurance. The mechanisms must be as specified in 
paragraphs (a), (b), (d), and (e), respectively, of this section, except 
that it is the combination of mechanisms, rather than the single 
mechanism, which must provide financial assurance for an amount at least 
equal to the adjusted plugging and abandonment cost. If an owner or 
operator uses a trust fund in combination with a surety bond or letter 
of credit, he may use that trust fund as the standby trust fund for the 
other mechanisms. A single standby trust may be established for two or 
more mechanisms. The Regional Administrator may invoke any or all of the 
mechanisms to provide for plugging and abandonment of the injection 
well.
    (h) Use of a financial mechanism for multiple facilities. An owner 
or operator may use a financial assurance mechanism specified in this 
section to meet the requirements of this section for more than one 
injection well. Evidence of financial assurance submitted to the 
Regional Administrator must include a list showing, for each injection 
well, the EPA Identification Number, name, address, and the amount of 
funds for plugging and abandonment assured by the mechanism. If the 
injection wells covered by the mechanism are in more than one Region, 
identical evidence of financial assurance must be submitted to and 
maintained with the Regional Administrators of all such Regions. The 
amount of funds available through the mechanism must be no less than the 
sum of funds that would be available if a separate mechanism had been 
established and maintained for each injection well. In directing funds 
available through the mechanism for plugging and abandonment of any of 
the injection wells covered by the mechanism, the Regional Administrator 
may direct only the amount of funds designated for that injection well, 
unless the owner or operator agrees to use additional funds available 
under the mechanism.
    (i) Release of the owner or operator from the requirements of this 
section. Within 60 days after receiving certifications from the owner or 
operator and an independent registered professional engineer that 
plugging and abandonment has been accomplished in accordance with the 
plugging and abandonment plan, the Regional Administrator will notify 
the owner or operator in writing that he is no longer required by this 
section to maintain financial assurance for plugging and abandonment of 
the injection well, unless the Regional Administrator has reason to 
believe that plugging and abandonment has not been in accordance with 
the plugging and abandonment plan.



Sec.  144.64  Incapacity of owners or operators, guarantors, 
or financial institutions.

    (a) An owner or operator must notify the Regional Administrator by 
certified mail of the commencement of a voluntary or involuntary 
proceeding under title 11 (Bankruptcy), U.S. Code, naming the owner or 
operator as debtor, within 10 business days after the commencement of 
the proceeding. A guarantor of a corporate guarantee as specified in 
Sec.  144.63(f) must make such a notification if he is named as debtor, 
as required under the terms of the guarantee (Sec.  144.70(f)).
    (b) An owner or operator who fulfills the requirements of Sec.  
144.63 by obtaining a letter of credit, surety bond, or insurance policy 
will be deemed to be without the required financial assurance or 
liability coverage in the event

[[Page 849]]

of bankruptcy, insolvency, or a suspension or revocation of the license 
or charter of the issuing institution. The owner or operator must 
establish other financial assurance or liability coverage within 60 days 
after such an event.



Sec.  144.65  Use of State-required mechanisms.

    (a) For a facility located in a State where EPA is administering the 
requirements of this subpart but where the State has plugging and 
abandonment regulations that include requirements for financial 
assurance of plugging and abandonment, an owner or operator may use 
State-required financial mechanisms to meet the requirements of this 
subpart if the Regional Administrator determines that the State 
mechanisms are at least equivalent to the mechanisms specified in this 
subpart. The Regional Administrator will evaluate the equivalency of the 
mechanisms mainly in terms of (1) certainty of the availability of funds 
for the required plugging and abandonment activities and (2) the amount 
of funds that will be made available. The Regional Administrator may 
also consider other factors. The owner or operator must submit to the 
Regional Administrator evidence of the establishment of the mechanism 
together with a letter requesting that the State-required mechanism be 
considered acceptable for meeting the requirements of this subpart. The 
submittal must include the following information: The facility's EPA 
Identification Number, name and address, and the amounts of funds for 
plugging and abandonment coverage assured by the mechanism. The Regional 
Administrator will notify the owner or operator of his determination 
regarding the mechanism's acceptability. The Regional Administrator may 
require the owner or operator to submit additional information as is 
deemed necessary for making this determination.
    (b) If a State-required mechanism is found acceptable as specified 
in paragraph (a) of this section except for the amount of funds 
available, the owner or operator may satisfy the requirements of this 
subpart by increasing the funds available through the State-required 
mechanism or using additional mechanisms as specified in this subpart. 
The amounts of funds available through the State and Federal mechanisms 
must at least equal the amounts required by this subpart.



Sec.  144.66  State assumption of responsibility.

    (a) If a State either assumes legal responsibility for an owner's or 
operator's compliance with the plugging and abandonment requirements of 
these regulations or assures that funds will be available from State 
sources to cover these requirements, the owner or operator will be in 
compliance with the requirements of this subpart if the Regional 
Administrator determines that the State's assumption of responsibility 
is at least equivalent to the mechanisms specified in this subpart. The 
Regional Administrator will evaluate the equivalency of State guarantees 
mainly in terms of (1) certainty of the availability of funds for the 
required plugging and abandonment coverage and (2) the amount of funds 
that will be made available. The Regional Administrator may also 
consider other factors. The owner or operator must submit to the 
Regional Administrator a letter from the State describing the nature of 
the State's assumption of responsibility together with a letter from the 
owner or operator requesting that the State's asumption of 
responsibility be considered acceptable for meeting the requirements of 
this subpart. The letter from the State must include, or have attached 
to it, the following information: the facility's EPA Identification 
Number, name and address, and the amounts of funds for plugging and 
abandonment coverage that are guaranteed by the State. The Regional 
Administrator will notify the owner or operator of his determination 
regarding the acceptability of the State's guarantee in lieu of 
mechanisms specified in this subpart. The Regional Administrator may 
require the owner or operator to submit additional information as is 
deemed necessary to make this determination. Pending this determination, 
the owner or operator will be deemed to be in compliance with Sec.  
144.63.

[[Page 850]]

    (b) If a State's assumption of responsibility is found acceptable as 
specified in paragraph (a) of this section except for the amount of 
funds available, the owner or operator may satisfy the requirements of 
this subpart by use of both the State's assurance and additional 
financial mechanisms as specified in this subpart. The amount of funds 
available through the State and Federal mechanisms must at least equal 
the amount required by this subpart.



Sec.  144.70  Wording of the instruments.

    (a)(1) A trust agreement for a trust fund, as specified in Sec.  
144.63(a) of this chapter, must be worded as follows, except that 
instructions in brackets are to be replaced with the relevant 
information and the brackets deleted:

                             Trust Agreement

    TRUST AGREEMENT, the ``Agreement,'' entered into as of [date] by and 
between [name of the owner or operator], a [name of State] [insert 
``corporation,'' ``partnership,'' ``association,'' or 
``proprietorship''], the ``Grantor,'' and [name of corporate trustee], 
[insert ``incorporated in the State of ___'' or ``a national bank''], 
the ``Trustee.''
    Whereas, the United States Environmental Protection Agency, ``EPA,'' 
an agency of the United States Government, has established certain 
regulations applicable to the Grantor, requiring that an owner or 
operator of an injection well shall provide assurance that funds will be 
available when needed for plugging and abandonment of the injection 
well,
    Whereas, the Grantor has elected to establish a trust to provide all 
or part of such financial assurance for the facility(ies) identified 
herein,
    Whereas, the Grantor, acting through its duly authorized officers, 
has selected the Trustee to be the trustee under this agreement, and the 
Trustee is willing to act as trustee,
    Now, therefore, the Grantor and the Trustee agree as follows:
    Section 1. Definitions. As used in this Agreement:
    (a) The term ``Grantor'' means the owner or operator who enters into 
this Agreement and any successors or assigns of the Grantor.
    (b) The term ``Trustee'' means the Trustee who enters into this 
Agreement and any successor Trustee.
    (c) Facility or activity means any ``underground injection well'' or 
any other facility or activity that is subject to regulation under the 
Underground Injection Control Program.
    Section 2. Identification of Facilities and Cost Estimates. This 
Agreement pertains to the facilities and cost estimates identified on 
attached Schedule A [on Schedule A, for each facility list the EPA 
Identification Number, name, address, and the current plugging and 
abandonment cost estimate, or portions thereof, for which financial 
assurance is demonstrated by this Agreement].
    Section 3. Establishment of Fund. The Grantor and the Trustee hereby 
establish a trust fund, the ``Fund,'' for the benefit of EPA. The 
Grantor and the Trustee intend that no third party have access to the 
Fund except as herein provided. The Fund is established initially as 
consisting of the property, which is acceptable to the Trustee, 
described in Schedule B attached hereto. Such property and any other 
property subsequently transferred to the Trustee is referred to as the 
Fund, together with all earnings and profits thereon, less any payments 
or distributions made by the Trustee pursuant to this Agreement. The 
Fund shall be held by the Trustee, IN TRUST, as hereinafter provided. 
The Trustee shall not be responsible nor shall it undertake any 
responsibility for the amount or adequacy of, nor any duty to collect 
from the Grantor, any payments necessary to discharge any liabilities of 
the Grantor established by EPA.
    Section 4. Payment for Plugging and Abandonment. The Trustee shall 
make payments from the Fund as the EPA Regional Administrator shall 
direct, in writing, to provide for the payment of the costs of plugging 
and abandonment of the injection wells covered by this Agreement. The 
Trustee shall reimburse the Grantor or other persons as specified by the 
EPA Regional Administrator from the Fund for plugging and abandonment 
expenditures in such amounts as the EPA Regional Administrator shall 
direct in writing. In addition, the Trustee shall refund to the Grantor 
such amounts as the EPA Regional Administrator specifies in writing. 
Upon refund, such funds shall no longer constitute part of the Fund as 
defined herein.
    Section 5. Payments Comprising the Fund. Payments made to the 
Trustee for the Fund shall consist of cash or securities acceptable to 
the Trustee.
    Section 6. Trustee Management. The Trustee shall invest and reinvest 
the principal and income of the Fund and keep the Fund invested as a 
single fund, without distinction between principal and income, in 
accordance with general investment policies and guidelines which the 
Grantor may communicate in writing to the Trustee from time to time, 
subject, however, to the provisions of this Section. In investing, 
reinvesting, exchanging, selling, and managing the Fund, the Trustee 
shall discharge his duties with respect to the trust fund solely in the 
interest of the beneficiary and with the care, skill,

[[Page 851]]

prudence, and diligence under the circumstances then prevailing which 
persons of prudence, acting in a like capacity and familiar with such 
matters, would use in the conduct of an enterprise of a like character 
and with like aims; except that:
    (i) Securities or other obligations of the Grantor, or any other 
owner or operator of the facilities, or any of their affiliates as 
defined in the Investment Company Act of 1940, as amended, 15 U.S.C. 
80a-2.(a), shall not be acquired or held, unless they are securities or 
other obligations of the Federal or a State government;
    (ii) The Trustee is authorized to invest the Fund in time or demand 
deposits of the Trustee, to the extent insured by an agency of the 
Federal or State government; and
    (iii) The Trustee is authorized to hold cash awaiting investment or 
distribution uninvested for a reasonable time and without liability for 
the payment of interest thereon.
    Section 7. Commingling and Investment. The Trustee is expressly 
authorized in its discretion:
    (a) To transfer from time to time any or all of the assets of the 
Fund to any common, commingled, or collective trust fund created by the 
Trustee in which the Fund is eligible to participate, subject to all of 
the provisions thereof, to be commingled with the assets of other trusts 
participating therein; and
    (b) To purchase shares in any investment company registered under 
the Investment Company Act of 1940, 15 U.S.C. 80a-1 et seq., including 
one which may be created, managed, underwritten, or to which investment 
advice is rendered or the shares of which are sold by the Trustee. The 
Trustee may vote shares in its discretion.
    Section 8. Express Powers of Trustee. Without in any way limiting 
the powers and discretions conferred upon the Trustee by the other 
provisions of this Agreement or by law, the Trustee is expressly 
authorized and empowered:
    (a) To sell, exchange, convey, transfer, or otherwise dispose of any 
property held by it, by public or private sale. No person dealing with 
the Trustee shall be bound to see to the application of the purchase 
money or to inquire into the validity or expediency of any such sale or 
other disposition;
    (b) To make, execute, acknowledge, and deliver any and all documents 
of transfer and conveyance and any and all other instruments that may be 
necessary or appropriate to carry out the powers herein granted;
    (c) To register any securities held in the Fund in its own name or 
in the name of a nominee and to hold any security in bearer form or in 
book entry, or to combine certificates representing such securities with 
certificates of the same issue held by the Trustee in other fiduciary 
capacities, or to deposit or arrange for the deposit of such securities 
in a qualified central depository even though, when so deposited, such 
securities may be merged and held in bulk in the name of the nominee of 
such depositary with other securities deposited therein by another 
person, or to deposit or arrange for the deposit of any securities 
issued by the United States Government, or any agency or instrumentality 
thereof, with a Federal Reserve bank, but the books and records of the 
Trustee shall at all times show that all such securities are part of the 
Fund;
    (d) To deposit any cash in the Fund in interest-bearing accounts 
maintained or savings certificates issued by the Trustee, in its 
separate corporate capacity, or in any other banking institution 
affiliated with the Trustee, to the extent insured by an agency of the 
Federal or State government; and
    (e) To compromise or otherwise adjust all claims in favor of or 
against the Fund.
    Section 9. Taxes and Expenses. All taxes of any kind that may be 
assessed or levied against or in respect of the Fund and all brokerage 
commissions incurred by the Fund shall be paid from the Fund. All other 
expenses incurred by the Trustee in connection with the administration 
of this Trust, including fees for legal services rendered to the 
Trustee, the compensation of the Trustee to the extent not paid directly 
by the Grantor, and all other proper charges and disbursements of the 
Trustee shall be paid from the Fund.
    Section 10. Annual Valuation. The Trustee shall annually, at least 
30 days prior to the anniversary date of establishment of the Fund, 
furnish to the Grantor and to the appropriate EPA Regional Administrator 
a statement confirming the value of the Trust. Any securities in the 
Fund shall be valued at market value as of no more than 60 days prior to 
the anniversary date of establishment of the Fund. The failure of the 
Grantor to object in writing to the Trustee within 90 days after the 
statement has been furnished to the Grantor and the EPA Regional 
Administrator shall constitute a conclusively binding assent by the 
Grantor, barring the Grantor from asserting any claim or liability 
against the Trustee with respect to matters disclosed in the statement.
    Section 11. Advice of Counsel. The Trustee may from time to time 
consult with counsel, who may be counsel to the Grantor, with respect to 
any question arising as to the construction of this Agreement of any 
action to be taken hereunder. The Trustee shall be fully protected, to 
the extent permitted by law, in acting upon the advice of counsel.
    Section 12. Trustee Compensation. The Trustee shall be entitled to 
reasonable compensation for its services as agreed upon in writing from 
time to time with the Grantor.
    Section 13. Successor Trustee. The Trustee may resign or the Grantor 
may replace the

[[Page 852]]

Trustee, but such resignation or replacement shall not be effective 
until the Grantor has appointed a successor trustee and this successor 
accepts the appointment. The successor trustee shall have the same 
powers and duties as those conferred upon the Trustee hereunder. Upon 
the successor trustee's acceptance of the appointment, the Trustee shall 
assign, transfer, and pay over to the successor trustee the funds and 
properties then constituting the Fund. If for any reason the Grantor 
cannot or does not act in the event of the resignation of the Trustee, 
the Trustee may apply to a court of competent jurisdiction for the 
appointment of a successor trustee or for instructions. The successor 
trustee shall specify the date on which it assumes administration of the 
trust in a writing sent to the Grantor, the EPA Regional Administrator, 
and the present Trustee by certified mail 10 days before such change 
becomes effective. Any expenses incurred by the Trustee as a result of 
any of the acts contemplated by this Section shall be paid as provided 
in Section 9.
    Section 14. Instructions to the Trustee. All orders, requests, and 
instructions by the Grantor to the Trustee shall be in writing, signed 
by such persons as are designated in the attached Exhibit A or such 
other designees as the Grantor may designate by amendment to Exhibit A. 
The Trustee shall be fully protected in acting without inquiry in 
accordance with the Grantor's orders, requests, and instructions. All 
orders, requests, and instructions by the EPA Regional Administrator to 
the Trustee shall be in writing, signed by the EPA Regional 
Administrators of the Regions in which the facilities are located, or 
their designees, and the Trustee shall act and shall be fully protected 
in acting in accordance with such orders, requests, and instructions. 
The Trustee shall have the right to assume, in the absence of written 
notice to the contrary, that no event constituting a change or a 
termination of the authority of any person to act on behalf of the 
Grantor or EPA hereunder has occurred. The Trustee shall have no duty to 
act in the absence of such orders, requests, and instructions from the 
Grantor and/or EPA, except as provided for herein.
    Section 15. Notice of Nonpayment. The Trustee shall notify the 
Grantor and the appropriate EPA Regional Administrator, by certified 
mail within 10 days following the expiration of the 30-day period after 
the anniversary of the establishment of the Trust, if no payment is 
received from the Grantor during that period. After the pay-in period is 
completed, the Trustee shall not be required to send a notice of 
nonpayment.
    Section 16. Amendment of Agreement. This Agreement may be amended by 
an instrument in writing executed by the Grantor, the Trustee, and the 
appropriate EPA Regional Administrator, or by the Trustee and the 
appropriate EPA Regional Administrator if the Grantor ceases to exist.
    Section 17. Irrevocability and Termination. Subject to the right of 
the parties to amend this Agreement as provided in Section 16, this 
Trust shall be irrevocable and shall continue until terminated at the 
written agreement of the Grantor, the Trustee, and the EPA Regional 
Administrator, or by the Trustee and the EPA Regional Administrator if 
the Grantor ceases to exist. Upon termination of the Trust, all 
remaining trust property, less final trust administration expenses, 
shall be delivered to the Grantor.
    Section 18. Immunity and Indemnification. The Trustee shall not 
incur personal liability of any nature in connection with any act or 
omission, made in good faith, in the administration of this Trust, or in 
carrying out any directions by the Grantor or the EPA Regional 
Administrator issued in accordance with this Agreement. The Trustee 
shall be indemnified and saved harmless by the Grantor or from the Trust 
Fund, or both, from and against any personal liability to which the 
Trustee may be subjected by reason of any act or conduct in its official 
capacity, including all expenses reasonably incurred in its defense in 
the event the Grantor fails to provide such defense.
    Section 19. Choice of Law. This Agreement shall be administered, 
construed, and enforced according to the laws of the State of [insert 
name of State].
    Section 20. Interpretation. As used in this Agreement, words in the 
singular include the plural and words in the plural include the 
singular. The descriptive headings for each Section of this Agreement 
shall not affect the interpretation or the legal efficacy of this 
Agreement.
    In Witness Whereof the parties have caused this Agreement to be 
executed by their respective officers duly authorized and their 
corporate seals to be hereunto affixed and attested as of the date first 
above written. The parties below certify that the wording of this 
Agreement is identical to the wording specified in 40 CFR 144.70(a)(1) 
as such regulations were constituted on the date first above written.

[Signature of Grantor]
    By [Title]
Attest:

                                 [Title]

                                 [Seal]

[Signature of Trustee]
    By
Attest:

[[Page 853]]

                                 [Title]

                                 [Seal]

    (2) The following is an example of the certification of 
acknowledgment which must accompany the trust agreement for a trust fund 
as specified in Sec.  144.63(a). State requirements may differ on the 
proper content of this acknowledgment.

State of________________________________________________________________
County of_______________________________________________________________

    On this [date], before me personally came [owner or operator] to me 
known, who, being by me duly sworn, did depose and say that she/he 
resides at [address], that she/he is [title] of [corporation], the 
corporation described in and which executed the above instrument; that 
she/he knows the seal of said corporation; that the seal affixed to such 
instrument is such corporate seal; that it was so affixed by order to 
the Board of Directors of said corporation, and that she/he signed her/
his name thereto by like order.

[Signature of Notary Public]

    (b) A surety bond guaranteeing payment into a trust fund, as 
specified in Sec.  144.63 of this chapter, must be worded as follows, 
except that instructions in brackets are to be replaced with the 
relevant information and the brackets deleted:

                        Financial Guarantee Bond

Dated bond executed:____________________________________________________
Effective date:_________________________________________________________
    Principal: [legal name and business address of owner or operator].
    Type of organization: [insert ``individual,'' ``joint venture,'' 
``partnership,'' or ``corporation''].
State of incorporation:_________________________________________________
    Surety(ies): [name(s) and business address(es)].
    EPA Identification Number, name, address, and plugging and 
abandonment amount(s) for each facility guaranteed by this bond 
[indicate plugging and abandonment amounts separately]: ___
    Total penal sum of bond: $___
    Surety's bond number: ___
    Know All Persons By These Presents, That we, the Principal and 
Surity(ies) hereto are firmly bound to the U.S. Environmental Protection 
Agency (hereinafter called EPA), in the above penal sum for the payment 
of which we bind ourselves, our heirs, executors, administrators, 
successors, and assigns jointly and severally; provided that, where the 
Surety(ies) are corporations acting as co-surties, we, the Sureties, 
bind ourselves in such sum ``jointly and severally'' only for the 
purpose of allowing a joint action or actions against any or all of us, 
and for all other purposes each Surety binds itself, jointly and 
severally with the Principal, for the payment of such sum only as is set 
forth opposite the name of such Surety, but if no limit of liability is 
indicated, the limit of liability shall be the full amount of the penal 
sum.
    Whereas said Principal is required, under the Underground Injection 
Control Regulations (UIC), to have a permit or comply with requirements 
to operate under rule in order to own or operate each injection well 
identified above, and
    Whereas said Principal is required to provide financial assurance 
for plugging and abandonment as a condition of the permit or provisions 
to operate under rule, and
    Whereas said Principal shall establish a standby trust fund as is 
required when a surety bond is used to provide such financial assurance;
    Now, therefore, the conditions of the obligation are such that if 
the Principal shall faithfully, before the beginning of plugging and 
abandonment of each injection well identified above, fund the standby 
trust fund in the amount(s) identified above for the injection well,
    Or if the Principal shall fund the standby trust fund in such 
amount(s) within 15 days after an order to begin plugging and 
abandonment is issued by an EPA Regional Administrator or a U.S. 
district court or other court of competent jurisdiction,
    Or, if the Principal shall provide alternate financial assurance, as 
specified in subpart F of 40 CFR part 144, as applicable, and obtain the 
EPA Regional Administrator's written approval of such assurance, within 
90 days after the date of notice of cancellation is received by both the 
Principal and the EPA Regional Administrator(s) from the Surety(ies), 
then this obligation shall be null and void, otherwise it is to remain 
in full force and effect.
    The Surety(ies) shall become liable on this bond obligation only 
when the Principal has failed to fulfill the conditions described above. 
Upon notification by an EPA Regional Administrator that the Principal 
has failed to perform as guaranteed by this bond, the Surety(ies) shall 
place funds in the amount guaranteed for the injection well(s) into the 
standby trust funds as directed by the EPA Regional Administrator.
    The liability of the Surety(ies) shall not be discharged by any 
payment or succession of payments hereunder, unless and until such 
payment or payments shall amount in the aggregate to the penal sum of 
the bond, but in no event shall the obligation of the Surety(ies) 
hereunder exceed the amount of said penal sum.
    The Surety(ies) may cancel the bond by sending notice of 
cancellation by certified

[[Page 854]]

mail to the Principal and to the EPA Regional Administrator(s) for the 
Region(s) in which the injection well(s) is (are) located, provided, 
however, that that cancellation shall not occur during the 120 days 
beginning on the date of receipt of the notice of cancellation by both 
the Principal and the EPA Regional Administrator(s), as evidenced by the 
return receipts.
    The Principal may terminate this bond by sending written notice to 
the Surety(ies), provided, however, that no such notice shall become 
effective until the Surety(ies) receive(s) written authorization for 
termination of the bond by the EPA Regional Administrator(s) of the 
Region(s) in which the bonded facility(ies) is (are) located.
    [The following paragraph is an optional rider that may be included 
but is not required.]
    Principal and Surety(ies) hereby agree to adjust the penal sum of 
the bond yearly so that it guarantees a new plugging and abandonment 
amount, provided that the penal sum does not increase by more than 20 
percent in any one year, and no decrease in the penal sum takes place 
without the written permission of the EPA Regional Administrator(s).
    In Witness Whereof, the Principal and Surety(ies) have executed this 
Financial Guarantee Bond and have affixed their seals on the date set 
forth above.
    The persons whose signatures appear below hereby certify that they 
are authorized to execute this surety bond on behalf of the Principal 
and Surety(ies) and that the wording of this surety bond is identical to 
the wording specified in 40 CFR 144.70(b) as such regulations were 
constituted on the date this bond was executed.

                                Principal

[Signature(s)]
[Name(s)]
[Title(s)]
[Corporate seal]

                          Corporate Surety(ies)

[Name and address]
    State of incorporation: ___.
    Liability limit: $___.
[Signature(s)]
[Name(s) and title(s)]
[Corporate seal]
[For every co-surety, provide signature(s), corporate seal, and other 
information in the same manner as for Surety above.]
    Bond premium: $___.

    (c) A surety bond guaranteeing performance of plugging and 
abandonment, as specified in Sec.  144.63(c), must be worded as follows, 
except that the instructions in brackets are to be replaced with the 
relevant information and the brackets deleted:

                            Performance Bond

    Date bond executed: ___.
    Effective date: ___.
    Principal: [legal name and business address of owner or operator].
    Type of organization: [insert ``individual,'' ``joint venture,'' 
``partnership,'' or ``corporation''].
    State of incorporation: ___.
    Surety(ies): [name(s) and business address(es)]
________________________________________________________________________
    EPA Identification Number, name, address, and plugging and 
abandonment amounts(s) for each injection well guaranteed by this bond 
[indicate plugging and abandonment amounts for each well]:
________________________________________________________________________
    Total penal sum of bond: $___.
    Surety's bond number: ___.
    Know All Persons By These Presents, That We, the Principal and 
Surety(ies) hereto are firmly bound to the U.S. Environmental Protection 
Agency [hereinafter called EPA], in the above penal sum for the payment 
of which we bind ourselves, our heirs, executors, administrators, 
successors, and assigns jointly and severally; provided that, where the 
Surety(ies) are corporations acting as co-sureties, we, the Sureties, 
bind ourselves in such sum ``jointly and severally'' only for the 
purpose of allowing a joint action or actions against any or all of us, 
and for all other purposes each Surety binds itself, jointly and 
severally with the Principal, for the payment of such sum only as is set 
forth opposite the name of such Surety, but if no limit of liability is 
indicated, the limit of liability shall be the full amount of the penal 
sum.
    Whereas said Principal is required, under the Undergound Injection 
Control Regulations, as amended, to have a permit or comply with 
provisions to operate under rule for each injection well identified 
above, and
    Whereas said Principal is required to provide financial assurance 
for plugging and abandonment as a condition of the permit or approval to 
operate under rule, and
    Whereas said Principal shall establish a standby trust fund as is 
required when a surety bond is used to provide such financial assurance;
    Now, Therefore, the conditions of this obligation are such that if 
the Principal shall faithfully perform plugging and abandonment, 
whenever required to do so, of each injection well for which this bond 
guarantees plugging and abandonment, in accordance with the plugging and 
abandonment plan and other rquirements of the permit or provisions for 
operating under rule and other requirements of the permit or provisions 
for

[[Page 855]]

operating under rule as may be amended, pursuant to all applicable laws, 
statutes, rules and regulations, as such laws, statutes, rules, and 
regulations may be amended,
    Or, if the Principal shall provide alternate financial assurance as 
specified in subpart F of 40 CFR part 144, and obtain the EPA Regional 
Administrator's written approval of such assurance, within 90 days after 
the date of notice of cancellation is received by both the Principal and 
the EPA Regional Administrator(s) from the Surety(ies), then this 
obligation shall be null and void, otherwise it is to remain in full 
force and effect.
    The Surety(ies) shall become liable on this bond obligation only 
when the Principal has failed to fulfill the conditions described above.
    Upon notification by an EPA Regional Administrator that the 
Principal has been found in violation of the plugging and abandonment 
requirements of 40 CFR part 144, for an injection well which this bond 
guarantees performances of plugging and abandonment, the Surety(ies) 
shall either perform plugging and abandonment in accordance with the 
plugging and abandonment plan and other permit requirements or 
provisions for operating under rule and other requirements or place the 
amount for plugging and abandonment into a standby trust fund as 
directed by the EPA Regional Administrator.
    Upon notification by an EPA Regional Administrator that the 
Principal has failed to provide alternate financial assurance as 
specified in subpart F of 40 CFR part 144, and obtain written approval 
of such assurance from the EPA Regional Administrator(s) during the 90 
days following receipt by both the Principal and the EPA Regional 
Administrator(s) of a notice of cancellation of the bond, the 
Surety(ies) shall place funds in the amount guaranteed for the injection 
well(s) into the standby trust fund as directed by the EPA Regional 
Administrator.
    The surety(ies) hereby waive(s) notification of amendments to 
plugging and abandonment plans, permits, applicable laws, statutes, 
rules, and regulations and agrees that no such amendment shall in any 
way alleviate its (their) obligation on this bond.
    The liability of the Surety(ies) shall not be discharged by any 
payment or succession of payments hereunder, unless and until such 
payment or payments shall amount in the aggregate to the penal sum of 
the bond, but in no event shall the obligation of the Surety(ies) 
hereunder exceed the amount of said penal sum.
    The Surety(ies) may cancel the bond by sending notice by certified 
mail to the owner or operator and to the EPA Regional Administrator(s) 
for the Region(s) in which the injection well(s) is (are) located, 
provided, however, that cancellation shall not occur during the 120 days 
beginning on the date of receipt of the notice of cancellation by both 
the Principal and the EPA Regional Administrator(s), as evidenced by the 
return receipts.
    The principal may terminate this bond by sending written notice to 
the Surety(ies), provided, however, that no such notice shall become 
effective until the Surety(ies) receive(s) written authorization for 
termination of the bond by the EPA Regional Administrator(s) of the EPA 
Region(s) in which the bonded injection well(s) is (are) located.
    [The following paragraph is an optional rider that may be included 
but is not required.]
    Principal and Surety(ies) hereby agree to adjust the penal sum of 
the bond yearly so that it guarantees a new plugging and abandonment 
amount, provided that the penal sum does not increase by more than 20 
percent in any one year, and no decrease in the penal sum takes place 
without the written permission of the EPA Regional Administrator(s).
    In Witness Whereof, The Principal and Surety(ies) have executed this 
Performance Bond and have affixed their seals on the date set forth 
above.
    The persons whose signatures appear below hereby certify that they 
are authorized to execute this surety bond on behalf of the Principal 
and Surety(ies) and that the wording on this surety bond is identical to 
the wording specified in 40 CFR 144.70(c) as such regulation was 
constituted on the date this bond was executed.
    Principal.
[Signature(s)]
[Name(s)]
[Title(s)]
[Corporate seal]
[Corporate Surety(ies)]
[Name and address]
    State of incorporation:
________________________________________________________________________
    Liability limit: $___.
[Signature(s)]
[Name(s) and title(s)]
    Corporate seal:
[For every co-surety, provide signature(s), corporate seal, and other 
information in the same manner as for Surety above.]
    Bond premium: $___.

    (d) A letter of credit, as specified in Sec.  144.63(d) of this 
chapter, must be worded as follows, except that instructions in brackets 
are to be replaced with the relevant information and the brackets 
deleted:

                  Irrevocable Standby Letter of Credit

    Regional Administrator(s)
Region(s)_______________________________________________________________
    U.S. Environmental Protection Agency.
    Dear Sir or Madam:
    We hereby establish our Irrevocable Standby Letter of Credit No. ___ 
in your favor,

[[Page 856]]

at the request and for the account of [owner's or operator's name and 
address] up to the aggregate amount of [in words] U.S. dollars $___, 
available upon presentation [insert, if more than one Regional 
Administrator is a beneficiary, ``by any one of you''] of
    (1) Your sight draft, bearing reference to this letter of credit No. 
___, and
    (2) Your signed statement reading as follows: ``I certify that the 
amount of the draft is payable pursuant to regulations issued under 
authority of the Safe Drinking Water Act.''
    This letter of credit is effective as of [date] and shall expire on 
[date at least 1 year later], but such expiration date shall be 
automatically extended for a period of [at least 1 year] on [date] and 
on each successive expiration date, unless, at least 120 days before the 
current expiration date, we notify both you and [owner's or operator's 
name] by certified mail that we have decided not to extend this letter 
of credit beyond the current expiration date. In the event you are so 
notified, any unused portion of the credit shall be available upon 
presentation of your sight draft for 120 days after the date of receipt 
by both you and [owner's or operator's name], as shown on the signed 
return receipts.
    Whenever this letter of credit is drawn on under and in compliance 
with the terms of this credit, we shall duly honor such draft upon 
presentation to us, and we shall deposit the amount of the draft 
directly into the standby trust fund of [owner's or operator's name] in 
accordance with your instructions.
    We certify that the wording of this letter of credit is identical to 
the wording specified in 40 CFR 144.70(d) as such regulations were 
constituted on the date shown immediately below.
[Signature(s) and title(s) of official(s) of issuing institution]
[Date]
    This credit is subject to [insert ``the most recent edition of the 
Uniform Customs and Practice for Documentary Credits, published and 
copyrighted by the International Chamber of Commerce,'' or ``the Uniform 
Commercial Code''].

    (e) A certificate of insurance, as specified in Sec.  144.63(e) of 
this chapter, must be worded as follows, except that instructions in 
brackets are to be replaced with the relevant information and the 
brackets deleted:

    Certificate of Insurance for Plugging and Abandonment
    Name and Address of Insurer (herein called the ``insurer''):
________________________________________________________________________
    Name and Address of Insurer (herein called the ``insurer''):
________________________________________________________________________
    Injection Wells covered: [list for each well: The EPA Identification 
Number, name, address, and the amount of insurance for plugging and 
abandonment (these amounts for all injection wells covered must total 
the face amount shown below).]
Face Amount:____________________________________________________________
Policy Number:__________________________________________________________
Effective Date:_________________________________________________________
    The insurer hereby certifies that it has issued to the Insured the 
policy of insurance identified above to provide financial assurance for 
plugging and abandonment for the injection wells identified above. The 
Insurer further warrants that such policy conforms in all respects with 
the requirements of 40 CFR 144.63(e), as applicable and as such 
regulations were constituted on the date shown immediately below. It is 
agreed that any provision of the policy inconsistent with such 
regulations is hereby amended to eliminate such inconsistency.
    Whenever requested by the EPA Regional Administrator(s) of the U.S. 
Environmental Protection Agency, the Insurer agrees to furnish to the 
EPA Regional Administrator(s) a duplicate original of the policy listed 
above, including all endorsements thereon.
    I hereby certify that the wording of this certificate is identical 
to the wording specified in 40 CFR 144.70(e) as such regulations were 
constituted on the date shown immediately below.
[Authorized signature of Insurer]
[Name of person signing]
[Title of person signing]
    [Signature of witness or notary:]
________________________________________________________________________
[Date]

    (f) A letter from the chief financial officer, as specified in Sec.  
144.63(f) of this chapter, must be worded as follows, except that 
instructions in brackets are to be replaced with the relevant 
information and the brackets deleted:

                   Letter From Chief Financial Officer

    [Address to Regional Administrator of every Region in which 
injection wells for which financial responsibility is to be demonstrated 
through the financial test are located.]
    I am the chief financial officer of [name and address of firm.] This 
letter is in support of this firm's use of the financial test to 
demonstrate financial assurance, as specified in subpart F of 40 CFR 
part 144.
    [Fill out the following four paragraphs regarding injection wells 
and associated cost estimates. If your firm has no injection wells that 
belong in a particular paragraph, write ``None'' in the space indicated. 
For each injection well, include its EPA Identification

[[Page 857]]

Number, name, address, and current plugging and abandonment cost 
estimate.]
    1. This firm is the owner or operator of the following injection 
wells for which financial assurance for plugging and abandonment is 
demonstrated through the financial test specified in subpart F of 40 CFR 
part 144. The current plugging and abandonment cost estimate covered by 
the test is shown for each injection well: ___.
    2. This firm guarantees, through the corporate guarantee specified 
in subpart F of 40 CFR part 144, the plugging and abandonment of the 
following injection wells owned or operated by subsidaries of this firm. 
The current cost estimate for plugging and abandonment so guaranteed is 
shown for each injection well: ___.
    3. In States where EPA is not administering the financial 
requirements of subpart F of 40 CFR part 144, this firm, as owner or 
operator or guarantor, is demonstrating financial assurance for the 
plugging and abandoment of the following injection wells through the use 
of a test equivalent or substantially equivalent to the financial test 
specified in subpart F of 40 CFR part 144. The current plugging and 
abandonment cost estimate covered by such a test is shown for each 
injection well: ___.
    4. This firm is the owner or operator of the following injection 
wells for which financial assurance for plugging and abandonment is not 
demonstrated either to EPA or a State through the financial test or any 
other financial assurance mechanism specified in subpart F of 40 CFR 
part 144 or equivalent or substantially equivalent State mechanisms. The 
current plugging and abandonment cost estimate not covered by such 
financial assurance is shown for each injection well: ___.
    This firm [insert ``is required'' or ``is not required''] to file a 
Form 10K with the Securities and Exchange Commission (SEC) for the 
latest fiscal year.
    The fiscal year of this firm ends on [month, day]. The figures for 
the following items marked with an asterisk are derived from this firm's 
independently audited, year-end financial statements for the latest 
completed fiscal year, ended [date].
    [Fill in Alternative I if the criteria of paragraph (f)(1)(i) of 
Sec.  144.63 of this chapter are used. Fill in Alternative II if the 
criteria of paragraph (f)(1)(ii) of Sec.  144.63 of this chapter are 
used.]

                              Alternative I
1. (a) Current plugging and abandonment cost...............        $____
  (b) Sum of the company's financial responsibilities under
   40 CFR Parts 264 and 265, Subpart H, currently met using
   the financial test or corporate guarantee...............
  (c) Total of lines a and b...............................
*2. Total liabilities [if any portion of the plugging and
 abandonment cost is included in total liabilities, you may
 deduct the amount of that portion from this line and add
 that amount to lines 3 and 4].............................
*3. Tangible net worth.....................................
*4. Net worth..............................................
*5. Current assets.........................................
*6. Current liabilities....................................
*7. Net working capital [line 5 minus line 6]..............
*8. The sum of net income plus depreciation, depletion and
 amortization..............................................
*9. Total assets in U.S. (required only if less than 90% of
 firm's assets are located in U.S.)........................
------------------------------------------------------------------------
                                                     Yes              No
------------------------------------------------------------------------
10. Is line 3 at least $10 million?.............
11. Is line 3 at least 6 times line 1(c)?.......
12. Is line 7 at least 6 times line 1(c)?.......
*13. Are at least 90% of firm's assets located
 in the U.S.? If not, complete line 14..........
14. Is line 9 at least 6 times line 1(c)?.......
15. Is line 2 divided by line 4 less than 2.0?..
16. Is line 8 divided by line 2 greater than
 0.1?...........................................
17. Is line 5 divided by line 6 greater than      .........  ...........
 1.5?...........................................
 


                             Alternative II
1. (a) Current plugging and abandonment cost...............        $____
  (b) Sum of the company's financial responsibilities under
   40 CFR Parts 264 and 265, Subpart H, currently met using
   the financial test or corporate guarantee...............
  (c) Total of lines a and b...............................
2. Current bond rating of most recent issuance of this firm
 and name of rating service................................
3. Date of issuance of bond................................
4. Date of maturity of bond................................
*5. Tangible net worth [if any portion of the plugging and
 abandonment cost estimate is included in ``total
 liabilities'' on your firm's financial statements, you may
 add the amount of that portion to this line]..............
*6. Total assets in U.S. (required only if less than 90% of
 firm's assets are located in U.S.)........................
------------------------------------------------------------------------
                                                        Yes           No
------------------------------------------------------------------------
7. Is line 5 at least $10 million?..............
8. Is line 5 at least 6 times line 1(c)?........
*9. Are at least 90% of the firm's assets
 located in the U.S.? If not, complete line 10..
10. Is line 6 at least 6 times line 1(c)?.......  .........  ...........
 

    I hereby certify that the wording of this letter is identical to the 
wording specified in 40 CFR 144.70(f) as such regulations were 
constituted on the date shown immediately below.
[Signature]
[Name]
[Title]

[[Page 858]]

[Date]

    (g) A corporate guarantee as specified in Sec.  144.63(e) must be 
worded as follows except that instructions in brackets are to be 
replaced with the relevant information and the bracketed material 
deleted:

                 Guarantee for Plugging and Abandonment

    Guarantee made this __ day of ___, 19__, by [name of guaranteeing 
entity], a business corporation organized under the laws of the State of 
____, herein referred to as guarantor, to the United States 
Environmental Protection Agency (EPA), obligee, on behalf of our 
subsidiary [owner or operator] of [business address].
Recitals
    1. Guarantor meets or exceeds the financial test criteria and agrees 
to comply with the reporting requirements for guarantors as specified in 
40 CFR 144.63(e).
    2. [Owner or operator] owns or operates the following Class I 
hazardous waste injection well covered by this guarantee: [List for each 
facility: EPA Identification Number, name, and address. Indicate for 
each whether guarantee is for closure, post-closure care, or both.]
    3. ``Plugging and abandonment plan'' as used below refers to the 
plans maintained as required by 40 CFR part 144 for the plugging and 
abandonment of injection wells as identified above.
    4. For value received from [owner or operator], guarantor guarantees 
to EPA that in the event that [owner or operator] fails to perform 
[``plugging and abandonment''] of the above facility(ies) in accordance 
with the plugging and abandonment plan and other requirements when 
required to do so, the guarantor will do so or fund a trust fund as 
specified in 40 CFR 144.63 in the name of [owner or operator] in the 
amount of the adjusted plugging and abandonment cost estimates prepared 
as specified in 40 CFR 144.62.
    5. Guarantor agrees that, if at the end of any fiscal year before 
termination of this guarantee, the guarantor fails to meet the financial 
test criteria, guarantor will send within 90 days, by certified mail, 
notice to the EPA Regional Administrator(s) for the Region(s) in which 
the facility(ies) is (are) located and to [owner or operator] that he 
intends to provide alternate financial assurance as specified in 40 CFR 
144.63 in the name of [owner or operator]. Within 30 days after sending 
such notice, the guarantor will establish such financial assurance if 
[owner or operator] has not done so.
    6. The guarantor agrees to notify the Regional Administrator, by 
certified mail, of a voluntary or involuntary case under Title 11, U.S. 
Code, naming guarantor as debtor, within 10 days after its commencement.
    7. Guarantor agrees that within 30 days after being notified by an 
EPA Regional Administrator of a determination that guarantor no longer 
meets the financial test criteria or that he is disallowed from 
continuing as a guarantor of plugging and adandonment, he will establish 
alternate financial assurance, as specified in 40 CFR 144.63, in the 
name of [owner or operator] if [owner or operator] has not done so.
    8. Guarantor agrees to remain bound under this guarantee 
notwithstanding any or all of the following: amendment or modification 
of the plugging and abandonment plan, the extension or reduction of the 
time of performance of plugging and abandonment or any other 
modification or alteration of an obligation of [owner or operator] 
pursuant to 40 CFR part 144.
    9. Guarantor agrees to remain bound under this guarantee for so long 
as [owner or operator] must comply with the applicable financial 
assurance requirements of 40 CFR part 144 for the above-listed 
facilities, except that guarantor may cancel this guarantee by sending 
notice by certified mail, to the EPA Regional Administrator(s) for the 
Region(s) in which the facility(ies) is (are) located and to [owner or 
operator], such cancellation to become effective no earlier than 120 
days after actual receipt of such notice by both EPA and [owner or 
operator] as evidenced by the return receipts.
    10. Guarantor agrees that if [owner or operator] fails to provide 
alternate financial assurance and obtain written approval of such 
assurance from the EPA Regional Administrator(s) within 90 days after a 
notice of cancellation by the guarantor is received by both the EPA 
Regional Administrator(s) and [owner or operator], guarantor will 
provide alternate financial assurance as specified in 40 CFR 144.63 in 
the name of [owner or operator].
    11. Guarantor expressly waives notice of acceptance of this 
guarantee by the EPA or by [owner or operator]. Guarantor also expressly 
waives notice of amendments or modifications of the plugging and 
abandonment plan.
    I hereby certify that the wording of this guarantee is identical to 
the wording specified in 40 CFR 144.70(f).
    Effective date: ___.
[Name of guarantor]
[Authorized signature for guarantor]
[Type name of person signing]
[Title of person signing]
    Signature of witness or notary: ___

[48 FR 14189, Apr. 1, 1983, as amended at 59 FR 29959, June 10, 1994]

[[Page 859]]



  Subpart G_Requirements for Owners and Operators of Class V Injection 
                                  Wells

    Source: 64 FR 68566, Dec. 7, 1999, unless otherwise noted.



Sec.  144.79  General.

    This subpart tells you what requirements apply if you own or operate 
a Class V injection well. You may also be required to follow additional 
requirements listed in the rest of this part. Where they may apply, 
these other requirements are referenced rather than repeated. The 
requirements described in this subpart and elsewhere in this part are to 
protect underground sources of drinking water and are part of the 
Underground Injection Control (UIC) Program established under the Safe 
Drinking Water Act. This subpart is written in a special format to make 
it easier to understand the regulatory requirements. Like other EPA 
regulations, it establishes enforceable legal requirements.

                  Definition of Class V Injection Wells



Sec.  144.80  What is a Class V injection well?

    As described in Sec.  144.6, injection wells are classified as 
follows:
    (a) Class I. (1) Wells used by generators of hazardous waste or 
owners or operators of hazardous waste management facilities to inject 
hazardous waste beneath the lowermost formation containing, within one-
quarter mile of the well bore, an underground source of drinking water.
    (2) Other industrial and municipal disposal wells which inject 
fluids beneath the lowermost formation containing, within one quarter 
mile of the well bore, an underground source of drinking water;
    (3) Radioactive waste disposal wells which inject fluids below the 
lowermost formation containing an underground source of drinking water 
within one quarter mile of the well bore.
    (b) Class II. Wells which inject fluids:
    (1) Which are brought to the surface in connection with natural gas 
storage operations, or conventional oil or natural gas production and 
may be commingled with waste waters from gas plants which are an 
integral part of production operations, unless those waters are 
classified as a hazardous waste at the time of injection.
    (2) For enhanced recovery of oil or natural gas; and
    (3) For storage of hydrocarbons which are liquid at standard 
temperature and pressure.
    (c) Class III. Wells which inject fluids for extraction of minerals 
including:
    (1) Mining of sulfur by the Frasch process;
    (2) In situ production of uranium or other metals; this category 
includes only in situ production from ore bodies which have not been 
conventionally mined. Solution mining of conventional mines such as 
stopes leaching is included in Class V.
    (3) Solution mining of salts or potash.
    (d) Class IV. (1) Wells used by generators of hazardous waste or of 
radioactive waste, by owners and operators of hazardous waste management 
facilities, or by owners or operators of radioactive waste disposal 
sites to dispose of hazardous waste or radioactive waste into a 
formation which within one quarter (\1/4\) mile of the well contains an 
underground source of drinking water.
    (2) Wells used by generators of hazardous waste or of radioactive 
waste, by owners and operators of hazardous waste management facilities, 
or by owners or operators of radioactive waste disposal sites to dispose 
of hazardous waste or radioactive waste above a formation which within 
one quarter (\1/4\) mile of the well contains an underground source of 
drinking water.
    (3) Wells used by generators of hazardous waste or owners or 
operators of hazardous waste management facilities to dispose of 
hazardous waste, which cannot be classified under paragraph (a)(1) or 
(d)(1) and (2) of this section (e.g., wells used to dispose of hazardous 
waste into or above a formation which contains an aquifer which has been 
exempted pursuant to 40 CFR 146.04).
    (e) Class V. Injection wells not included in Class I, II, III, IV or 
VI. Typically, Class V wells are shallow wells

[[Page 860]]

used to place a variety of fluids directly below the land surface. 
However, if the fluids you place in the ground qualify as a hazardous 
waste under the Resource Conservation and Recovery Act (RCRA), your well 
is either a Class I or Class IV well, not a Class V well. Examples of 
Class V wells are described in Sec.  144.81.
    (f) Class VI. Wells used for geologic sequestration of carbon 
dioxide beneath the lowermost formation containing a USDW, except those 
wells that are experimental in nature; or, wells used for geologic 
sequestration of carbon dioxide that have been granted a waiver of the 
injection depth requirements pursuant to requirements at Sec.  146.95 of 
this chapter; or, wells used for geologic sequestration of carbon 
dioxide that have received an expansion to the areal extent of a 
existing Class II enhanced oil recovery or enhanced gas recovery aquifer 
exemption pursuant to Sec.  146.4 of this chapter and Sec.  144.7(d).

[64 FR 68566, Dec. 7, 1999, as amended at 75 FR 77290, Dec. 10, 2010]



Sec.  144.81  Does this subpart apply to me?

    This subpart applies to you if you own or operate a Class V well, 
for example:
    (1) Air conditioning return flow wells used to return to the supply 
aquifer the water used for heating or cooling in a heat pump;
    (2) Large capacity cesspools including multiple dwelling, community 
or regional cesspools, or other devices that receive sanitary wastes, 
containing human excreta, which have an open bottom and sometimes 
perforated sides. The UIC requirements do not apply to single family 
residential cesspools nor to non-residential cesspools which receive 
solely sanitary waste and have the capacity to serve fewer than 20 
persons a day.
    (3) Cooling water return flow wells used to inject water previously 
used for cooling;
    (4) Drainage wells used to drain surface fluids, primarily storm 
runoff, into a subsurface formation;
    (5) Dry wells used for the injection of wastes into a subsurface 
formation;
    (6) Recharge wells used to replenish the water in an aquifer;
    (7) Salt water intrusion barrier wells used to inject water into a 
fresh aquifer to prevent the intrusion of salt water into the fresh 
water;
    (8) Sand backfill and other backfill wells used to inject a mixture 
of water and sand, mill tailings or other solids into mined out portions 
of subsurface mines whether what is injected is a radioactive waste or 
not.
    (9) Septic system wells used to inject the waste or effluent from a 
multiple dwelling, business establishment, community or regional 
business establishment septic tank. The UIC requirements do not apply to 
single family residential septic system wells, nor to non-residential 
septic system wells which are used solely for the disposal of sanitary 
waste and have the capacity to serve fewer than 20 persons a day.
    (10) Subsidence control wells (not used for the purpose of oil or 
natural gas production) used to inject fluids into a non-oil or gas 
producing zone to reduce or eliminate subsidence associated with the 
overdraft of fresh water;
    (11) Injection wells associated with the recovery of geothermal 
energy for heating, aquaculture and production of electric power;
    (12) Wells used for solution mining of conventional mines such as 
stopes leaching;
    (13) Wells used to inject spent brine into the same formation from 
which it was withdrawn after extraction of halogens or their salts;
    (14) Injection wells used in experimental technologies.
    (15) Injection wells used for in situ recovery of lignite, coal, tar 
sands, and oil shale.
    (16) Motor vehicle waste disposal wells that receive or have 
received fluids from vehicular repair or maintenance activities, such as 
an auto body repair shop, automotive repair shop, new and used car 
dealership, specialty repair shop (e.g., transmission and muffler repair 
shop), or any facility that does any vehicular repair work. Fluids 
disposed in these wells may contain organic and inorganic chemicals in 
concentrations that exceed the maximum contaminant levels (MCLs) 
established by the primary drinking water regulations (see 40 CFR part 
141).

[[Page 861]]

These fluids also may include waste petroleum products and may contain 
contaminants, such as heavy metals and volatile organic compounds, which 
pose risks to human health.

[64 FR 68566, Dec. 7, 1999, as amended at 67 FR 39593, June 7, 2002]

              Requirements for All Class V Injection Wells



Sec.  144.82  What must I do to protect underground sources of drinking water?

    If you own or operate any type of Class V well, the regulations 
below require that you cannot allow movement of fluid into USDWs that 
might cause endangerment, you must comply with other Federal UIC 
requirements in 40 CFR parts 144 through 147, and you must comply with 
any other measures required by your State or EPA Regional Office UIC 
Program to protect USDWs, and you must properly close your well when you 
are through using it. You also must submit basic information about your 
well, as described in Sec.  144.83.
    (a) Prohibition of fluid movement. (1) As described in Sec.  
144.12(a), your injection activity cannot allow the movement of fluid 
containing any contaminant into USDWs, if the presence of that 
contaminant may cause a violation of the primary drinking water 
standards under 40 CFR part 141, other health based standards, or may 
otherwise adversely affect the health of persons. This prohibition 
applies to your well construction, operation, maintenance, conversion, 
plugging, closure, or any other injection activity.
    (2) If the Director of the UIC Program in your State or EPA Region 
learns that your injection activity may endanger USDWs, he or she may 
require you to close your well, require you to get a permit, or require 
other actions listed in Sec.  144.12(c), (d), or (e).
    (b) Closure requirements. You must close the well in a manner that 
complies with the above prohibition of fluid movement. Also, you must 
dispose or otherwise manage any soil, gravel, sludge, liquids, or other 
materials removed from or adjacent to your well in accordance with all 
applicable Federal, State, and local regulations and requirements.
    (c) Other requirements in Parts 144 through 147. Beyond this 
subpart, you are subject to other UIC Program requirements in 40 CFR 
parts 144 through 147. While most of the relevant requirements are 
repeated or referenced in this subpart for convenience, you need to read 
these other parts to understand the entire UIC Program.
    (d) Other State or EPA requirements. 40 CFR parts 144 through 147 
define minimum Federal UIC requirements. EPA Regional Offices 
administering the UIC Program have the flexibility to establish 
additional or more stringent requirements based on the authorities in 
parts 144 through 147, if believed to be necessary to protect USDWs. 
States can have their own authorities to establish additional or more 
stringent requirements if needed to protect USDWs. You must comply with 
these additional requirements, if any exist in your area. Contact the 
UIC Program Director in your State or EPA Region to learn more.



Sec.  144.83  Do I need to notify anyone about my Class V injection well?

    Yes, you need to provide basic ``inventory information'' about your 
well to the UIC Director, if you haven't already. You also need to 
provide any additional information that your UIC Program Director 
requests in accordance with the provisions of the UIC regulations.
    (a) Inventory requirements. Unless you know you have already 
satisfied the inventory requirements in Sec.  144.26 that were in effect 
prior to the issuance of this Subpart G, you must give your UIC Program 
Director certain information about yourself and your injection 
operation.

    Note: This information is requested on national form ``Inventory of 
Injection Wells,'' OMB No. 2040-0042.

    (1) The requirements differ depending on your well status and 
location, as described in the following table:

[[Page 862]]



------------------------------------------------------------------------
                              And you're in one of
                                 these locations
                              (``Primacy'' States,
                              where the State runs
                                 the Class V UIC
                               Program): Alabama,
                                    Arkansas,        Or you're in one of
                                 Commonwealth of       these locations
                                Northern Mariana          (``Direct
                                    Islands,         Implementation'' or
                                  Connecticut,       DI Programs, where
                               Delaware, Florida,   EPA runs the Class V
                                 Georgia, Guam,         UIC Program):
                                Idaho, Illinois,      Alaska, American
                               Kansas, Louisiana,      Samoa, Arizona,
                                Maine, Maryland,         California,
    If your well is . . .        Massachusetts,       Colorado, Hawaii,
                                  Mississippi,         Indiana, Iowa,
                               Missouri, Nebraska,   Kentucky, Michigan,
                                   Nevada, New       Minnesota, Montana,
                                 Hampshire, New           New York,
                               Jersey, New Mexico,   Pennsylvania, South
                                 North Carolina,     Dakota, Tennessee,
                               North Dakota, Ohio,    Virginia, Virgin
                                Oklahoma, Oregon,   Islands, Washington,
                               Puerto Rico, Rhode     DC, or any Indian
                                  Island, South            Country
                                Carolina, Texas,
                                 Utah, Vermont,
                                Washington, West
                              Virginia, Wisconsin,
                                   or Wyoming
------------------------------------------------------------------------
(i) New (prior to             . . . then you must   . . . then you must
 construction of your well).   contact your State    submit the
                               UIC Program to        inventory
                               determine what you    information
                               must submit and by    described in (a)(2)
                               when..                of this section
                                                     prior to
                                                     constructing your
                                                     well.
------------------------------------------------------------------------
(ii) Existing (construction   . . . then you must   . . . then you must
 underway or completed).       contact your State    cease injection and
                               UIC Program to        submit the
                               determine what you    inventory
                               must submit and by    information. You
                               when..                may resume
                                                     injection 90 days
                                                     after you submit
                                                     the information
                                                     unless the UIC
                                                     Program Director
                                                     notifies you that
                                                     injection may not
                                                     resume or may
                                                     resume sooner.
------------------------------------------------------------------------

    (2) If your well is in a Primacy State or a DI Program State, here 
is the information you must submit:
    (i) No matter what type of Class V well you own or operate, you must 
submit at least the following information for each Class V well: 
facility name and location; name and address of legal contact; ownership 
of facility; nature and type of injection well(s); and operating status 
of injection well(s).
    (ii) Additional information. If you are in a Direct Implementation 
State and you own or operate a well listed below you must also provide 
the information listed in paragraph (a) (2) (iii) as follows:
    (A) Sand or other backfill wells (40 CFR 144.81(8) and 146.5(e)(8) 
of this chapter);
    (B) Geothermal energy recovery wells (40 CFR 144.81(11) and 146.5 
(e)(12) of this chapter);
    (C) Brine return flow wells (40 CFR 144.81(13) and 146.5 (e)(14) of 
this chapter);
    (D) Wells used in experimental technology (40 CFR 144.81(14) and 
146.5 (e)(15) of this chapter);
    (E) Municipal and industrial disposal wells other than Class I; and
    (F) Any other Class V wells at the discretion of the Regional 
Administrator.
    (iii) You must provide a list of all wells owned or operated along 
with the following information for each well. (A single description of 
wells at a single facility with substantially the same characteristics 
is acceptable).
    (A) Location of each well or project given by Township, Range, 
Section, and Quarter-Section, or by latitude and longitude to the 
nearest second, according to the conventional practice in your State;
    (B) Date of completion of each well;
    (C) Identification and depth of the underground formation(s) into 
which each well is injecting;
    (D) Total depth of each well;
    (E) Construction narrative and schematic (both plan view and cross-
sectional drawings);
    (F) Nature of the injected fluids;
    (G) Average and maximum injection pressure at the wellhead;
    (H) Average and maximum injection rate; and
    (I) Date of the last inspection.
    (3) Regardless of whether your well is in a Primacy State or DI 
Program you are responsible for knowing about, understanding, and 
complying with these inventory requirements.
    (b) Information in response to requests. If you are in one of the DI 
Programs listed in the table above, the UIC Program Director may require 
you to submit other information believed necessary to protect 
underground sources of drinking water.
    (1) Such information requirements may include, but are not limited 
to:

[[Page 863]]

    (i) Perform ground water monitoring and periodically submit your 
monitoring results;
    (ii) Analyze the fluids you inject and periodically submit the 
results of your analyses;
    (iii) Describe the geologic layers through which and into which you 
are injecting; and
    (iv) Conduct other analyses and submit other information, if needed 
to protect underground sources of drinking water.
    (2) If the Director requires this other information, he or she will 
request it from you in writing, along with a brief statement on why the 
information is required. This written notification also will tell you 
when to submit the information.
    (3) You are prohibited from using your injection well if you fail to 
comply with the written request within the time frame specified. You can 
start injecting again only if you receive a permit.



Sec.  144.84  Do I need to get a permit?

    No, unless you fall within an exception described below:
    (a) General authorization by rule. With certain exceptions listed in 
paragraph (b) of this section, your Class V injection activity is 
``authorized by rule,'' meaning you have to comply with all the 
requirements of this subpart and the rest of the UIC Program but you 
don't have to get an individual permit. Well authorization expires once 
you have properly closed your well, as described in Sec.  144.82(b).
    (b) Circumstances in which permits or other actions are required. If 
you fit into one of the categories listed below, your Class V well is no 
longer authorized by rule. This means that you have to either get a 
permit or close your injection well. You can find out by contacting the 
UIC Program Director in your State or EPA Region if this is the case. 
Subpart D of this part tells you how to apply for a permit and describes 
other aspects of the permitting process. Subpart E of this part outlines 
some of the requirements that apply to you if you get a permit.
    (1) You fail to comply with the prohibition of fluid movement 
standard in Sec.  144.12(a) and described in Sec.  144.82(a) (in which 
case, you have to get a permit, close your well, and/or comply with 
other conditions determined by the UIC Program Director in your State or 
EPA Region);
    (2) You own or operate a Class V large-capacity cesspool (in which 
case, you must close your well as specified in the additional 
requirements below) or a Class V motor vehicle waste disposal well in a 
ground water protection area or sensitive ground water area (in which 
case, you must either close your well or get a permit as specified in 
the additional requirements in this subsection). New motor vehicle waste 
disposal wells and new cesspools are prohibited as of April 5, 2000;
    (3) You are specifically required by the UIC Program Director in 
your State or EPA Region to get a permit (in which case, rule 
authorization expires upon the effective date of the permit issued, or 
you are prohibited from injecting into your well upon:
    (i) Failure to submit a permit application in a timely manner as 
specified in a notice from the Director; or
    (ii) Upon the effective date of permit denial);
    (4) You have failed to submit inventory information to your UIC 
Program Director, as described in Sec.  144.83(a) (in which case, you 
are prohibited from injecting into your well until you comply with the 
inventory requirements); or
    (5) If you are in a DI State and you received a request from your 
UIC Program Director for additional information under Sec.  144.83(b), 
and have failed to comply with the request in a timely manner (in which 
case, you are prohibited from injecting into your well until you get a 
permit).

 Additional Requirements for Class V Large-Capacity Cesspools and Motor 
                      Vehicle Waste Disposal Wells



Sec.  144.85  Do these additional requirements apply to me?

    (a) Large-capacity cesspools. The additional requirements apply to 
all new and existing large-capacity cesspools regardless of their 
location. If you are using a septic system for these type of wastes you 
are not subject to the additional requirements in this subpart.

[[Page 864]]

    (b) Motor vehicle waste disposal wells existing on April 5, 2000. If 
you have a Class V motor vehicle waste disposal well these requirements 
apply to you if your well is located in a ground water protection area 
or other sensitive ground water area that is identified by your State or 
EPA Region. If your State or EPA Region fails to identify ground water 
protection areas and/or other sensitive ground water areas these 
requirements apply to all Class V motor vehicle wells in the State.
    (c) New motor vehicle waste disposal wells. The additional 
requirements apply to all new motor vehicle waste disposal wells as of 
April 5, 2000.



Sec.  144.86  What are the definitions I need to know?

    (a) State Drinking Water Source Assessment and Protection Program. 
This is a new approach to protecting drinking water sources, specified 
in the 1996 Amendments to the Safe Drinking Water Act at Section 1453. 
States must prepare and submit for EPA approval a program that sets out 
how States will conduct local assessments, including: delineating the 
boundaries of areas providing source waters for public water systems; 
identifying significant potential sources of contaminants in such areas; 
and determining the susceptibility of public water systems in the 
delineated areas to the inventoried sources of contamination.
    (b) Complete local source water assessment for ground water 
protection areas. When EPA has approved a State's Drinking Water Source 
Assessment and Protection Program, States will begin to conduct local 
assessments for each public water system in their State. For the 
purposes of this rule, local assessments for community water systems and 
non-transient non-community systems are complete when four requirements 
are met: First, a State must delineate the boundaries of the assessment 
area for community and non-transient non-community water systems. 
Second, the State must identify significant potential sources of 
contamination in these delineated areas. Third, the State must 
``determine the susceptibility of community and non-transient non-
community water systems in the delineated area to such contaminants.'' 
Lastly, each State will develop its own plan for making the completed 
assessments available to the public.
    (c) Ground water protection area. A ground water protection area is 
a geographic area near and/or surrounding community and non-transient 
non-community water systems that use ground water as a source of 
drinking water. These areas receive priority for the protection of 
drinking water supplies and States are required to delineate and assess 
these areas under section 1453 of the Safe Drinking Water Act. The 
additional requirements in Sec.  144.88 apply to you if your Class V 
motor vehicle waste disposal well is in a ground water protection area 
for either a community water system or a non-transient non-community 
water system, in many States, these areas will be the same as Wellhead 
Protection Areas that have been or will be delineated as defined in 
section 1428 of the SDWA.
    (d) Community water system. A community water system is a public 
water system that serves at least 15 service connections used by year-
round residents or regularly serves at least 25 year-round residents.
    (e) Non-transient non-community water system. A public water system 
that is not a community water system and that regularly serves at least 
25 of the same people over six months a year. These may include systems 
that provide water to schools, day care centers, government/military 
installations, manufacturers, hospitals or nursing homes, office 
buildings, and other facilities.
    (f) Delineation. Once a State's Drinking Water Source Assessment and 
Protection Program is approved, the States will begin delineating their 
local assessment areas. Delineation is the first step in the assessment 
process in which the boundaries of ground water protection areas are 
identified.
    (g) Other sensitive ground water areas. States may also identify 
other areas in the State in addition to ground water protection areas 
that are critical to protecting underground sources of drinking water 
from contamination. These other sensitive ground water areas may include 
areas such as areas

[[Page 865]]

overlying sole-source aquifers; highly productive aquifers supplying 
private wells; continuous and highly productive aquifers at points 
distant from public water supply wells; areas where water supply 
aquifers are recharged; karst aquifers that discharge to surface 
reservoirs serving as public water supplies; vulnerable or sensitive 
hydrogeologic settings, such as glacial outwash deposits, eolian sands, 
and fractured volcanic rock; and areas of special concern selected based 
on a combination of factors, such as hydrogeologic sensitivity, depth to 
ground water, significance as a drinking water source, and prevailing 
land-use practices.



Sec.  144.87  How does the identification of ground water protection areas 
and other sensitive ground water areas affect me?

    (a) You are subject to these new requirements if you own or operate 
an existing motor vehicle well and you are located in a ground water 
protection area or an other sensitive ground water area. If your State 
or EPA Region fails to identify these areas within the specified time 
frames these requirements apply to all existing motor vehicle waste 
disposal wells within your State.
    (b) Ground water protection areas. (1) For the purpose of this 
subpart, States are required to complete all local source water 
assessments for ground water protection areas by January 1, 2004. Once a 
local assessment for a ground water protection area is complete every 
existing motor vehicle waste disposal well owner in that ground water 
protection area has one year to close the well or receive a permit. If a 
State fails to complete all local assessments for ground water 
protection areas by January 1, 2004, the following may occur:
    (i) The new requirements in this subpart will apply to all existing 
motor vehicle waste disposal wells in the State and owners and operators 
of motor vehicle waste disposal wells located outside of completed 
assessments for ground water protection areas must close their well or 
receive a permit by January 1, 2005.
    (ii) EPA may grant a State an extension for up to one year from the 
January 1, 2004 deadline if the State is making reasonable progress in 
completing the source water assessments for ground water protection 
areas. States must apply for the extension by June 1, 2003. If a State 
fails to complete the assessments for the remaining ground water 
protection areas by the extended date the rule requirements will apply 
to all motor vehicle waste disposal wells in the State and owners and 
operators of motor vehicle waste disposal wells located outside of 
ground water protection areas with completed assessments must close 
their well or receive a permit by January 1, 2006.
    (2) The UIC Program Director may extend the compliance deadline for 
specific motor vehicle waste disposal wells for up to one year if the 
most efficient compliance option for the well is connection to a 
sanitary sewer or installation of new treatment technology.
    (c) Other sensitive ground water areas. States may also delineate 
other sensitive ground water areas by January 1, 2004. Existing motor 
vehicle waste disposal well owners and operators within other sensitive 
ground water areas have until January 1, 2007 to receive a permit or 
close the well. If a State or EPA Region fails to identify these 
additional sensitive ground water areas by January 1, 2004, the new 
requirements of this rule will apply to all motor vehicle waste disposal 
wells in the State effective January 1, 2007 unless they are subject to 
a different compliance date pursuant to paragraph (b) of this section. 
Again, EPA may extend the January 1, 2004 deadline for up to one year 
for States to delineate other sensitive ground water areas if the State 
is making reasonable progress in identifying the sensitive areas. States 
must apply for this extension by June 1, 2003. If a State has been 
granted an extension, existing motor vehicle waste disposal well owners 
and operators within the sensitive ground water areas have until January 
1, 2008 to close the well or receive a permit, unless they are subject 
to a different compliance date pursuant to paragraph (b) of this 
section. If a State has been granted an extension and fails to delineate 
sensitive areas by the extended date, the rule requirements will apply 
to all motor vehicle waste disposal

[[Page 866]]

wells in the State and owners and operators have until January 1, 2008 
to close the well or receive a permit, unless they are subject to a 
different compliance date pursuant to paragraph (b) of this section.
    (d) How to find out if your well is in a ground water protection 
area or sensitive ground water area. States are required to make their 
local source water assessments widely available to the public through a 
variety of methods after the assessments are complete. You can find out 
if your Class V well is in a ground water protection area by contacting 
the State agency responsible for the State Drinking Water Source 
Assessment and Protection Program in your area. You may call the Safe 
Drinking Water Hotline at 1-800-426-4791 to find out who to call in your 
State for this information. The State office responsible for 
implementing the Drinking Water Source Assessment and Protection Program 
makes the final and official determination of boundaries for ground 
water protection areas. Because States that choose to delineate other 
sensitive ground water areas are also required to make the information 
on these areas accessible to the public, they may do so in a manner 
similar to the process used by the States in publicizing the EPA 
approved Drinking Water Source Assessment and Protection Program. You 
can find out if your Class V well is in an other sensitive ground water 
area by contacting the State or Federal agency responsible for the 
Underground Injection Control Program. You may call the Safe Drinking 
Water Hotline at 1-800-426-4791 to find out who to call for information.
    (e) Changes in the status of the EPA approved state drinking water 
source assessment and protection program. After January 1, 2004 your 
State may assess a ground water protection area for ground water 
supplying a new community water system or a new non-transient non-
community water system that includes your Class V injection well. Also, 
your State may officially re-delineate the boundaries of a previously 
delineated ground water protection area to include additional areas that 
includes your motor vehicle waste disposal well. This would make the 
additional regulations apply to you if your motor vehicle waste disposal 
well is in such an area. The additional regulations start applying to 
you one year after the State completes the local assessment for the 
ground water protection area for the new drinking water system or the 
new re-delineated area. The UIC Program Director responsible for your 
area may extend this deadline for up to one year if the most efficient 
compliance option for the well is connection to a sanitary sewer or 
installation of new treatment technology.
    (f) What happens if my state doesn't designate other sensitive 
ground water areas? If your State or EPA Region elects not to delineate 
the additional sensitive ground water areas, the additional regulations 
apply to you regardless of the location of your well by January 1, 2007, 
or January 2008 if an extension has been granted as explained in 
paragraph (c) of this section, except for wells in ground water 
protection areas which are subject to different compliance deadlines 
explained in paragraph (b) of this section.
    (g) [Reserved]
    (h) Application of requirements outside of ground water protection 
areas and sensitive ground water areas. EPA expects and strongly 
encourages States to use existing authorities in the UIC program to take 
whatever measures are needed to ensure Class V wells are not endangering 
USDWs in any other areas outside of delineated ground water protection 
areas and sensitive ground water areas. Such measures could include, if 
believed to be necessary by a UIC Program Director, applying the 
additional requirements below to other areas and/or other types of Class 
V wells. Therefore, the Director may apply the additional requirements 
to you, even if you are not located in the areas listed in paragraph (a) 
of this section.



Sec.  144.88  What are the additional requirements?

    The additional requirements are specified in the following tables:

[[Page 867]]



    (a) Table 1--Additional Requirements for Large-Capacity Cesspools
                                Statewide
 [See Sec.   144.85 to determine if these additional requirements apply
                                 to you]
------------------------------------------------------------------------
         Well Status               Requirement            Deadline
------------------------------------------------------------------------
If your cesspool is. . .      Then you. . ........  By. . .
------------------------------------------------------------------------
(1) Existing (operational or  (i) Must close the    April 5, 2005.
 under construction by April   well.
 5, 2000).
                              (ii) Must notify the  At least 30 days
                               UIC Program           prior to closure.
                               Director (both
                               Primacy States and
                               Direct
                               Implementation
                               States) of your
                               intent to close the
                               well..
                              Note: This
                               information is
                               requested on
                               national form
                               ``Preclosure
                               Notification for
                               Closure of
                               Injection Wells,''.
(2) New or converted          Are prohibited......  April 5, 2000.
 (construction not started
 before April 5, 2000).
------------------------------------------------------------------------


  (b) Table 2--Additional Requirements for Motor Vehicle Waste Disposal
                                  Wells
 [See Sec.   144.85 to determine if these additional requirements apply
                                 to you]
------------------------------------------------------------------------
         Well status               Requirement            Deadline
------------------------------------------------------------------------
If your motor vehicle waste   Then. . ............  By. . .
 disposal well is
------------------------------------------------------------------------
(1) Existing (operational or  (i) If your well is   Within 1 year of the
 under construction by April   in a ground water     completion of your
 5, 2000).                     protection area,      local source water
                               you must close the    assessment; your
                               well or obtain a      UIC Program
                               permit.               Director may extend
                                                     the closure
                                                     deadline, but not
                                                     the permit
                                                     application
                                                     deadline, for up to
                                                     one year if the
                                                     most efficient
                                                     compliance option
                                                     is connection to a
                                                     sanitary sewer or
                                                     installation of new
                                                     treatment
                                                     technology.
                             -------------------------------------------
                              (ii) If your well is  By January 1, 2007;
                               in an other           your UIC Program
                               sensitive ground      Director may extend
                               water area, you       the closure
                               must close the well   deadline, but not
                               or obtain a permit.   the permit
                                                     application
                                                     deadline, for up to
                                                     one year if the
                                                     most efficient
                                                     compliance option
                                                     is connection to a
                                                     sanitary sewer or
                                                     installation of new
                                                     treatment
                                                     technology.
                             -------------------------------------------
                              (iii) If you plan to  The date you submit
                               seek a waiver from    your permit
                               the ban and apply     application.
                               for a permit, you
                               must meet MCLs at
                               the point of
                               injection while
                               your permit
                               application is
                               under review, if
                               you choose to keep
                               operating your well.
                             -------------------------------------------
                              (iv) If you receive   The date(s)
                               a permit, you must    specified in your
                               comply with all       permit.
                               permit conditions,
                               if you choose to
                               keep operating your
                               well, including
                               requirements to
                               meet MCLs and other
                               health based
                               standards at the
                               point of injection,
                               follow best
                               management
                               practices, and
                               monitor your
                               injectate and
                               sludge quality.
                             -------------------------------------------
                              (v) If your well is   January 1, 2005
                               in a State which      unless your State
                               has not completed     obtains an
                               all their local       extension as
                               assessments by        described in 144.87
                               January 1, 2004 or    (b) in which case
                               by the extended       your deadline is
                               date if your State    January 1, 2006;
                               has obtained an       your UIC Program
                               extension as          Director may extend
                               described in          the closure
                               144.87, and you are   deadline, but not
                               outside an area       the permit
                               with a completed      application
                               assessment you must   deadline, for up to
                               close the well or     one year if the
                               obtain a permit.      most efficient
                                                     compliance option
                                                     is connection to a
                                                     sanitary sewer or
                                                     installation of new
                                                     treatment
                                                     technology.
                             -------------------------------------------

[[Page 868]]

 
                              (vi) If your well is  January 1, 2007
                               in a State that has   unless your State
                               not delineated        obtains an
                               other sensitive       extension as
                               ground water areas    described in
                               by January 1, 2004    144.87(c) in which
                               and you are outside   case your deadline
                               of an area with a     is January 2008.
                               completed
                               assessment you must
                               close the well or
                               obtain a permit
                               regardless of your
                               location.
                             -------------------------------------------
                              (vii) If you plan to  At least 30 days
                               close your well,      prior to closure.
                               you must notify the
                               UIC Program
                               Director of your
                               intent to close the
                               well (this includes
                               closing your well
                               prior to
                               conversion).
                              Note: This
                               information is
                               requested on
                               national form
                               ``Preclosure
                               Notification for
                               Closure of
                               Injection Wells''..
------------------------------------------------------------------------
(2) New or converted          Are prohibited......  April 5, 2000.
 (construction not started
 before April 5, 2000).
------------------------------------------------------------------------


[64 FR 68566, Dec. 7, 1999; 64 FR 70316, Dec. 16, 1999]



Sec.  144.89  How do I close my Class V injection well?

    The following describes the requirements for closing your Class V 
injection well.
    (a) Closure. (1) Prior to closing a Class V large-capacity cesspool 
or motor vehicle waste disposal well, you must plug or otherwise close 
the well in a manner that complies with the prohibition of fluid 
movement standard in Sec.  144.12 and summarized in Sec.  144.82(a). If 
the UIC Program Director in your State or EPA Region has any additional 
or more specific closure standards, you have to meet those standards 
too. You also must dispose or otherwise manage any soil, gravel, sludge, 
liquids, or other materials removed from or adjacent to your well in 
accordance with all applicable Federal, State, and local regulations and 
requirements, as in Sec.  144.82(b).
    (2) Closure does not mean that you need to cease operations at your 
facility, only that you need to close your well. A number of 
alternatives are available for disposing of waste fluids. Examples of 
alternatives that may be available to motor vehicle stations include: 
recycling and reusing wastewater as much as possible; collecting and 
recycling petroleum-based fluids, coolants, and battery acids drained 
from vehicles; washing parts in a self-contained, recirculating solvent 
sink, with spent solvents being recovered and replaced by the supplier; 
using absorbents to clean up minor leaks and spills, and placing the 
used materials in approved waste containers and disposing of them 
properly; using a wet vacuum or mop to pick up accumulated rain or snow 
melt, and if allowed, connecting floor drains to a municipal sewer 
system or holding tank, and if allowed, disposing of the holding tank 
contents through a publicly owned treatment works. You should check with 
the publicly owned treatment works you might use to see if they would 
accept your wastes. Alternatives that may be available to owners and 
operators of a large-capacity cesspool include: conversion to a septic 
system; connection to sewer; and installation of an on-site treatment 
unit.
    (b) Conversions. In limited cases, the UIC Director may authorize 
the conversion (reclassification) of a motor vehicle waste disposal well 
to another type of Class V well. Motor vehicle wells may only be 
converted if: all motor vehicle fluids are segregated by

[[Page 869]]

physical barriers and are not allowed to enter the well; and, injection 
of motor vehicle waste is unlikely based on a facility's compliance 
history and records showing proper waste disposal. The use of a semi-
permanent plug as the means to segregate waste is not sufficient to 
convert a motor vehicle waste disposal well to another type of Class V 
well.

[64 FR 68566, Dec. 7, 1999; 65 FR 5024, Feb. 2, 2000]



PART 145_STATE UIC PROGRAM REQUIREMENTS--Table of Contents



                 Subpart A_General Program Requirements

Sec.
145.1 Purpose and scope.
145.2 Definitions.

                Subpart B_Requirements for State Programs

145.11 Requirements for permitting.
145.12 Requirements for compliance evaluation programs.
145.13 Requirements for enforcement authority.
145.14 Sharing of information.

                   Subpart C_State Program Submissions

145.21 General requirements for program approvals.
145.22 Elements of a program submission.
145.23 Program description.
145.24 Attorney General's statement.
145.25 Memorandum of Agreement with the Regional Administrator.

           Subpart D_Program Approval, Revision and Withdrawal

145.31 Approval process.
145.32 Procedures for revision of State programs.
145.33 Criteria for withdrawal of State programs.
145.34 Procedures for withdrawal of State programs.

                         Subpart E_Indian Tribes

145.52 Requirements for Tribal eligibility.
145.56 Request by an Indian Tribe for a determination of eligibility.
145.58 Procedure for processing an Indian Tribe's application.

    Authority: 42 U.S.C. 300f et seq.

    Source: 48 FR 14202, Apr. 1, 1983, unless otherwise noted.



                 Subpart A_General Program Requirements



Sec.  145.1  Purpose and scope.

    (a) This part specifies the procedures EPA will follow in approving, 
revising, and withdrawing State programs under section 1422 (underground 
injection control--UIC) of SDWA, and includes the elements which must be 
part of submissions to EPA for program approval and the substantive 
provisions which must be present in State programs for them to be 
approved.
    (b) State submissions for program approval must be made in 
accordance with the procedures set out in subpart C. This includes 
developing and submitting to EPA a program description (Sec.  145.23), 
an Attorney General's Statement (Sec.  145.24), and a Memorandum of 
Agreement with the Regional Administrator (Sec.  145.25).
    (c) The substantive provisions which must be included in State 
programs to obtain approval include requirements for permitting, 
compliance evaluation, enforcement, public participation, and sharing of 
information. The requirements are found in subpart B. Many of the 
requirements for State programs are made applicable to States by cross-
referencing other EPA regulations. In particular, many of the provisions 
of parts 144 and 124 are made applicable to States by the references 
contained in Sec.  145.11.
    (d) Upon submission of a complete program, EPA will conduct a public 
hearing, if interest is shown, and determine whether to approve or 
disapprove the program taking into consideration the requirements of 
this part, the Safe Drinking Water Act and any comments received.
    (e) Upon approval of a State program, the Administrator shall 
suspend the issuance of Federal permits for those activities subject to 
the approved State program.
    (f) Any State program approved by the Administrator shall at all 
times be conducted in accordance with the requirements of this part.
    (g) Nothing in this part precludes a State from:
    (1) Adopting or enforcing requirements which are more stringent or

[[Page 870]]

more extensive than those required under this part;
    (2) Operating a program with a greater scope of coverage than that 
required under this part. Where an approved State program has a greater 
scope of coverage than required by Federal law the additional coverage 
is not part of the federally approved program.
    (h) Section 1451 of the SDWA authorizes the Administrator to 
delegate primary enforcement responsibility for the Underground 
Injection Control Program to eligible Indian Tribes. An Indian Tribe 
must establish its eligibility to be treated as a State before it is 
eligible to apply for Underground Injection Control grants and primary 
enforcement responsibility. All requirements of parts 124, 144, 145, and 
146 that apply to States with UIC primary enforcement responsibility 
also apply to Indian Tribes except where specifically noted.
    (i) States seeking primary enforcement responsibility for Class VI 
wells must submit a primacy application in accordance with subpart C of 
this part and meet all requirements of this part. States may apply for 
primary enforcement responsibility for Class VI wells independently of 
other injection well classes.

[48 FR 14202, Apr. 1, 1983, as amended at 53 FR 37412, Sept. 26, 1988; 
59 FR 64345, Dec. 14, 1994; 75 FR 77290, Dec. 10, 2010]



Sec.  145.2  Definitions.

    The definitions of part 144 apply to all subparts of this part.



                Subpart B_Requirements for State Programs



Sec.  145.11  Requirements for permitting.

    (a) All State programs under this part must have legal authority to 
implement each of the following provisions and must be administered in 
conformance with each; except that States are not precluded from 
omitting or modifying any provisions to impose more stringent 
requirements.
    (1) Section 144.5(b)-(Confidential information);
    (2) Section 144.6--(Classification of injection wells);
    (3) Section 144.7--(Identification of underground sources of 
drinking water and exempted aquifers);
    (4) Section 144.8--(Noncompliance reporting);
    (5) Section 144.11--(Prohibition of unauthorized injection);
    (6) Section 144.12--(Prohibition of movement of fluids into 
underground sources of drinking water);
    (7) Section 144.13--(Elimination of Class IV wells);
    (8) Section 144.14--(Requirements for wells managing hazardous 
waste);
    (9) Sections 144.21-144.26--(Authorization by rule);
    (10) Section 144.31--(Application for a permit);
    (11) Section 144.32--(Signatories);
    (12) Section 144.33--(Area Permits);
    (13) Section 144.34--(Emergency permits);
    (14) Section 144.35--(Effect of permit);
    (15) Section 144.36--(Duration);
    (16) Section 144.38--(Permit transfer);
    (17) Section 144.39--(Permit modification);
    (18) Section 144.40--(Permit termination);
    (19) Section 144.51--(Applicable permit conditions);
    (20) Section 144.52--(Establishing permit conditions);
    (21) Section 144.53(a)--(Schedule of compliance);
    (22) Section 144.54--(Monitoring requirements);
    (23) Section 144.55--(Corrective Action);
    (24) Section 124.3(a)--(Application for a permit);
    (25) Section 124.5 (a), (c), (d), and (f)--(Modification of 
permits);
    (26) Section 124.6 (a), (c), (d), and (e)--(Draft Permit);
    (27) Section 124.8--(Fact sheets);
    (28) Section 124.10 (a)(1)(ii), (a)(1)(iii), (a)(1)(v), (b), (c), 
(d), and (e)--(Public notice);
    (29) Section 124.11--(Public comments and requests for hearings);
    (30) Section 124.12(a)--(Public hearings);
    (31) Section 124.17 (a) and (c)--(Response to comments);
    (32) Section 144.88--(What are the additional requirements?); and

[[Page 871]]

    (33) For states that wish to receive electronic documents, 40 CFR 
part 3--(Electronic reporting).
    (b)(1) States need not implement provisions identical to the 
provisions listed in paragraphs (a)(1) through (a)(32) of this section. 
Implemented provisions must, however, establish requirements at least as 
stringent as the corresponding listed provisions. While States may 
impose more stringent requirements, they may not make one requirement 
more lenient as a tradeoff for making another requirement more 
stringent; for example, by requiring that public hearings be held prior 
to issuing any permit while reducing the amount of advance notice of 
such a hearing.
    (2) State programs may, if they have adequate legal authority, 
implement any of the provisions of parts 144 and 124. See, for example 
Sec.  144.37(d) (continuation of permits) and Sec.  124.4 (consolidation 
of permit processing).

[48 FR 14202, Apr. 1, 1983, as amended at 64 FR 78572, Dec. 7, 1999; 70 
FR 59888, Oct. 13, 2005]



Sec.  145.12  Requirements for compliance evaluation programs.

    (a) State programs shall have procedures for receipt, evaluation, 
retention and investigation for possible enforcement of all notices and 
reports required of permittees and other regulated persons (and for 
investigation for possible enforcement of failure to submit these 
notices and reports).
    (b) State programs shall have inspection and surveillance procedures 
to determine, independent of information supplied by regulated persons, 
compliance or noncompliance with applicable program requirements. The 
State shall maintain:
    (1) A program which is capable of making comprehensive surveys of 
all facilities and activities subject to the State Director's authority 
to identify persons subject to regulation who have failed to comply with 
permit application or other program requirements. Any compilation, 
index, or inventory of such facilities and activities shall be made 
available to the Regional Administrator upon request;
    (2) A program for periodic inspections of the facilities and 
activities subject to regulation. These inspections shall be conducted 
in a manner designed to:
    (i) Determine compliance or noncompliance with issued permit 
conditions and other program requirements;
    (ii) Verify the accuracy of information submitted by permittees and 
other regulated persons in reporting forms and other forms supplying 
monitoring data; and
    (iii) Verify the adequacy of sampling, monitoring, and other methods 
used by permittees and other regulated persons to develop that 
information;
    (3) A program for investigating information obtained regarding 
violations of applicable program and permit requirements; and
    (4) Procedures for receiving and ensuring proper consideration of 
information submitted by the public about violations. Public effort in 
reporting violations shall be encouraged and the State Director shall 
make available information on reporting procedures.
    (c) The State Director and State officers engaged in compliance 
evaluation shall have authority to enter any site or premises subject to 
regulation or in which records relevant to program operation are kept in 
order to copy any records, inspect, monitor or otherwise investigate 
compliance with permit conditions and other program requirements. States 
whose law requires a search warrant before entry conform with this 
requirement.
    (d) Investigatory inspections shall be conducted, samples shall be 
taken and other information shall be gathered in a manner [e.g., using 
proper ``chain of custody'' procedures] that will produce evidence 
admissible in an enforcement proceeding or in court.



Sec.  145.13  Requirements for enforcement authority.

    (a) Any State agency administering a program shall have available 
the following remedies for violations of State program requirements:
    (1) To restrain immediately and effectively any person by order or 
by suit in State court from engaging in any unauthorized activity which 
is endangering or causing damage to public health or environment;

    Note: This paragraph requires that States have a mechanism (e.g., an 
administrative

[[Page 872]]

cease and desist order or the ability to seek a temporary restraining 
order) to stop any unauthorized activity endangering public health or 
the environment.

    (2) To sue in courts of competent jurisdiction to enjoin any 
threatened or continuing violation of any program requirement, including 
permit conditions, without the necessity of a prior revocation of the 
permit;
    (3) To assess or sue to recover in court civil penalties and to seek 
criminal remedies, including fines, as follows:
    (i) For all wells except Class II wells, civil penalties shall be 
recoverable for any program violation in at least the amount of $2,500 
per day. For Class II wells, civil penalties shall be recoverable for 
any program violation in at least the amount of $1,000 per day.
    (ii) Criminal fines shall be recoverable in at least the amount of 
$5,000 per day against any person who willfully violates any program 
requirement, or for Class II wells, pipeline (production) severance 
shall be imposable against any person who willfully violates any program 
requirement.

    Note: In many States the State Director will be represented in State 
courts by the State Attorney General or other appropriate legal officer. 
Although the State Director need not appear in court actions he or she 
should have power to request that any of the above actions be brought.

    (b)(1) The maximum civil penalty or criminal fine (as provided in 
paragraph (a)(3) of this section) shall be assessable for each instance 
of violation and, if the violation is continuous, shall be assessable up 
to the maximum amount for each day of violation.
    (2) The burden of proof and degree of knowledge or intent required 
under State law for establishing violations under paragraph (a)(3) of 
this section, shall be no greater than the burden of proof or degree of 
knowledge or intent EPA must provide when it brings an action under the 
Safe Drinking Water Act.

    Note: For example, this requirement is not met if State law includes 
mental state as an element of proof for civil violations.

    (c) A civil penalty assessed, sought, or agreed upon by the State 
Director under paragraph (a)(3) of this section shall be appropriate to 
the violation.

    Note: To the extent that State judgments or settlements provide 
penalties in amounts which EPA believes to be substantially inadequate 
in comparison to the amounts which EPA would require under similar 
facts, EPA, when authorized by the applicable statute, may commence 
separate actions for penalties.
    In addition to the requirements of this paragraph, the State may 
have other enforcement remedies. The following enforcement options, 
while not mandatory, are highly recommended:
    Procedures for assessment by the State of the costs of 
investigations, inspections, or monitoring surveys which lead to the 
establishment of violations;
    Procedures which enable the State to assess or to sue any persons 
responsible for unauthorized activities for any expenses incurred by the 
State in removing, correcting, or terminating any adverse effects upon 
human health and the environment resulting from the unauthorized 
activity, or both; and
    Procedures for the administrative assessment of penalties by the 
Director.

    (d) Any State administering a program shall provide for public 
participation in the State enforcement process by providing either:
    (1) Authority which allows intervention as of right in any civil or 
administrative action to obtain remedies specified in paragraph (a) (1), 
(2) or (3) of this section by any citizen having an interest which is or 
may be adversely affected; or
    (2) Assurance that the State agency or enforcement authority will:
    (i) Investigate and provide written responses to all citizen 
complaints submitted pursuant to the procedures specified in Sec.  
145.12(b)(4);
    (ii) Not oppose intervention by any citizen when permissive 
intervention may be authorized by statute, rule, or regulation; and
    (iii) Publish notice of and provide at least 30 days for public 
comment on any proposed settlement of a State enforcement action.
    (e) To the extent that an Indian Tribe does not assert or is 
precluded from asserting criminal enforcement authority the 
Administrator will assume primary enforcement responsibility for 
criminal violations. The Memorandum of Agreement in Sec.  145.25 shall 
reflect a system where the Tribal agency will refer such violations to 
the

[[Page 873]]

Administrator in an appropriate and timely manner.

(Clean Water Act (33 U.S.C. 1251 et seq.), Safe Drinking Water Act (42 
U.S.C. 300f et seq.), Clean Air Act (42 U.S.C. 7401 et seq.), Resource 
Conservation and Recovery Act (42 U.S.C. 6901 et seq.))

[48 FR 14202, Apr. 1, 1983, as amended at 48 FR 39621, Sept. 1, 1983; 53 
FR 37412, Sept. 26, 1988]



Sec.  145.14  Sharing of information.

    (a) Any information obtained or used in the administration of a 
State program shall be available to EPA upon request without 
restriction. If the information has been submitted to the State under a 
claim of confidentiality, the State must submit that claim to EPA when 
providing information under this section. Any information obtained from 
a State and subject to a claim of confidentiality will be treated in 
accordance with the regulations in 40 CFR part 2. If EPA obtains from a 
State information that is not claimed to be confidential, EPA may make 
that information available to the public without further notice.
    (b) EPA shall furnish to States with approved programs the 
information in its files not submitted under a claim of confidentiality 
which the State needs to implement its approved program. EPA shall 
furnish to States with approved programs information submitted to EPA 
under a claim of confidentiality, which the State needs to implement its 
approved program, subject to the conditions in 40 CFR part 2.



                   Subpart C_State Program Submissions



Sec.  145.21  General requirements for program approvals.

    (a) States shall submit to the Administrator a proposed State UIC 
program complying with Sec.  145.22 of this part within 270 days of the 
date of promulgation of the UIC regulations on June 24, 1980. The 
administrator may, for good cause, extend the date for submission of a 
proposed State UIC program for up to an additional 270 days.
    (b) States shall submit to the Administrator 6 months after the date 
of promulgation of the UIC regulations a report describing the State's 
progress in developing a UIC program. If the Administrator extends the 
time for submission of a UIC program an additional 270 days, pursuant to 
Sec.  145.21(a), the State shall submit a second report six months after 
the first report is due. The Administrator may prescribe the manner and 
form of the report.
    (c) The requirements of Sec.  145.21 (a) and (b) shall not apply to 
Indian Tribes.
    (d) EPA will establish a UIC program in any State which does not 
comply with paragraph (a) of this section. EPA will continue to operate 
a UIC program in such a State until the State receives approval of a UIC 
program in accordance with the requirements of this part.

    Note: States which are authorized to administer the NPDES permit 
program under section 402 of CWA are encouraged to rely on existing 
statutory authority, to the extent possible, in developing a State UIC 
program. Section 402(b)(1)(D) of CWA requires that NPDES States have the 
authority ``to issue permits which control the disposal of pollutants 
into wells.'' In many instances, therefore, NPDES States will have 
existing statutory authority to regulate well disposal which satisfies 
the requirements of the UIC program. Note, however, that CWA excludes 
certain types of well injections from the definition of ``pollutant.'' 
If the State's statutory authority contains a similar exclusion it may 
need to be modified to qualify for UIC program approval.

    (e) If a State can demonstrate to EPA's satisfaction that there are 
no underground injections within the State for one or more classes of 
injection wells (other than Class IV wells) subject to SDWA and that 
such injections cannot legally occur in the State until the State has 
developed an approved program for those classes of injections, the State 
need not submit a program to regulate those injections and a partial 
program may be approved. The demonstration of legal prohibition shall be 
made by either explicitly banning new injections of the class not 
covered by the State program or providing a certification from the State 
Attorney General that such new injections cannot legally occur until the 
State has developed an approved program for that class. The State shall 
submit a program to regulate both those classes of injections for which 
a

[[Page 874]]

demonstration is not made and class IV wells.
    (f) When a State UIC program is fully approved by EPA to regulate 
all classes of injections, the State assumes primary enforcement 
authority under section 1422(b)(3) of SDWA. EPA retains primary 
enforcement responsibility whenever the State program is disapproved in 
whole or in part. States which have partially approved programs have 
authority to enforce any violation of the approved portion of their 
program. EPA retains authority to enforce violations of State 
underground injection control programs, except that, when a State has a 
fully approved program, EPA will not take enforcement actions without 
providing prior notice to the State and otherwise complying with section 
1423 of SDWA.
    (g) A State can assume primary enforcement responsibility for the 
UIC program, notwithstanding Sec.  145.21(3), when the State program is 
unable to regulate activities on Indian lands within the State. EPA will 
administer the program on Indian lands if the State does not seek this 
authority.
    (h) To establish a Federal UIC Class VI program in States not 
seeking full UIC primary enforcement responsibility approval, pursuant 
to the SDWA section 1422(c), States shall, by September 6, 2011, submit 
to the Administrator a new or revised State UIC program complying with 
Sec. Sec.  145.22 or 145.32 of this part. Beginning on September 6, 2011 
the requirements of subpart H of part 146 of this chapter will be 
applicable and enforceable by EPA in each State that has not received 
approval of a new Class VI program application under section 1422 of the 
Safe Drinking Water Act or a revision of its UIC program under section 
1422 of the Safe Drinking Water Act to incorporate subpart H of part 
146. Following September 6, 2011, EPA will publish a list of the States 
where subpart H of part 146 has become applicable.

[48 FR 14202, Apr. 1, 1983, as amended at 53 FR 37412, Sept. 26, 1988; 
75 FR 77290, Dec. 10, 2010]



Sec.  145.22  Elements of a program submission.

    (a) Any State that seeks to administer a program under this part 
shall submit to the Administrator at least three copies of a program 
submission. For Class VI programs, the entire submission can be sent 
electronically. The submission shall contain the following:
    (1) A letter from the Governor of the State requesting program 
approval;
    (2) A complete program description, as required by Sec.  145.23, 
describing how the State intends to carry out its responsibilities under 
this part;
    (3) An Attorney General's statement as required by Sec.  145.24;
    (4) A Memorandum of Agreement with the Regional Administrator as 
required by Sec.  145.25;
    (5) Copies of all applicable State statutes and regulations, 
including those governing State administrative procedures;
    (6) The showing required by Sec.  145.31(b) of the State's public 
participation activities prior to program submission.
    (b) Within 30 days of receipt by EPA of a State program submission, 
EPA will notify the State whether its submission is complete. If EPA 
finds that a State's submission is complete, the statutory review period 
(i.e., the period of time allotted for formal EPA review of a proposed 
State program under the Safe Drinking Water Act) shall be deemed to have 
begun on the date of receipt of the State's submission. If EPA finds 
that a State's submission is incomplete, the statutory review period 
shall not begin until all the necessary information is received by EPA.
    (c) If the State's submission is materially changed during the 
statutory review period, the statutory review period shall begin again 
upon receipt of the revised submission.
    (d) The State and EPA may extend the statutory review period by 
agreement.

[48 FR 14202, Apr. 1, 1983, as amended at 75 FR 77290, Dec. 10, 2010]



Sec.  145.23  Program description.

    Any State that seeks to administer a program under this part shall 
submit a description of the program it proposes to administer in lieu of 
the Federal program under State law or under an interstate compact. For 
Class VI programs, the entire submission can be sent electronically. The 
program description shall include:

[[Page 875]]

    (a) A description in narrative form of the scope, structure, 
coverage and processes of the State program.
    (b) A description (including organization charts) of the 
organization and structure of the State agency or agencies which will 
have responsibility for administering the program, including the 
information listed below. If more than one agency is responsible for 
administration of a program, each agency must have statewide 
jurisdiction over a class of activities. The responsibilities of each 
agency must be delineated, their procedures for coordination set forth, 
and an agency may be designated as a ``lead agency'' to facilitate 
communications between EPA and the State agencies having program 
responsibility. When the State proposes to administer a program of 
greater scope of coverage than is required by Federal law, the 
information provided under this paragraph shall indicate the resources 
dedicated to administering the Federally required portion of the 
program.
    (1) A description of the State agency staff who will carry out the 
State program, including the number, occupations, and general duties of 
the employees. The State need not submit complete job descriptions for 
every employee carrying out the State program.
    (2) An itemization of the estimated costs of establishing and 
administering the program for the first two years after approval, 
including cost of the personnel listed in paragraph (b)(1) of this 
section, cost of administrative support, and cost of technical support.
    (3) An itemization of the sources and amounts of funding, including 
an estimate of Federal grant money, available to the State Director for 
the first two years after approval to meet the costs listed in paragraph 
(b)(2) of this section, identifying any restrictions or limitations upon 
this funding.
    (c) A description of applicable State procedures, including 
permitting procedures and any State administrative or judicial review 
procedures.
    (d) Copies of the permit form(s), application form(s), reporting 
form(s), and manifest format the State intends to employ in its program. 
Forms used by States need not be identical to the forms used by EPA but 
should require the same basic information. The State need not provide 
copies of uniform national forms it intends to use but should note its 
intention to use such forms. For Class VI programs, submit copies of the 
current forms in use by the State, if any.
    (e) A complete description of the State's compliance tracking and 
enforcement program.
    (f) A State UIC program description shall also include:
    (1) A schedule for issuing permits within five years after program 
approval to all injection wells within the State which are required to 
have permits under this part and 40 CFR part 144. For Class VI programs, 
a schedule for issuing permits within two years after program approval;
    (2) The priorities (according to criteria set forth in Sec.  146.9 
of this chapter) for issuing permits, including the number of permits in 
each class of injection well which will be issued each year during the 
first five years of program operation. For Class VI programs, include 
the priorities for issuing permits and the number of permits which will 
be issued during the first two years of program operation;
    (3) A description of how the Director will implement the mechanical 
integrity testing requirements of Sec.  146.8 of this chapter, or, for 
Class VI wells, the mechanical integrity testing requirements of Sec.  
146.89 of this chapter, including the frequency of testing that will be 
required and the number of tests that will be reviewed by the Director 
each year;
    (4) A description of the procedure whereby the Director will notify 
owners or operators of injection wells of the requirement that they 
apply for and obtain a permit. The notification required by this 
paragraph shall require applications to be filed as soon as possible, 
but not later than four years after program approval for all injection 
wells requiring a permit. For Class VI programs approved before December 
10, 2011, a description of the procedure whereby the Director will 
notify owners or operators of any Class I wells previously permitted for 
the purpose of geologic sequestration or Class V experimental technology 
wells no longer being used for experimental purposes

[[Page 876]]

that will continue injection of carbon dioxide for the purpose of GS 
that they must apply for a Class VI permit pursuant to requirements at 
Sec.  146.81(c) within one year of December 10, 2011. For Class VI 
programs approved following December 10, 2011, a description of the 
procedure whereby the Director will notify owners or operators of any 
Class I wells previously permitted for the purpose of geologic 
sequestration or Class V experimental technology wells no longer being 
used for experimental purposes that will continue injection of carbon 
dioxide for the purpose of GS or Class VI wells previously permitted by 
EPA that they must apply for a Class VI permit pursuant to requirements 
at Sec.  146.81(c) within one year of Class VI program approval;
    (5) A description of any rule under which the Director proposes to 
authorize injections, including the text of the rule;
    (6) For any existing enhanced recovery and hydrocarbon storage wells 
which the Director proposes to authorize by rule, a description of the 
procedure for reviewing the wells for compliance with applicable 
monitoring, reporting, construction, and financial responsibility 
requirements of Sec. Sec.  144.51 and 144.52, and 40 CFR part 146;
    (7) A description of and schedule for the State's program to 
establish and maintain a current inventory of injection wells which must 
be permitted under State law;
    (8) Where the Director had designated underground sources of 
drinking water in accordance with Sec.  144.7(a), a description and 
identification of all such designated sources in the State;
    (9) A description of aquifers, or parts thereof, which the Director 
has identified under Sec.  144.7(b) as exempted aquifers, and a summary 
of supporting data. For Class VI programs only, States must incorporate 
information related to any EPA approved exemptions expanding the areal 
extent of existing aquifer exemptions for Class II enhanced oil recovery 
or enhanced gas recovery wells transitioning to Class VI injection for 
geologic sequestration pursuant to requirements at Sec. Sec.  146.4(d) 
and 144.7(d), including a summary of supporting data and the specific 
location of the aquifer exemption expansions. Other than expansions of 
the areal extent of Class II enhanced oil recovery or enhanced gas 
recovery well aquifer exemptions for Class VI injection, new aquifer 
exemptions shall not be issued for Class VI wells or injection 
activities;
    (10) A description of and schedule for the State's program to ban 
Class IV wells prohibited under Sec.  144.13; and
    (11) A description of and schedule for the State's program to 
establish an inventory of Class V wells and to assess the need for a 
program to regulate Class V wells.
    (12) For Class V programs only. A description of and a schedule for 
the State's plan to identify and delineate other sensitive ground water 
areas. States should consider geologic and hydrogeologic settings, 
ground water flow and occurrence, topographic and geographic features, 
depth to ground water, significance as a drinking water source, 
prevailing land use practices and any other existing information 
relating to the susceptibility of ground water to contamination from 
Class V injection wells when developing their plan. Within the schedule 
for the plan, States must commit to: completing all delineations of 
other sensitive ground water areas by no later than Jan. 1, 2004; making 
these delineation available to the public; implementing the Class V 
regulations, effective April 5, 2000, in these delineated areas by no 
later than January 1, 2007. Alternately, if a State chooses not to 
identify other sensitive ground water areas, the requirements for motor 
vehicle waste disposal wells would apply statewide by January 1, 2007.
    (13) For Class VI programs, a description of the procedure whereby 
the Director must notify, in writing, any States, Tribes, and 
Territories of any permit applications for geologic sequestration of 
carbon dioxide wherein the area of review crosses State, Tribal, or 
Territory boundaries, resulting in the need for trans-boundary 
coordination related to an injection operation.

[48 FR 14202, Apr. 1, 1983, as amended at 64 FR 68572, Dec. 7, 1999; 75 
FR 77290, Dec. 10, 2010]

[[Page 877]]



Sec.  145.24  Attorney General's statement.

    (a) Any State that seeks to administer a program under this part 
shall submit a statement from the State Attorney General (or the 
attorney for those State or interstate agencies which have independent 
legal counsel) that the laws of the State, or an interstate compact, 
provide adequate authority to carry out the program described under 
Sec.  145.23 and to meet the requirements of this part. This statement 
shall include citations to the specific statutes, administrative 
regulations, and, where appropriate, judicial decisions which 
demonstrate adequate authority. State statutes and regulations cited by 
the State Attorney General or independent legal counsel shall be in the 
form of lawfully adopted State statutes and regulations at the time the 
statement is signed and shall be fully effective by the time the program 
is approved. To qualify as ``independent legal counsel'' the attorney 
signing the statement required by this section must have full authority 
to independently represent the State agency in court on all matters 
pertaining to the State program.

    Note: EPA will supply States with an Attorney General's statement 
format on request.

    (b) When a State seeks authority over activities on Indian lands, 
the statement shall contain an appropriate analysis of the State's 
authority.



Sec.  145.25  Memorandum of Agreement with the Regional Administrator.

    (a) Any State that seeks to administer a program under this part 
shall submit a Memorandum of Agreement. The Memorandum of Agreement 
shall be executed by the State Director and the Regional Administrator 
and shall become effective when approved by the Administrator. In 
addition to meeting the requirements of paragraph (b) of this section, 
the Memorandum of Agreement may include other terms, conditions, or 
agreements consistent with this part and relevant to the administration 
and enforcement of the State's regulatory program. The Administrator 
shall not approve any Memorandum of Agreement which contains provisions 
which restrict EPA's statutory oversight responsibility.
    (b) The Memorandum of Agreement shall include the following:
    (1) Provisions for the prompt transfer from EPA to the State of 
pending permit applications and any other information relevant to 
program operation not already in the possession of the State Director 
(e.g., support files for permit issuance, compliance reports, etc.). 
When existing permits are transferred from EPA to State for 
administration, the Memorandum of Agreement shall contain provisions 
specifying a procedure for transferring the administration of these 
permits. If a State lacks the authority to directly administer permits 
issued by the Federal government, a procedure may be established to 
transfer responsibility for these permits.

    Note: For example, EPA and the State and the permittee could agree 
that the State would issue a permit(s) identical to the outstanding 
Federal permit which would simultaneously be terminated.

    (2) Provisions specifying classes and categories of permit 
applications, draft permits, and proposed permits that the State will 
send to the Regional Administrator for review, comment and, where 
applicable, objection.
    (3) Provisions specifying the frequency and content of reports, 
documents and other information which the State is required to submit to 
EPA. The State shall allow EPA to routinely review State records, 
reports, and files relevant to the administration and enforcement of the 
approved program. State reports may be combined with grant reports where 
appropriate.
    (4) Provisions on the State's compliance monitoring and enforcement 
program, including:
    (i) Provisions for coordination of compliance monitoring activities 
by the State and by EPA. These may specify the basis on which the 
Regional Administrator will select facilities or activities within the 
State for EPA inspection. The Regional Administrator will normally 
notify the State at least 7 days before any such inspection; and
    (ii) Procedures to assure coordination of enforcement activities.
    (5) When appropriate, provisions for joint processing of permits by 
the State and EPA, for facilities or activities which require permits 
from both

[[Page 878]]

EPA and the State under different programs. See Sec.  124.4.
    (6) Provisions for modification of the Memorandum of Agreement in 
accordance with this part.
    (c) The Memorandum of Agreement, the annual program and grant and 
the State/EPA Agreement should be consistent. If the State/EPA Agreement 
indicates that a change is needed in the Memorandum of Agreement, the 
Memorandum of Agreement may be amended through the procedures set forth 
in this part. The State/EPA Agreement may not override the Memorandum of 
Agreement.

    Note: Detailed program priorities and specific arrangements for EPA 
support of the State program will change and are therefore more 
appropriately negotiated in the context of annual agreements rather than 
in the MOA. However, it may still be appropriate to specify in the MOA 
the basis for such detailed agreements, e.g., a provision in the MOA 
specifying that EPA will select facilities in the State for inspection 
annually as part of the State/EPA agreement.



           Subpart D_Program Approval, Revision and Withdrawal



Sec.  145.31  Approval process.

    (a) Prior to submitting an application to the Administrator for 
approval of a State UIC program, the State shall issue public notice of 
its intent to adopt a UIC program and to seek program approval from EPA. 
This public notice shall:
    (1) Be circulated in a manner calculated to attract the attention of 
interested persons. Circulation of the public notice shall include 
publication in enough of the largest newspapers in the State to attract 
Statewide attention and mailing to persons on appropriate State mailing 
lists and to any other persons whom the agency has reason to believe are 
interested;
    (2) Indicate when and where the State's proposed program submission 
may be reviewed by the public;
    (3) Indicate the cost of obtaining a copy of the submission;
    (4) Provide for a comment period of not less than 30 days during 
which interested persons may comment on the proposed UIC program;
    (5) Schedule a public hearing on the State program for no less than 
30 days after notice of the hearing is published;
    (6) Briefly outline the fundamental aspects of the State UIC 
program; and
    (7) Identify a person that an interested member of the public may 
contact for further information.
    (b) After complying with the requirements of paragraph (a) of this 
section any State may submit a proposed UIC program under section 1422 
of SDWA and Sec.  145.22 of this part to EPA for approval. Such a 
submission shall include a showing of compliance with paragraph (a) of 
this section; copies of all written comments received by the State; a 
transcript, recording or summary of any public hearing which was held by 
the State; and a responsiveness summary which identifies the public 
participation activities conducted, describes the matters presented to 
the public, summarizes significant comments received, and responds to 
these comments. A copy of the responsiveness summary shall be sent to 
those who testified at the hearing, and others upon request.
    (c) After determining that a State's submission for UIC program 
approval is complete the Administrator shall issue public notice of the 
submission in the Federal Register and in accordance with paragraph 
(a)(1) of this section. Such notice shall:
    (1) Indicate that a public hearing will be held by EPA no earlier 
than 30 days after notice of the hearing. The notice may require persons 
wishing to present testimony to file a request with the Regional 
Administrator, who may cancel the public hearing if sufficient public 
interest in a hearing is not expressed;
    (2) Afford the public 30 days after the notice to comment on the 
State's submission; and
    (3) Note the availability of the State submission for inspection and 
copying by the public.
    (d) The Administrator shall approve State programs which conform to 
the applicable requirements of this part.
    (e) Within 90 days of the receipt of a complete submission (as 
provided in

[[Page 879]]

Sec.  145.22) or material amendment thereto, the Administrator shall by 
rule either fully approve, disapprove, or approve in part the State's 
UIC program taking into account any comments submitted. The 
Administrator shall give notice of this rule in the Federal Register and 
in accordance with paragraph (a)(1) of this section. If the 
Administrator determines not to approve the State program or to approve 
it only in part, the notice shall include a concise statement of the 
reasons for this determination. A responsiveness summary shall be 
prepared by the Regional Office which identifies the public 
participation activities conducted, describes the matters presented to 
the public, summarizes significant comments received, and explains the 
Agency's response to these comments. The responsiveness summary shall be 
sent to those who testified at the public hearing, and to others upon 
request.



Sec.  145.32  Procedures for revision of State programs.

    (a) Either EPA or the approved State may initiate program revision. 
Program revision may be necessary when the controlling Federal or State 
statutory or regulatory authority is modified or supplemented. The state 
shall keep EPA fully informed of any proposed modifications to its basic 
statutory or regulatory authority, its forms, procedures, or priorities.
    (b) Revision of a State program shall be accomplished as follows:
    (1) The State shall submit a modified program description, Attorney 
General's statement, Memorandum of Agreement, or such other documents as 
EPA determines to be necessary under the circumstances.
    (2) Whenever EPA determines that the proposed program revision is 
substantial, EPA shall issue public notice and provide an opportunity to 
comment for a period of at least 30 days. The public notice shall be 
mailed to interested persons and shall be published in the Federal 
Register and in enough of the largest newspapers in the State to provide 
Statewide coverage. The public notice shall summarize the proposed 
revisions and provide for the opportunity to request a public hearing. 
Such a hearing will be held is there if significant public interest 
based on requests received. All requests for expansions to the areal 
extent of Class II enhanced oil recovery or enhanced gas recovery 
aquifer exemptions for Class VI wells must be treated as substantial 
program revisions.
    (3) The Administrator shall approve or disapprove program revisions 
based on the requirements of this part and of the Safe Drinking Water 
Act.
    (4) A program revision shall become effective upon the approval of 
the Administrator. Notice of approval of any substantial revision shall 
be published in the Federal Register. Notice of approval of non-
substantial program revisions may be given by a letter from the 
Administrator to the State Governor or his designee.
    (c) States with approved programs shall notify EPA whenever they 
propose to transfer all or part of any program from the approved State 
agency to any other State agency, and shall identify any new division of 
responsibilities among the agencies involved. The new agency is not 
authorized to administer the program until approval by the Administrator 
under paragraph (b) of this section. Organizational charts required 
under Sec.  145.23(b) shall be revised and resubmitted.
    (d) Whenever the Administrator has reason to believe that 
circumstances have changed with respect to a State program, he may 
request, and the State shall provide, a supplemental Attorney General's 
statement, program description, or such other documents or information 
as are necessary.
    (e) The State shall submit the information required under paragraph 
(b)(1) of this section within 270 days of any amendment to this part or 
40 CFR part 144, 146, or 124 which revises or adds any requirement 
respecting an approved UIC program.

[48 FR 14202, Apr. 1, 1983, as amended at 75 FR 77291, Dec. 10, 2010]



Sec.  145.33  Criteria for withdrawal of State programs.

    (a) The Administrator may withdraw program approval when a State 
program no longer complies with the requirements of this part, and the 
State fails to take corrective action. Such circumstances include the 
following:

[[Page 880]]

    (1) When the State's legal authority no longer meets their 
requirements of this part, including:
    (i) Failure of the State to promulgate or enact new authorities when 
necessary; or
    (ii) Action by a State legislature or court striking down or 
limiting State authorities.
    (2) When the operation of the State program fails to comply with the 
requirements of this part, including:
    (i) Failure to exercise control over activities required to be 
regulated under this part, including failure to issue permits;
    (ii) Repeated issuance of permits which do not conform to the 
requirements of this part; or
    (iii) Failure to comply with the public participation requirements 
of this part.
    (3) When the State's enforcement program fails to comply with the 
requirements of this part, including:
    (i) Failure to act on violations of permits or other program 
requirements;
    (ii) Failure to seek adequate enforcement penalties or to collect 
administrative fines when imposed; or
    (iii) Failure to inspect and monitor activities subject to 
regulation.
    (4) When the State program fails to comply with the terms of the 
Memorandum of Agreement required under Sec.  145.24.



Sec.  145.34  Procedures for withdrawal of State programs.

    (a) A State with a program approved under this part may voluntarily 
transfer program responsibilities required by Federal law to EPA by 
taking the following actions, or in such other manner as may be agreed 
upon with the Administrator.
    (1) The State shall give the Administrator 180 days notice of the 
proposed transfer and shall submit a plan for the orderly transfer of 
all relevant program information not in the possession of EPA (such as 
permits, permit files, compliance files, reports, permit applications) 
which are necessary for EPA to administer the program.
    (2) Within 60 days of receiving the notice and transfer plan, the 
Administrator shall evaluate the State's transfer plan and shall 
identify any additional information needed by the Federal government for 
program administration and/or identify any other deficiencies in the 
plan.
    (3) At least 30 days before the transfer is to occur the 
Administrator shall publish notice of the transfer in the Federal 
Register and in enough of the largest newspapers in the State to provide 
Statewide coverage, and shall mail notice to all permit holders, permit 
applicants, other regulated persons and other interested persons on 
appropriate EPA and State mailing lists.
    (b) Approval of a State UIC program may be withdrawn and a Federal 
program established in its place when the Administrator determines, 
after holding a public hearing, that the State program is not in 
compliance with the requirements of SDWA and this part.
    (1) Notice to State of public hearing. If the Administrator has 
cause to believe that a State is not administering or enforcing its 
authorized program in compliance with the requirements of SDWA and this 
part, he or she shall inform the State by registered mail of the 
specific areas of alleged noncompliance. If the State demonstrates to 
the Administrator within 30 days of such notification that the State 
program is in compliance, the Administrator shall take no further action 
toward withdrawal and shall so notify the State by registered mail.
    (2) Public hearing. If the State has not demonstrated its compliance 
to the satisfaction of the Administrator within 30 days after 
notification, the Administrator shall inform the State Director and 
schedule a public hearing to discuss withdrawal of the State program. 
Notice of such public hearing shall be published in the Federal Register 
and in enough of the largest newspapers in the State to attract 
statewide attention, and mailed to persons on appropriate State and EPA 
mailing lists. This hearing shall be convened not less than 60 days nor 
more than 75 days following the publication of the notice of the 
hearing. Notice of the hearing shall identify the Administrator's 
concerns. All interested persons shall be given opportunity to make 
written or oral presentation on the State's program at the public 
hearing.

[[Page 881]]

    (3) Notice to State of findings. When the Administrator finds after 
the public hearing that the State is not in compliance, he or she shall 
notify the State by registered mail of the specific deficiencies in the 
State program and of necessary remedial actions. Within 90 days of 
receipt of the above letter, the State shall either carry out the 
required remedial action or the Administrator shall withdraw program 
approval. If the State carries out the remedial action or, as a result 
of the hearing is found to be in compliance, the Administrator shall so 
notify the State by registered mail and conclude the withdrawal 
proceedings.



                         Subpart E_Indian Tribes

    Source: 53 FR 37412, Sept. 26, 1988, unless otherwise noted.



Sec.  145.52  Requirements for Tribal eligibility.

    The Administrator is authorized to treat an Indian Tribe as eligible 
to apply for primary enforcement responsibility for the Underground 
Injection Control Program if it meets the following criteria:
    (a) The Indian Tribe is recognized by the Secretary of the Interior.
    (b) The Indian Tribe has a Tribal governing body which is currently 
``carrying out substantial governmental duties and powers'' over a 
defined area, (i.e., is currently performing governmental functions to 
promote the health, safety, and welfare of the affected population 
within a defined geographic area).
    (c) The Indian Tribe demonstrates that the functions to be performed 
in regulating the underground injection wells that the applicant intends 
to regulate are within the area of the Indian Tribal government's 
jurisdiction.
    (d) The Indian Tribe is reasonably expected to be capable, in the 
Administrator's judgment, of administering (in a manner consistent with 
the terms and purposes of the Act and all applicable regulations) an 
effective Underground Injection Control Program.

[53 FR 37412, Sept. 26, 1988, as amended at 59 FR 64345, Dec. 14, 1994]



Sec.  145.56  Request by an Indian Tribe for a determination of eligibility.

    An Indian Tribe may apply to the Administrator for a determination 
that it meets the criteria of section 1451 of the Act. The application 
shall be concise and describe how the Indian Tribe will meet each of the 
requirements of Sec.  145.52. The application shall consist of the 
following:
    (a) A statement that the Tribe is recognized by the Secretary of the 
Interior.
    (b) A descriptive statement demonstrating that the Tribal governing 
body is currently carrying out substantial governmental duties and 
powers over a defined area. The statement should:
    (1) Describe the form of the Tribal government;
    (2) Describe the types of governmental functions currently performed 
by the Tribal governing body such as, but not limited to, the exercise 
of police powers affecting (or relating to) the health, safety, and 
welfare of the affected population; taxation; and the exercise of the 
power of eminent domain; and
    (3) Identify the sources of the Tribal government's authority to 
carry out the governmental functions currently being performed.
    (c) A map or legal description of the area over which the Indian 
Tribe asserts jurisdiction; a statement by the Tribal Attorney General 
(or equivalent official) which describes the basis for the Tribe's 
jurisdictional assertion (including the nature or subject matter of the 
asserted jurisdiction); a copy of those documents such as Tribal 
constitutions, by-laws, charters, executive orders, codes, ordinances, 
and/or resolutions which the Tribe believes are relevant to its 
assertions regarding jurisdiction; and a description of the locations of 
the underground injection wells the Tribe proposes to regulate.
    (d) A narrative statement describing the capability of the Indian 
Tribe to administer an effective Underground Injection Control program 
which should include:
    (1) A description of the Indian Tribe's previous management 
experience which may include, the administration of programs and 
services authorized

[[Page 882]]

under the Indian Self-Determination and Education Assistance Act (25 
U.S.C. 450 et seq.), the Indian Mineral Development Act (25 U.S.C. 2101 
et seq.), or the Indian Sanitation Facilities Construction Activity Act 
(42 U.S.C. 2004a).
    (2) A list of existing environmental or public health programs 
administered by the Tribal governing body and a copy of related Tribal 
laws, regulations and policies.
    (3) A description of the Indian Tribe's accounting and procurement 
systems.
    (4) A description of the entity (or entities) which exercise the 
executive, legislative, and judicial functions of the Tribal government.
    (5) A description of the existing, or proposed, agency of the Indian 
Tribe which will assume primary enforcement responsibility, including a 
description of the relationship between owners/operators of the 
underground injection wells and the agency.
    (6) A description of the technical and administrative capabilities 
of the staff to administer and manage an effective Underground Injection 
Control Program or a plan which proposes how the Tribe will acquire 
additional administrative and/or technical expertise. The plan must 
address how the Tribe will obtain the funds to acquire the additional 
administrative and technical expertise.
    (e) The Adminstrator may, in his discretion, request further 
documentation necessary to support a Tribe's eligibility.
    (f) If the Administrator has previously determined that a Tribe has 
met the prerequisites that make it eligible to assume a role similar to 
that of a State as provided by statute under the Safe Drinking Water 
Act, the Clean Water Act, or the Clean Air Act, then that Tribe need 
provide only that information unique to the Underground Injection 
Control program (Sec.  145.76(c) and (d)(6)).

[53 FR 37412, Sept. 26, 1988, as amended at 59 FR 64345, Dec. 14, 1994]



Sec.  145.58  Procedure for processing an Indian Tribe's application.

    (a) The Administrator shall process a completed application of an 
Indian Tribe in a timely manner. He shall promptly notify the Indian 
Tribe of receipt of the application.
    (b) A tribe that meets the requirements of Sec.  145.52 is eligible 
to apply for development grants and primary enforcement responsibility 
for an Underground Injection Control program and the associated funding 
under section 1443(b) of the Act and primary enforcement responsibility 
for the Underground Injection Control Program under sections 1422 and/or 
1425 of the Act.

[53 FR 37412, Sept. 26, 1988, as amended at 59 FR 64345, Dec. 14, 1994]



PART 146_UNDERGROUND INJECTION CONTROL PROGRAM: CRITERIA AND STANDARDS--
Table of Contents



                      Subpart A_General Provisions

Sec.
146.1 Applicability and scope.
146.2 Law authorizing these regulations.
146.3 Definitions.
146.4 Criteria for exempted aquifers.
146.5 Classification of injection wells.
146.6 Area of review.
146.7 Corrective action.
146.8 Mechanical integrity.
146.9 Criteria for establishing permitting priorities.
146.10 Plugging and abandoning Class I-III wells.

      Subpart B_Criteria and Standards Applicable to Class I Wells

146.11 Criteria and standards applicable to Class I nonhazardous wells.
146.12 Construction requirements.
146.13 Operating, monitoring and reporting requirements.
146.14 Information to be considered by the Director.
146.15 Class I municipal disposal well alternative authorization in 
          certain parts of Florida.
146.16 Requirements for new Class I municipal wells in certain parts of 
          Florida.

      Subpart C_Criteria and Standards Applicable to Class II Wells

146.21 Applicability.
146.22 Construction requirements.
146.23 Operating, monitoring, and reporting requirements.
146.24 Information to be considered by the Director.

[[Page 883]]

     Subpart D_Criteria and Standards Applicable to Class III Wells

146.31 Applicability.
146.32 Construction requirements.
146.33 Operating, monitoring, and reporting requirements.
146.34 Information to be considered by the Director.

Subpart E--Criteria and Standards Applicable to Class IV Injection Wells 
[Reserved]

 Subpart F_Criteria and Standards Applicable to Class V Injection Wells

146.51 Applicability.

 Subpart G_Criteria and Standards Applicable to Class I Hazardous Waste 
                             Injection Wells

146.61 Applicability.
146.62 Minimum criteria for siting.
146.63 Area of review.
146.64 Corrective action for wells in the area of review.
146.65 Construction requirements.
146.66 Logging, sampling, and testing prior to new well operation.
146.67 Operating requirements.
146.68 Testing and monitoring requirements.
146.69 Reporting requirements.
146.70 Information to be evaluated by the Director.
146.71 Closure.
146.72 Post-closure care.
146.73 Financial responsibility for post-closure care.

      Subpart H_Criteria and Standards Applicable to Class VI Wells

146.81 Applicability.
146.82 Required Class VI permit information.
146.83 Minimum criteria for siting.
146.84 Area of review and corrective action.
146.85 Financial responsibility.
146.86 Injection well construction requirements.
146.87 Logging, sampling, and testing prior to injection well operation.
146.88 Injection well operating requirements.
146.89 Mechanical integrity.
146.90 Testing and monitoring requirements.
146.91 Reporting requirements.
146.92 Injection well plugging.
146.93 Post-injection site care and site closure.
146.94 Emergency and remedial response.
146.95 Class VI injection depth waiver requirements.

    Authority: Safe Drinking Water Act, 42 U.S.C. 300f et seq.; Resource 
Conservation and Recovery Act, 42 U.S.C. 6901 et seq.

    Source: 45 FR 42500, June 24, 1980, unless otherwise noted.



                      Subpart A_General Provisions



Sec.  146.1  Applicability and scope.

    (a) This part sets forth technical criteria and standards for the 
Underground Injection Control Program. This part should be read in 
conjunction with 40 CFR parts 124, 144, and 145, which also apply to UIC 
programs. 40 CFR part 144 defines the regulatory framework of EPA 
administered permit programs. 40 CFR part 145 describes the elements of 
an approvable State program and procedures for EPA approval of State 
participation in the permit programs. 40 CFR part 124 describes the 
procedures the Agency will use for issuing permits under the covered 
programs. Certain of these procedures will also apply to State-
administered programs as specified in 40 CFR part 145.
    (b) Upon the approval, partial approval or promulgation of a State 
UIC program by the Administrator, any underground injection which is not 
authorized by the Director by rule or by permit is unlawful.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 48 FR 14293, Apr. 1, 1983]



Sec.  146.2  Law authorizing these regulations.

    The Safe Drinking Water Act, 42 U.S.C. 300f et seq. authorizes these 
regulations and all other UIC program regulations referenced in 40 CFR 
part 144. Certain regulations relating to the injection of hazardous 
waste are also authorized by the Resource Conservation and Recovery Act, 
42 U.S.C. 6901 et seq.

[58 FR 63898, Dec. 3, 1993]



Sec.  146.3  Definitions.

    The following definitions apply to the underground injection control 
program.

[[Page 884]]

    Abandoned well means a well whose use has been permanently 
discontinued or which is in a state of disrepair such that it cannot be 
used for its intended purpose or for observation purposes.
    Administrator means the Administrator of the United States 
Environmental Protection Agency, or an authorized representative.
    Application means the EPA standard national forms for applying for a 
permit, including any additions, revisions or modifications to the 
forms; or forms approved by EPA for use in approved States, including 
any approved modifications or revisions. For RCRA, application also 
includes the information required by the Director under Sec.  122.25 
(contents of Part B of the RCRA application).
    Aquifer means a geological formation, group of formations, or part 
of a formation that is capable of yielding a significant amount of water 
to a well or spring.
    Area of review means the area surrounding an injection well 
described according to the criteria set forth in Sec.  146.06 or in the 
case of an area permit, the project area plus a circumscribing area the 
width of which is either \1/4\ of a mile or a number calculated 
according to the criteria set forth in Sec.  146.06.
    Casing means a pipe or tubing of appropriate material, of varying 
diameter and weight, lowered into a borehole during or after drilling in 
order to support the sides of the hole and thus prevent the walls from 
caving, to prevent loss of drilling mud into porous ground, or to 
prevent water, gas, or other fluid from entering or leaving the hole.
    Catastrophic collapse means the sudden and utter failure of 
overlying ``strata'' caused by removal of underlying materials.
    Cementing means the operation whereby a cement slurry is pumped into 
a drilled hole and/or forced behind the casing.
    Cesspool means a ``drywell'' that receives untreated sanitary waste 
containing human excreta, and which sometimes has an open bottom and/or 
perforated sides.
    Confining bed means a body of impermeable or distinctly less 
permeable material stratigraphically adjacent to one or more aquifers.
    Confining zone means a geological formation, group of formations, or 
part of a formation that is capable of limiting fluid movement above an 
injection zone.
    Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    Conventional mine means an open pit or underground excavation for 
the production of minerals.
    Director means the Regional Administrator, the State director or the 
Tribal director as the context requires, or an authorized 
representative. When there is no approved State or Tribal program, and 
there is an EPA administered program, ``Director'' means the Regional 
Administrator. When there is an approved State or Tribal program, 
``Director'' normally means the State or Tribal director. In some 
circumstances, however, EPA retains the authority to take certain 
actions even when there is an approved State or Tribal program. (For 
example, when EPA has issued an NPDES permit prior to the approval of a 
State program, EPA may retain jurisdiction over that permit after 
program approval; see Sec.  123.69). In such cases, the term Director 
means the Regional Administrator and not the State or Tribal director.
    Disposal well means a well used for the disposal of waste into a 
subsurface stratum.
    Drywell means a well, other than an improved sinkhole or subsurface 
fluid distribution system, completed above the water table so that its 
bottom and sides are typically dry except when receiving fluids.
    Effective date of a UIC program means the date that a State UIC 
program is approved or established by the Administrator.
    Environmental Protection Agency (``EPA'') means the United States 
Environmental Protection Agency.
    EPA means the United States ``Environmental Protection Agency.''
    Exempted aquifer means an aquifer or its portion that meets the 
criteria in the definition of ``underground source of drinking water'' 
but which has been exempted according to the procedures of Sec.  
144.8(b).

[[Page 885]]

    Existing injection well means an ``injection well'' other than a 
``new injection well.''
    Experimental technology means a technology which has not been proven 
feasible under the conditions in which it is being tested.
    Facility or activity means any ``HWM facility,'' UIC ``injection 
well,'' NPDES ``point source,'' or State 404 dredge and fill activity, 
or any other facility or activity (including land or appurtenances 
thereto) that is subject to regulation under the RCRA, UIC, NPDES, or 
404 programs.
    Fault means a surface or zone of rock fracture along which there has 
been displacement.
    Flow rate means the volume per time unit given to the flow of gases 
or other fluid substance which emerges from an orifice, pump, turbine or 
passes along a conduit or channel.
    Fluid means material or substance which flows or moves whether in a 
semisolid, liquid, sludge, gas, or any other form or state.
    Formation means a body of rock characterized by a degree of 
lithologic homogeneity which is prevailingly, but not necessarily, 
tabular and is mappable on the earth's surface or traceable in the 
subsurface.
    Formation fluid means ``fluid'' present in a ``formation'' under 
natural conditions as opposed to introduced fluids, such as drilling 
mud.
    Generator means any person, by site location, whose act or process 
produces hazardous waste identified or listed in 40 CFR part 261.
    Ground water means water below the land surface in a zone of 
saturation.
    Hazardous waste means a hazardous waste as defined in 40 CFR 261.3.
    Hazardous Waste Management facility (``HWM facility'') means all 
contiguous land, and structures, other appurtenances, and improvements 
on the land used for treating, storing, or disposing of hazardous waste. 
A facility may consist of several treatment, storage, or disposal 
operational units (for example, one or more landfills, surface 
impoundments, or combination of them).
    HWM facility means ``Hazardous Waste Management facility.''
    Improved sinkhole means a naturally occurring karst depression or 
other natural crevice found in volcanic terrain and other geologic 
settings which have been modified by man for the purpose of directing 
and emplacing fluids into the subsurface.
    Indian Tribe means any Indian Tribe having a Federally recognized 
governing body carrying out substantial governmental duties and powers 
over a defined area.
    Injection well means a ``well'' into which ``fluids'' are being 
injected.
    Injection zone means a geological ``formation'', group of 
formations, or part of a formation receiving fluids through a well.
    Lithology means the description of rocks on the basis of their 
physical and chemical characteristics.
    Owner or operator means the owner or operator of any facility or 
activity subject to regulation under the RCRA, UIC, NPDES, or 404 
programs.
    Packer means a device lowered into a well to produce a fluid-tight 
seal.
    Permit means an authorization, license, or equivalent control 
document issued by EPA or an ``approved State'' to implement the 
requirements of this part and parts 124, 144, and 145. Permit does not 
include RCRA interim status (Sec.  122.23), UIC authorization by rule 
(Sec. Sec.  144.21 to 144.26 and 144.15), or any permit which has not 
yet been the subject of final agency action, such as a ``draft permit'' 
or a ``proposed permit.''
    Plugging means the act or process of stopping the flow of water, oil 
or gas into or out of a formation through a borehole or well penetrating 
that formation.
    Plugging record means a systematic listing of permanent or temporary 
abandonment of water, oil, gas, test, exploration and waste injection 
wells, and may contain a well log, description of amounts and types of 
plugging material used, the method employed for plugging, a description 
of formations which are sealed and a graphic log of the well showing 
formation location, formation thickness, and location of plugging 
structures.
    Point of injection for Class V wells means the last accessible 
sampling point prior to waste fluids being released into the subsurface 
environment

[[Page 886]]

through a Class V injection well. For example, the point of injection of 
a Class V septic system might be the distribution box--the last 
accessible sampling point before the waste fluids drain into the 
underlying soils. For a dry well, it is likely to be the well bore 
itself.
    Pressure means the total load or force per unit area acting on a 
surface.
    Project means a group of wells in a single operation.
    Radioactive waste means any waste which contains radioactive 
material in concentrations which exceed those listed in 10 CFR part 20, 
appendix B, table II column 2.
    RCRA means the Solid Waste Disposal Act as amended by the Resource 
Conservation and Recovery Act of 1976 (Pub. L. 94-580, as amended by 
Pub. L. 95-609, 42 U.S.C. 6901 et seq.).
    Sanitary waste means liquid or solid wastes originating solely from 
humans and human activities, such as wastes collected from toilets, 
showers, wash basins, sinks used for cleaning domestic areas, sinks used 
for food preparation, clothes washing operations, and sinks or washing 
machines where food and beverage serving dishes, glasses, and utensils 
are cleaned. Sources of these wastes may include single or multiple 
residences, hotels and motels, restaurants, bunkhouses, schools, ranger 
stations, crew quarters, guard stations, campgrounds, picnic grounds, 
day-use recreation areas, other commercial facilities, and industrial 
facilities provided the waste is not mixed with industrial waste.
    SDWA means the Safe Drinking Water Act (Pub. L. 95-523, as amended 
by Pub. L. 95-190, 42 U.S.C. 300(f) et seq.).
    Septic system means a ``well'' that is used to emplace sanitary 
waste below the surface and is typically comprised of a septic tank and 
subsurface fluid distribution system or disposal system.
    Site means the land or water area where any facility or activity is 
physically located or conducted, including adjacent land used in 
connection with the facility or activity.
    Sole or principal source aquifer means an aquifer which has been 
designated by the Administrator pursuant to section 1424 (a) or (e) of 
the SDWA.
    State Director means the chief administrative officer of any State, 
interstate, or Tribal agency operating an ``approved program,'' or the 
delegated representative of the State Director. If the responsibility is 
divided among two or more State, interstate, or Tribal agencies, ``State 
Director'' means the chief administrative officer of the State, 
interstate, or Tribal agency authorized to perform the particular 
procedure or function to which reference is made.
    Stratum (plural strata) means a single sedimentary bed or layer, 
regardless of thickness, that consists of generally the same kind of 
rock material.
    Subsidence means the lowering of the natural land surface in 
response to: Earth movements; lowering of fluid pressure; removal of 
underlying supporting material by mining or solution of solids, either 
artificially or from natural causes; compaction due to wetting 
(Hydrocompaction); oxidation of organic matter in soils; or added load 
on the land surface.
    Subsurface fluid distribution system means an assemblage of 
perforated pipes, drain tiles, or other similar mechanisms intended to 
distribute fluids below the surface of the ground.
    Surface casing means the first string of well casing to be installed 
in the well.
    Total dissolved solids (``TDS'') means the total dissolved 
(filterable) solids as determined by use of the method specified in 40 
CFR part 136.
    UIC means the Underground Injection Control program under Part C of 
the Safe Drinking Water Act, including an ``approved program.''
    Underground injection means a ``well injection.''
    Underground source of drinking water (USDW) means an aquifer or its 
portion:

    (1)(i) Which supplies any public water system; or
    (ii) Which contains a sufficient quantity of ground water to supply 
a public water system; and
    (A) Currently supplies drinking water for human consumption; or
    (B) Contains fewer than 10,000 mg/l total dissolved solids; and
    (2) Which is not an exempted aquifer.

[[Page 887]]

    USDW means ``underground source of drinking water.''
    Well means: A bored, drilled, or driven shaft whose depth is greater 
than the largest surface dimension; or, a dug hole whose depth is 
greater than the largest surface dimension; or, an improved sinkhole; 
or, a subsurface fluid distribution system.
    Well injection means the subsurface emplacement of fluids through a 
well.
    Well plug means a watertight and gastight seal installed in a 
borehole or well to prevent movement of fluids.
    Well stimulation means several processes used to clean the well 
bore, enlarge channels, and increase pore space in the interval to be 
injected thus making it possible for wastewater to move more readily 
into the formation, and includes (1) surging, (2) jetting, (3) blasting, 
(4) acidizing, (5) hydraulic fracturing.
    Well monitoring means the measurement, by on-site instruments or 
laboratory methods, of the quality of water in a well.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43161, Aug. 27, 1981; 
47 FR 4998, Feb. 3, 1982; 48 FR 14293, Apr. 1, 1983; 53 FR 37414, Sept. 
26, 1988; 64 FR 68573, Dec. 7, 1999]



Sec.  146.4  Criteria for exempted aquifers.

    An aquifer or a portion thereof which meets the criteria for an 
``underground source of drinking water'' in Sec.  146.3 may be 
determined under Sec.  144.7 of this chapter to be an ``exempted 
aquifer'' for Class I-V wells if it meets the criteria in paragraphs (a) 
through (c) of this section. Class VI wells must meet the criteria under 
paragraph (d) of this section:
    (a) It does not currently serve as a source of drinking water; and
    (b) It cannot now and will not in the future serve as a source of 
drinking water because:
    (1) It is mineral, hydrocarbon or geothermal energy producing, or 
can be demonstrated by a permit applicant as part of a permit 
application for a Class II or III operation to contain minerals or 
hydrocarbons that considering their quantity and location are expected 
to be commercially producible.
    (2) It is situated at a depth or location which makes recovery of 
water for drinking water purposes economically or technologically 
impractical;
    (3) It is so contaminated that it would be economically or 
technologically impractical to render that water fit for human 
consumption; or
    (4) It is located over a Class III well mining area subject to 
subsidence or catastrophic collapse; or
    (c) The total dissolved solids content of the ground water is more 
than 3,000 and less than 10,000 mg/l and it is not reasonably expected 
to supply a public water system.
    (d) The areal extent of an aquifer exemption for a Class II enhanced 
oil recovery or enhanced gas recovery well may be expanded for the 
exclusive purpose of Class VI injection for geologic sequestration under 
Sec.  144.7(d) of this chapter if it meets the following criteria:
    (1) It does not currently serve as a source of drinking water; and
    (2) The total dissolved solids content of the ground water is more 
than 3,000 mg/l and less than 10,000 mg/l; and
    (3) It is not reasonably expected to supply a public water system.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 47 FR 4998, Feb. 3, 1982; 48 
FR 14293, Apr. 1, 1983; 75 FR 77291, Dec. 10, 2010]



Sec.  146.5  Classification of injection wells.

    Injection wells are classified as follows:
    (a) Class I. (1) Wells used by generators of hazardous waste or 
owners or operators of hazardous waste management facilities to inject 
hazardous waste beneath the lowermost formation containing, within one 
quarter (\1/4\) mile of the well bore, an underground source of drinking 
water.
    (2) Other industrial and municipal disposal wells which inject 
fluids beneath the lowermost formation containing, within one quarter 
mile of the well bore, an underground source of drinking water.

[[Page 888]]

    (3) Radioactive waste disposal wells which inject fluids below the 
lowermost formation containing an underground source of drinking water 
within one quarter mile of the well bore.
    (b) Class II. Wells which inject fluids:
    (1) Which are brought to the surface in connection with conventional 
oil or natural gas production and may be commingled with waste waters 
from gas plants which are an integral part of production operations, 
unless those waters are classified as a hazardous waste at the time of 
injection.
    (2) For enhanced recovery of oil or natural gas; and
    (3) For storage of hydrocarbons which are liquid at standard 
temperature and pressure.
    (c) Class III. Wells which inject for extraction of minerals 
including:
    (1) Mining of sulfur by the Frasch process;
    (2) In situ production of uranium or other metals. This category 
includes only in-situ production from ore bodies which have not been 
conventionally mined. Solution mining of conventional mines such as 
stopes leaching is included in Class V.
    (3) Solution mining of salts or potash.
    (d) Class IV. (1) Wells used by generators of hazardous waste or of 
radioactive waste, by owners or operators of hazardous waste management 
facilities, or by owners or operators of radioactive waste disposal 
sites to dispose of hazardous waste or radioactive waste into a 
formation which within one quarter (\1/4\) mile of the well contains an 
underground source of drinking water.
    (2) Wells used by generators of hazardous waste or of radioactive 
waste, by owners or operators of hazardous waste management facilities, 
or by owners or operators of radioactive waste disposal sites to dispose 
of hazardous waste or radioactive waste above a formation which within 
one quarter (\1/4\) mile of the well contains an underground source of 
drinking water.
    (3) Wells used by generators of hazardous waste or owners or 
operators of hazardous waste management facilities to dispose of 
hazardous waste, which cannot be classified under Sec.  146.05(a)(1) or 
Sec.  146.05(d) (1) and (2) (e.g., wells used to dispose of hazardous 
wastes into or above a formation which contains an aquifer which has 
been exempted pursuant to Sec.  146.04).
    (e) Class V. Injection wells not included in Class I, II, III, IV or 
VI. Specific types of Class V injection wells are also described in 40 
CFR 144.81. Class V wells include:
    (1) Air conditioning return flow wells used to return to the supply 
aquifer the water used for heating or cooling in a heat pump;
    (2) Cesspools including multiple dwelling, community or regional 
cesspools, or other devices that receive wastes which have an open 
bottom and sometimes have perforated sides. The UIC requirements do not 
apply to single family residential cesspools nor to non-residential 
cesspools which receive solely sanitary wastes and have the capacity to 
serve fewer than 20 persons a day.
    (3) Cooling water return flow wells used to inject water previously 
used for cooling;
    (4) Drainage wells used to drain surface fluid, primarily storm 
runoff, into a subsurface formation;
    (5) Dry wells used for the injection of wastes into a subsurface 
formation;
    (6) Recharge wells used to replenish the water in an aquifer;
    (7) Salt water intrusion barrier wells used to inject water into a 
fresh water aquifer to prevent the intrusion of salt water into the 
fresh water;
    (8) Sand backfill and other backfill wells used to inject a mixture 
of water and sand, mill tailings or other solids into mined out portions 
of subsurface mines whether what is injected is a radioactive waste or 
not.
    (9) Septic system wells used to inject the waste or effluent from a 
multiple dwelling, business establishment, community or regional 
business establishment septic tank. The UIC requirements do not apply to 
single family residential septic system wells, nor to non-residential 
septic system wells which are used solely for the disposal of sanitary 
waste and have the capacity to serve fewer than 20 persons a day.
    (10) Subsidence control wells (not used for the purpose of oil or 
natural

[[Page 889]]

gas production) used to inject fluids into a non-oil or gas producing 
zone to reduce or eliminate subsidence associated with the overdraft of 
fresh water;
    (11) Radioactive waste disposal wells other than Class IV;
    (12) Injection wells associated with the recovery of geothermal 
energy for heating, aquaculture and production of electric power.
    (13) Wells used for solution mining of conventional mines such as 
stopes leaching;
    (14) Wells used to inject spent brine into the same formation from 
which it was withdrawn after extraction of halogens or their salts;
    (15) Injection wells used in experimental technologies.
    (16) Injection wells used for in situ recovery of lignite, coal, tar 
sands, and oil shale.
    (f) Class VI. Wells that are not experimental in nature that are 
used for geologic sequestration of carbon dioxide beneath the lowermost 
formation containing a USDW; or, wells used for geologic sequestration 
of carbon dioxide that have been granted a waiver of the injection depth 
requirements pursuant to requirements at Sec.  146.95; or, wells used 
for geologic sequestration of carbon dioxide that have received an 
expansion to the areal extent of an existing Class II enhanced oil 
recovery or enhanced gas recovery aquifer exemption pursuant to 
Sec. Sec.  146.4 and 144.7(d) of this chapter.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43161, Aug. 27, 1981; 
47 FR 4999, Feb. 3, 1982; 64 FR 68573, Dec. 7, 1999; 75 FR 77291, Dec. 
10, 2010]



Sec.  146.6  Area of review.

    The area of review for each injection well or each field, project or 
area of the State shall be determined according to either paragraph (a) 
or (b) of this section. The Director may solicit input from the owners 
or operators of injection wells within the State as to which method is 
most appropriate for each geographic area or field.
    (a) Zone of endangering influence. (1) The zone of endangering 
influence shall be:
    (i) In the case of application(s) for well permit(s) under Sec.  
122.38 that area the radius of which is the lateral distance in which 
the pressures in the injection zone may cause the migration of the 
injection and/or formation fluid into an underground source of drinking 
water; or
    (ii) In the case of an application for an area permit under Sec.  
122.39, the project area plus a circumscribing area the width of which 
is the lateral distance from the perimeter of the project area, in which 
the pressures in the injection zone may cause the migration of the 
injection and/or formation fluid into an underground source of drinking 
water.
    (2) Computation of the zone of endangering influence may be based 
upon the parameters listed below and should be calculated for an 
injection time period equal to the expected life of the injection well 
or pattern. The following modified Theis equation illustrates one form 
which the mathematical model may take.
[GRAPHIC] [TIFF OMITTED] TC15NO91.140

where:
[GRAPHIC] [TIFF OMITTED] TC15NO91.141

r = Radius of endangering influence from injection well (length)
k = Hydraulic conductivity of the injection zone (length/time)
H = Thickness of the injection zone (length)
t = Time of injection (time)
S = Storage coefficient (dimensionless)
Q = Injection rate (volume/time)
hbo = Observed original hydrostatic head of injection zone 
          (length) measured from the base of the lowermost underground 
          source of drinking water
hw = Hydrostatic head of underground source of drinking water 
          (length) measured from the base of the lowest underground 
          source of drinking water
Sp Gb = Specific gravity of fluid in the injection 
          zone (dimensionless)
[pi] = 3.142 (dimensionless)


The above equation is based on the following assumptions:
    (i) The injection zone is homogenous and isotropic;
    (ii) The injection zone has infinite area extent;
    (iii) The injection well penetrates the entire thickness of the 
injection zone;

[[Page 890]]

    (iv) The well diameter is infinitesimal compared to ``r'' when 
injection time is longer than a few minutes; and
    (v) The emplacement of fluid into the injection zone creates 
instantaneous increase in pressure.
    (b) Fixed radius. (1) In the case of application(s) for well 
permit(s) under Sec.  122.38 a fixed radius around the well of not less 
than one-fourth (\1/4\) mile may be used.
    (2) In the case of an application for an area permit under Sec.  
122.39 a fixed width of not less than one-fourth (\1/4\) mile for the 
circumscribing area may be used.

In determining the fixed radius, the following factors shall be taken 
into consideration: Chemistry of injected and formation fluids; 
hydrogeology; population and ground-water use and dependence; and 
historical practices in the area.
    (c) If the area of review is determined by a mathematical model 
pursuant to paragraph (a) of this section, the permissible radius is the 
result of such calculation even if it is less than one-fourth (\1/4\) 
mile.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43161, Aug. 27, 1981; 
47 FR 4999, Feb. 3, 1982]



Sec.  146.7  Corrective action.

    In determining the adequacy of corrective action proposed by the 
applicant under 40 CFR 144.55 and in determining the additional steps 
needed to prevent fluid movement into underground sources of drinking 
water, the following criteria and factors shall be considered by the 
Director:
    (a) Nature and volume of injected fluid;
    (b) Nature of native fluids or by-products of injection;
    (c) Potentially affected population;
    (d) Geology;
    (e) Hydrology;
    (f) History of the injection operation;
    (g) Completion and plugging records;
    (h) Abandonment procedures in effect at the time the well was 
abandoned; and
    (i) Hydraulic connections with underground sources of drinking 
water.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
48 FR 14293, Apr. 1, 1983]



Sec.  146.8  Mechanical integrity.

    (a) An injection well has mechanical integrity if:
    (1) There is no significant leak in the casing, tubing or packer; 
and
    (2) There is no significant fluid movement into an underground 
source of drinking water through vertical channels adjacent to the 
injection well bore.
    (b) One of the following methods must be used to evaluate the 
absence of significant leaks under paragraph (a)(1) of this section:
    (1) Following an initial pressure test, monitoring of the tubing-
casing annulus pressure with sufficient frequency to be representative, 
as determined by the Director, while maintaining an annulus pressure 
different from atmospheric pressure measured at the surface;
    (2) Pressure test with liquid or gas; or
    (3) Records of monitoring showing the absence of significant changes 
in the relationship between injection pressure and injection flow rate 
for the following Class II enhanced recovery wells:
    (i) Existing wells completed without a packer provided that a 
pressure test has been performed and the data is available and provided 
further that one pressure test shall be performed at a time when the 
well is shut down and if the running of such a test will not cause 
further loss of significant amounts of oil or gas; or
    (ii) Existing wells constructed without a long string casing, but 
with surface casing which terminates at the base of fresh water provided 
that local geological and hydrological features allow such construction 
and provided further that the annular space shall be visually inspected. 
For these wells, the Director shall prescribe a monitoring program which 
will verify the absence

[[Page 891]]

of significant fluid movement from the injection zone into an USDW.
    (c) One of the following methods must be used to determine the 
absence of significant fluid movement under paragraph (a)(2) of this 
section:
    (1) The results of a temperature or noise log; or
    (2) For Class II only, cementing records demonstrating the presence 
of adequate cement to prevent such migration; or
    (3) For Class III wells where the nature of the casing precludes the 
use of the logging techniques prescribed at paragraph (c)(1) of this 
section, cementing records demonstrating the presence of adequate cement 
to prevent such migration;
    (4) For Class III wells where the Director elects to rely on 
cementing records to demonstrate the absence of significant fluid 
movement, the monitoring program prescribed by Sec.  146.33(b) shall be 
designed to verify the absence of significant fluid movement.
    (d) The Director may allow the use of a test to demonstrate 
mechanical integrity other than those listed in paragraphs (b) and 
(c)(2) of this section with the written approval of the Administrator. 
To obtain approval, the Director shall submit a written request to the 
Administrator, which shall set forth the proposed test and all technical 
data supporting its use. The Administrator shall approve the request if 
it will reliably demonstrate the mechanical integrity of wells for which 
its use is proposed. Any alternate method approved by the Administrator 
shall be published in the Federal Register and may be used in all States 
unless its use is restricted at the time of approval by the 
Administrator.
    (e) In conducting and evaluating the tests enumerated in this 
section or others to be allowed by the Director, the owner or operator 
and the Director shall apply methods and standards generally accepted in 
the industry. When the owner or operator reports the results of 
mechanical integrity tests to the Director, he shall include a 
description of the test(s) and the method(s) used. In making his/her 
evaluation, the Director shall review monitoring and other test data 
submitted since the previous evaluation.
    (f) The Director may require additional or alternative tests if the 
results presented by the owner or operator under Sec.  146.8(e) are not 
satisfactory to the Director to demonstrate that there is no movement of 
fluid into or between USDWs resulting from the injection activity.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
47 FR 4999, Feb. 3, 1982; 58 FR 63898, Dec. 3, 1993]



Sec.  146.9  Criteria for establishing permitting priorities.

    In determining priorities for setting times for owners or operators 
to submit applications for authorization to inject under the procedures 
of Sec.  144.31 (a), (c), (g) or Sec.  144.22(f), the Director shall 
base these priorities upon consideration of the following factors:
    (a) Injection wells known or suspected to be contaminating 
underground sources of drinking water;
    (b) Injection wells known to be injecting fluids containing 
hazardous contaminants;
    (c) Likelihood of contamination of underground sources of drinking 
water;
    (d) Potentially affected population;
    (e) Injection wells violating existing State requirements;
    (f) Coordination with the issuance of permits required by other 
State or Federal permit programs;
    (g) Age and depth of the injection well; and
    (h) Expiration dates of existing State permits, if any.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 48 FR 14293, Apr. 1, 1983]



Sec.  146.10  Plugging and abandoning Class I, II, III, IV, and V wells.

    (a) Requirements for Class I, II and III wells. (1) Prior to 
abandoning Class I, II and III wells, the well shall be plugged with 
cement in a manner which will not allow the movement of fluids either 
into or between underground sources of drinking water. The Director may 
allow Class III wells to use other plugging materials if the Director is 
satisfied that such materials will prevent movement of fluids into or

[[Page 892]]

between underground sources of drinking water.
    (2) Placement of the cement plugs shall be accomplished by one of 
the following:
    (i) The Balance method;
    (ii) The Dump Bailer method;
    (iii) The Two-Plug method; or
    (iv) An alternative method approved by the Director, which will 
reliably provide a comparable level of protection to underground sources 
of drinking water.
    (3) The well to be abandoned shall be in a state of static 
equilibrium with the mud weight equalized top to bottom, either by 
circulating the mud in the well at least once or by a comparable method 
prescribed by the Director, prior to the placement of the cement 
plug(s).
    (4) The plugging and abandonment plan required in 40 CFR 144.51(o) 
and 144.52(a)(6) shall, in the case of a Class III project which 
underlies or is in an aquifer which has been exempted under Sec.  
146.04, also demonstrate adequate protection of USDWs. The Director 
shall prescribe aquifer cleanup and monitoring where he deems it 
necessary and feasible to insure adequate protection of USDWs.
    (b) Requirements for Class IV wells. Prior to abandoning a Class IV 
well, the owner or operator shall close the well in accordance with 40 
CFR 144.23(b).
    (c) Requirements for Class V wells. (1) Prior to abandoning a Class 
V well, the owner or operator shall close the well in a manner that 
prevents the movement of fluid containing any contaminant into an 
underground source of drinking water, if the presence of that 
contaminant may cause a violation of any primary drinking water 
regulation under 40 CFR part 141 or may otherwise adversely affect the 
health of persons. Closure requirements for motor vehicle waste disposal 
wells and large-capacity cesspools are reiterated at Sec.  144.89.
    (2) The owner or operator shall dispose of or otherwise manage any 
soil, gravel, sludge, liquids, or other materials removed from or 
adjacent to the well in accordance with all applicable Federal, State, 
and local regulations and requirements.

[64 FR 68573, Dec. 7, 1999]



      Subpart B_Criteria and Standards Applicable to Class I Wells



Sec.  146.11  Criteria and standards applicable to Class I nonhazardous wells.

    This subpart establishes criteria and standards for underground 
injection control programs to regulate Class I nonhazardous wells.

[53 FR 28148, July 26, 1988]



Sec.  146.12  Construction requirements.

    (a) All Class I wells shall be sited in such a fashion that they 
inject into a formation which is beneath the lowermost formation 
containing, within one quarter mile of the well bore, an underground 
source of drinking water.
    (b) All Class I wells shall be cased and cemented to prevent the 
movement of fluids into or between underground sources of drinking 
water. The casing and cement used in the construction of each newly 
drilled well shall be designed for the life expectancy of the well. In 
determining and specifying casing and cementing requirements, the 
following factors shall be considered:
    (1) Depth to the injection zone;
    (2) Injection pressure, external pressure, internal pressure, and 
axial loading;
    (3) Hole size;
    (4) Size and grade of all casing strings (wall thickness, diameter, 
nominal weight, length, joint specification, and construction material);
    (5) Corrosiveness of injected fluid, formation fluids, and 
temperatures;
    (6) Lithology of injection and confining intervals; and
    (7) Type or grade of cement.
    (c) All Class I injection wells, except those municipal wells 
injecting non-corrosive wastes, shall inject fluids through tubing with 
a packer set immediately above the injection zone, or tubing with an 
approved fluid seal as an alternative. The tubing, packer, and fluid 
seal shall be designed for the expected service.

[[Page 893]]

    (1) The use of other alternatives to a packer may be allowed with 
the written approval of the Director. To obtain approval, the operator 
shall submit a written request to the Director, which shall set forth 
the proposed alternative and all technical data supporting its use. The 
Director shall approve the request if the alternative method will 
reliably provide a comparable level of protection to underground sources 
of drinking water. The Director may approve an alternative method solely 
for an individual well or for general use.
    (2) In determining and specifying requirements for tubing, packer, 
or alternatives the following factors shall be considered:
    (i) Depth of setting;
    (ii) Characteristics of injection fluid (chemical content, 
corrosiveness, and density);
    (iii) Injection pressure;
    (iv) Annular pressure;
    (v) Rate, temperature and volume of injected fluid; and
    (vi) Size of casing.
    (d) Appropriate logs and other tests shall be conducted during the 
drilling and construction of new Class I wells. A descriptive report 
interpreting the results of such logs and tests shall be prepared by a 
knowledgeable log analyst and submitted to the Director. At a minimum, 
such logs and tests shall include:
    (1) Deviation checks on all holes constructed by first drilling a 
pilot hole, and then enlarging the pilot hole by reaming or another 
method. Such checks shall be at sufficiently frequent intervals to 
assure that vertical avenues for fluid migration in the form of 
diverging holes are not created during drilling.
    (2) Such other logs and tests as may be needed after taking into 
account the availability of similar data in the area of the drilling 
site, the construction plan, and the need for additional information, 
that may arise from time to time as the construction of the well 
progresses. In determining which logs and tests shall be required, the 
following logs shall be considered for use in the following situations:
    (i) For surface casing intended to protect underground sources of 
drinking water:
    (A) Resistivity, spontaneous potential, and caliper logs before the 
casing is installed; and
    (B) A cement bond, temperature, or density log after the casing is 
set and cemented.
    (ii) For intermediate and long strings of casing intended to 
facilitate injection:
    (A) Resistivity, spontaneous potential, porosity, and gamma ray logs 
before the casing is installed;
    (B) Fracture finder logs; and
    (C) A cement bond, temperature, or density log after the casing is 
set and cemented.
    (e) At a minimum, the following information concerning the injection 
formation shall be determined or calculated for new Class I wells:
    (1) Fluid pressure;
    (2) Temperature;
    (3) Fracture pressure;
    (4) Other physical and chemical characteristics of the injection 
matrix; and
    (5) Physical and chemical characteristics of the formation fluids.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981]



Sec.  146.13  Operating, monitoring and reporting requirements.

    (a) Operating requirements. Operating requirements shall at a 
minimum, specify that:
    (1) Except during stimulation injection pressure at the wellhead 
shall not exceed a maximum which shall be calculated so as to assure 
that the pressure in the injection zone during injection does not 
initiate new fractures or propagate existing fractures in the injection 
zone. In no case shall injection pressure initiate fractures in the 
confining zone or cause the movement of injection or formation fluids 
into an underground source of drinking water.
    (2) Injection between the outermost casing protecting underground 
sources of drinking water and the well bore is prohibited.
    (3) Unless an alternative to a packer has been approved under Sec.  
146.12(c), the annulus between the tubing and the long string of casings 
shall be filled with a fluid approved by the Director and a pressure, 
also approved by the Director, shall be maintained on the annulus.

[[Page 894]]

    (b) Monitoring requirements. Monitoring requirements shall, at a 
minimum, include:
    (1) The analysis of the injected fluids with sufficient frequency to 
yield representative data of their characteristics;
    (2) Installation and use of continuous recording devices to monitor 
injection pressure, flow rate and volume, and the pressure on the 
annulus between the tubing and the long string of casing;
    (3) A demonstration of mechanical integrity pursuant to Sec.  146.8 
at least once every five years during the life of the well; and
    (4) The type, number and location of wells within the area of review 
to be used to monitor any migration of fluids into and pressure in the 
underground sources of drinking water, the parameters to be measured and 
the frequency of monitoring.
    (c) Reporting requirements. Reporting requirements shall, at a 
minimum, include:
    (1) Quarterly reports to the Director on:
    (i) The physical, chemical and other relevant characteristics of 
injection fluids;
    (ii) Monthly average, maximum and minimum values for injection 
pressure, flow rate and volume, and annular pressure; and
    (iii) The results of monitoring prescribed under paragraph (b)(4) of 
this section.
    (2) Reporting the results, with the first quarterly report after the 
completion, of:
    (i) Periodic tests of mechanical integrity;
    (ii) Any other test of the injection well conducted by the permittee 
if required by the Director; and
    (iii) Any well work over.
    (d) Ambient monitoring. (1) Based on a site-specific assessment of 
the potential for fluid movement from the well or injection zone and on 
the potential value of monitoring wells to detect such movement, the 
Director shall require the owner or operator to develop a monitoring 
program. At a minimum, the Director shall require monitoring of the 
pressure buildup in the injection zone annually, including at a minimum, 
a shut down of the well for a time sufficient to conduct a valid 
observation of the pressure fall-off curve.
    (2) When prescribing a monitoring system the Director may also 
require:
    (i) Continuous monitoring for pressure changes in the first aquifer 
overlying the confining zone. When such a well is installed, the owner 
or operator shall, on a quarterly basis, sample the aquifer and analyze 
for constituents specified by the Director;
    (ii) The use of indirect, geophysical techniques to determine the 
position of the waste front, the water quality in a formation designated 
by the Director, or to provide other site specific data;
    (iii) Periodic monitoring of the ground water quality in the first 
aquifer overlying the injection zone;
    (iv) Periodic monitoring of the ground water quality in the 
lowermost USDW; and
    (v) Any additional monitoring necessary to determine whether fluids 
are moving into or between USDWs.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
47 FR 32129, July 26, 1982; 53 FR 28148, July 26, 1988]



Sec.  146.14  Information to be considered by the Director.

    This section sets forth the information which must be considered by 
the Director in authorizing Class I wells. For an existing or converted 
new Class I well the Director may rely on the existing permit file for 
those items of information listed below which are current and accurate 
in the file. For a newly drilled Class I well, the Director shall 
require the submission of all the information listed below. For both 
existing and new Class I wells certain maps, cross-sections, tabulations 
of wells within the area of review and other data may be included in the 
application by reference provided they are current, readily available to 
the Director (for example, in the permitting agency's files) and 
sufficiently identified to be retrieved. In cases where EPA issues the 
permit all the information in this section must be submitted to the 
Administrator.
    (a) Prior to the issuance of a permit for an existing Class I well 
to operate or the construction or conversion of a new Class I well the 
Director shall consider the following:

[[Page 895]]

    (1) Information required in 40 CFR 144.31 and 144.31(g);
    (2) A map showing the injection well(s) for which a permit is sought 
and the applicable area of review. Within the area of review, the map 
must show the number, or name, and location of all producing wells, dry 
holes, surface bodies of water, springs, mines (surface and subsurface), 
quarries, water wells and other pertinent surface features including 
residences and roads. The map should also show faults, if known or 
suspected. Only information of public record is required to be included 
on this map;
    (3) A tabulation of data on all wells within the area of review 
which penetrate into the proposed injection zone. Such data shall 
include a description of each well's type, construction, date drilled, 
location, depth, record of plugging and/or completion, and any 
additional information the Director may require;
    (4) Maps and cross sections indicating the general vertical and 
lateral limits of all underground sources of drinking water within the 
area of review, their position relative to the injection formation and 
the direction of water movement, where known, in each underground source 
of drinking water which may be affected by the proposed injection;
    (5) Maps and cross sections detailing the geologic structure of the 
local area;
    (6) Generalized maps and cross sections illustrating the regional 
geologic setting;
    (7) Proposed operating data:
    (i) Average and maximum daily rate and volume of the fluid to be 
injected;
    (ii) Average and maximum injection pressure; and
    (iii) Source and an analysis of the chemical, physical, radiological 
and biological characteristics of injection fluids;
    (8) Proposed formation testing program to obtain an analysis of the 
chemical, physical and radiological characteristics of and other 
information on the receiving formation;
    (9) Proposed stimulation program;
    (10) Proposed injection procedure;
    (11) Schematic or other appropriate drawings of the surface and 
subsurface construction details of the well.
    (12) Contingency plans to cope with all shut-ins or well failures so 
as to prevent migration of fluids into any underground source of 
drinking water;
    (13) Plans (including maps) for meeting the monitoring requirements 
in Sec.  146.13(b);
    (14) For wells within the area of review which penetrate the 
injection zone but are not properly completed or plugged, the corrective 
action proposed to be taken under 40 CFR 144.55;
    (15) Construction procedures including a cementing and casing 
program, logging procedures, deviation checks, and a drilling, testing, 
and coring program; and
    (16) A certificate that the applicant has assured, through a 
performance bond or other appropriate means, the resources necessary to 
close, plug or abandon the well as required by 40 CFR 122.42(g).
    (b) Prior to granting approval for the operation of a Class I well 
the Director shall consider the following information:
    (1) All available logging and testing program data on the well;
    (2) A demonstration of mechanical integrity pursuant to Sec.  146.8;
    (3) The anticipated maximum pressure and flow rate at which the 
permittee will operate;
    (4) The results of the formation testing program;
    (5) The actual injection procedure;
    (6) The compatibility of injected waste with fluids in the injection 
zone and minerals in both the injection zone and the confining zone; and
    (7) The status of corrective action on defective wells in the area 
of review.
    (c) Prior to granting approval for the plugging and abandonment of a 
Class I well the Director shall consider the following information:
    (1) The type and number of plugs to be used;
    (2) The placement of each plug including the elevation of the top 
and bottom;
    (3) The type and grade and quantity of cement to be used;
    (4) The method for placement of the plugs; and

[[Page 896]]

    (5) The procedure to be used to meet the requirement of Sec.  
146.10(c).

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
48 FR 14293, Apr. 1, 1983]



Sec.  146.15  Class I municipal disposal well alternative authorization 
in certain parts of Florida.

    (a) Existing Class I municipal disposal wells in specific geographic 
regions as defined in paragraph (f) of this section may continue to 
inject without violating the regulatory prohibitions in Parts 144 and 
146 of this chapter against the movement of injection or formation 
fluids into a USDW, provided that such wells meet the requirements of 
this section, even if the Director determines they have caused or may 
cause fluid movement into a USDW. Nothing in this section excuses such 
Class I municipal disposal wells from meeting all other applicable State 
and Federal requirements including 40 CFR 144.12(a).
    (b) For purposes of this section, an existing Class I municipal 
disposal well is defined as a well for which a complete UIC construction 
permit application was received by the Director on or before December 
22, 2005.
    (c) For purposes of this section, the determination that a Class I 
municipal disposal well has caused or may cause movement of injection or 
formation fluids into a USDW may be made by the Director based on any 
relevant data available to him/her, including ground water monitoring 
data generated pursuant to regulatory requirements governing operation 
of Class I municipal disposal wells.
    (d) In order for a Class I municipal disposal well to qualify for 
authorization to inject pursuant to paragraph (a) of this section, the 
Owner/Operator of that well shall:
    (1) Develop and implement a pretreatment program that is no less 
stringent than the requirements of Chapter 62-625, Florida 
Administrative Code, or have no significant industrial users as defined 
in that chapter.
    (2) Treat the injectate using secondary treatment in a manner that 
is no less stringent than the requirements of Florida Rule 62-
600.420(1)(d), and using high-level disinfection in a manner that is no 
less stringent than the requirements of Florida Rule 62-600.440(5)(a)-
(f), within five years after notification by the Director that the well 
has caused or may cause fluid movement into a USDW.
    (e) Where the Director issued such notice for a well prior to 
December 22, 2005, in order for that well to qualify for authorization 
to inject pursuant to paragraph (a) of this section, the Owner/Operator 
shall:
    (1) Develop and implement a pretreatment program that is no less 
stringent than the requirements of Chapter 62-625, Florida 
Administrative Code, or have no significant industrial users as defined 
in that chapter; and
    (2) Treat the injectate using secondary treatment in a manner that 
is no less stringent than the requirements of Florida Rule 62-
600.420(1)(d), and using high-level disinfection in a manner that is no 
less stringent than the requirements of Florida Rule 62-600.440(5)(a)-
(f), within five years after December 22, 2005.
    (f) Authorization to inject wastewater into existing Class I 
municipal disposal wells pursuant to this section is limited to Class I 
municipal disposal wells in Florida in the following counties: Brevard, 
Broward, Charlotte, Collier, Flagler, Glades, Hendry, Highlands, 
Hillsborough, Indian River, Lee, Manatee, Martin, Miami-Dade, Monroe, 
Okeechobee, Orange, Osceola, Palm Beach, Pinellas, St. Johns, St. Lucie, 
Sarasota, and Volusia.

[70 FR 70531, Nov. 22, 2005]



Sec.  146.16  Requirements for new Class I municipal wells 
in certain parts of Florida.

    Prior to commencing injection, any Class I municipal disposal well 
in one of the counties identified in Sec.  146.15(f) that is not an 
existing Class I municipal disposal well as defined in Sec.  146.15(b) 
of this section shall meet all of the requirements for existing wells

[[Page 897]]

seeking authorization to inject pursuant to Sec.  146.15.

[70 FR 70532, Nov. 22, 2005]



      Subpart C_Criteria and Standards Applicable to Class II Wells



Sec.  146.21  Applicability.

    This subpart establishes criteria and standards for underground 
injection control programs to regulate Class II wells.



Sec.  146.22  Construction requirements.

    (a) All new Class II wells shall be sited in such a fashion that 
they inject into a formation which is separated from any USDW by a 
confining zone that is free of known open faults or fractures within the 
area of review.
    (b)(1) All Class II injection wells shall be cased and cemented to 
prevent movement of fluids into or between underground sources of 
drinking water. The casing and cement used in the construction of each 
newly drilled well shall be designed for the life expectancy of the 
well. In determining and specifying casing and cementing requirements, 
the following factors shall be considered:
    (i) Depth to the injection zone;
    (ii) Depth to the bottom of all USDWs; and
    (iii) Estimated maximum and average injection pressures;
    (2) In addition the Director may consider information on:
    (i) Nature of formation fluids;
    (ii) Lithology of injection and confining zones;
    (iii) External pressure, internal pressure, and axial loading;
    (iv) Hole size;
    (v) Size and grade of all casing strings; and
    (vi) Class of cement.
    (c) The requirements in paragraph (b) of this section need not apply 
to existing or newly converted Class II wells located in existing fields 
if:
    (1) Regulatory controls for casing and cementing existed for those 
wells at the time of drilling and those wells are in compliance with 
those controls; and
    (2) Well injection will not result in the movement of fluids into an 
underground source of drinking water so as to create a significant risk 
to the health of persons.
    (d) The requirements in paragraph (b) of this section need not apply 
to newly drilled wells in existing fields if;
    (1) They meet the requirements of the State for casing and cementing 
applicable to that field at the time of submission of the State program 
to the Administrator; and
    (2) Well injection will not result in the movement of fluids into an 
underground source of drinking water so as to create a significant risk 
to the health of persons.
    (e) Where a State did not have regulatory controls for casing and 
cementing prior to the time of the submission of the State program to 
the Administrator, the Director need not apply the casing and cementing 
requirements in paragraph (b) of this section if he submits as a part of 
his application for primacy, an appropriate plan for casing and 
cementing of existing, newly converted, and newly drilled wells in 
existing fields, and the Administrator approves the plan.
    (f) Appropriate logs and other tests shall be conducted during the 
drilling and construction of new Class II wells. A descriptive report 
interpreting the results of that portion of those logs and tests which 
specifically relate to (1) an USDW and the confining zone adjacent to 
it, and (2) the injection and adjacent formations shall be prepared by a 
knowledgeable log analyst and submitted to the director. At a minimum, 
these logs and tests shall include:
    (1) Deviation checks on all holes constructed by first drilling a 
pilot hole and then enlarging the pilot hole, by reaming or another 
method. Such checks shall be at sufficiently frequent intervals to 
assure that vertical avenues for fluid movement in the form of diverging 
holes are not created during drilling.
    (2) Such other logs and tests as may be needed after taking into 
account the availability of similar data in the area of the drilling 
site, the construction plan, and the need for additional information 
that may arise from time to time as the construction of the well 
progresses. In determining which logs

[[Page 898]]

and tests shall be required the following shall be considered by the 
Director in setting logging and testing requirements:
    (i) For surface casing intended to protect underground sources of 
drinking water in areas where the lithology has not been determined:
    (A) Electric and caliper logs before casing is installed; and
    (B) A cement bond, temperature, or density log after the casing is 
set and cemented.
    (ii) for intermediate and long strings of casing intended to 
facilitate injection:
    (A) Electric porosity and gamma ray logs before the casing is 
installed;
    (B) Fracture finder logs; and
    (C) A cement bond, temperature, or density log after the casing is 
set and cemented.
    (g) At a minimum, the following information concerning the injection 
formation shall be determined or calculated for new Class II wells or 
projects:
    (1) Fluid pressure;
    (2) Estimated fracture pressure;
    (3) Physical and chemical characteristics of the injection zone.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
47 FR 5000, Feb. 3, 1982]



Sec.  146.23  Operating, monitoring, and reporting requirements.

    (a) Operating requirements. Operating requirements shall, at a 
minimum, specify that:
    (1) Injection pressure at the wellhead shall not exceed a maximum 
which shall be calculated so as to assure that the pressure during 
injection does not initiate new fractures or propagate existing 
fractures in the confining zone adjacent to the USDWs. In no case shall 
injection pressure cause the movement of injection or formation fluids 
into an underground source of drinking water
    (2) Injection between the outermost casing protecting underground 
sources of drinking water and the well bore shall be prohibited.
    (b) Monitoring requirements. Monitoring requirements shall, at a 
minimum, include:
    (1) Monitoring of the nature of injected fluids at time intervals 
sufficiently frequent to yield data representative of their 
characteristics;
    (2) Observation of injection pressure, flow rate, and cumulative 
volume at least with the following frequencies:
    (i) Weekly for produced fluid disposal operations;
    (ii) Monthly for enhanced recovery operations;
    (iii) Daily during the injection of liquid hydrocarbons and 
injection for withdrawal of stored hydrocarbons; and
    (iv) Daily during the injection phase of cyclic steam operations

And recording of one observation of injection pressure, flow rate and 
cumulative volume at reasonable intervals no greater than 30 days.
    (3) A demonstration of mechanical integrity pursuant to Sec.  146.8 
at least once every five years during the life of the injection well;
    (4) Maintenance of the results of all monitoring until the next 
permit review (see 40 CFR 144.52(a)(5)); and
    (5) Hydrocarbon storage and enhanced recovery may be monitored on a 
field or project basis rather than on an individual well basis by 
manifold monitoring. Manifold monitoring may be used in cases of 
facilities consisting of more than one injection well, operating with a 
common manifold. Separate monitoring systems for each well are not 
required provided the owner/operator demonstrates that manifold 
monitoring is comparable to individual well monitoring.
    (c) Reporting requirements. (1) Reporting requirements shall at a 
minimum include an annual report to the Director summarizing the results 
of monitoring required under paragraph (b) of this section. Such summary 
shall include monthly records of injected fluids, and any major changes 
in characteristics or sources of injected fluid. Previously submitted 
information may be included by reference.
    (2) Owners or operators of hydrocarbon storage and enhanced recovery 
projects may report on a field or project basis rather than an 
individual

[[Page 899]]

well basis where manifold monitoring is used.

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act; 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
47 FR 5000, Feb. 3, 1982; 48 FR 14293, Apr. 1, 1983; 48 FR 31404, July 
8, 1983]



Sec.  146.24  Information to be considered by the Director.

    This section sets forth the information which must be considered by 
the Director in authorizing Class II wells. Certain maps, cross-
sections, tabulations of wells within the area of review, and other data 
may be included in the application by reference provided they are 
current, readily available to the Director (for example, in the 
permitting agency's files) and sufficiently identified to be retrieved. 
In cases where EPA issues the permit, all the information in this 
section is to be submitted to the Administrator.
    (a) Prior to the issuance of a permit for an existing Class II well 
to operate or the construction or conversion of a new Class II well the 
Director shall consider the following:
    (1) Information required in 40 CFR 144.31 and 144.31(g);
    (2) A map showing the injection well or project area for which a 
permit is sought and the applicable area of review. Within the area of 
review, the map must show the number or name and location of all 
existing producing wells, injection wells, abandoned wells, dry holes, 
and water wells. The map may also show surface bodies of waters, mines 
(surface and subsurface), quarries and other pertinent surface features 
including residences and roads, and faults if known or suspended. Only 
information of public record and pertinent information known to the 
applicant is required to be included on this map. This requirement does 
not apply to existing Class II wells; and
    (3) A tabulation of data reasonably available from public records or 
otherwise known to the applicant on all wells within the area of review 
included on the map required under paragraph (a)(2) of this section 
which penetrate the proposed injection zone or, in the case of Class II 
wells operating over the fracture pressure of the injection formation, 
all known wells within the area of review which penetrate formations 
affected by the increase in pressure. Such data shall include a 
description of each well's type, construction, date drilled, location, 
depth, record of plugging and complete, and any additional information 
the Director may require. In cases where the information would be 
repetitive and the wells are of similar age, type, and construction the 
Director may elect to only require data on a representative number of 
wells. This requirement does not apply to existing Class II wells.
    (4) Proposed operating data:
    (i) Average and maximum daily rate and volume of fluids to be 
injected.
    (ii) Average and maximum injection pressure; and
    (iii) Source and an appropriate analysis of the chemical and 
physical characteristics of the injection fluid.
    (5) Appropriate geological data on the injection zone and confining 
zone including lithologic description, geological name, thickness and 
depth;
    (6) Geologic name and depth to bottom of all underground sources of 
drinking water which may be affected by the injection;
    (7) Schematic or other appropriate drawings of the surface and 
subsurface construction details of the well;
    (8) In the case of new injection wells the corrective action 
proposed to be taken by the applicant under 40 CFR 122.44;
    (9) A certificate that the applicant has assured through a 
performance bond or other appropriate means, the resources necessary to 
close plug or abandon the well as required by 40 CFR 122.42(g);
    (b) In addition the Director may consider the following:
    (1) Proposed formation testing program to obtain the information 
required by Sec.  146.22(g);
    (2) Proposed stimulation program;
    (3) Proposed injection procedure;
    (4) Proposed contingency plans, if any, to cope with well failures 
so as to prevent migration of contaminating fluids into an underground 
source of drinking water;

[[Page 900]]

    (5) Plans for meeting the monitoring requirements of Sec.  
146.23(b).
    (c) Prior to granting approval for the operation of a Class II well 
the Director shall consider the following information:
    (1) All available logging and testing program data on the well;
    (2) A demonstration of mechanical integrity pursuant to Sec.  146.8;
    (3) The anticipated maximum pressure and flow rate at which the 
permittee will operate.
    (4) The results of the formation testing program;
    (5) The actual injection procedure; and
    (6) For new wells the status of corrective action on defective wells 
in the area of review.
    (d) Prior to granting approval for the plugging and abandonment of a 
Class II well the Director shall consider the following information:
    (1) The type, and number of plugs to be used;
    (2) The placement of each plug including the elevation of top and 
bottom;
    (3) The type, grade, and quantity of cement to be used;
    (4) The method of placement of the plugs; and
    (5) The procedure to be used to meet the requirements of Sec.  
146.10(c).

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43162, Aug. 27, 1981; 
47 FR 5000, Feb. 3, 1982; 48 FR 14293, Apr. 1, 1983]



     Subpart D_Criteria and Standards Applicable to Class III Wells



Sec.  146.31  Applicability.

    This subpart establishes criteria and standards for underground 
injection control programs to regulate Class III wells.



Sec.  146.32  Construction requirements.

    (a) All new Class III wells shall be cased and cemented to prevent 
the migration of fluids into or between underground sources of drinking 
water. The Director may waive the cementing requirement for new wells in 
existing projects or portions of existing projects where he has 
substantial evidence that no contamination of underground sources of 
drinking water would result. The casing and cement used in the 
construction of each newly drilled well shall be designed for the life 
expectancy of the well. In determining and specifying casing and 
cementing requirements, the following factors shall be considered:
    (1) Depth to the injection zone;
    (2) Injection pressure, external pressure, internal pressure, axial 
loading, etc.;
    (3) Hole size;
    (4) Size and grade of all casing strings (wall thickness, diameter, 
nominal weight, length, joint specification, and construction material);
    (5) Corrosiveness of injected fluids and formation fluids;
    (6) Lithology of injection and confining zones; and
    (7) Type and grade of cement.
    (b) Appropriate logs and other tests shall be conducted during the 
drilling and construction of new Class III wells. A descriptive report 
interpreting the results of such logs and tests shall be prepared by a 
knowledgeable log analyst and submitted to the Director. The logs and 
tests appropriate to each type of Class III well shall be determined 
based on the intended function, depth, construction and other 
characteristics of the well, availability of similar data in the area of 
the drilling site and the need for additional information that may arise 
from time to time as the construction of the well progresses. Deviation 
checks shall be conducted on all holes where pilot holes and reaming are 
used, unless the hole will be cased and cemented by circulating cement 
to the surface. Where deviation checks are necessary they shall be 
conducted at sufficiently frequent intervals to assure that vertical 
avenues for fluid migration in the form of diverging holes are not 
created during drillings.
    (c) Where the injection zone is a formation which is naturally 
water-bearing the following information concerning the injection zone 
shall be determined or calculated for new Class III wells or projects:
    (1) Fluid pressure;
    (2) Fracture pressure; and

[[Page 901]]

    (3) Physical and chemical characteristics of the formation fluids.
    (d) Where the injection formation is not a water-bearing formation, 
the information in paragraph (c)(2) of this section must be submitted.
    (e) Where injection is into a formation which contains water with 
less than 10,000 mg/l TDS monitoring wells shall be completed into the 
injection zone and into any underground sources of drinking water above 
the injection zone which could be affected by the mining operation. 
These wells shall be located in such a fashion as to detect any 
excursion of injection fluids, process by-products, or formation fluids 
outside the mining area or zone. If the operation may be affected by 
subsidence or catastrophic collapse the monitoring wells shall be 
located so that they will not be physically affected.
    (f) Where injection is into a formation which does not contain water 
with less than 10,000 mg/l TDS, no monitoring wells are necessary in the 
injection stratum.
    (g) Where the injection wells penetrate an USDW in an area subject 
to subsidence or catastrophic collapse an adequate number of monitoring 
wells shall be completed into the USDW to detect any movement of 
injected fluids, process by-products or formation fluids into the USDW. 
The monitoring wells shall be located outside the physical influence of 
the subsidence or catastrophic collapse.
    (h) In determining the number, location, construction and frequency 
of monitoring of the monitoring wells the following criteria shall be 
considered:
    (1) The population relying on the USDW affected or potentially 
affected by the injection operation;
    (2) The proximity of the injection operation to points of withdrawal 
of drinking water;
    (3) The local geology and hydrology;
    (4) The operating pressures and whether a negative pressure gradient 
is being maintained;
    (5) The nature and volume of the injected fluid, the formation 
water, and the process by-products; and
    (6) The injection well density.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43163, Aug. 27, 1981; 
47 FR 5000, Feb. 3, 1982]



Sec.  146.33  Operating, monitoring, and reporting requirements.

    (a) Operating requirements. Operating requirements prescribed shall, 
at a minimum, specify that:
    (1) Except during well stimulation injection pressure at the 
wellhead shall be calculated so as to assure that the pressure in the 
injection zone during injection does not initiate new fractures or 
propagate existing fractures in the injection zone. In no case, shall 
injection pressure initiate fractures in the confining zone or cause the 
migration of injection or formation fluids into an underground source of 
drinking water.
    (2) Injection between the outermost casing protecting underground 
sources of drinking water and the well bore is prohibited.
    (b) Monitoring requirements. Monitoring requirements shall, at a 
minimum, specify:
    (1) Monitoring of the nature of injected fluids with sufficient 
frequency to yield representative data on its characteristics. Whenever 
the injection fluid is modified to the extent that the analysis required 
by Sec.  146.34(a)(7)(iii) is incorrect or incomplete, a new analysis as 
required by Sec.  146.34(a)(7)(iii) shall be provided to the Director.
    (2) Monitoring of injection pressure and either flow rate or volume 
semi-monthly, or metering and daily recording of injected and produced 
fluid volumes as appropriate.
    (3) Demonstration of mechanical integrity pursuant to Sec.  146.08 
at least once every five years during the life of the well for salt 
solution mining.
    (4) Monitoring of the fluid level in the injection zone semi-
monthly, where appropriate and monitoring of the parameters chosen to 
measure water quality in the monitoring wells required by Sec.  
146.32(e), semi-monthly.
    (5) Quarterly monitoring of wells required by Sec.  146.32(g).
    (6) All Class III wells may be monitored on a field or project basis 
rather than an individual well basis by manifold monitoring. Manifold 
monitoring may be used in cases of facilities consisting of more than 
one injection well, operating with a common manifold. Separate 
monitoring systems for each well are not required provided the

[[Page 902]]

owner/operator demonstrates that manifold monitoring is comparable to 
individual well monitoring.
    (c) Reporting requirements. Reporting requirements shall, at a 
minimum, include:
    (1) Quarterly reporting to the Director on required monitoring;
    (2) Results of mechanical integrity and any other periodic test 
required by the Director reported with the first regular quarterly 
report after the completion of the test; and
    (3) Monitoring may be reported on a project or field basis rather 
than individual well basis where manifold monitoring is used.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43163, Aug. 27, 1981; 
46 FR 5001, Feb. 3, 1982; 48 FR 31404, July 8, 1983]



Sec.  146.34  Information to be considered by the Director.

    This section sets forth the information which must be considered by 
the Director in authorizing Class III wells. Certain maps, cross 
sections, tabulations of wells within the area of review, and other data 
may be included in the application by reference provided they are 
current, readily available to the Director (for example, in the 
permitting agency's files) and sufficiently identified to be retrieved. 
In cases where EPA issues the permit, all the information in this 
section must be submitted to the Administrator.
    (a) Prior to the issuance of a permit for an existing Class III well 
or area to operate or the construction of a new Class III well the 
Director shall consider the following:
    (1) Information required in 40 CFR 144.31 and 144.31(g);
    (2) A map showing the injection well or project area for which a 
permit is sought and the applicable area of review. Within the area of 
review, the map must show the number or name and location of all 
existing producing wells, injection wells, abandoned wells, dry holes, 
public water systems and water wells. The map may also show surface 
bodies of waters, mines (surface and subsurface), quarries and other 
pertinent surface features including residences and roads, and faults if 
known or suspected. Only information of public record and pertinent 
information known to the applicant is required to be included on this 
map.
    (3) A tabulation of data reasonably available from public records or 
otherwise known to the applicant on wells within the area of review 
included on the map required under paragraph (a)(2) of this section 
which penetrate the proposed injection zone. Such data shall include a 
description of each well's type, construction, date drilled, location, 
depth, record of plugging and completion, and any additional information 
the Director may require. In cases where the information would be 
repetitive and the wells are of similar age, type, and construction the 
Director may elect to only require data on a representative number of 
wells.
    (4) Maps and cross sections indicating the vertical limits of all 
underground sources of drinking water within the area of review, their 
position relative to the injection formation, and the direction of water 
movement, where known, in every underground source of drinking water 
which may be affected by the proposed injection:
    (5) Maps and cross sections detailing the geologic structure of the 
local area;
    (6) Generalized map and cross sections illustrating the regional 
geologic setting;
    (7) Proposed operating data:
    (i) Average and maximum daily rate and volume of fluid to be 
injected;
    (ii) Average and maximum injection pressure; and
    (iii) Qualitative analysis and ranges in concentrations of all 
constituents of injected fluids. The applicant may request Federal 
confidentiality as specified in 40 CFR part 2. If the information is 
proprietary an applicant may, in lieu of the ranges in concentrations, 
choose to submit maximum concentrations which shall not be exceeded. In 
such a case the applicant shall retain records of the undisclosed 
concentrations and provide them upon request to the Director as part of 
any enforcement investigation.
    (8) Proposed formation testing program to obtain the information 
required by Sec.  146.32(c).
    (9) Proposed stimulation program;
    (10) Proposed injection procedure;

[[Page 903]]

    (11) Schematic or other appropriate drawings of the surface and 
subsurface construction details of the well;
    (12) Plans (including maps) for meeting the monitoring requirements 
of Sec.  146.33(b);
    (13) Expected changes in pressure, native fluid displacement, 
direction of movement of injection fluid;
    (14) Contingency plans to cope with all shut-ins or well failures so 
as to prevent the migration of contaminating fluids into underground 
sources of drinking water;
    (15) A certificate that the applicant has assured, through a 
performance bond, or other appropriate means, the resources necessary to 
close, plug, or abandon the well as required by 40 CFR 144.52(a)(7) and
    (16) The corrective action proposed to be taken under 40 CFR 144.55.
    (b) Prior to granting approval for the operation of a Class III well 
the Director shall consider the following information:
    (1) All available logging and testing data on the well;
    (2) A satisfactory demonstration of mechanical integrity for all new 
wells and for all existing salt solution wells pursuant to Sec.  146.08;
    (3) The anticipated maximum pressure and flow rate at which the 
permittee will operate;
    (4) The results of the formation testing program;
    (5) The actual injection procedures; and
    (6) The status of corrective action on defective wells in the area 
of review.
    (c) Prior to granting approval for the plugging and abandonment of a 
Class III well the Director shall consider the following information:
    (1) The type and number of plugs to be used;
    (2) The placement of each plug including the elevation of the top 
and bottom;
    (3) The type, grade, and quantity of cement to be used;
    (4) The method of placement of the plugs; and
    (5) The procedure to be used to meet the requirements of Sec.  
146.10(c).

(Clean Water Act, Safe Drinking Water Act, Clean Air Act, Resource 
Conservation and Recovery Act: 42 U.S.C. 6905, 6912, 6925, 6927, 6974)

[45 FR 42500, June 24, 1980, as amended at 46 FR 43163, Aug. 27, 1981; 
47 FR 5001, Feb. 3, 1982; 48 FR 14293, Apr. 1, 1983]

Subpart E--Criteria and Standards Applicable to Class IV Injection Wells 
[Reserved]



 Subpart F_Criteria and Standards Applicable to Class V Injection Wells



Sec.  146.51  Applicability.

    This subpart sets forth criteria and standards for underground 
injection control programs to regulate all injection not regulated in 
subparts B, C, D, and E.
    (a) Generally, wells covered by this subpart inject non-hazardous 
fluids into or above formations that contain underground sources of 
drinking water. It includes all wells listed in Sec.  146.5(e) but is 
not limited to those types of injection wells.
    (b) It also includes wells not covered in Class IV that inject 
radioactive material listed in 10 CFR part 20, appendix B, table II, 
column 2.

[45 FR 42500, June 24, 1980, as amended at 47 FR 5001, Feb. 3, 1982]



 Subpart G_Criteria and Standards Applicable to Class I Hazardous Waste 
                             Injection Wells

    Source: 53 FR 28148, July 26, 1988, unless otherwise noted.



Sec.  146.61  Applicability.

    (a) This subpart establishes criteria and standards for underground 
injection control programs to regulate Class I hazardous waste injection 
wells. Unless otherwise noted this subpart supplements the requirements 
of subpart A and applies instead of subpart B to Class I hazardous waste 
injection wells.
    (b) Definitions.
    Cone of influence means that area around the well within which 
increased

[[Page 904]]

injection zone pressures caused by injection into the hazardous waste 
injection well would be sufficient to drive fluids into an underground 
source of drinking water (USDW).
    Existing well means a Class I well which was authorized prior to 
August 25, 1988, by an approved State program, or an EPA-administered 
program or a well which has become a Class I well as a result of a 
change in the definition of the injected waste which would render the 
waste hazardous under Sec.  261.3 of this part.
    Injection interval means that part of the injection zone in which 
the well is screened, or in which the waste is otherwise directly 
emplaced.
    New well means any Class I hazardous waste injection well which is 
not an existing well.
    Transmissive fault or fracture is a fault or fracture that has 
sufficient permeability and vertical extent to allow fluids to move 
between formations.



Sec.  146.62  Minimum criteria for siting.

    (a) All Class I hazardous waste injection wells shall be sited such 
that they inject into a formation that is beneath the lowermost 
formation containing within one quarter mile of the well bore an 
underground source of drinking water.
    (b) The siting of Class I hazardous waste injection wells shall be 
limited to areas that are geologically suitable. The Director shall 
determine geologic suitability based upon:
    (1) An analysis of the structural and stratigraphic geology, the 
hydrogeology, and the seismicity of the region;
    (2) An analysis of the local geology and hydrogeology of the well 
site, including, at a minimum, detailed information regarding 
stratigraphy, structure and rock properties, aquifer hydrodynamics and 
mineral resources; and
    (3) A determination that the geology of the area can be described 
confidently and that limits of waste fate and transport can be 
accurately predicted through the use of models.
    (c) Class I hazardous waste injection wells shall be sited such 
that:
    (1) The injection zone has sufficient permeability, porosity, 
thickness and areal extent to prevent migration of fluids into USDWs.
    (2) The confining zone:
    (i) Is laterally continuous and free of transecting, transmissive 
faults or fractures over an area sufficient to prevenet the movement of 
fluids into a USDW; and
    (ii) Contains at least one formation of sufficient thickness and 
with lithologic and stress characteristics capable of preventing 
vertical propagation of fractures.
    (d) The owner or operator shall demonstrate to the satisfaction of 
the Director that:
    (1) The confining zone is separated from the base of the lowermost 
USDW by at least one sequence of permeable and less permeable strata 
that will provide an added layer of protection for the USDW in the event 
of fluid movement in an unlocated borehole or transmissive fault; or
    (2) Within the area of review, the piezometric surface of the fluid 
in the injection zone is less than the piezometric surface of the 
lowermost USDW, considering density effects, injection pressures and any 
significant pumping in the overlying USDW; or
    (3) There is no USDW present.
    (4) The Director may approve a site which does not meet the 
requirements in paragraphs (d) (1), (2), or (3) of this section if the 
owner or operator can demonstrate to the Director that because of the 
geology, nature of the waste, or other considerations, abandoned 
boreholes or other conduits would not cause endangerment of USDWs.



Sec.  146.63  Area of review.

    For the purposes of Class I hazardous waste wells, this section 
shall apply to the exclusion of Sec.  146.6. The area of review for 
Class I hazardous waste injection wells shall be a 2-mile radius around 
the well bore. The Director may specify a larger area of review based on 
the calculated cone of influence of the well.



Sec.  146.64  Corrective action for wells in the area of review.

    For the purposes of Class I hazardous waste wells, this section 
shall apply to the exclusion of Sec. Sec.  144.55 and 146.07.

[[Page 905]]

    (a) The owner or operator of a Class I hazardous waste well shall as 
part of the permit application submit a plan to the Director outlining 
the protocol used to:
    (1) Identify all wells penetrating the confining zone or injection 
zone within the area of review; and
    (2) Determine whether wells are adequately completed or plugged.
    (b) The owner or operator of a Class I hazardous waste well shall 
identify the location of all wells within the area of review that 
penetrate the injection zone or the confining zone and shall submit as 
required in Sec.  146.70(a):
    (1) A tabulation of all wells within the area of review that 
penetrate the injection zone or the confining zone; and
    (2) A description of each well or type of well and any records of 
its plugging or completion.
    (c) For wells that the Director determines are improperly plugged, 
completed, or abandoned, or for which plugging or completion information 
is unavailable, the applicant shall also submit a plan consisting of 
such steps or modification as are necessary to prevent movement of 
fluids into or between USDWs. Where the plan is adequate, the Director 
shall incorporate it into the permit as a condition. Where the 
Director's review of an application indicates that the permittee's plan 
is inadequate (based at a minimum on the factors in paragraph (e) of 
this section), the Director shall:
    (1) Require the applicant to revise the plan;
    (2) Prescribe a plan for corrective action as a condition of the 
permit; or
    (3) Deny the application.
    (d) Requirements:
    (1) Existing injection wells. Any permit issued for an existing 
Class I hazardous waste injection well requiring corrective action other 
than pressure limitations shall include a compliance schedule requiring 
any corrective action accepted or prescribed under paragraph (c) of this 
section. Any such compliance schedule shall provide for compliance no 
later than 2 years following issuance of the permit and shall require 
observance of appropriate pressure limitations under paragraph (d)(3) 
until all other corrective action measures have been implemented.
    (2) New injection wells. No owner or operator of a new Class I 
hazardous waste injection well may begin injection until all corrective 
actions required under this section have been taken.
    (3) The Director may require pressure limitations in lieu of 
plugging. If pressure limitations are used in lieu of plugging, the 
Director shall require as a permit condition that injection pressure be 
so limited that pressure in the injection zone at the site of any 
improperly completed or abandoned well within the area of review would 
not be sufficient to drive fluids into or between USDWs. This pressure 
limitation shall satisfy the corrective action requirement. 
Alternatively, such injection pressure limitation may be made part of a 
compliance schedule and may be required to be maintained until all other 
required corrective actions have been implemented.
    (e) In determining the adequacy of corrective action proposed by the 
applicant under paragraph (c) of this section and in determining the 
additional steps needed to prevent fluid movement into and between 
USDWs, the following criteria and factors shall be considered by the 
Director:
    (1) Nature and volume of injected fluid;
    (2) Nature of native fluids or byproducts of injection;
    (3) Geology;
    (4) Hydrology;
    (5) History of the injection operation;
    (6) Completion and plugging records;
    (7) Closure procedures in effect at the time the well was closed;
    (8) Hydraulic connections with USDWs;
    (9) Reliability of the procedures used to identify abandoned wells; 
and
    (10) Any other factors which might affect the movement of fluids 
into or between USDWs.



Sec.  146.65  Construction requirements.

    (a) General. All existing and new Class I hazardous waste injection 
wells shall be constructed and completed to:
    (1) Prevent the movement of fluids into or between USDWs or into any 
unauthorized zones;

[[Page 906]]

    (2) Permit the use of appropriate testing devices and workover 
tools; and
    (3) Permit continuous monitoring of injection tubing and long string 
casing as required pursuant to Sec.  146.67(f).
    (b) Compatibility. All well materials must be compatible with fluids 
with which the materials may be expected to come into contact. A well 
shall be deemed to have compatibility as long as the materials used in 
the construction of the well meet or exceed standards developed for such 
materials by the American Petroleum Institute, The American Society for 
Testing Materials, or comparable standards acceptable to the Director.
    (c) Casing and Cementing of New Wells. (1) Casing and cement used in 
the construction of each newly drilled well shall be designed for the 
life expectancy of the well, including the post-closure care period. The 
casing and cementing program shall be designed to prevent the movement 
of fluids into or between USDWs, and to prevent potential leaks of 
fluids from the well. In determining and specifying casing and cementing 
requirements, the Director shall consider the following information as 
required by Sec.  146.70:
    (i) Depth to the injection zone;
    (ii) Injection pressure, external pressure, internal pressure and 
axial loading;
    (iii) Hole size;
    (iv) Size and grade of all casing strings (well thickness, diameter, 
nominal weight, length, joint specification and construction material);
    (v) Corrosiveness of injected fluid, formation fluids and 
temperature;
    (vi) Lithology of injection and confining zones;
    (vii) Type or grade of cement; and
    (viii) Quantity and chemical composition of the injected fluid.
    (2) One surface casing string shall, at a minimum, extend into the 
confining bed below the lowest formation that contains a USDW and be 
cemented by circulating cement from the base of the casing to the 
surface, using a minimum of 120% of the calculated annual volume. The 
Director may require more than 120% when the geology or other 
circumstances warrant it.
    (3) At least one long string casing, using a sufficient number of 
centralizers, shall extend to the injection zone and shall be cemented 
by circulating cement to the surface in one or more stages:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure; and
    (ii) In a quantity no less than 120% of the calculated volume 
necessary to fill the annular space. The Director may require more than 
120% when the geology or other circumstances warrant it.
    (4) Circulation of cement may be accomplished by staging. The 
Director may approve an alternative method of cementing in cases where 
the cement cannot be recirculated to the surface, provided the owner or 
operator can demonstrate by using logs that the cement is continuous and 
does not allow fluid movement behind the well bore.
    (5) Casings, including any casing connections, must be rated to have 
sufficient structural strength to withstand, for the design life of the 
well:
    (i) The maximum burst and collapse pressures which may be 
experienced during the construction, operation and closure of the well; 
and
    (ii) The maximum tensile stress which may be experienced at any 
point along the length of the casing during the construction, operation, 
and closure of the well.
    (6) At a minimum, cement and cement additivies must be of sufficient 
quality and quantity to maintain integrity over the design life of the 
well.
    (d) Tubing and packer. (1) All Class I hazardous waste injection 
wells shall inject fluids through tubing with a packer set at a point 
specified by the Director.
    (2) In determining and specifying requirements for tubing and 
packer, the following factors shall be considered:
    (i) Depth of setting;
    (ii) Characteristics of injection fluid (chemical content, 
corrosiveness, temperature and density);
    (iii) Injection pressure;
    (iv) Annular pressure;
    (v) Rate (intermittent or continuous), temperature and volume of 
injected fluid;
    (vi) Size of casing; and
    (vii) Tubing tensile, burst, and collapse strengths.

[[Page 907]]

    (3) The Director may approve the use of a fluid seal if he 
determines that the following conditions are met:
    (i) The operator demonstrates that the seal will provide a level of 
protection comparable to a packer;
    (ii) The operator demonstrates that the staff is, and will remain, 
adequately trained to operate and maintain the well and to identify and 
interpret variations in parameters of concern;
    (iii) The permit contains specific limitations on variations in 
annular pressure and loss of annular fluid;
    (iv) The design and construction of the well allows continuous 
monitoring of the annular pressure and mass balance of annular fluid; 
and
    (v) A secondary system is used to monitor the interface between the 
annulus fluid and the injection fluid and the permit contains 
requirements for testing the system every three months and recording the 
results.



Sec.  146.66  Logging, sampling, and testing prior to new well operation.

    (a) During the drilling and construction of a new Class I hazardous 
waste injection well, appropriate logs and tests shall be run to 
determine or verify the depth, thickness, porosity, permeability, and 
rock type of, and the salinity of any entrained fluids in, all relevant 
geologic units to assure conformance with performance standards in Sec.  
146.65, and to establish accurate baseline data against which future 
measurements may be compared. A descriptive report interpreting results 
of such logs and tests shall be prepared by a knowledgeable log analyst 
and submitted to the Director. At a minimum, such logs and tests shall 
include:
    (1) Deviation checks during drilling on all holes constructed by 
drilling a pilot hole which are enlarged by reaming or another method. 
Such checks shall be at sufficiently frequent intervals to determine the 
location of the borehole and to assure that vertical avenues for fluid 
movement in the form of diverging holes are not created during drilling; 
and
    (2) Such other logs and tests as may be needed after taking into 
account the availability of similar data in the area of the drilling 
site, the construction plan, and the need for additional information 
that may arise from time to time as the construction of the well 
progresses. At a minimum, the following logs shall be required in the 
following situations:
    (i) Upon installation of the surface casing:
    (A) Resistivity, spontaneous potential, and caliper logs before the 
casing is installed; and
    (B) A cement bond and variable density log, and a temperature log 
after the casing is set and cemented.
    (ii) Upon installation of the long string casing:
    (A) Resistivity, spontaneous potential, porosity, caliper, gamma 
ray, and fracture finder logs before the casing is installed; and
    (B) A cement bond and variable density log, and a temperature log 
after the casing is set and cemented.
    (iii) The Director may allow the use of an alternative to the above 
logs when an alternative will provide equivalent or better information; 
and
    (3) A mechanical integrity test consisting of:
    (i) A pressure test with liquid or gas;
    (ii) A radioactive tracer survey;
    (iii) A temperature or noise log;
    (iv) A casing inspection log, if required by the Director; and
    (v) Any other test required by the Director.
    (b) Whole cores or sidewall cores of the confining and injection 
zones and formation fluid samples from the injection zone shall be 
taken. The Director may accept cores from nearby wells if the owner or 
operator can demonstrate that core retrieval is not possible and that 
such cores are representative of conditions at the well. The Director 
may require the owner or operator to core other formations in the 
borehole.
    (c) The fluid temperature, pH, conductivity, pressure and the static 
fluid level of the injection zone must be recorded.
    (d) At a minimum, the following information concerning the injection 
and confining zones shall be determined or calculated for Class I 
hazardous waste injection wells:
    (1) Fracture pressure;

[[Page 908]]

    (2) Other physical and chemical characteristics of the injection and 
confining zones; and
    (3) Physical and chemical characteristics of the formation fluids in 
the injection zone.
    (e) Upon completion, but prior to operation, the owner or operator 
shall conduct the following tests to verify hydrogeologic 
characteristics of the injection zone:
    (1) A pump test; or
    (2) Injectivity tests.
    (f) The Director shall have the opportunity to witness all logging 
and testing by this subpart. The owner or operator shall submit a 
schedule of such activities to the Director 30 days prior to conducting 
the first test.



Sec.  146.67  Operating requirements.

    (a) Except during stimulation, the owner or operator shall assure 
that injection pressure at the wellhead does not exceed a maximum which 
shall be calculated so as to assure that the pressure in the injection 
zone during injection does not initiate new fractures or propagate 
existing fractures in the injection zone. The owner or operator shall 
assure that the injection pressure does not initiate fractures or 
propagate existing fractures in the confining zone, nor cause the 
movement of injection or formation fluids into a USDW.
    (b) Injection between the outermost casing protecting USDWs and the 
well bore is prohibited.
    (c) The owner or operator shall maintain an annulus pressure that 
exceeds the operating injection pressure, unless the Director determines 
that such a requirement might harm the integrity of the well. The fluid 
in the annulus shall be noncorrosive, or shall contain a corrosion 
inhibitor.
    (d) The owner or operator shall maintain mechanical integrity of the 
injection well at all times.
    (e) Permit requirements for owners or operators of hazardous waste 
wells which inject wastes which have the potential to react with the 
injection formation to generate gases shall include:
    (1) Conditions limiting the temperature, pH or acidity of the 
injected waste; and
    (2) Procedures necessary to assure that pressure imbalances which 
might cause a backflow or blowout do not occur.
    (f) The owner or operator shall install and use continuous recording 
devices to monitor: the injection pressure; the flow rate, volume, and 
temperature of injected fluids; and the pressure on the annulus between 
the tubing and the long string casing, and shall install and use:
    (1) Automatic alarm and automatic shut-off systems, designed to 
sound and shut-in the well when pressures and flow rates or other 
parameters approved by the Director exceed a range and/or gradient 
specified in the permit; or
    (2) Automatic alarms, designed to sound when the pressures and flow 
rates or other parameters approved by the Director exceed a rate and/or 
gradient specified in the permit, in cases where the owner or operator 
certifies that a trained operator will be on-site at all times when the 
well is operating.
    (g) If an automatic alarm or shutdown is triggered, the owner or 
operator shall immediately investigate and identify as expeditiously as 
possible the cause of the alarm or shutoff. If, upon such investigation, 
the well appears to be lacking mechanical integrity, or if monitoring 
required under paragraph (f) of this section otherwise indicates that 
the well may be lacking mechanical integrity, the owner or operator 
shall:
    (1) Cease injection of waste fluids unless authorized by the 
Director to continue or resume injection.
    (2) Take all necessary steps to determine the presence or absence of 
a leak; and
    (3) Notify the Director within 24 hours after the alarm or shutdown.
    (h) If a loss of mechanical integrity is discovered pursuant to 
paragraph (g) of this section or during periodic mechanical integrity 
testing, the owner or operator shall:
    (1) Immediately cease injection of waste fluids;
    (2) Take all steps reasonably necessary to determine whether there 
may have been a release of hazardous wastes or hazardous waste 
constituents into any unauthorized zone;

[[Page 909]]

    (3) Notify the Director within 24 hours after loss of mechanical 
integrity is discovered;
    (4) Notify the Director when injection can be expected to resume; 
and
    (5) Restore and demonstrate mechanical integrity to the satisfaction 
of the Director prior to resuming injection of waste fluids.
    (i) Whenever the owner or operator obtains evidence that there may 
have been a release of injected wastes into an unauthorized zone:
    (1) The owner or operator shall immediately case injection of waste 
fluids, and:
    (i) Notify the Director within 24 hours of obtaining such evidence;
    (ii) Take all necessary steps to identify and characterize the 
extent of any release;
    (iii) Comply with any remediation plan specified by the Director;
    (iv) Implement any remediation plan approved by the Director; and
    (v) Where such release is into a USDW currently serving as a water 
supply, place a notice in a newspaper of general circulation.
    (2) The Director may allow the operator to resume injection prior to 
completing cleanup action if the owner or operator demonstrates that the 
injection operation will not endanger USDWs.
    (j) The owner or operator shall notify the Director and obtain his 
approval prior to conducting any well workover.



Sec.  146.68  Testing and monitoring requirements.

    Testing and monitoring requirements shall at a minimum include:
    (a) Monitoring of the injected wastes. (1) The owner or operator 
shall develop and follow an approved written waste analysis plan that 
describes the procedures to be carried out to obtain a detailed chemical 
and physical analysis of a representative sample of the waste, including 
the quality assurance procedures used. At a minimum, the plan shall 
specify:
    (i) The paramenters for which the waste will be analyzed and the 
rationale for the selection of these parameters;
    (ii) The test methods that will be used to test for these 
parameters; and
    (iii) The sampling method that will be used to obtain a 
representative sample of the waste to be analyzed.
    (2) The owner or operator shall repeat the analysis of the injected 
wastes as described in the waste analysis plan at frequencies specified 
in the waste analysis plan and when process or operating changes occur 
that may significantly alter the characteristics of the waste stream.
    (3) The owner or operator shall conduct continuous or periodic 
monitoring of selected parameters as required by the Director.
    (4) The owner or operator shall assure that the plan remains 
accurate and the analyses remain representative.
    (b) Hydrogeologic compatibility determination. The owner or operator 
shall submit information demonstrating to the satisfaction of the 
Director that the waste stream and its anticipated reaction products 
will not alter the permeability, thickness or other relevant 
characteristics of the confining or injection zones such that they would 
no longer meet the requirements specified in Sec.  146.62.
    (c) Compatibility of well materials. (1) The owner or operator shall 
demonstrate that the waste stream will be compatible with the well 
materials with which the waste is expected to come into contact, and 
submit to the Director a description of the methodology used to make 
that determination. Compatibility for purposes of this requirement is 
established if contact with injected fluids will not cause the well 
materials to fail to satisfy any design requirement imposed under Sec.  
146.65(b).
    (2) The Director shall require continuous corrosion monitoring of 
the construction materials used in the well for wells injecting 
corrosive waste, and may require such monitoring for other waste, by:
    (i) Placing coupons of the well construction materials in contact 
with the waste stream; or
    (ii) Routing the waste stream through a loop constructed with the 
material used in the well; or
    (iii) Using an alternative method approved by the Director.

[[Page 910]]

    (3) If a corrosion monitoring program is required:
    (i) The test shall use materials identical to those used in the 
construction of the well, and such materials must be continuously 
exposed to the operating pressures and temperatures (measured at the 
well head) and flow rates of the injection operation; and
    (ii) The owner or operator shall monitor the materials for loss of 
mass, thickness, cracking, pitting and other signs of corrosion on a 
quarterly basis to ensure that the well components meet the minimum 
standards for material strength and performance set forth in Sec.  
146.65(b).
    (d) Periodic mechanical integrity testing. In fulfilling the 
requirements of Sec.  146.8, the owner or operator of a Class I 
hazardous waste injection well shall conduct the mechanical integrity 
testing as follows:
    (1) The long string casing, injection tube, and annular seal shall 
be tested by means of an approved pressure test with a liquid or gas 
annually and whenever there has been a well workover;
    (2) The bottom-hole cement shall be tested by means of an approved 
radioactive tracer survey annually;
    (3) An approved temperature, noise, or other approved log shall be 
run at least once every five years to test for movement of fluid along 
the borehole. The Director may require such tests whenever the well is 
worked over;
    (4) Casing inspection logs shall be run whenever the owner or 
operator conducts a workover in which the injection string is pulled, 
unless the Director waives this requirement due to well construction or 
other factors which limit the test's reliability, or based upon the 
satisfactory results of a casing inspection log run within the previous 
five years. The Director may require that a casing inspection log be run 
every five years, if he has reason to believe that the integrity of the 
long string casing of the well may be adversely affected by naturally-
occurring or man-made events;
    (5) Any other test approved by the Director in accordance with the 
procedures in Sec.  146.8(d) may also be used.
    (e) Ambient monitoring. (1) Based on a site-specific assessment of 
the potential for fluid movement from the well or injection zone, and on 
the potential value of monitoring wells to detect such movement, the 
Director shall require the owner or operator to develop a monitoring 
program. At a minimum, the Director shall require monitoring of the 
pressure buildup in the injection zone annually, including at a minimum, 
a shut down of the well for a time sufficient to conduct a valid 
observation of the pressure fall-off curve.
    (2) When prescribing a monitoring system the Director may also 
require:
    (i) Continuous monitoring for pressure changes in the first aquifer 
overlying the confining zone. When such a well is installed, the owner 
or operator shall, on a quarterly basis, sample the aquifer and analyze 
for constituents specified by the Director;
    (ii) The use of indirect, geophysical techniques to determine the 
position of the waste front, the water quality in a formation designated 
by the Director, or to provide other site specific data;
    (iii) Periodic monitoring of the ground water quality in the first 
aquifer overlying the injection zone;
    (iv) Periodic monitoring of the ground water quality in the 
lowermost USDW; and
    (v) Any additional monitoring necessary to determine whether fluids 
are moving into or between USDWs.
    (f) The Director may require seismicity monitoring when he has 
reason to believe that the injection activity may have the capacity to 
cause seismic disturbances.

[53 FR 28148, July 26, 1988, as amended at 57 FR 46294, Oct. 7, 1992]



Sec.  146.69  Reporting requirements.

    Reporting requirements shall, at a minimum, include:
    (a) Quarterly reports to the Director containing:
    (1) The maximum injection pressure;
    (2) A description of any event that exceeds operating parameters for 
annulus pressure or injection pressure as specified in the permit;
    (3) A description of any event which triggers an alarm or shutdown 
device required pursuant to Sec.  146.67(f) and the response taken;
    (4) The total volume of fluid injected;
    (5) Any change in the annular fluid volume;

[[Page 911]]

    (6) The physical, chemical and other relevant characteristics of 
injected fluids; and
    (7) The results of monitoring prescribed under Sec.  146.68.
    (b) Reporting, within 30 days or with the next quarterly report 
whichever comes later, the results of:
    (1) Periodic tests of mechanical integrity;
    (2) Any other test of the injection well conducted by the permittee 
if required by the Director; and
    (3) Any well workover.



Sec.  146.70  Information to be evaluated by the Director.

    This section sets forth the information which must be evaluated by 
the Director in authorizing Class I hazardous waste injection wells. For 
a new Class I hazardous waste injection well, the owner or operator 
shall submit all the information listed below as part of the permit 
application. For an existing or converted Class I hazardous waste 
injection well, the owner or operator shall submit all information 
listed below as part of the permit application except for those items of 
information which are current, accurate, and available in the existing 
permit file. For both existing and new Class I hazardous waste injection 
wells, certain maps, cross-sections, tabulations of wells within the 
area of review and other data may be included in the application by 
reference provided they are current and readily available to the 
Director (for example, in the permitting agency's files) and 
sufficiently identifiable to be retrieved. In cases where EPA issues the 
permit, all the information in this section must be submitted to the 
Administrator or his designee.
    (a) Prior to the issuance of a permit for an existing Class I 
hazardous waste injection well to operate or the construction or 
conversion of a new Class I hazardous waste injection well, the Director 
shall review the following to assure that the requirements of this part 
and part 144 are met:
    (1) Information required in Sec.  144.31;
    (2) A map showing the injection well for which a permit is sought 
and the applicable area of review. Within the area of review, the map 
must show the number or name and location of all producing wells, 
injection wells, abandoned wells, dry holes, surface bodies of water, 
springs, mines (surface and subsurface), quarries, water wells and other 
pertinent surface features, including residences and roads. The map 
should also show faults, if known or suspected;
    (3) A tabulation of all wells within the area of review which 
penetrate the proposed injection zone or confining zone. Such data shall 
include a description of each well's type, construction, date drilled, 
location, depth, record of plugging and/or completion and any additional 
information the Director may require;
    (4) The protocol followed to identify, locate and ascertain the 
condition of abandoned wells within the area of review which penetrate 
the injection or the confining zones;
    (5) Maps and cross-sections indicating the general vertical and 
lateral limits of all underground sources of drinking water within the 
area of review, their position relative to the injection formation and 
the direction of water movement, where known, in each underground source 
of drinking water which may be affected by the proposed injection;
    (6) Maps and cross-sections detailing the geologic structure of the 
local area;
    (7) Maps and cross-sections illustrating the regional geologic 
setting;
    (8) Proposed operating data;
    (i) Average and maximum daily rate and volume of the fluid to be 
injected; and
    (ii) Average and maximum injection pressure;
    (9) Proposed formation testing program to obtain an analysis of the 
chemical, physical and radiological characteristics of and other 
information on the injection formation and the confining zone;
    (10) Proposed stimulation program;
    (11) Proposed injection procedure;
    (12) Schematic or other appropriate drawings of the surface and 
subsurface construction details of the well;
    (13) Contingency plans to cope with all shut-ins or well failures so 
as to prevent migration of fluids into any USDW;

[[Page 912]]

    (14) Plans (including maps) for meeting monitoring requirements of 
Sec.  146.68;
    (15) For wells within the area of review which penetrate the 
injection zone or the confining zone but are not properly completed or 
plugged, the corrective action to be taken under Sec.  146.64;
    (16) Construction procedures including a cementing and casing 
program, well materials specifications and their life expectancy, 
logging procedures, deviation checks, and a drilling, testing and coring 
program; and
    (17) A demonstration pursuant to part 144, subpart F, that the 
applicant has the resources necessary to close, plug or abandon the well 
and for post-closure care.
    (b) Prior to the Director's granting approval for the operation of a 
Class I hazardous waste injection well, the owner or operator shall 
submit and the Director shall review the following information, which 
shall be included in the completion report:
    (1) All available logging and testing program data on the well;
    (2) A demonstration of mechanical integrity pursuant to Sec.  
146.68;
    (3) The anticipated maximum pressure and flow rate at which the 
permittee will operate;
    (4) The results of the injection zone and confining zone testing 
program as required in Sec.  146.70(a)(9);
    (5) The actual injection procedure;
    (6) The compatibility of injected waste with fluids in the injection 
zone and minerals in both the injection zone and the confining zone and 
with the materials used to construct the well;
    (7) The calculated area of review based on data obtained during 
logging and testing of the well and the formation, and where necessary 
revisions to the information submitted under Sec.  146.70(a) (2) and 
(3).
    (8) The status of corrective action on wells identified in Sec.  
146.70(a)(15).
    (c) Prior to granting approval for the plugging and abandonment 
(i.e., closure) of a Class I hazardous waste injection well, the 
Director shall review the information required in Sec. Sec.  
146.71(a)(4) and 146.72(a).
    (d) Any permit issued for a Class I hazardous waste injection well 
for disposal on the premises where the waste is generated shall contain 
a certification by the owner or operator that:
    (1) The generator of the hazardous waste has a program to reduce the 
volume or quantity and toxicity of such waste to the degree determined 
by the generator to be economically practicable; and
    (2) Injection of the waste is that practicable method of disposal 
currently available to the generator which minimizes the present and 
future threat to human health and the environment.



Sec.  146.71  Closure.

    (a) Closure Plan. The owner or operator of a Class I hazardous waste 
injection well shall prepare, maintain, and comply with a plan for 
closure of the well that meets the requirements of paragraph (d) of this 
section and is acceptable to the Director. The obligation to implement 
the closure plan survives the termination of a permit or the cessation 
of injection activities. The requirement to maintain and implement an 
approved plan is directly enforceable regardless of whether the 
requirement is a condition of the permit.
    (1) The owner or operator shall submit the plan as a part of the 
permit application and, upon approval by the Director, such plan shall 
be a condition of any permit issued.
    (2) The owner or operator shall submit any proposed significant 
revision to the method of closure reflected in the plan for approval by 
the Director no later than the date on which notice of closure is 
required to be submitted to the Director under paragraph (b) of this 
section.
    (3) The plan shall assure financial responsibility as required in 
Sec.  144.52(a)(7).
    (4) The plan shall include the following information:
    (i) The type and number of plugs to be used;
    (ii) The placement of each plug including the elevation of the top 
and bottom of each plug;
    (iii) The type and grade and quantity of material to be used in 
plugging;
    (iv) The method of placement of the plugs;
    (v) Any proposed test or measure to be made;

[[Page 913]]

    (vi) The amount, size, and location (by depth) of casing and any 
other materials to be left in the well;
    (vii) The method and location where casing is to be parted, if 
applicable;
    (viii) The procedure to be used to meet the requirements of 
paragraph (d)(5) of this section;
    (ix) The estimated cost of closure; and
    (x) Any proposed test or measure to be made.
    (5) The Director may modify a closure plan following the procedures 
of Sec.  124.5.
    (6) An owner or operator of a Class I hazardous waste injection well 
who ceases injection temporarily, may keep the well open provided he:
    (i) Has received authorization from the Director; and
    (ii) Has described actions or procedures, satisfactory to the 
Director, that the owner or operator will take to ensure that the well 
will not endanger USDWs during the period of temporary disuse. These 
actions and procedures shall include compliance with the technical 
requirements applicable to active injection wells unless waived by the 
Director.
    (7) The owner or operator of a well that has ceased operations for 
more than two years shall notify the Director 30 days prior to resuming 
operation of the well.
    (b) Notice of intent to close. The owner or operator shall notify 
the Director at least 60 days before closure of a well. At the 
discretion of the Director, a shorter notice period may be allowed.
    (c) Closure report. Within 60 days after closure or at the time of 
the next quarterly report (whichever is less) the owner or operator 
shall submit a closure report to the Director. If the quarterly report 
is due less than 15 days after completion of closure, then the report 
shall be submitted within 60 days after closure. The report shall be 
certified as accurate by the owner or operator and by the person who 
performed the closure operation (if other than the owner or operator). 
Such report shall consist of either:
    (1) A statement that the well was closed in accordance with the 
closure plan previously submitted and approved by the Director; or
    (2) Where actual closure differed from the plan previously 
submitted, a written statement specifying the differences between the 
previous plan and the actual closure.
    (d) Standards for well closure. (1) Prior to closing the well, the 
owner or operator shall observe and record the pressure decay for a time 
specified by the Director. The Director shall analyze the pressure decay 
and the transient pressure observations conducted pursuant to Sec.  
146.68(e)(1)(i) and determine whether the injection activity has 
conformed with predicted values.
    (2) Prior to well closure, appropriate mechanical integrity testing 
shall be conducted to ensure the integrity of that portion of the long 
string casing and cement that will be left in the ground after closure. 
Testing methods may include:
    (i) Pressure tests with liquid or gas;
    (ii) Radioactive tracer surveys;
    (iii) Noise, temperature, pipe evaluation, or cement bond logs; and
    (iv) Any other test required by the Director.
    (3) Prior to well closure, the well shall be flushed with a buffer 
fluid.
    (4) Upon closure, a Class I hazardous waste well shall be plugged 
with cement in a manner that will not allow the movement of fluids into 
or between USDWs.
    (5) Placement of the cement plugs shall be accomplished by one of 
the following:
    (i) The Balance Method;
    (ii) The Dump Bailer Method;
    (iii) The Two-Plug Method; or
    (iv) An alternate method, approved by the Director, that will 
reliably provide a comparable level of protection.
    (6) Each plug used shall be appropriately tagged and tested for seal 
and stability before closure is completed.
    (7) The well to be closed shall be in a state of static equilibrium 
with the mud weight equalized top to bottom, either by circulating the 
mud in the well at least once or by a comparable method prescribed by 
the Director, prior to the placement of the cement plug(s).



Sec.  146.72  Post-closure care.

    (a) The owner or operator of a Class I hazardous waste well shall 
prepare,

[[Page 914]]

maintain, and comply with a plan for post-closure care that meets the 
requirements of paragraph (b) of this section and is acceptable to the 
Director. The obligation to implement the post-closure plan survives the 
termination of a permit or the cessation of injection activities. The 
requirement to maintain an approved plan is directly enforceable 
regardless of whether the requirement is a condition of the permit.
    (1) The owner or operator shall submit the plan as a part of the 
permit application and, upon approval by the Director, such plan shall 
be a condition of any permit issued.
    (2) The owner or operator shall submit any proposed significant 
revision to the plan as appropriate over the life of the well, but no 
later than the date of the closure report required under Sec.  
146.71(c).
    (3) The plan shall assure financial responsibility as required in 
Sec.  146.73.
    (4) The plan shall include the following information:
    (i) The pressure in the injection zone before injection began;
    (ii) The anticipated pressure in the injection zone at the time of 
closure;
    (iii) The predicted time until pressure in the injection zone decays 
to the point that the well's cone of influence no longer intersects the 
base of the lowermost USDW;
    (iv) Predicted position of the waste front at closure;
    (v) The status of any cleanups required under Sec.  146.64; and
    (vi) The estimated cost of proposed post-closure care.
    (5) At the request of the owner or operator, or on his own 
initiative, the Director may modify the post-closure plan after 
submission of the closure report following the procedures in Sec.  
124.5.
    (b) The owner or operator shall:
    (1) Continue and complete any cleanup action required under Sec.  
146.64, if applicable;
    (2) Continue to conduct any groundwater monitoring required under 
the permit until pressure in the injection zone decays to the point that 
the well's cone of influence no longer intersects the base of the 
lowermost USDW. The Director may extend the period of post-closure 
monitoring if he determines that the well may endanger a USDW.
    (3) Submit a survey plat to the local zoning authority designated by 
the Director. The plat shall indicate the location of the well relative 
to permanently surveyed benchmarks. A copy of the plat shall be 
submitted to the Regional Administrator of the appropriate EPA Regional 
Office.
    (4) Provide appropriate notification and information to such State 
and local authorities as have cognizance over drilling activities to 
enable such State and local authorities to impose appropriate conditions 
on subsequent drilling activities that may penetrate the well's 
confining or injection zone.
    (5) Retain, for a period of three years following well closure, 
records reflecting the nature, composition and volume of all injected 
fluids. The Director shall require the owner or operator to deliver the 
records to the Director at the conclusion of the retention period, and 
the records shall thereafter be retained at a location designated by the 
Director for that purpose.
    (c) Each owner of a Class I hazardous waste injection well, and the 
owner of the surface or subsurface property on or in which a Class I 
hazardous waste injection well is located, must record a notation on the 
deed to the facility property or on some other instrument which is 
normally examined during title search that will in perpetuity provide 
any potential purchaser of the property the following information:
    (1) The fact that land has been used to manage hazardous waste;
    (2) The name of the State agency or local authority with which the 
plat was filed, as well as the address of the Regional Environmental 
Protection Agency Office to which it was submitted;
    (3) The type and volume of waste injected, the injection interval or 
intervals into which it was injected, and the period over which 
injection occurred.



Sec.  146.73  Financial responsibility for post-closure care.

    The owner or operator shall demonstrate and maintain financial 
responsibility for post-closure by using a

[[Page 915]]

trust fund, surety bond, letter of credit, financial test, insurance or 
corporate guarantee that meets the specifications for the mechanisms and 
instruments revised as appropriate to cover closure and post-closure 
care in 40 CFR part 144, subpart F. The amount of the funds available 
shall be no less than the amount identified in Sec.  146.72(a)(4)(vi). 
The obligation to maintain financial responsibility for post-closure 
care survives the termination of a permit or the cessation of injection. 
The requirement to maintain financial responsibility is enforceable 
regardless of whether the requirement is a condition of the permit.



      Subpart H_Criteria and Standards Applicable to Class VI Wells

    Source: 75 FR 77291, Dec. 10, 2010, unless otherwise noted.



Sec.  146.81  Applicability.

    (a) This subpart establishes criteria and standards for underground 
injection control programs to regulate any Class VI carbon dioxide 
geologic sequestration injection wells.
    (b) This subpart applies to any wells used to inject carbon dioxide 
specifically for the purpose of geologic sequestration, i.e., the long-
term containment of a gaseous, liquid, or supercritical carbon dioxide 
stream in subsurface geologic formations.
    (c) This subpart also applies to owners or operators of permit- or 
rule-authorized Class I, Class II, or Class V experimental carbon 
dioxide injection projects who seek to apply for a Class VI geologic 
sequestration permit for their well or wells. Owners or operators 
seeking to convert existing Class I, Class II, or Class V experimental 
wells to Class VI geologic sequestration wells must demonstrate to the 
Director that the wells were engineered and constructed to meet the 
requirements at Sec.  146.86(a) and ensure protection of USDWs, in lieu 
of requirements at Sec. Sec.  146.86(b) and 146.87(a). By December 10, 
2011, owners or operators of either Class I wells previously permitted 
for the purpose of geologic sequestration or Class V experimental 
technology wells no longer being used for experimental purposes that 
will continue injection of carbon dioxide for the purpose of GS must 
apply for a Class VI permit. A converted well must still meet all other 
requirements under part 146.
    (d) Definitions. The following definitions apply to this subpart. To 
the extent that these definitions conflict with those in Sec.  144.3 or 
Sec.  146.3 of this chapter these definitions govern for Class VI wells:
    Area of review means the region surrounding the geologic 
sequestration project where USDWs may be endangered by the injection 
activity. The area of review is delineated using computational modeling 
that accounts for the physical and chemical properties of all phases of 
the injected carbon dioxide stream and displaced fluids, and is based on 
available site characterization, monitoring, and operational data as set 
forth in Sec.  146.84.
    Carbon dioxide plume means the extent underground, in three 
dimensions, of an injected carbon dioxide stream.
    Carbon dioxide stream means carbon dioxide that has been captured 
from an emission source (e.g., a power plant), plus incidental 
associated substances derived from the source materials and the capture 
process, and any substances added to the stream to enable or improve the 
injection process. This subpart does not apply to any carbon dioxide 
stream that meets the definition of a hazardous waste under 40 CFR part 
261.
    Confining zone means a geologic formation, group of formations, or 
part of a formation stratigraphically overlying the injection zone(s) 
that acts as barrier to fluid movement. For Class VI wells operating 
under an injection depth waiver, confining zone means a geologic 
formation, group of formations, or part of a formation stratigraphically 
overlying and underlying the injection zone(s).
    Corrective action means the use of Director-approved methods to 
ensure that wells within the area of review do not serve as conduits for 
the movement of fluids into underground sources of drinking water 
(USDW).
    Geologic sequestration means the long-term containment of a gaseous, 
liquid, or supercritical carbon dioxide stream in subsurface geologic 
formations. This

[[Page 916]]

term does not apply to carbon dioxide capture or transport.
    Geologic sequestration project means an injection well or wells used 
to emplace a carbon dioxide stream beneath the lowermost formation 
containing a USDW; or, wells used for geologic sequestration of carbon 
dioxide that have been granted a waiver of the injection depth 
requirements pursuant to requirements at Sec.  146.95; or, wells used 
for geologic sequestration of carbon dioxide that have received an 
expansion to the areal extent of an existing Class II enhanced oil 
recovery or enhanced gas recovery aquifer exemption pursuant to 
Sec. Sec.  146.4 and 144.7(d) of this chapter. It includes the 
subsurface three-dimensional extent of the carbon dioxide plume, 
associated area of elevated pressure, and displaced fluids, as well as 
the surface area above that delineated region.
    Injection zone means a geologic formation, group of formations, or 
part of a formation that is of sufficient areal extent, thickness, 
porosity, and permeability to receive carbon dioxide through a well or 
wells associated with a geologic sequestration project.
    Post-injection site care means appropriate monitoring and other 
actions (including corrective action) needed following cessation of 
injection to ensure that USDWs are not endangered, as required under 
Sec.  146.93.
    Pressure front means the zone of elevated pressure that is created 
by the injection of carbon dioxide into the subsurface. For the purposes 
of this subpart, the pressure front of a carbon dioxide plume refers to 
a zone where there is a pressure differential sufficient to cause the 
movement of injected fluids or formation fluids into a USDW.
    Site closure means the point/time, as determined by the Director 
following the requirements under Sec.  146.93, at which the owner or 
operator of a geologic sequestration site is released from post-
injection site care responsibilities.
    Transmissive fault or fracture means a fault or fracture that has 
sufficient permeability and vertical extent to allow fluids to move 
between formations.



Sec.  146.82  Required Class VI permit information.

    This section sets forth the information which must be considered by 
the Director in authorizing Class VI wells. For converted Class I, Class 
II, or Class V experimental wells, certain maps, cross-sections, 
tabulations of wells within the area of review and other data may be 
included in the application by reference provided they are current, 
readily available to the Director, and sufficiently identified to be 
retrieved. In cases where EPA issues the permit, all the information in 
this section must be submitted to the Regional Administrator.
    (a) Prior to the issuance of a permit for the construction of a new 
Class VI well or the conversion of an existing Class I, Class II, or 
Class V well to a Class VI well, the owner or operator shall submit, 
pursuant to Sec.  146.91(e), and the Director shall consider the 
following:
    (1) Information required in Sec.  144.31(e)(1) through (6) of this 
chapter;
    (2) A map showing the injection well for which a permit is sought 
and the applicable area of review consistent with Sec.  146.84. Within 
the area of review, the map must show the number or name, and location 
of all injection wells, producing wells, abandoned wells, plugged wells 
or dry holes, deep stratigraphic boreholes, State- or EPA-approved 
subsurface cleanup sites, surface bodies of water, springs, mines 
(surface and subsurface), quarries, water wells, other pertinent surface 
features including structures intended for human occupancy, State, 
Tribal, and Territory boundaries, and roads. The map should also show 
faults, if known or suspected. Only information of public record is 
required to be included on this map;
    (3) Information on the geologic structure and hydrogeologic 
properties of the proposed storage site and overlying formations, 
including:
    (i) Maps and cross sections of the area of review;
    (ii) The location, orientation, and properties of known or suspected 
faults and fractures that may transect the confining zone(s) in the area 
of review and a determination that they would not interfere with 
containment;

[[Page 917]]

    (iii) Data on the depth, areal extent, thickness, mineralogy, 
porosity, permeability, and capillary pressure of the injection and 
confining zone(s); including geology/facies changes based on field data 
which may include geologic cores, outcrop data, seismic surveys, well 
logs, and names and lithologic descriptions;
    (iv) Geomechanical information on fractures, stress, ductility, rock 
strength, and in situ fluid pressures within the confining zone(s);
    (v) Information on the seismic history including the presence and 
depth of seismic sources and a determination that the seismicity would 
not interfere with containment; and
    (vi) Geologic and topographic maps and cross sections illustrating 
regional geology, hydrogeology, and the geologic structure of the local 
area.
    (4) A tabulation of all wells within the area of review which 
penetrate the injection or confining zone(s). Such data must include a 
description of each well's type, construction, date drilled, location, 
depth, record of plugging and/or completion, and any additional 
information the Director may require;
    (5) Maps and stratigraphic cross sections indicating the general 
vertical and lateral limits of all USDWs, water wells and springs within 
the area of review, their positions relative to the injection zone(s), 
and the direction of water movement, where known;
    (6) Baseline geochemical data on subsurface formations, including 
all USDWs in the area of review;
    (7) Proposed operating data for the proposed geologic sequestration 
site:
    (i) Average and maximum daily rate and volume and/or mass and total 
anticipated volume and/or mass of the carbon dioxide stream;
    (ii) Average and maximum injection pressure;
    (iii) The source(s) of the carbon dioxide stream; and
    (iv) An analysis of the chemical and physical characteristics of the 
carbon dioxide stream.
    (8) Proposed pre-operational formation testing program to obtain an 
analysis of the chemical and physical characteristics of the injection 
zone(s) and confining zone(s) and that meets the requirements at Sec.  
146.87;
    (9) Proposed stimulation program, a description of stimulation 
fluids to be used and a determination that stimulation will not 
interfere with containment;
    (10) Proposed procedure to outline steps necessary to conduct 
injection operation;
    (11) Schematics or other appropriate drawings of the surface and 
subsurface construction details of the well;
    (12) Injection well construction procedures that meet the 
requirements of Sec.  146.86;
    (13) Proposed area of review and corrective action plan that meets 
the requirements under Sec.  146.84;
    (14) A demonstration, satisfactory to the Director, that the 
applicant has met the financial responsibility requirements under Sec.  
146.85;
    (15) Proposed testing and monitoring plan required by Sec.  146.90;
    (16) Proposed injection well plugging plan required by Sec.  
146.92(b);
    (17) Proposed post-injection site care and site closure plan 
required by Sec.  146.93(a);
    (18) At the Director's discretion, a demonstration of an alternative 
post-injection site care timeframe required by Sec.  146.93(c);
    (19) Proposed emergency and remedial response plan required by Sec.  
146.94(a);
    (20) A list of contacts, submitted to the Director, for those 
States, Tribes, and Territories identified to be within the area of 
review of the Class VI project based on information provided in 
paragraph (a)(2) of this section; and
    (21) Any other information requested by the Director.
    (b) The Director shall notify, in writing, any States, Tribes, or 
Territories within the area of review of the Class VI project based on 
information provided in paragraphs (a)(2) and (a)(20) of this section of 
the permit application and pursuant to the requirements at Sec.  
145.23(f)(13) of this chapter.
    (c) Prior to granting approval for the operation of a Class VI well, 
the Director shall consider the following information:
    (1) The final area of review based on modeling, using data obtained 
during logging and testing of the well and the formation as required by 
paragraphs

[[Page 918]]

(c)(2), (3), (4), (6), (7), and (10) of this section;
    (2) Any relevant updates, based on data obtained during logging and 
testing of the well and the formation as required by paragraphs (c)(3), 
(4), (6), (7), and (10) of this section, to the information on the 
geologic structure and hydrogeologic properties of the proposed storage 
site and overlying formations, submitted to satisfy the requirements of 
paragraph (a)(3) of this section;
    (3) Information on the compatibility of the carbon dioxide stream 
with fluids in the injection zone(s) and minerals in both the injection 
and the confining zone(s), based on the results of the formation testing 
program, and with the materials used to construct the well;
    (4) The results of the formation testing program required at 
paragraph (a)(8) of this section;
    (5) Final injection well construction procedures that meet the 
requirements of Sec.  146.86;
    (6) The status of corrective action on wells in the area of review;
    (7) All available logging and testing program data on the well 
required by Sec.  146.87;
    (8) A demonstration of mechanical integrity pursuant to Sec.  
146.89;
    (9) Any updates to the proposed area of review and corrective action 
plan, testing and monitoring plan, injection well plugging plan, post-
injection site care and site closure plan, or the emergency and remedial 
response plan submitted under paragraph (a) of this section, which are 
necessary to address new information collected during logging and 
testing of the well and the formation as required by all paragraphs of 
this section, and any updates to the alternative post-injection site 
care timeframe demonstration submitted under paragraph (a) of this 
section, which are necessary to address new information collected during 
the logging and testing of the well and the formation as required by all 
paragraphs of this section; and
    (10) Any other information requested by the Director.
    (d) Owners or operators seeking a waiver of the requirement to 
inject below the lowermost USDW must also refer to Sec.  146.95 and 
submit a supplemental report, as required at Sec.  146.95(a). The 
supplemental report is not part of the permit application.



Sec.  146.83  Minimum criteria for siting.

    (a) Owners or operators of Class VI wells must demonstrate to the 
satisfaction of the Director that the wells will be sited in areas with 
a suitable geologic system. The owners or operators must demonstrate 
that the geologic system comprises:
    (1) An injection zone(s) of sufficient areal extent, thickness, 
porosity, and permeability to receive the total anticipated volume of 
the carbon dioxide stream;
    (2) Confining zone(s) free of transmissive faults or fractures and 
of sufficient areal extent and integrity to contain the injected carbon 
dioxide stream and displaced formation fluids and allow injection at 
proposed maximum pressures and volumes without initiating or propagating 
fractures in the confining zone(s).
    (b) The Director may require owners or operators of Class VI wells 
to identify and characterize additional zones that will impede vertical 
fluid movement, are free of faults and fractures that may interfere with 
containment, allow for pressure dissipation, and provide additional 
opportunities for monitoring, mitigation, and remediation.



Sec.  146.84  Area of review and corrective action.

    (a) The area of review is the region surrounding the geologic 
sequestration project where USDWs may be endangered by the injection 
activity. The area of review is delineated using computational modeling 
that accounts for the physical and chemical properties of all phases of 
the injected carbon dioxide stream and is based on available site 
characterization, monitoring, and operational data.
    (b) The owner or operator of a Class VI well must prepare, maintain, 
and comply with a plan to delineate the area of review for a proposed 
geologic sequestration project, periodically reevaluate the delineation, 
and perform

[[Page 919]]

corrective action that meets the requirements of this section and is 
acceptable to the Director. The requirement to maintain and implement an 
approved plan is directly enforceable regardless of whether the 
requirement is a condition of the permit. As a part of the permit 
application for approval by the Director, the owner or operator must 
submit an area of review and corrective action plan that includes the 
following information:
    (1) The method for delineating the area of review that meets the 
requirements of paragraph (c) of this section, including the model to be 
used, assumptions that will be made, and the site characterization data 
on which the model will be based;
    (2) A description of:
    (i) The minimum fixed frequency, not to exceed five years, at which 
the owner or operator proposes to reevaluate the area of review;
    (ii) The monitoring and operational conditions that would warrant a 
reevaluation of the area of review prior to the next scheduled 
reevaluation as determined by the minimum fixed frequency established in 
paragraph (b)(2)(i) of this section.
    (iii) How monitoring and operational data (e.g., injection rate and 
pressure) will be used to inform an area of review reevaluation; and
    (iv) How corrective action will be conducted to meet the 
requirements of paragraph (d) of this section, including what corrective 
action will be performed prior to injection and what, if any, portions 
of the area of review will have corrective action addressed on a phased 
basis and how the phasing will be determined; how corrective action will 
be adjusted if there are changes in the area of review; and how site 
access will be guaranteed for future corrective action.
    (c) Owners or operators of Class VI wells must perform the following 
actions to delineate the area of review and identify all wells that 
require corrective action:
    (1) Predict, using existing site characterization, monitoring and 
operational data, and computational modeling, the projected lateral and 
vertical migration of the carbon dioxide plume and formation fluids in 
the subsurface from the commencement of injection activities until the 
plume movement ceases, until pressure differentials sufficient to cause 
the movement of injected fluids or formation fluids into a USDW are no 
longer present, or until the end of a fixed time period as determined by 
the Director. The model must:
    (i) Be based on detailed geologic data collected to characterize the 
injection zone(s), confining zone(s) and any additional zones; and 
anticipated operating data, including injection pressures, rates, and 
total volumes over the proposed life of the geologic sequestration 
project;
    (ii) Take into account any geologic heterogeneities, other 
discontinuities, data quality, and their possible impact on model 
predictions; and
    (iii) Consider potential migration through faults, fractures, and 
artificial penetrations.
    (2) Using methods approved by the Director, identify all 
penetrations, including active and abandoned wells and underground 
mines, in the area of review that may penetrate the confining zone(s). 
Provide a description of each well's type, construction, date drilled, 
location, depth, record of plugging and/or completion, and any 
additional information the Director may require; and
    (3) Determine which abandoned wells in the area of review have been 
plugged in a manner that prevents the movement of carbon dioxide or 
other fluids that may endanger USDWs, including use of materials 
compatible with the carbon dioxide stream.
    (d) Owners or operators of Class VI wells must perform corrective 
action on all wells in the area of review that are determined to need 
corrective action, using methods designed to prevent the movement of 
fluid into or between USDWs, including use of materials compatible with 
the carbon dioxide stream, where appropriate.
    (e) At the minimum fixed frequency, not to exceed five years, as 
specified in the area of review and corrective action plan, or when 
monitoring and operational conditions warrant, owners or operators must:

[[Page 920]]

    (1) Reevaluate the area of review in the same manner specified in 
paragraph (c)(1) of this section;
    (2) Identify all wells in the reevaluated area of review that 
require corrective action in the same manner specified in paragraph (c) 
of this section;
    (3) Perform corrective action on wells requiring corrective action 
in the reevaluated area of review in the same manner specified in 
paragraph (d) of this section; and
    (4) Submit an amended area of review and corrective action plan or 
demonstrate to the Director through monitoring data and modeling results 
that no amendment to the area of review and corrective action plan is 
needed. Any amendments to the area of review and corrective action plan 
must be approved by the Director, must be incorporated into the permit, 
and are subject to the permit modification requirements at Sec.  144.39 
or Sec.  144.41 of this chapter, as appropriate.
    (f) The emergency and remedial response plan (as required by Sec.  
146.94) and the demonstration of financial responsibility (as described 
by Sec.  146.85) must account for the area of review delineated as 
specified in paragraph (c)(1) of this section or the most recently 
evaluated area of review delineated under paragraph (e) of this section, 
regardless of whether or not corrective action in the area of review is 
phased.
    (g) All modeling inputs and data used to support area of review 
reevaluations under paragraph (e) of this section shall be retained for 
10 years.



Sec.  146.85  Financial responsibility.

    (a) The owner or operator must demonstrate and maintain financial 
responsibility as determined by the Director that meets the following 
conditions:
    (1) The financial responsibility instrument(s) used must be from the 
following list of qualifying instruments:
    (i) Trust Funds.
    (ii) Surety Bonds.
    (iii) Letter of Credit.
    (iv) Insurance.
    (v) Self Insurance (i.e., Financial Test and Corporate Guarantee).
    (vi) Escrow Account.
    (vii) Any other instrument(s) satisfactory to the Director.
    (2) The qualifying instrument(s) must be sufficient to cover the 
cost of:
    (i) Corrective action (that meets the requirements of Sec.  146.84);
    (ii) Injection well plugging (that meets the requirements of Sec.  
146.92);
    (iii) Post injection site care and site closure (that meets the 
requirements of Sec.  146.93); and
    (iv) Emergency and remedial response (that meets the requirements of 
Sec.  146.94).
    (3) The financial responsibility instrument(s) must be sufficient to 
address endangerment of underground sources of drinking water.
    (4) The qualifying financial responsibility instrument(s) must 
comprise protective conditions of coverage.
    (i) Protective conditions of coverage must include at a minimum 
cancellation, renewal, and continuation provisions, specifications on 
when the provider becomes liable following a notice of cancellation if 
there is a failure to renew with a new qualifying financial instrument, 
and requirements for the provider to meet a minimum rating, minimum 
capitalization, and ability to pass the bond rating when applicable.
    (A) Cancellation--for purposes of this part, an owner or operator 
must provide that their financial mechanism may not cancel, terminate or 
fail to renew except for failure to pay such financial instrument. If 
there is a failure to pay the financial instrument, the financial 
institution may elect to cancel, terminate, or fail to renew the 
instrument by sending notice by certified mail to the owner or operator 
and the Director. The cancellation must not be final for 120 days after 
receipt of cancellation notice. The owner or operator must provide an 
alternate financial responsibility demonstration within 60 days of 
notice of cancellation, and if an alternate financial responsibility 
demonstration is not acceptable (or possible), any funds from the 
instrument being cancelled must be released within 60 days of 
notification by the Director.
    (B) Renewal--for purposes of this part, owners or operators must 
renew all financial instruments, if an instrument expires, for the 
entire term of the

[[Page 921]]

geologic sequestration project. The instrument may be automatically 
renewed as long as the owner or operator has the option of renewal at 
the face amount of the expiring instrument. The automatic renewal of the 
instrument must, at a minimum, provide the holder with the option of 
renewal at the face amount of the expiring financial instrument.
    (C) Cancellation, termination, or failure to renew may not occur and 
the financial instrument will remain in full force and effect in the 
event that on or before the date of expiration: The Director deems the 
facility abandoned; or the permit is terminated or revoked or a new 
permit is denied; or closure is ordered by the Director or a U.S. 
district court or other court of competent jurisdiction; or the owner or 
operator is named as debtor in a voluntary or involuntary proceeding 
under Title 11 (Bankruptcy), U.S. Code; or the amount due is paid.
    (5) The qualifying financial responsibility instrument(s) must be 
approved by the Director.
    (i) The Director shall consider and approve the financial 
responsibility demonstration for all the phases of the geologic 
sequestration project prior to issue a Class VI permit (Sec.  146.82).
    (ii) The owner or operator must provide any updated information 
related to their financial responsibility instrument(s) on an annual 
basis and if there are any changes, the Director must evaluate, within a 
reasonable time, the financial responsibility demonstration to confirm 
that the instrument(s) used remain adequate for use. The owner or 
operator must maintain financial responsibility requirements regardless 
of the status of the Director's review of the financial responsibility 
demonstration.
    (iii) The Director may disapprove the use of a financial instrument 
if he determines that it is not sufficient to meet the requirements of 
this section.
    (6) The owner or operator may demonstrate financial responsibility 
by using one or multiple qualifying financial instruments for specific 
phases of the geologic sequestration project.
    (i) In the event that the owner or operator combines more than one 
instrument for a specific geologic sequestration phase (e.g., well 
plugging), such combination must be limited to instruments that are not 
based on financial strength or performance (i.e., self insurance or 
performance bond), for example trust funds, surety bonds guaranteeing 
payment into a trust fund, letters of credit, escrow account, and 
insurance. In this case, it is the combination of mechanisms, rather 
than the single mechanism, which must provide financial responsibility 
for an amount at least equal to the current cost estimate.
    (ii) When using a third-party instrument to demonstrate financial 
responsibility, the owner or operator must provide a proof that the 
third-party providers either have passed financial strength requirements 
based on credit ratings; or has met a minimum rating, minimum 
capitalization, and ability to pass the bond rating when applicable.
    (iii) An owner or operator using certain types of third-party 
instruments must establish a standby trust to enable EPA to be party to 
the financial responsibility agreement without EPA being the beneficiary 
of any funds. The standby trust fund must be used along with other 
financial responsibility instruments (e.g., surety bonds, letters of 
credit, or escrow accounts) to provide a location to place funds if 
needed.
    (iv) An owner or operator may deposit money to an escrow account to 
cover financial responsibility requirements; this account must segregate 
funds sufficient to cover estimated costs for Class VI (geologic 
sequestration) financial responsibility from other accounts and uses.
    (v) An owner or operator or its guarantor may use self insurance to 
demonstrate financial responsibility for geologic sequestration 
projects. In order to satisfy this requirement the owner or operator 
must meet a Tangible Net Worth of an amount approved by the Director, 
have a Net working capital and tangible net worth each at least six 
times the sum of the current well plugging, post injection site care and 
site closure cost, have assets located in the United States amounting to 
at least 90 percent of total assets or at least six times the sum of the 
current well plugging, post injection site care and site closure cost, 
and must

[[Page 922]]

submit a report of its bond rating and financial information annually. 
In addition the owner or operator must either: Have a bond rating test 
of AAA, AA, A, or BBB as issued by Standard & Poor's or Aaa, Aa, A, or 
Baa as issued by Moody's; or meet all of the following five financial 
ratio thresholds: A ratio of total liabilities to net worth less than 
2.0; a ratio of current assets to current liabilities greater than 1.5; 
a ratio of the sum of net income plus depreciation, depletion, and 
amortization to total liabilities greater than 0.1; A ratio of current 
assets minus current liabilities to total assets greater than -0.1; and 
a net profit (revenues minus expenses) greater than 0.
    (vi) An owner or operator who is not able to meet corporate 
financial test criteria may arrange a corporate guarantee by 
demonstrating that its corporate parent meets the financial test 
requirements on its behalf. The parent's demonstration that it meets the 
financial test requirement is insufficient if it has not also guaranteed 
to fulfill the obligations for the owner or operator.
    (vii) An owner or operator may obtain an insurance policy to cover 
the estimated costs of geologic sequestration activities requiring 
financial responsibility. This insurance policy must be obtained from a 
third party provider.
    (b) The requirement to maintain adequate financial responsibility 
and resources is directly enforceable regardless of whether the 
requirement is a condition of the permit.
    (1) The owner or operator must maintain financial responsibility and 
resources until:
    (i) The Director receives and approves the completed post-injection 
site care and site closure plan; and
    (ii) The Director approves site closure.
    (2) The owner or operator may be released from a financial 
instrument in the following circumstances:
    (i) The owner or operator has completed the phase of the geologic 
sequestration project for which the financial instrument was required 
and has fulfilled all its financial obligations as determined by the 
Director, including obtaining financial responsibility for the next 
phase of the GS project, if required; or
    (ii) The owner or operator has submitted a replacement financial 
instrument and received written approval from the Director accepting the 
new financial instrument and releasing the owner or operator from the 
previous financial instrument.
    (c) The owner or operator must have a detailed written estimate, in 
current dollars, of the cost of performing corrective action on wells in 
the area of review, plugging the injection well(s), post-injection site 
care and site closure, and emergency and remedial response.
    (1) The cost estimate must be performed for each phase separately 
and must be based on the costs to the regulatory agency of hiring a 
third party to perform the required activities. A third party is a party 
who is not within the corporate structure of the owner or operator.
    (2) During the active life of the geologic sequestration project, 
the owner or operator must adjust the cost estimate for inflation within 
60 days prior to the anniversary date of the establishment of the 
financial instrument(s) used to comply with paragraph (a) of this 
section and provide this adjustment to the Director. The owner or 
operator must also provide to the Director written updates of 
adjustments to the cost estimate within 60 days of any amendments to the 
area of review and corrective action plan (Sec.  146.84), the injection 
well plugging plan (Sec.  146.92), the post-injection site care and site 
closure plan (Sec.  146.93), and the emergency and remedial response 
plan (Sec.  146.94).
    (3) The Director must approve any decrease or increase to the 
initial cost estimate. During the active life of the geologic 
sequestration project, the owner or operator must revise the cost 
estimate no later than 60 days after the Director has approved the 
request to modify the area of review and corrective action plan (Sec.  
146.84), the injection well plugging plan (Sec.  146.92), the post-
injection site care and site closure plan (Sec.  146.93), and the 
emergency and response plan (Sec.  146.94), if the change in the plan 
increases the cost. If the change to the plans decreases the cost,

[[Page 923]]

any withdrawal of funds must be approved by the Director. Any decrease 
to the value of the financial assurance instrument must first be 
approved by the Director. The revised cost estimate must be adjusted for 
inflation as specified at paragraph (c)(2) of this section.
    (4) Whenever the current cost estimate increases to an amount 
greater than the face amount of a financial instrument currently in use, 
the owner or operator, within 60 days after the increase, must either 
cause the face amount to be increased to an amount at least equal to the 
current cost estimate and submit evidence of such increase to the 
Director, or obtain other financial responsibility instruments to cover 
the increase. Whenever the current cost estimate decreases, the face 
amount of the financial assurance instrument may be reduced to the 
amount of the current cost estimate only after the owner or operator has 
received written approval from the Director.
    (d) The owner or operator must notify the Director by certified mail 
of adverse financial conditions such as bankruptcy that may affect the 
ability to carry out injection well plugging and post-injection site 
care and site closure.
    (1) In the event that the owner or operator or the third party 
provider of a financial responsibility instrument is going through a 
bankruptcy, the owner or operator must notify the Director by certified 
mail of the commencement of a voluntary or involuntary proceeding under 
Title 11 (Bankruptcy), U.S. Code, naming the owner or operator as 
debtor, within 10 days after commencement of the proceeding.
    (2) A guarantor of a corporate guarantee must make such a 
notification to the Director if he/she is named as debtor, as required 
under the terms of the corporate guarantee.
    (3) An owner or operator who fulfills the requirements of paragraph 
(a) of this section by obtaining a trust fund, surety bond, letter of 
credit, escrow account, or insurance policy will be deemed to be without 
the required financial assurance in the event of bankruptcy of the 
trustee or issuing institution, or a suspension or revocation of the 
authority of the trustee institution to act as trustee of the 
institution issuing the trust fund, surety bond, letter of credit, 
escrow account, or insurance policy. The owner or operator must 
establish other financial assurance within 60 days after such an event.
    (e) The owner or operator must provide an adjustment of the cost 
estimate to the Director within 60 days of notification by the Director, 
if the Director determines during the annual evaluation of the 
qualifying financial responsibility instrument(s) that the most recent 
demonstration is no longer adequate to cover the cost of corrective 
action (as required by Sec.  146.84), injection well plugging (as 
required by Sec.  146.92), post-injection site care and site closure (as 
required by Sec.  146.93), and emergency and remedial response (as 
required by Sec.  146.94).
    (f) The Director must approve the use and length of pay-in-periods 
for trust funds or escrow accounts.



Sec.  146.86  Injection well construction requirements.

    (a) General. The owner or operator must ensure that all Class VI 
wells are constructed and completed to:
    (1) Prevent the movement of fluids into or between USDWs or into any 
unauthorized zones;
    (2) Permit the use of appropriate testing devices and workover 
tools; and
    (3) Permit continuous monitoring of the annulus space between the 
injection tubing and long string casing.
    (b) Casing and cementing of Class VI wells. (1) Casing and cement or 
other materials used in the construction of each Class VI well must have 
sufficient structural strength and be designed for the life of the 
geologic sequestration project. All well materials must be compatible 
with fluids with which the materials may be expected to come into 
contact and must meet or exceed standards developed for such materials 
by the American Petroleum Institute, ASTM International, or comparable 
standards acceptable to the Director. The casing and cementing program 
must be designed to prevent the movement of fluids into or between 
USDWs. In order to allow the Director to determine and specify casing 
and cementing requirements, the owner or operator

[[Page 924]]

must provide the following information:
    (i) Depth to the injection zone(s);
    (ii) Injection pressure, external pressure, internal pressure, and 
axial loading;
    (iii) Hole size;
    (iv) Size and grade of all casing strings (wall thickness, external 
diameter, nominal weight, length, joint specification, and construction 
material);
    (v) Corrosiveness of the carbon dioxide stream and formation fluids;
    (vi) Down-hole temperatures;
    (vii) Lithology of injection and confining zone(s);
    (viii) Type or grade of cement and cement additives; and
    (ix) Quantity, chemical composition, and temperature of the carbon 
dioxide stream.
    (2) Surface casing must extend through the base of the lowermost 
USDW and be cemented to the surface through the use of a single or 
multiple strings of casing and cement.
    (3) At least one long string casing, using a sufficient number of 
centralizers, must extend to the injection zone and must be cemented by 
circulating cement to the surface in one or more stages.
    (4) Circulation of cement may be accomplished by staging. The 
Director may approve an alternative method of cementing in cases where 
the cement cannot be recirculated to the surface, provided the owner or 
operator can demonstrate by using logs that the cement does not allow 
fluid movement behind the well bore.
    (5) Cement and cement additives must be compatible with the carbon 
dioxide stream and formation fluids and of sufficient quality and 
quantity to maintain integrity over the design life of the geologic 
sequestration project. The integrity and location of the cement shall be 
verified using technology capable of evaluating cement quality radially 
and identifying the location of channels to ensure that USDWs are not 
endangered.
    (c) Tubing and packer. (1) Tubing and packer materials used in the 
construction of each Class VI well must be compatible with fluids with 
which the materials may be expected to come into contact and must meet 
or exceed standards developed for such materials by the American 
Petroleum Institute, ASTM International, or comparable standards 
acceptable to the Director.
    (2) All owners or operators of Class VI wells must inject fluids 
through tubing with a packer set at a depth opposite a cemented interval 
at the location approved by the Director.
    (3) In order for the Director to determine and specify requirements 
for tubing and packer, the owner or operator must submit the following 
information:
    (i) Depth of setting;
    (ii) Characteristics of the carbon dioxide stream (chemical content, 
corrosiveness, temperature, and density) and formation fluids;
    (iii) Maximum proposed injection pressure;
    (iv) Maximum proposed annular pressure;
    (v) Proposed injection rate (intermittent or continuous) and volume 
and/or mass of the carbon dioxide stream;
    (vi) Size of tubing and casing; and
    (vii) Tubing tensile, burst, and collapse strengths.



Sec.  146.87  Logging, sampling, and testing prior to injection well operation.

    (a) During the drilling and construction of a Class VI injection 
well, the owner or operator must run appropriate logs, surveys and tests 
to determine or verify the depth, thickness, porosity, permeability, and 
lithology of, and the salinity of any formation fluids in all relevant 
geologic formations to ensure conformance with the injection well 
construction requirements under Sec.  146.86 and to establish accurate 
baseline data against which future measurements may be compared. The 
owner or operator must submit to the Director a descriptive report 
prepared by a knowledgeable log analyst that includes an interpretation 
of the results of such logs and tests. At a minimum, such logs and tests 
must include:
    (1) Deviation checks during drilling on all holes constructed by 
drilling a pilot hole which is enlarged by reaming or another method. 
Such checks must be at sufficiently frequent intervals to determine the 
location of the borehole and to ensure that vertical avenues for

[[Page 925]]

fluid movement in the form of diverging holes are not created during 
drilling; and
    (2) Before and upon installation of the surface casing:
    (i) Resistivity, spontaneous potential, and caliper logs before the 
casing is installed; and
    (ii) A cement bond and variable density log to evaluate cement 
quality radially, and a temperature log after the casing is set and 
cemented.
    (3) Before and upon installation of the long string casing:
    (i) Resistivity, spontaneous potential, porosity, caliper, gamma 
ray, fracture finder logs, and any other logs the Director requires for 
the given geology before the casing is installed; and
    (ii) A cement bond and variable density log, and a temperature log 
after the casing is set and cemented.
    (4) A series of tests designed to demonstrate the internal and 
external mechanical integrity of injection wells, which may include:
    (i) A pressure test with liquid or gas;
    (ii) A tracer survey such as oxygen-activation logging;
    (iii) A temperature or noise log;
    (iv) A casing inspection log; and
    (5) Any alternative methods that provide equivalent or better 
information and that are required by and/or approved of by the Director.
    (b) The owner or operator must take whole cores or sidewall cores of 
the injection zone and confining system and formation fluid samples from 
the injection zone(s), and must submit to the Director a detailed report 
prepared by a log analyst that includes: Well log analyses (including 
well logs), core analyses, and formation fluid sample information. The 
Director may accept information on cores from nearby wells if the owner 
or operator can demonstrate that core retrieval is not possible and that 
such cores are representative of conditions at the well. The Director 
may require the owner or operator to core other formations in the 
borehole.
    (c) The owner or operator must record the fluid temperature, pH, 
conductivity, reservoir pressure, and static fluid level of the 
injection zone(s).
    (d) At a minimum, the owner or operator must determine or calculate 
the following information concerning the injection and confining 
zone(s):
    (1) Fracture pressure;
    (2) Other physical and chemical characteristics of the injection and 
confining zone(s); and
    (3) Physical and chemical characteristics of the formation fluids in 
the injection zone(s).
    (e) Upon completion, but prior to operation, the owner or operator 
must conduct the following tests to verify hydrogeologic characteristics 
of the injection zone(s):
    (1) A pressure fall-off test; and,
    (2) A pump test; or
    (3) Injectivity tests.
    (f) The owner or operator must provide the Director with the 
opportunity to witness all logging and testing by this subpart. The 
owner or operator must submit a schedule of such activities to the 
Director 30 days prior to conducting the first test and submit any 
changes to the schedule 30 days prior to the next scheduled test.



Sec.  146.88  Injection well operating requirements.

    (a) Except during stimulation, the owner or operator must ensure 
that injection pressure does not exceed 90 percent of the fracture 
pressure of the injection zone(s) so as to ensure that the injection 
does not initiate new fractures or propagate existing fractures in the 
injection zone(s). In no case may injection pressure initiate fractures 
in the confining zone(s) or cause the movement of injection or formation 
fluids that endangers a USDW. Pursuant to requirements at Sec.  
146.82(a)(9), all stimulation programs must be approved by the Director 
as part of the permit application and incorporated into the permit.
    (b) Injection between the outermost casing protecting USDWs and the 
well bore is prohibited.
    (c) The owner or operator must fill the annulus between the tubing 
and the long string casing with a non-corrosive fluid approved by the 
Director. The owner or operator must maintain on the annulus a pressure 
that exceeds the operating injection pressure, unless the Director 
determines that such requirement might harm the integrity of the well or 
endanger USDWs.

[[Page 926]]

    (d) Other than during periods of well workover (maintenance) 
approved by the Director in which the sealed tubing-casing annulus is 
disassembled for maintenance or corrective procedures, the owner or 
operator must maintain mechanical integrity of the injection well at all 
times.
    (e) The owner or operator must install and use:
    (1) Continuous recording devices to monitor: The injection pressure; 
the rate, volume and/or mass, and temperature of the carbon dioxide 
stream; and the pressure on the annulus between the tubing and the long 
string casing and annulus fluid volume; and
    (2) Alarms and automatic surface shut-off systems or, at the 
discretion of the Director, down-hole shut-off systems (e.g., automatic 
shut-off, check valves) for onshore wells or, other mechanical devices 
that provide equivalent protection; and
    (3) Alarms and automatic down-hole shut-off systems for wells 
located offshore but within State territorial waters, designed to alert 
the operator and shut-in the well when operating parameters such as 
annulus pressure, injection rate, or other parameters diverge beyond 
permitted ranges and/or gradients specified in the permit.
    (f) If a shutdown (i.e., down-hole or at the surface) is triggered 
or a loss of mechanical integrity is discovered, the owner or operator 
must immediately investigate and identify as expeditiously as possible 
the cause of the shutoff. If, upon such investigation, the well appears 
to be lacking mechanical integrity, or if monitoring required under 
paragraph (e) of this section otherwise indicates that the well may be 
lacking mechanical integrity, the owner or operator must:
    (1) Immediately cease injection;
    (2) Take all steps reasonably necessary to determine whether there 
may have been a release of the injected carbon dioxide stream or 
formation fluids into any unauthorized zone;
    (3) Notify the Director within 24 hours;
    (4) Restore and demonstrate mechanical integrity to the satisfaction 
of the Director prior to resuming injection; and
    (5) Notify the Director when injection can be expected to resume.



Sec.  146.89  Mechanical integrity.

    (a) A Class VI well has mechanical integrity if:
    (1) There is no significant leak in the casing, tubing, or packer; 
and
    (2) There is no significant fluid movement into a USDW through 
channels adjacent to the injection well bore.
    (b) To evaluate the absence of significant leaks under paragraph 
(a)(1) of this section, owners or operators must, following an initial 
annulus pressure test, continuously monitor injection pressure, rate, 
injected volumes; pressure on the annulus between tubing and long-string 
casing; and annulus fluid volume as specified in Sec.  146.88 (e);
    (c) At least once per year, the owner or operator must use one of 
the following methods to determine the absence of significant fluid 
movement under paragraph (a)(2) of this section:
    (1) An approved tracer survey such as an oxygen-activation log; or
    (2) A temperature or noise log.
    (d) If required by the Director, at a frequency specified in the 
testing and monitoring plan required at Sec.  146.90, the owner or 
operator must run a casing inspection log to determine the presence or 
absence of corrosion in the long-string casing.
    (e) The Director may require any other test to evaluate mechanical 
integrity under paragraphs (a)(1) or (a)(2) of this section. Also, the 
Director may allow the use of a test to demonstrate mechanical integrity 
other than those listed above with the written approval of the 
Administrator. To obtain approval for a new mechanical integrity test, 
the Director must submit a written request to the Administrator setting 
forth the proposed test and all technical data supporting its use. The 
Administrator may approve the request if he or she determines that it 
will reliably demonstrate the mechanical integrity of wells for which 
its use is proposed. Any alternate method approved by the Administrator 
will be published in the Federal Register and may be used in all States 
in accordance with applicable State law unless its use is restricted at 
the time of approval by the Administrator.

[[Page 927]]

    (f) In conducting and evaluating the tests enumerated in this 
section or others to be allowed by the Director, the owner or operator 
and the Director must apply methods and standards generally accepted in 
the industry. When the owner or operator reports the results of 
mechanical integrity tests to the Director, he/she shall include a 
description of the test(s) and the method(s) used. In making his/her 
evaluation, the Director must review monitoring and other test data 
submitted since the previous evaluation.
    (g) The Director may require additional or alternative tests if the 
results presented by the owner or operator under paragraphs (a) through 
(d) of this section are not satisfactory to the Director to demonstrate 
that there is no significant leak in the casing, tubing, or packer, or 
to demonstrate that there is no significant movement of fluid into a 
USDW resulting from the injection activity as stated in paragraphs 
(a)(1) and (2) of this section.



Sec.  146.90  Testing and monitoring requirements.

    The owner or operator of a Class VI well must prepare, maintain, and 
comply with a testing and monitoring plan to verify that the geologic 
sequestration project is operating as permitted and is not endangering 
USDWs. The requirement to maintain and implement an approved plan is 
directly enforceable regardless of whether the requirement is a 
condition of the permit. The testing and monitoring plan must be 
submitted with the permit application, for Director approval, and must 
include a description of how the owner or operator will meet the 
requirements of this section, including accessing sites for all 
necessary monitoring and testing during the life of the project. Testing 
and monitoring associated with geologic sequestration projects must, at 
a minimum, include:
    (a) Analysis of the carbon dioxide stream with sufficient frequency 
to yield data representative of its chemical and physical 
characteristics;
    (b) Installation and use, except during well workovers as defined in 
Sec.  146.88(d), of continuous recording devices to monitor injection 
pressure, rate, and volume; the pressure on the annulus between the 
tubing and the long string casing; and the annulus fluid volume added;
    (c) Corrosion monitoring of the well materials for loss of mass, 
thickness, cracking, pitting, and other signs of corrosion, which must 
be performed on a quarterly basis to ensure that the well components 
meet the minimum standards for material strength and performance set 
forth in Sec.  146.86(b), by:
    (1) Analyzing coupons of the well construction materials placed in 
contact with the carbon dioxide stream; or
    (2) Routing the carbon dioxide stream through a loop constructed 
with the material used in the well and inspecting the materials in the 
loop; or
    (3) Using an alternative method approved by the Director;
    (d) Periodic monitoring of the ground water quality and geochemical 
changes above the confining zone(s) that may be a result of carbon 
dioxide movement through the confining zone(s) or additional identified 
zones including:
    (1) The location and number of monitoring wells based on specific 
information about the geologic sequestration project, including 
injection rate and volume, geology, the presence of artificial 
penetrations, and other factors; and
    (2) The monitoring frequency and spatial distribution of monitoring 
wells based on baseline geochemical data that has been collected under 
Sec.  146.82(a)(6) and on any modeling results in the area of review 
evaluation required by Sec.  146.84(c).
    (e) A demonstration of external mechanical integrity pursuant to 
Sec.  146.89(c) at least once per year until the injection well is 
plugged; and, if required by the Director, a casing inspection log 
pursuant to requirements at Sec.  146.89(d) at a frequency established 
in the testing and monitoring plan;
    (f) A pressure fall-off test at least once every five years unless 
more frequent testing is required by the Director based on site-specific 
information;
    (g) Testing and monitoring to track the extent of the carbon dioxide 
plume and the presence or absence of elevated pressure (e.g., the 
pressure front) by using:
    (1) Direct methods in the injection zone(s); and,

[[Page 928]]

    (2) Indirect methods (e.g., seismic, electrical, gravity, or 
electromagnetic surveys and/or down-hole carbon dioxide detection 
tools), unless the Director determines, based on site-specific geology, 
that such methods are not appropriate;
    (h) The Director may require surface air monitoring and/or soil gas 
monitoring to detect movement of carbon dioxide that could endanger a 
USDW.
    (1) Design of Class VI surface air and/or soil gas monitoring must 
be based on potential risks to USDWs within the area of review;
    (2) The monitoring frequency and spatial distribution of surface air 
monitoring and/or soil gas monitoring must be decided using baseline 
data, and the monitoring plan must describe how the proposed monitoring 
will yield useful information on the area of review delineation and/or 
compliance with standards under Sec.  144.12 of this chapter;
    (3) If an owner or operator demonstrates that monitoring employed 
under Sec. Sec.  98.440 to 98.449 of this chapter (Clean Air Act, 42 
U.S.C. 7401 et seq.) accomplishes the goals of paragraphs (h)(1) and (2) 
of this section, and meets the requirements pursuant to Sec.  
146.91(c)(5), a Director that requires surface air/soil gas monitoring 
must approve the use of monitoring employed under Sec. Sec.  98.440 to 
98.449 of this chapter. Compliance with Sec. Sec.  98.440 to 98.449 of 
this chapter pursuant to this provision is considered a condition of the 
Class VI permit;
    (i) Any additional monitoring, as required by the Director, 
necessary to support, upgrade, and improve computational modeling of the 
area of review evaluation required under Sec.  146.84(c) and to 
determine compliance with standards under Sec.  144.12 of this chapter;
    (j) The owner or operator shall periodically review the testing and 
monitoring plan to incorporate monitoring data collected under this 
subpart, operational data collected under Sec.  146.88, and the most 
recent area of review reevaluation performed under Sec.  146.84(e). In 
no case shall the owner or operator review the testing and monitoring 
plan less often than once every five years. Based on this review, the 
owner or operator shall submit an amended testing and monitoring plan or 
demonstrate to the Director that no amendment to the testing and 
monitoring plan is needed. Any amendments to the testing and monitoring 
plan must be approved by the Director, must be incorporated into the 
permit, and are subject to the permit modification requirements at Sec.  
144.39 or Sec.  144.41 of this chapter, as appropriate. Amended plans or 
demonstrations shall be submitted to the Director as follows:
    (1) Within one year of an area of review reevaluation;
    (2) Following any significant changes to the facility, such as 
addition of monitoring wells or newly permitted injection wells within 
the area of review, on a schedule determined by the Director; or
    (3) When required by the Director.
    (k) A quality assurance and surveillance plan for all testing and 
monitoring requirements.



Sec.  146.91  Reporting requirements.

    The owner or operator must, at a minimum, provide, as specified in 
paragraph (e) of this section, the following reports to the Director, 
for each permitted Class VI well:
    (a) Semi-annual reports containing:
    (1) Any changes to the physical, chemical, and other relevant 
characteristics of the carbon dioxide stream from the proposed operating 
data;
    (2) Monthly average, maximum, and minimum values for injection 
pressure, flow rate and volume, and annular pressure;
    (3) A description of any event that exceeds operating parameters for 
annulus pressure or injection pressure specified in the permit;
    (4) A description of any event which triggers a shut-off device 
required pursuant to Sec.  146.88(e) and the response taken;
    (5) The monthly volume and/or mass of the carbon dioxide stream 
injected over the reporting period and the volume injected cumulatively 
over the life of the project;
    (6) Monthly annulus fluid volume added; and
    (7) The results of monitoring prescribed under Sec.  146.90.
    (b) Report, within 30 days, the results of:

[[Page 929]]

    (1) Periodic tests of mechanical integrity;
    (2) Any well workover; and,
    (3) Any other test of the injection well conducted by the permittee 
if required by the Director.
    (c) Report, within 24 hours:
    (1) Any evidence that the injected carbon dioxide stream or 
associated pressure front may cause an endangerment to a USDW;
    (2) Any noncompliance with a permit condition, or malfunction of the 
injection system, which may cause fluid migration into or between USDWs;
    (3) Any triggering of a shut-off system (i.e., down-hole or at the 
surface);
    (4) Any failure to maintain mechanical integrity; or.
    (5) Pursuant to compliance with the requirement at Sec.  146.90(h) 
for surface air/soil gas monitoring or other monitoring technologies, if 
required by the Director, any release of carbon dioxide to the 
atmosphere or biosphere.
    (d) Owners or operators must notify the Director in writing 30 days 
in advance of:
    (1) Any planned well workover;
    (2) Any planned stimulation activities, other than stimulation for 
formation testing conducted under Sec.  146.82; and
    (3) Any other planned test of the injection well conducted by the 
permittee.
    (e) Regardless of whether a State has primary enforcement 
responsibility, owners or operators must submit all required reports, 
submittals, and notifications under subpart H of this part to EPA in an 
electronic format approved by EPA.
    (f) Records shall be retained by the owner or operator as follows:
    (1) All data collected under Sec.  146.82 for Class VI permit 
applications shall be retained throughout the life of the geologic 
sequestration project and for 10 years following site closure.
    (2) Data on the nature and composition of all injected fluids 
collected pursuant to Sec.  146.90(a) shall be retained until 10 years 
after site closure. The Director may require the owner or operator to 
deliver the records to the Director at the conclusion of the retention 
period.
    (3) Monitoring data collected pursuant to Sec.  146.90(b) through 
(i) shall be retained for 10 years after it is collected.
    (4) Well plugging reports, post-injection site care data, including, 
if appropriate, data and information used to develop the demonstration 
of the alternative post-injection site care timeframe, and the site 
closure report collected pursuant to requirements at Sec. Sec.  
146.93(f) and (h) shall be retained for 10 years following site closure.
    (5) The Director has authority to require the owner or operator to 
retain any records required in this subpart for longer than 10 years 
after site closure.



Sec.  146.92  Injection well plugging.

    (a) Prior to the well plugging, the owner or operator must flush 
each Class VI injection well with a buffer fluid, determine bottomhole 
reservoir pressure, and perform a final external mechanical integrity 
test.
    (b) Well plugging plan. The owner or operator of a Class VI well 
must prepare, maintain, and comply with a plan that is acceptable to the 
Director. The requirement to maintain and implement an approved plan is 
directly enforceable regardless of whether the requirement is a 
condition of the permit. The well plugging plan must be submitted as 
part of the permit application and must include the following 
information:
    (1) Appropriate tests or measures for determining bottomhole 
reservoir pressure;
    (2) Appropriate testing methods to ensure external mechanical 
integrity as specified in Sec.  146.89;
    (3) The type and number of plugs to be used;
    (4) The placement of each plug, including the elevation of the top 
and bottom of each plug;
    (5) The type, grade, and quantity of material to be used in 
plugging. The material must be compatible with the carbon dioxide 
stream; and
    (6) The method of placement of the plugs.
    (c) Notice of intent to plug. The owner or operator must notify the 
Director in writing pursuant to Sec.  146.91(e), at least 60 days before 
plugging of a well. At this time, if any changes have been made to the 
original well plugging

[[Page 930]]

plan, the owner or operator must also provide the revised well plugging 
plan. The Director may allow for a shorter notice period. Any amendments 
to the injection well plugging plan must be approved by the Director, 
must be incorporated into the permit, and are subject to the permit 
modification requirements at Sec.  144.39 or Sec.  144.41 of this 
chapter, as appropriate.
    (d) Plugging report. Within 60 days after plugging, the owner or 
operator must submit, pursuant to Sec.  146.91(e), a plugging report to 
the Director. The report must be certified as accurate by the owner or 
operator and by the person who performed the plugging operation (if 
other than the owner or operator.) The owner or operator shall retain 
the well plugging report for 10 years following site closure.



Sec.  146.93  Post-injection site care and site closure.

    (a) The owner or operator of a Class VI well must prepare, maintain, 
and comply with a plan for post-injection site care and site closure 
that meets the requirements of paragraph (a)(2) of this section and is 
acceptable to the Director. The requirement to maintain and implement an 
approved plan is directly enforceable regardless of whether the 
requirement is a condition of the permit.
    (1) The owner or operator must submit the post-injection site care 
and site closure plan as a part of the permit application to be approved 
by the Director.
    (2) The post-injection site care and site closure plan must include 
the following information:
    (i) The pressure differential between pre-injection and predicted 
post-injection pressures in the injection zone(s);
    (ii) The predicted position of the carbon dioxide plume and 
associated pressure front at site closure as demonstrated in the area of 
review evaluation required under Sec.  146.84(c)(1);
    (iii) A description of post-injection monitoring location, methods, 
and proposed frequency;
    (iv) A proposed schedule for submitting post-injection site care 
monitoring results to the Director pursuant to Sec.  146.91(e); and,
    (v) The duration of the post-injection site care timeframe and, if 
approved by the Director, the demonstration of the alternative post-
injection site care timeframe that ensures non-endangerment of USDWs.
    (3) Upon cessation of injection, owners or operators of Class VI 
wells must either submit an amended post-injection site care and site 
closure plan or demonstrate to the Director through monitoring data and 
modeling results that no amendment to the plan is needed. Any amendments 
to the post-injection site care and site closure plan must be approved 
by the Director, be incorporated into the permit, and are subject to the 
permit modification requirements at Sec.  144.39 or Sec.  144.41 of this 
chapter, as appropriate.
    (4) At any time during the life of the geologic sequestration 
project, the owner or operator may modify and resubmit the post-
injection site care and site closure plan for the Director's approval 
within 30 days of such change.
    (b) The owner or operator shall monitor the site following the 
cessation of injection to show the position of the carbon dioxide plume 
and pressure front and demonstrate that USDWs are not being endangered.
    (1) Following the cessation of injection, the owner or operator 
shall continue to conduct monitoring as specified in the Director-
approved post-injection site care and site closure plan for at least 50 
years or for the duration of the alternative timeframe approved by the 
Director pursuant to requirements in paragraph (c) of this section, 
unless he/she makes a demonstration under (b)(2) of this section. The 
monitoring must continue until the geologic sequestration project no 
longer poses an endangerment to USDWs and the demonstration under (b)(2) 
of this section is submitted and approved by the Director.
    (2) If the owner or operator can demonstrate to the satisfaction of 
the Director before 50 years or prior to the end of the approved 
alternative timeframe based on monitoring and other site-specific data, 
that the geologic sequestration project no longer poses an endangerment 
to USDWs, the Director may approve an amendment to the post-injection 
site care and site closure

[[Page 931]]

plan to reduce the frequency of monitoring or may authorize site closure 
before the end of the 50-year period or prior to the end of the approved 
alternative timeframe, where he or she has substantial evidence that the 
geologic sequestration project no longer poses a risk of endangerment to 
USDWs.
    (3) Prior to authorization for site closure, the owner or operator 
must submit to the Director for review and approval a demonstration, 
based on monitoring and other site-specific data, that no additional 
monitoring is needed to ensure that the geologic sequestration project 
does not pose an endangerment to USDWs.
    (4) If the demonstration in paragraph (b)(3) of this section cannot 
be made (i.e., additional monitoring is needed to ensure that the 
geologic sequestration project does not pose an endangerment to USDWs) 
at the end of the 50-year period or at the end of the approved 
alternative timeframe, or if the Director does not approve the 
demonstration, the owner or operator must submit to the Director a plan 
to continue post-injection site care until a demonstration can be made 
and approved by the Director.
    (c) Demonstration of alternative post-injection site care timeframe. 
At the Director's discretion, the Director may approve, in consultation 
with EPA, an alternative post-injection site care timeframe other than 
the 50 year default, if an owner or operator can demonstrate during the 
permitting process that an alternative post-injection site care 
timeframe is appropriate and ensures non-endangerment of USDWs. The 
demonstration must be based on significant, site-specific data and 
information including all data and information collected pursuant to 
Sec. Sec.  146.82 and 146.83, and must contain substantial evidence that 
the geologic sequestration project will no longer pose a risk of 
endangerment to USDWs at the end of the alternative post-injection site 
care timeframe.
    (1) A demonstration of an alternative post-injection site care 
timeframe must include consideration and documentation of:
    (i) The results of computational modeling performed pursuant to 
delineation of the area of review under Sec.  146.84;
    (ii) The predicted timeframe for pressure decline within the 
injection zone, and any other zones, such that formation fluids may not 
be forced into any USDWs; and/or the timeframe for pressure decline to 
pre-injection pressures;
    (iii) The predicted rate of carbon dioxide plume migration within 
the injection zone, and the predicted timeframe for the cessation of 
migration;
    (iv) A description of the site-specific processes that will result 
in carbon dioxide trapping including immobilization by capillary 
trapping, dissolution, and mineralization at the site;
    (v) The predicted rate of carbon dioxide trapping in the immobile 
capillary phase, dissolved phase, and/or mineral phase;
    (vi) The results of laboratory analyses, research studies, and/or 
field or site-specific studies to verify the information required in 
paragraphs (iv) and (v) of this section;
    (vii) A characterization of the confining zone(s) including a 
demonstration that it is free of transmissive faults, fractures, and 
micro-fractures and of appropriate thickness, permeability, and 
integrity to impede fluid (e.g., carbon dioxide, formation fluids) 
movement;
    (viii) The presence of potential conduits for fluid movement 
including planned injection wells and project monitoring wells 
associated with the proposed geologic sequestration project or any other 
projects in proximity to the predicted/modeled, final extent of the 
carbon dioxide plume and area of elevated pressure;
    (ix) A description of the well construction and an assessment of the 
quality of plugs of all abandoned wells within the area of review;
    (x) The distance between the injection zone and the nearest USDWs 
above and/or below the injection zone; and
    (xi) Any additional site-specific factors required by the Director.
    (2) Information submitted to support the demonstration in paragraph 
(c)(1) of this section must meet the following criteria:
    (i) All analyses and tests performed to support the demonstration 
must be accurate, reproducible, and performed in accordance with the 
established quality assurance standards;

[[Page 932]]

    (ii) Estimation techniques must be appropriate and EPA-certified 
test protocols must be used where available;
    (iii) Predictive models must be appropriate and tailored to the site 
conditions, composition of the carbon dioxide stream and injection and 
site conditions over the life of the geologic sequestration project;
    (iv) Predictive models must be calibrated using existing information 
(e.g., at Class I, Class II, or Class V experimental technology well 
sites) where sufficient data are available;
    (v) Reasonably conservative values and modeling assumptions must be 
used and disclosed to the Director whenever values are estimated on the 
basis of known, historical information instead of site-specific 
measurements;
    (vi) An analysis must be performed to identify and assess aspects of 
the alternative post-injection site care timeframe demonstration that 
contribute significantly to uncertainty. The owner or operator must 
conduct sensitivity analyses to determine the effect that significant 
uncertainty may contribute to the modeling demonstration.
    (vii) An approved quality assurance and quality control plan must 
address all aspects of the demonstration; and,
    (viii) Any additional criteria required by the Director.
    (d) Notice of intent for site closure. The owner or operator must 
notify the Director in writing at least 120 days before site closure. At 
this time, if any changes have been made to the original post-injection 
site care and site closure plan, the owner or operator must also provide 
the revised plan. The Director may allow for a shorter notice period.
    (e) After the Director has authorized site closure, the owner or 
operator must plug all monitoring wells in a manner which will not allow 
movement of injection or formation fluids that endangers a USDW.
    (f) The owner or operator must submit a site closure report to the 
Director within 90 days of site closure, which must thereafter be 
retained at a location designated by the Director for 10 years. The 
report must include:
    (1) Documentation of appropriate injection and monitoring well 
plugging as specified in Sec.  146.92 and paragraph (e) of this section. 
The owner or operator must provide a copy of a survey plat which has 
been submitted to the local zoning authority designated by the Director. 
The plat must indicate the location of the injection well relative to 
permanently surveyed benchmarks. The owner or operator must also submit 
a copy of the plat to the Regional Administrator of the appropriate EPA 
Regional Office;
    (2) Documentation of appropriate notification and information to 
such State, local and Tribal authorities that have authority over 
drilling activities to enable such State, local, and Tribal authorities 
to impose appropriate conditions on subsequent drilling activities that 
may penetrate the injection and confining zone(s); and
    (3) Records reflecting the nature, composition, and volume of the 
carbon dioxide stream.
    (g) Each owner or operator of a Class VI injection well must record 
a notation on the deed to the facility property or any other document 
that is normally examined during title search that will in perpetuity 
provide any potential purchaser of the property the following 
information:
    (1) The fact that land has been used to sequester carbon dioxide;
    (2) The name of the State agency, local authority, and/or Tribe with 
which the survey plat was filed, as well as the address of the 
Environmental Protection Agency Regional Office to which it was 
submitted; and
    (3) The volume of fluid injected, the injection zone or zones into 
which it was injected, and the period over which injection occurred.
    (h) The owner or operator must retain for 10 years following site 
closure, records collected during the post-injection site care period. 
The owner or operator must deliver the records to the Director at the 
conclusion of the retention period, and the records must thereafter be 
retained at a location designated by the Director for that purpose.



Sec.  146.94  Emergency and remedial response.

    (a) As part of the permit application, the owner or operator must 
provide the

[[Page 933]]

Director with an emergency and remedial response plan that describes 
actions the owner or operator must take to address movement of the 
injection or formation fluids that may cause an endangerment to a USDW 
during construction, operation, and post-injection site care periods. 
The requirement to maintain and implement an approved plan is directly 
enforceable regardless of whether the requirement is a condition of the 
permit.
    (b) If the owner or operator obtains evidence that the injected 
carbon dioxide stream and associated pressure front may cause an 
endangerment to a USDW, the owner or operator must:
    (1) Immediately cease injection;
    (2) Take all steps reasonably necessary to identify and characterize 
any release;
    (3) Notify the Director within 24 hours; and
    (4) Implement the emergency and remedial response plan approved by 
the Director.
    (c) The Director may allow the operator to resume injection prior to 
remediation if the owner or operator demonstrates that the injection 
operation will not endanger USDWs.
    (d) The owner or operator shall periodically review the emergency 
and remedial response plan developed under paragraph (a) of this 
section. In no case shall the owner or operator review the emergency and 
remedial response plan less often than once every five years. Based on 
this review, the owner or operator shall submit an amended emergency and 
remedial response plan or demonstrate to the Director that no amendment 
to the emergency and remedial response plan is needed. Any amendments to 
the emergency and remedial response plan must be approved by the 
Director, must be incorporated into the permit, and are subject to the 
permit modification requirements at Sec.  144.39 or Sec.  144.41 of this 
chapter, as appropriate. Amended plans or demonstrations shall be 
submitted to the Director as follows:
    (1) Within one year of an area of review reevaluation;
    (2) Following any significant changes to the facility, such as 
addition of injection or monitoring wells, on a schedule determined by 
the Director; or
    (3) When required by the Director.



Sec.  146.95  Class VI injection depth waiver requirements.

    This section sets forth information which an owner or operator 
seeking a waiver of the Class VI injection depth requirements must 
submit to the Director; information the Director must consider in 
consultation with all affected Public Water System Supervision 
Directors; the procedure for Director--Regional Administrator 
communication and waiver issuance; and the additional requirements that 
apply to owners or operators of Class VI wells granted a waiver of the 
injection depth requirements.
    (a) In seeking a waiver of the requirement to inject below the 
lowermost USDW, the owner or operator must submit a supplemental report 
concurrent with permit application. The supplemental report must include 
the following,
    (1) A demonstration that the injection zone(s) is/are laterally 
continuous, is not a USDW, and is not hydraulically connected to USDWs; 
does not outcrop; has adequate injectivity, volume, and sufficient 
porosity to safely contain the injected carbon dioxide and formation 
fluids; and has appropriate geochemistry.
    (2) A demonstration that the injection zone(s) is/are bounded by 
laterally continuous, impermeable confining units above and below the 
injection zone(s) adequate to prevent fluid movement and pressure 
buildup outside of the injection zone(s); and that the confining unit(s) 
is/are free of transmissive faults and fractures. The report shall 
further characterize the regional fracture properties and contain a 
demonstration that such fractures will not interfere with injection, 
serve as conduits, or endanger USDWs.
    (3) A demonstration, using computational modeling, that USDWs above 
and below the injection zone will not be endangered as a result of fluid 
movement. This modeling should be conducted in conjunction with the area 
of review determination, as described in Sec.  146.84, and is subject to 
requirements, as described in Sec.  146.84(c), and periodic 
reevaluation, as described in Sec.  146.84(e).

[[Page 934]]

    (4) A demonstration that well design and construction, in 
conjunction with the waiver, will ensure isolation of the injectate in 
lieu of requirements at 146.86(a)(1) and will meet well construction 
requirements in paragraph (f) of this section.
    (5) A description of how the monitoring and testing and any 
additional plans will be tailored to the geologic sequestration project 
to ensure protection of USDWs above and below the injection zone(s), if 
a waiver is granted.
    (6) Information on the location of all the public water supplies 
affected, reasonably likely to be affected, or served by USDWs in the 
area of review.
    (7) Any other information requested by the Director to inform the 
Regional Administrator's decision to issue a waiver.
    (b) To inform the Regional Administrator's decision on whether to 
grant a waiver of the injection depth requirements at Sec. Sec.  144.6 
of this chapter, 146.5(f), and 146.86(a)(1), the Director must submit, 
to the Regional Administrator, documentation of the following:
    (1) An evaluation of the following information as it relates to 
siting, construction, and operation of a geologic sequestration project 
with a waiver:
    (i) The integrity of the upper and lower confining units;
    (ii) The suitability of the injection zone(s) (e.g., lateral 
continuity; lack of transmissive faults and fractures; knowledge of 
current or planned artificial penetrations into the injection zone(s) or 
formations below the injection zone);
    (iii) The potential capacity of the geologic formation(s) to 
sequester carbon dioxide, accounting for the availability of alternative 
injection sites;
    (iv) All other site characterization data, the proposed emergency 
and remedial response plan, and a demonstration of financial 
responsibility;
    (v) Community needs, demands, and supply from drinking water 
resources;
    (vi) Planned needs, potential and/or future use of USDWs and non-
USDWs in the area;
    (vii) Planned or permitted water, hydrocarbon, or mineral resource 
exploitation potential of the proposed injection formation(s) and other 
formations both above and below the injection zone to determine if there 
are any plans to drill through the formation to access resources in or 
beneath the proposed injection zone(s)/formation(s);
    (viii) The proposed plan for securing alternative resources or 
treating USDW formation waters in the event of contamination related to 
the Class VI injection activity; and,
    (ix) Any other applicable considerations or information requested by 
the Director.
    (2) Consultation with the Public Water System Supervision Directors 
of all States and Tribes having jurisdiction over lands within the area 
of review of a well for which a waiver is sought.
    (3) Any written waiver-related information submitted by the Public 
Water System Supervision Director(s) to the (UIC) Director.
    (c) Pursuant to requirements at Sec.  124.10 of this chapter and 
concurrent with the Class VI permit application notice process, the 
Director shall give public notice that a waiver application has been 
submitted. The notice shall clearly state:
    (1) The depth of the proposed injection zone(s);
    (2) The location of the injection well(s);
    (3) The name and depth of all USDWs within the area of review;
    (4) A map of the area of review;
    (5) The names of any public water supplies affected, reasonably 
likely to be affected, or served by USDWs in the area of review; and,
    (6) The results of UIC-Public Water System Supervision consultation 
required under paragraph (b)(2) of this section.
    (d) Following public notice, the Director shall provide all 
information received through the waiver application process to the 
Regional Administrator. Based on the information provided, the Regional 
Administrator shall provide written concurrence or non-concurrence 
regarding waiver issuance.
    (1) If the Regional Administrator determines that additional 
information is required to support a decision, the Director shall 
provide the information. At his or her discretion, the Regional 
Administrator may require that public

[[Page 935]]

notice of the new information be initiated.
    (2) In no case shall a Director of a State-approved program issue a 
waiver without receipt of written concurrence from the Regional 
Administrator.
    (e) If a waiver is issued, within 30 days of waiver issuance, EPA 
shall post the following information on the Office of Water's Web site:
    (1) The depth of the proposed injection zone(s);
    (2) The location of the injection well(s);
    (3) The name and depth of all USDWs within the area of review;
    (4) A map of the area of review;
    (5) The names of any public water supplies affected, reasonably 
likely to be affected, or served by USDWs in the area of review; and
    (6) The date of waiver issuance.
    (f) Upon receipt of a waiver of the requirement to inject below the 
lowermost USDW for geologic sequestration, the owner or operator of the 
Class VI well must comply with:
    (1) All requirements at Sec. Sec.  146.84, 146.85, 146.87, 146.88, 
146.89, 146.91, 146.92, and 146.94;
    (2) All requirements at Sec.  146.86 with the following modified 
requirements:
    (i) The owner or operator must ensure that Class VI wells with a 
waiver are constructed and completed to prevent movement of fluids into 
any unauthorized zones including USDWs, in lieu of requirements at Sec.  
146.86(a)(1).
    (ii) The casing and cementing program must be designed to prevent 
the movement of fluids into any unauthorized zones including USDWs in 
lieu of requirements at Sec.  146.86(b)(1).
    (iii) The surface casing must extend through the base of the nearest 
USDW directly above the injection zone and be cemented to the surface; 
or, at the Director's discretion, another formation above the injection 
zone and below the nearest USDW above the injection zone.
    (3) All requirements at Sec.  146.90 with the following modified 
requirements:
    (i) The owner or operator shall monitor the groundwater quality, 
geochemical changes, and pressure in the first USDWs immediately above 
and below the injection zone(s); and in any other formations at the 
discretion of the Director.
    (ii) Testing and monitoring to track the extent of the carbon 
dioxide plume and the presence or absence of elevated pressure (e.g., 
the pressure front) by using direct methods to monitor for pressure 
changes in the injection zone(s); and, indirect methods (e.g., seismic, 
electrical, gravity, or electromagnetic surveys and/or down-hole carbon 
dioxide detection tools), unless the Director determines, based on site-
specific geology, that such methods are not appropriate.
    (4) All requirements at Sec.  146.93 with the following, modified 
post-injection site care monitoring requirements:
    (i) The owner or operator shall monitor the groundwater quality, 
geochemical changes and pressure in the first USDWs immediately above 
and below the injection zone; and in any other formations at the 
discretion of the Director.
    (ii) Testing and monitoring to track the extent of the carbon 
dioxide plume and the presence or absence of elevated pressure (e.g., 
the pressure front) by using direct methods in the injection zone(s); 
and indirect methods (e.g., seismic, electrical, gravity, or 
electromagnetic surveys and/or down-hole carbon dioxide detection 
tools), unless the Director determines based on site-specific geology, 
that such methods are not appropriate;
    (5) Any additional requirements requested by the Director designed 
to ensure protection of USDWs above and below the injection zone(s).



PART 147_STATE, TRIBAL, AND EPA-ADMINISTERED UNDERGROUND 
INJECTION CONTROL PROGRAMS--Table of Contents



                      Subpart A_General Provisions

Sec.
147.1 Purpose and scope.
147.2 Severability of provisions.

                            Subpart B_Alabama

147.50 State-administered program--Class II wells.
147.51 State-administered program--Class I, III, IV, and V wells.
147.52 State-administered program--Hydraulic Fracturing of Coal Beds.

[[Page 936]]

147.60 EPA-administered program--Indian lands.

                            Subpart C_Alaska

147.100 State-administered program--Class II wells.
147.101 EPA-administered program.
147.102 Aquifer exemptions.
147.103 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.104 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.

                            Subpart D_Arizona

147.150 State-administered program. [Reserved]
147.151 EPA-administered program.
147.152 Aquifer exemptions. [Reserved]

                           Subpart E_Arkansas

147.200 State-administered program--Class I, III, IV, and V wells.
147.201 State-administered program--Class II wells. [Reserved]
147.205 EPA-administered program--Indian lands.

                          Subpart F_California

147.250 State-administered program--Class II wells.
147.251 EPA-administered program--Class I, III, IV, and V wells and 
          Indian lands.
147.252 Aquifer exemptions. [Reserved]
147.253 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.

                           Subpart G_Colorado

147.300 State-administered program--Class II wells.
147.301 EPA-administered program--Class I, III, IV, V wells and Indian 
          lands.
147.302 Aquifer exemptions.
147.303 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.304 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.305 Requirements for all wells.

                          Subpart H_Connecticut

147.350 State-administered program.
147.351-147.352 [Reserved]
147.353 EPA-administered program--Indian lands.
147.354-147.359 [Reserved]

                           Subpart I_Delaware

147.400 State-administered program.
147.401-147.402 [Reserved]
147.403 EPA-administered program--Indian lands.
147.404-147.449 [Reserved]

                     Subpart J_District of Columbia

147.450 State-administered program. [Reserved]
147.451 EPA-administered program.
147.452 Aquifer exemptions. [Reserved]

                            Subpart K_Florida

147.500 State-administered program--Class I, III, IV, and V wells.
147.501 EPA-administered program--Class II wells and Indian lands.
147.502 Aquifer exemptions. [Reserved]
147.503 Existing Class II (except enhanced recovery and hydrocarbon 
          storage) wells authorized by rule.
147.504 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.

                            Subpart L_Georgia

147.550 State-administered program.
147.551-147.552 [Reserved]
147.553 EPA-administered program--Indian lands.
147.554-147.559 [Reserved]

                            Subpart M_Hawaii

147.600 State-administered program. [Reserved]
147.601 EPA-administered program.

                             Subpart N_Idaho

147.650 State-administrative program--Class I, II, III, IV, and V wells.
147.651 EPA-administered program--Indian lands.
147.652 Aquifer exemptions. [Reserved]

                           Subpart O_Illinois

147.700 State-administered program--Class I, III, IV, and V wells.
147.701 State-administered program--Class II wells.
147.703 EPA-administered program--Indian lands.

                            Subpart P_Indiana

147.750 State-administered program--Class II wells.
147.751 EPA-administered program.
147.752 Aquifer exemptions. [Reserved]
147.753 Existing Class I and III wells authorized by rule.

[[Page 937]]

                             Subpart Q_Iowa

147.800 State-administered program. [Reserved]
147.801 EPA-administered program.
147.802 Aquifer exemptions. [Reserved]

                            Subpart R_Kansas

147.850 State-administered program--Class I, III, IV and V wells.
147.851 State-administered program--Class II wells.
147.852-147.859 [Reserved]
147.860 EPA-administered program--Indian lands.

                           Subpart S_Kentucky

147.900 State-administered program--Class II wells.
147.901 EPA-administered program--Class I, III, IV, V, and VI wells and 
          Indian lands.EPA-administered program.
147.902 Aquifer exemptions.
147.903 Existing Class I and III wells authorized by rule.
147.904 [Reserved]
147.905 Requirements for all wells--area of review.

                           Subpart T_Louisiana

147.950 State-administered program.
147.951 EPA-administered program--Indian lands.

                             Subpart U_Maine

147.1000 State-administered program.
147.1001 EPA-administered program--Indian lands.

                           Subpart V_Maryland

147.1050 State-administered program--Class I, II, III, IV, and V wells.
147.1051-147.1052 [Reserved]
147.1053 EPA-administered program--Indian lands.
147.1054-147.1099 [Reserved]

                         Subpart W_Massachusetts

147.1100 State-administered program.
147.1101 EPA-administered program--Indian lands.

                           Subpart X_Michigan

147.1150 State-administered program. [Reserved]
147.1151 EPA-administered program.
147.1152 Aquifer exemptions. [Reserved]
147.1153 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.1154 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.1155 Requirements for all wells.

                           Subpart Y_Minnesota

147.1200 State-administered program. [Reserved]
147.1201 EPA-administered program.
147.1202 Aquifer exemptions. [Reserved]
147.1210 Requirements for Indian lands.

                          Subpart Z_Mississippi

147.1250 State-administered program--Class I, III, IV, and V wells.
147.1251 State-administered program--Class II wells.
147.1252 EPA-administered program--Indian lands.

                           Subpart AA_Missouri

147.1300 State-administered program.
147.1301 State-administered program--Class I, III, IV, and V wells.
147.1302 Aquifer exemptions. [Reserved]
147.1303 EPA-administered program--Indian lands.

                           Subpart BB_Montana

147.1350 State-administered programs--Class II wells.
147.1351 EPA-administered program.
147.1352 Aquifer exemptions.
147.1353 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.1354 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.1355 Requirements for all wells.

Appendix A to Subpart BB of Part 147--State Requirements Incorporated by 
          Reference in Subpart BB of Part 147 of the Code of Federal 
          Regulations.

                           Subpart CC_Nebraska

147.1400 State-administered program--Class II wells.
147.1401 State-administered program--Class I, III, IV, and V wells.
147.1402 Aquifer exemptions. [Reserved]
147.1403 EPA-administered program--Indian lands.

                            Subpart DD_Nevada

147.1450 State-administered program.
147.1451 EPA-administered program--Indian lands.
147.1452 Aquifer exemptions. [Reserved]
147.1453 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.

[[Page 938]]

147.1454 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.

                        Subpart EE_New Hampshire

147.1500 State-administered program.
147.1501 EPA-administered program--Indian lands.

                          Subpart FF_New Jersey

147.1550 State-administered program.
147.1551 EPA-administered program--Indian lands.

                          Subpart GG_New Mexico

147.1600 State-administered program--Class II wells.
147.1601 State-administered program--Class I, III, IV and V wells.
147.1603 EPA-administered program--Indian lands.

                           Subpart HH_New York

147.1650 State-administered program. [Reserved]
147.1651 EPA-administered program.
147.1652 Aquifer exemptions.
147.1653 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.1654 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.1655 Requirements for wells authorized by permit.

                        Subpart II_North Carolina

147.1700 State-administered program.
147.1701-147.1702 [Reserved]
147.1703 EPA-administered program--Indian lands.
147.1704-147.1749 [Reserved]

                         Subpart JJ_North Dakota

147.1750 State-administered program--Class II wells.
147.1751 State-administered program--Class I, III, IV, V and VI wells.
147.1752 EPA-administered program--Indian lands.

                             Subpart KK_Ohio

147.1800 State-administered program--Class II wells.
147.1801 State-administered program--Class I, III, IV and V wells.
147.1802 Aquifer exemptions. [Reserved]
147.1803 Existing Class I and III wells authorized by rule--maximum 
          injection pressure.
147.1805 EPA-administered program--Indian lands.

                           Subpart LL_Oklahoma

147.1850 State-administered program--Class I, III, IV and V wells.
147.1851 State-administered program--Class II wells.
147.1852 EPA-administered program--Indian lands.

                            Subpart MM_Oregon

147.1900 State-administered program.
147.1901 EPA-administered program--Indian lands.

                         Subpart NN_Pennsylvania

147.1950 State-administered program. [Reserved]
147.1951 EPA-administered program.
147.1952 Aquifer exemptions.
147.1953 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.1954 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.1955 Requirements for wells authorized by permit.

                         Subpart OO_Rhode Island

147.2000 State-administered program--Class I, II, III, IV, and V wells.
147.2001 EPA-administered program--Indian lands.

                        Subpart PP_South Carolina

147.2050 State-administered program.
147.2051 EPA-administered program--Indian lands.

                         Subpart QQ_South Dakota

147.2100 State-administered program--Class II wells.
147.2101 EPA-administered program--Class I, III, IV and V wells and all 
          wells on Indian lands.
147.2102 Aquifer exemptions.
147.2103 Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.2104 Requirements for all wells.

                          Subpart RR_Tennessee

147.2150 State-administered program. [Reserved]
147.2151 EPA-administered program Class VI and Indian lands.
147.2152 Aquifer exemptions. [Reserved]
147.2153 Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.

[[Page 939]]

                            Subpart SS_Texas

147.2200 State-administered program--Class I, III, IV, and V wells.
147.2201 State-administered program--Class II wells.
147.2205 EPA-administered program--Indian lands.

                             Subpart TT_Utah

147.2250 State-administered program--Class I, III, IV, and V wells.
147.2251 State-administered program--Class II wells.
147.2253 EPA-administered program--Indian lands.

                           Subpart UU_Vermont

147.2300 State-administered program.
147.2301-147.2302 [Reserved]
147.2303 EPA-administered program--Indian lands.
147.2304-147.2349 [Reserved]

                           Subpart VV_Virginia

147.2350 State-administered program. [Reserved]
147.2351 EPA-administered program.
147.2352 Aquifer exemptions. [Reserved]

                          Subpart WW_Washington

147.2400 State-administered program--Class I, II, III, IV, and V wells.
147.2403 EPA-administered program--Indian lands.
147.2404 EPA-administered program--Colville Reservation.

                        Subpart XX_West Virginia

147.2450-147.2452 [Reserved]
147.2453 EPA-administered program--Indian lands.
147.2454-147.2499 [Reserved]

                          Subpart YY_Wisconsin

147.2500 State-administered program.
147.2510 EPA-administered program--Indian lands.

                           Subpart ZZ_Wyoming

147.2550 State-administered program--Class I, III, IV, and V wells.
147.2551 State-administered program--Class II wells.
147.2553 EPA-administered program--Indian lands.
147.2554 Aquifer exemptions.
147.2555 Aquifer exemptions since January 1, 1999.

                            Subpart AAA_Guam

147.2600 State-administered program.
147.2601 EPA-administered program--Indian lands.

                         Subpart BBB_Puerto Rico

147.2650 State-administered program--Class I, II, III, IV, and V wells.
147.2651 EPA-administered program--Indian lands.

                       Subpart CCC_Virgin Islands

147.2700 State-administered program. [Reserved]
147.2701 EPA-administered program.

                       Subpart DDD_American Samoa

147.2750 State administered program. [Reserved]
147.2751 EPA-administered program.
147.2752 Aquifer exemptions. [Reserved]

        Subpart EEE_Commonwealth of the Northern Mariana Islands

147.2800 State-administered program--Class I, II, III, IV, and V wells.
147.2801 EPA-administered program.
147.2802 Aquifer exemptions. [Reserved]

           Subpart FFF_Trust Territory of the Pacific Islands

147.2850 State-administered program. [Reserved]
147.2851 EPA-administered program.
147.2852 Aquifer exemptions. [Reserved]

            Subpart GGG_Osage Mineral Reserve_Class II Wells

147.2901 Applicability and scope.
147.2902 Definitions.
147.2903 Prohibition of unauthorized injection.
147.2904 Area of review.
147.2905 Plugging and abandonment.
147.2906 Emergency permits.
147.2907 Confidentiality of information.
147.2908 Aquifer exemptions.
147.2909 Authorization of existing wells by rule.
147.2910 Duration of authorization by rule.
147.2911 Construction requirements for wells authorized by rule.
147.2912 Operating requirements for wells authorized by rule.
147.2913 Monitoring and reporting requirements for wells authorized by 
          rule.
147.2914 Corrective action for wells authorized by rule.
147.2915 Requiring a permit for wells authorized by rule.

[[Page 940]]

147.2916 Coverage of permitting requirements.
147.2917 Duration of permits.
147.2918 Permit application information.
147.2919 Construction requirements for wells authorized by permit.
147.2920 Operating requirements for wells authorized by permit.
147.2921 Schedule of compliance.
147.2922 Monitoring and reporting requirements for wells authorized by 
          permit.
147.2923 Corrective action for wells authorized by permit.
147.2924 Area permits.
147.2925 Standard permit conditions.
147.2926 Permit transfers.
147.2927 Permit modification.
147.2928 Permit termination.
147.2929 Administrative permitting procedures.

  Subpart HHH_Lands of the Navajo, Ute Mountain Ute, and All Other New 
                              Mexico Tribes

147.3000 EPA-administered program.
147.3001 Definition.
147.3002 Public notice of permit actions.
147.3003 Aquifer exemptions.
147.3004 Duration of rule authorization for existing Class I and III 
          wells.
147.3005 Radioactive waste injection wells.
147.3006 Injection pressure for existing Class II wells authorized by 
          rule.
147.3007 Application for a permit.
147.3008 Criteria for aquifer exemptions.
147.3009 Area of review.
147.3010 Mechanical integrity tests.
147.3011 Plugging and abandonment of Class III wells.
147.3012 Construction requirements for Class I wells.
147.3013 Information to be considered for Class I wells.
147.3014 Construction requirements for Class III wells.
147.3015 Information to be considered for Class III wells.
147.3016 Criteria and standards applicable to Class V wells.

Appendix A to Subpart HHH of Part 147--Exempted Aquifers in New Mexico.

           Subpart III_Lands of Certain Oklahoma Indian Tribes

147.3100 EPA-administered program.
147.3101 Public notice of permit actions.
147.3102 Plugging and abandonment plans.
147.3103 Fluid seals.
147.3104 Notice of abandonment.
147.3105 Plugging and abandonment report.
147.3106 Area of review.
147.3107 Mechanical integrity.
147.3108 Plugging Class I, II, and III wells.
147.3109 Timing of mechanical integrity test.

                Subpart JJJ_Assiniboine and Sioux Tribes

147.3200 Fort Peck Indian Reservation: Assiniboine & Sioux Tribes--Class 
          II wells.

Subpart KKK [Reserved]

                     Subpart LLL_Navajo Indian Lands

147.3400 Navajo Indian lands--Class II wells.

    Authority: 42 U.S.C. 300h-4.

    Source: 49 FR 20197, May 11, 1984, unless otherwise noted.

    Editorial Note: Nomenclature changes to part 147 appear at 69 FR 
18803, Apr. 9, 2004.



                      Subpart A_General Provisions



Sec.  147.1  Purpose and scope.

    (a) This part sets forth the applicable Underground Injection 
Control (UIC) programs for each of the States, territories, and 
possessions identified pursuant to the Safe Drinking Water Act (SDWA) as 
needing a UIC program, including any Indian country geographically 
located within those States, territories, and possessions.
    (b) The applicable UIC programs set forth in this part may be State-
administered programs approved by EPA, Tribally-administered programs 
approved by EPA, or Federally-administered programs promulgated by EPA. 
In some cases, the applicable UIC program for a particular area may 
consist of a State-administered or Tribally-administered program 
applicable to some classes of wells and a Federally-administered program 
applicable to other classes of wells. Approval of a State or Tribal 
program is based upon a determination by the Administrator that the 
program meets the requirements of section 1422 or section 1425 of the 
SDWA, any other applicable provisions of this subpart, and the 
applicable provisions of 40 CFR parts 124, 144, 145 and 146. A 
Federally-administered program is promulgated in those instances where 
the State or Tribe has not submitted any program for approval or where 
the submitted program does not meet the minimum Federal statutory and 
regulatory requirements.
    (c) In the case of each State or Tribal program approved by EPA 
pursuant to section 1422 of the SDWA, the relevant subpart describes the 
major elements of that program, including the relevant

[[Page 941]]

State or Tribal statutes and regulations, the Statement(s) of Legal 
Authority, the Memorandum of Agreement, and the Program Description. 
State or Tribal statutes and regulations that contain standards, 
requirements, and procedures applicable to owners or operators have been 
incorporated by reference pursuant to regulations of the Office of the 
Federal Register. Material incorporated by reference is available for 
inspection in the appropriate EPA Regional office, in EPA Headquarters, 
and at the National Archives and Records Administration (NARA). For 
information on the availability of this material at NARA, call (202) 
741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html. Other State or Tribal 
statutes and regulations containing standards and procedures that 
constitute elements of a State or Tribal program but do not apply 
directly to owners or operators have been listed but have not been 
incorporated by reference.
    (d) In the case of any program promulgated under section 1422 for a 
State or Tribe that is to be administered by EPA, the relevant State or 
Tribal subpart makes applicable the provisions of 40 CFR parts 124, 144, 
146, and 148, and any other additional requirements pertinent to the 
specific State or Tribal program.
    (e) Regulatory provisions incorporated by reference (in the case of 
approved State or Tribal programs) or promulgated by EPA (in the case of 
EPA-administered programs), and all permit conditions or permit denials 
issued pursuant to such regulations, are enforceable by the 
Administrator pursuant to section 1423 of the SDWA.
    (f) Class VI well owners or operators must comply with Sec.  
146.91(e) notwithstanding any State program approvals.

[73 FR 63646, Oct. 27, 2008, as amended at 75 FR 77303, Dec. 10, 2010]



Sec.  147.2  Severability of provisions.

    The provisions in this part and the various applications thereof are 
distinct and severable. If any provision of this part or the application 
thereof to any person or circumstances is held invalid, such invalidity 
shall not affect other provisions or application of such provision to 
other persons or circumstances which can be given effect without the 
invalid provision or application.



                            Subpart B_Alabama



Sec.  147.50  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Alabama, except 
those on Indian lands, is the program administered by the State Oil and 
Gas Board of Alabama, approved by EPA pursuant to section 1425 of the 
SDWA. Notice of this approval was published in the Federal Register on 
August 2, 1982 (47 FR 33268); the effective date of this program is 
August 2, 1982. This program consists of the following elements, as 
submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Alabama. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Code of Alabama Sections 9-17-1 through 9-17-109 (Cumm. Supp. 
1989);
    (2) State Oil and Gas Board of Alabama Administrative Code, Oil and 
Gas Report 1 (supplemented through May 1989), Rules and Regulations 
Governing the Conservation of Oil and Gas in Alabama, and Oil and Gas 
Statutes of Alabama with Oil and Gas Board Forms, Sec.  400-1-2 and 
Sec.  400-1-5-.04.
    (b) The Memorandum of Agreement between EPA Region IV and the 
Alabama Oil and Gas Board, signed by the EPA Regional Administrator on 
June 15, 1982.
    (c) Statement of legal authority. ``State Oil and Gas Board has 
Authority to Carry Out Underground Injection Control Program Relating to 
Class II Wells as Described in Federal Safe Drinking Water Act--Opinion 
by Assistant Attorney General,'' May 28, 1982.
    (d) The Program Description and any other materials submitted as 
part of

[[Page 942]]

the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43086, Oct. 25, 1988; 56 
FR 9411, Mar. 6, 1991]



Sec.  147.51  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Alabama, except those on Indian lands, is the program administered by 
the Alabama Department of Environmental Management, approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on August 25, 1983 (48 FR 38640); the 
effective date of this program is August 25, 1983. This program consists 
of the following elements, as submitted to EPA in the State's program 
application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Alabama. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Alabama Water Pollution Control Act, Code of Alabama 1975, 
sections 22-22-1 through 22-22-14 (1980 and Supp. 1983);
    (2) Regulations, Policies and Procedures of the Alabama Water 
Improvement Commission, Title I (Regulations) (Rev. December 1980), as 
amended May 17, 1982, to add Chapter 9, Underground Injection Control 
Regulations (effective June 10, 1982), as amended April 6, 1983 
(effective May 11, 1983).
    (b) The Memorandum of Agreement between EPA Region IV and the 
Alabama Department of Environment Management, signed by the EPA Regional 
Administrator on May 24, 1983.
    (c) Statement of legal authority. (1) ``Water Pollution--Public 
Health--State has Authority to Carry Out Underground Injection Control 
Program Described in Federal Safe Drinking Water Act--Opinion by Legal 
Counsel for the Water Improvement Commission,'' June 25, 1982;
    (2) Letter from Attorney, Alabama Water Improvement Commission, to 
Regional Administrator, EPA Region IV, ``Re: AWIC Response to Phillip 
Tate's (U.S. EPA, Washington) Comments on AWIC's Final Application for 
Class I, III, IV, and V UIC Program,'' September 21, 1982;
    (3) Letter from Alabama Chief Assistant Attorney General to Regional 
Counsel, EPA Region IV, ``Re: Status of Independent Legal Counsel in 
Alabama Water Improvement Commission's Underground Injection Control 
Program,'' September 14, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43086, Oct. 25, 1988]



Sec.  147.52  State-administered program--Hydraulic Fracturing of Coal Beds.

    The UIC program for hydraulic fracturing of coal beds in the State 
of Alabama, except those on Indian lands, is the program administered by 
the State Oil and Gas Board of Alabama, approved by EPA pursuant to 
Section 1425 of the SDWA on December 22, 1999 and effective on January 
19, 2000. The Alabama program consists of the following elements, as 
submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in State 
Oil and Gas Board of Alabama Rule 400-4-1-.02, Definitions, and Rule 
400-4-5-.04, Protection of Underground Sources of Drinking Water during 
the Hydraulic Fracturing of Coal Beds, are hereby incorporated by 
reference and made a part of the applicable UIC program under the SDWA 
for the State of Alabama. This incorporation by reference was approved 
by the Director of the Federal Register on January 19, 2000 in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be 
obtained at the State Oil and Gas Board of Alabama, 420 Hackberry Lane, 
Tuscaloosa, AL 35489-9780. Copies may be inspected at the Environmental 
Protection Agency, Region 4, Water Management Division, Ground Water/
Drinking Water Branch, Ground Water & UIC Section, Sam Nunn Atlanta 
Federal Center, 61

[[Page 943]]

Forsyth Street, S.W., Room15-T53, Atlanta, GA 30303-8960, or at the 
National Archives and Records Administration (NARA). For information on 
the availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (b) Addendum One, Underground Injection Control Program, Memorandum 
of Agreement Between the State of Alabama and the USEPA Region 4, signed 
by the Supervisor, Alabama State Oil and Gas Board on December 10, 1999, 
and the Regional Administrator, U.S. Environmental Protection Agency 
Region 4, on December 13, 1999.
    (c) Statement of Legal Authority. ``I hereby certify, pursuant to my 
authority as Attorney General for the State of Alabama and for reasons 
set forth in this statement, that in my opinion, the laws of the State 
of Alabama provide the State Oil and Gas Board (hereinafter referred to 
as ``the Board'') adequate authority to carry out an Underground 
Injection Program for the control of underground injection activity 
related to the hydraulic fracturing of coal beds.'' Opinion by Alabama's 
Attorney General Office, extracted from Letter from R. Craig Kneisel, 
Chief, Environmental Division, Office of the Attorney General, dated 
October 8, 1999, to Dr. Donald F. Oltz, Supervisor, State Oil and Gas 
Board of Alabama, Subject: Attorney General's Statement for Final 
Authorization of Alabama Class II Underground injection Control Program.
    (d) The Program Description for the Regulation of Hydraulic 
Fracturing of Coal Beds As required by 40 CFR 145.23--State Oil and Gas 
Board of Alabama, including Appendices A through F.

[65 FR 2897, Jan. 19, 2000]



Sec.  147.60  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in Alabama is administered by EPA. This program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148 and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Alabama is November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9411, Mar. 6, 1991]



                            Subpart C_Alaska



Sec.  147.100  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Alaska, other 
than those on Indian lands, is the program administered by the Alaska 
Oil and Gas Conservation Commission approved by EPA pursuant to section 
1425 of the SDWA. Notice of this approval was published in the Federal 
Register [May 6, 1986]; the effective date of this program is June 19, 
1986. This program consists of the following elements, as submitted to 
EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Alaska. This incorporation by reference 
was approved by the Director of the Federal Register effective June 19, 
1986.
    (1) Alaska Statutes, Alaska Oil and Gas Conservation Act, Title 31, 
Sec. Sec.  31.05.005 through 31.30.010 (1979 and Cum. Supp. 1984);
    (2) Alaska Statutes, Administrative Procedures Act, Title 44, 
Sec. Sec.  44.62.010 through 44.62.650 (1984);
    (3) Alaska Administrative Code, Alaska Oil and Gas Conservation 
Commission, 20 AAC 25.005 through 20 AAC 25.570 (Supp. 1986).
    (b) Memorandum of Agreement. The Memorandum of Agreement between EPA 
Region 10, and the Alaska Oil and Gas Conservation Commission, signed by 
the EPA Regional Administrator on January 29, 1986, as amended on June 
21, 1988.
    (c) Statement of Legal Authority. Statement from the Attorney 
General of the State of Alaska, signed by the Assistant Attorney General 
on December 10, 1985.

[[Page 944]]

    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[51 FR 16684, May 6, 1986, as amended at 56 FR 9411, Mar. 6, 1991]



Sec.  147.101  EPA-administered program.

    (a) Contents. The UIC program in the State of Alaska for Class I, 
III, IV, and V wells, and for all classes of wells on Indian lands, is 
administered by EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date of the UIC program for all 
non-Class II wells in Alaska and for all wells on Indian lands, is June 
25, 1984.

[52 FR 17680, May 11, 1987, as amended at 56 FR 9412, Mar. 6, 1991]



Sec.  147.102  Aquifer exemptions.

    (a) This section identifies any aquifers or their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter at the 
time of program promulgation. EPA may in the future exempt other 
aquifers or portions, according to applicable procedures, without 
codifying such exemptions in this section. An updated list of exemptions 
will be maintained in the Regional office.
    (b) The following aquifers are exempted in accordance with the 
provisions of Sec. Sec.  144.7(b) and 146.4 of this chapter for Class II 
injection activities only:
    (1) The portions of aquifers in the Kenai Peninsula, greater than 
the indicated depths below the ground surface, and described by a \1/4\ 
mile area beyond and lying directly below the following oil and gas 
producing fields:
    (i) Swanson River Field--1700 feet.
    (ii) Beaver Creek Field--1650 feet.
    (iii) Kenai Gas Field--1300 feet.
    (2) The portion of aquifers beneath Cook Inlet described by a \1/4\ 
mile area beyond and lying directly below the following oil and gas 
producing fields:
    (i) Granite Point.
    (ii) McArthur River Field.
    (iii) Middle Ground Shoal Field.
    (iv) Trading Bay Field.
    (3) The portions of aquifers on the North Slope described by a \1/4\ 
mile area beyond and lying directly below the Kuparuk River Unit oil and 
gas producing field.



Sec.  147.103  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.



Sec.  147.104  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
maximum injection pressures after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may

[[Page 945]]

grant such a request after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressure based on data provided pursuant to 
paragraph (a)(2)(ii) of this section the owner or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within 1 year of the effective date of this 
program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) as needed to protect USDWs.



                            Subpart D_Arizona



Sec.  147.150  State-administered program. [Reserved]



Sec.  147.151  EPA-administered program.

    (a) Contents. The UIC program that applies to all injection 
activities in Arizona, including those on Indian lands, except for Class 
II wells on Navajo Indian lands for which EPA has granted the Navajo 
Nation primacy for the SDWA Class II UIC program (as defined in Sec.  
147.3400), is administered by EPA. The UIC program for Navajo Indian 
lands, except for Class II wells on Navajo Indian lands for which EPA 
has granted the Navajo Nation primacy for the SDWA Class II UIC program, 
consists of the requirements contained in subpart HHH of this part. The 
program for all injection activity except that on Navajo Indian lands 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date for the UIC program in 
Arizona, except for the lands of the Navajo Indians, is June 25, 1984. 
The effective date for the UIC program on the lands of the Navajo, 
except for Class II wells on Navajo Indian lands for which EPA has 
granted the Navajo Nation primacy for the SDWA Class II UIC program (as 
defined in Sec.  147.3400), is November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9412, Mar. 6, 1991; 73 
FR 65564, Nov. 4, 2008]

[[Page 946]]



Sec.  147.152  Aquifer exemptions. [Reserved]



                           Subpart E_Arkansas



Sec.  147.200  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Arkansas, except those wells on Indian lands, is the program 
administered by the Arkansas Department of Pollution Control and Ecology 
approved by EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the Federal Register on July 6, 1982 (47 FR 
29236); the effective date of this program is July 6, 1982. This program 
consists of the following elements, as submitted to EPA in the State's 
program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Arkansas. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Arkansas Water and Air Pollution Control Act, Act 472 of 1949 as 
amended, Arkansas Statutes Annotated sections 82-1901 through 82-1943 
(1976);
    (2) Act 105 of 1939, Arkansas Statutes Annotated sections 53-101 
through 53-130 (1971 and Supp. 1981); Act 937 of 1979, Arkansas Statutes 
Annotated sections 53-1301 through 53-1320 (Supp. 1981); Act 523 of 
1981;
    (3) Arkansas Underground Injection Control Code, Department of 
Pollution Control and Ecology, promulgated January 22, 1982;
    (4) General Rule and Regulations, Arkansas Oil and Gas Commission 
(Order No. 2-39, revised July 1972);
    (5) Arkansas Hazardous Waste Management Code, Department of 
Pollution Control and Ecology, promulgated August 21, 1981.
    (b) The Memorandum of Agreement and Addendum No. 1 to the Memorandum 
of Agreement, between EPA Region VI and the Arkansas Department of 
Pollution Control and Ecology and the Arkansas Oil and Gas Commission, 
signed by the EPA Regional Administrator on May 25, 1982.
    (c) Statement of legal authority. (1) Letter from Chief Attorney, 
Arkansas Department of Pollution Control and Ecology, to Acting Regional 
Administrator, EPA Region VI, ``Re: Legal Authority of the Department of 
Pollution Control and Ecology of the State of Arkansas to Administer an 
Underground Injection Control Program,'' July 29, 1981;
    (2) Letter from Chief Attorney, Arkansas Department of Pollution 
Control and Ecology, to Acting Regional Counsel, EPA Region VI, ``Re: 
Addendum to Legal Statement--Underground Injection Control Program,'' 
October 13, 1981;
    (3) Letter from General Counsel, Arkansas Oil and Gas Commission, to 
Acting Regional Counsel, EPA Region VI, ``Re: Supplemental Addendum to 
Legal Statement--Underground Injection Control Program,'' October 20, 
1981;
    (4) Letter from Chief Attorney, Arkansas Department of Pollution 
Control and Ecology, to Attorney, Office of Regional Counsel, EPA Region 
VI (re: status as independent legal counsel), December 31, 1981;
    (5) Letter from General Counsel, Arkansas Oil and Gas Commission, to 
Acting Regional Counsel, EPA Region VI, ``Re: Supplemental Addendum to 
Legal Statement--Underground Injection Control Program,'' January 13, 
1982;
    (6) Letter from Chief Counsel, Arkansas Department of Pollution 
Control and Ecology, to Acting Regional Counsel, EPA Region VI, ``Re: 
Addendum to Legal Statement--Underground Injection Control Program,'' 
February 15, 1982;
    (7) Letter from Chief Counsel, Arkansas Department of Pollution 
Control and Ecology, to Acting Regional Counsel, EPA Region VI, ``Re: 
Addendum to Legal Statement--Underground Injection Control Program,'' 
May 13, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43086, Oct. 25, 1988]

[[Page 947]]



Sec.  147.201  State-administered program--Class II wells. [Reserved]



Sec.  147.205  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in Arkansas is administered by EPA. This program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148 and any 
additional requirements set forth in this subpart. Injection well owners 
and operators, and EPA shall comply with these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Arkansas is November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9412, Mar. 6, 1991]



                          Subpart F_California



Sec.  147.250  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of California, 
except those on Indian lands, is the program administered by the 
California Division of Oil and Gas, approved by EPA pursuant to SDWA 
section 1425.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of California. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) California Laws for Conservation of Petroleum and Gas, 
California Public Resources Code Div. 3, Chapt. 1, Sec. Sec.  3000-3359 
(1989);
    (2) California Administrative Code, title 14, Sec. Sec.  1710 to 
1724.10 (May 28, 1988).
    (b) The Memorandum of Agreement between EPA Region IX and the 
California Division of Oil and Gas, signed by the EPA Regional 
Administrator on September 29, 1982.
    (c) Statement of legal authority. (1) Letter from California Deputy 
Attorney General to the Administrator of EPA, ``Re: Legal Authority of 
California Division of Oil and Gas to Carry Out Class II Injection Well 
Program,'' April 1, 1981;
    (2) Letter from California Deputy Attorney General to Chief of 
California Branch, EPA Region IX, ``Re: California Application for 
Primacy, Class II UIC Program,'' December 3, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 52 FR 17681, May 11, 1987; 56 
FR 9412, Mar. 6, 1991]



Sec.  147.251  EPA-administered program--Class I, III, IV and V wells 
and Indian lands.

    (a) Contents. The UIC program in the State of California for Class 
I, III, IV and V wells, and for all classes of wells on Indian lands, is 
administered by EPA. The program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program for all 
lands in California, including Indian lands, is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9412, Mar. 6, 1991]



Sec.  147.252  Aquifer exemptions. [Reserved]



Sec.  147.253  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.

[[Page 948]]



                           Subpart G_Colorado



Sec.  147.300  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Colorado, except 
those wells on Indian Lands, is the program administered by the Colorado 
Oil and Gas Commission approved by EPA pursuant to section 1425 of the 
SDWA. Notice of this approval was published in the FR on April 2, 1984 
(49 FR 13040); the effective date of this program is April 2, 1984. This 
program consists of the following elements, as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Colorado. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained at the State of 
Colorado Oil and Gas Conservation Commission, Department of Natural 
Resources, Suite 380 Logan Tower Building, 1580 Logan Street, Denver, 
Colorado, 80203. Copies may be inspected at the Environmental Protection 
Agency, Region VIII, 999 18th Street, Suite 500, Denver, Colorado, 
80202-2405, or at the National Archives and Records Administration 
(NARA). For information on the availability of this material at NARA, 
call 202-741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Colorado Revised Statutes, 1989 replacement volume, Section 34-
60-101 through 34-60-123;
    (2) Colorado Revised Statutes, 1989 replacement volume, Section 25-
8-101 through 25-8-612;
    (3) Rules and Regulations, Rules of Practice and Procedure, and Oil 
and Gas Conservation Act (As Amended) Department of Natural Resources, 
Oil and Gas Conservation Commission of the State of Colorado (revised 
July 1989);
    (4) Oil and Gas Conservation Commission Revised Rules and 
Regulations in the 300, 400, 500, and 600 series, effective March 20, 
1989.
    (b) Memorandum of agreement. The Memorandum of Agreement between EPA 
Region VIII and the Colorado Oil and Gas Conservation Commission, signed 
by the EPA Regional Administrator on March 3, 1984 and amended on August 
30, 1989.
    (c) Statement of legal authority. (1) Letter from Colorado Assistant 
Attorney General to the Acting Regional Counsel, EPA Region VIII, ``Re: 
Class II Well Underground Injection Control Program of Colorado Oil and 
Gas Conservation Commission'', March 15, 1983;
    (2) Letter from Colorado Assistant Attorney General to the Acting 
Regional Counsel, EPA Region VIII, ``Re: Class II Well Injection Control 
Program of Colorado Oil and Gas Conservation Commission'', April 29, 
1983;
    (3) Letter from Colorado Assistant Attorney General to the Acting 
Regional Counsel, EPA Region VIII, ``Re: Class II Underground Injection 
Control Program of Colorado Oil and Gas Conservation Commission, 
interpretation of C.R.S. 1973, 34-60-110'', July 11, 1983;
    (4) Letter from Colorado Assistant Attorney General to the Acting 
Regional Counsel, EPA Region VIII, ``Re: Class II Well Underground 
Injection Control Program of Colorado Oil and Gas Conservation 
Commission'', February 17, 1984;
    (5) Memorandum from Colorado Assistant Attorney General to the 
Acting Regional Counsel, EPA Region VIII, ``Re: Authority to set and 
enforce maximum pressure for injecting fluids into Class II wells with 
existing permits'', March 7, 1984.
    (d) Program description. The Program Description and any other 
materials submitted as part of the application or as supplements 
thereto:
    (1) Application and accompanying materials for approval of 
Colorado's UIC program for Class II wells submitted by the Director of 
the Colorado Oil and Gas Conservation Commission to the Regional 
Administrator, May 3, 1983;
    (2) Supplemental amendment to Colorado's application for primacy for 
the UIC program for Class II wells describing the process through which 
the State will ensure enforceable limits for

[[Page 949]]

maximum injection pressure, describing the Commission's plan of 
administration for Class II wells, and describing Mechanical Integrity 
Test procedures for Class II wells, March 7, 1984;
    (3) Official correspondence concerning various program issues 
between the Colorado Oil and Gas Conservation Commission and EPA Region 
VIII, for the period from March 7, 1984 to May 8, 1989.

[56 FR 9412, Mar. 6, 1991]



Sec.  147.301  EPA-administered program--Class I, III, IV, V wells 
and Indian lands.

    (a) Contents. The UIC program for Class I, III, IV and V wells on 
all lands in Colorado, including Indian lands, and for Class II wells on 
Indian lands, is administered by EPA. The program for all EPA-
administered wells in Colorado other than Class II wells on the lands of 
the Ute Mountain Ute consists of the UIC program requirements of 40 CFR 
parts 124, 144, 146, 148, and any additional requirements set forth in 
the remainder of this subpart. Injection well owners and operators, and 
EPA shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program on all 
lands in Colorado, including Indian lands, except for Class II wells on 
lands of the Ute Mountain Ute, is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9413, Mar. 6, 1991]



Sec.  147.302  Aquifer exemptions.

    (a) This section identifies any aquifers of their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter at the 
time of program promulgation. EPA may in the future exempt other 
aquifers or portions according to applicable procedures without 
codifying such exemptions in this section. An updated list of exemptions 
will be maintained in the Regional office.
    (b) For all aquifers into which existing Class II wells are 
injecting, those portions within a \1/4\ mile radius of the well are 
exempted for the purpose of Class II injection activities only.



Sec.  147.303  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for wellhead pressure calculated by using the following 
formula;

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the wellhead in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.



Sec.  147.304  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may grant such a request after notice, opportunity for 
comment, and opportunity for a public hearing, according to the 
provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressures based on

[[Page 950]]

data provided pursuant to paragraph (a)(2)(ii) of this section the owner 
or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within one year of the effective date of this 
program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistent to deterioration from formation and 
injection fluids; and
    (iii) In quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) as needed to protect USDWs.



Sec.  147.305  Requirements for all wells.

    (a) The owner or operator converting an existing well to an 
injection well shall check the condition of the casing with one of the 
following logging tools:
    (1) A Pipe analysis log; or
    (2) A Caliper log.
    (b) The owner or operator of a new injection well cased with plastic 
(PVC, ABS, and others) casings shall:
    (1) Not construct a well deeper than 500 feet;
    (2) Use cement and additives compatible with such casing material;
    (3) Cement the annular space above the injection interval from the 
bottom of the blank casing to the surface.
    (c) The owner or operator of a newly drilled well shall install 
centralizers as directed by the Regional Administrator.
    (d) The owner or operator shall as required by the Regional 
Administrator:
    (1) Protect USDWs by:
    (i) Setting surface casing 50 feet below the base of the lowermost 
USDW;
    (ii) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (iii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may approve alternate casing and 
cementing practices provided that the owner or operator demonstrates 
that such practices will adequately protect USDWs.
    (e) Area of review. Notwithstanding the alternatives presented in 
Sec.  146.6 of this chapter, the area of review shall be

[[Page 951]]

a fixed radius as described in Sec.  146.6(b) of this chapter.
    (f) The applicant must give separate notice of intent to apply for a 
permit to each owner or tenant of the land within one-quarter mile of 
the site. The addresses of those to whom notice is given, and a 
description of how notice is given, shall be submitted with the permit 
application. The notice shall include:
    (1) Name and address of applicant;
    (2) A brief description of the planned injection activities, 
including well location, name and depth of the injection zone, maximum 
injection pressure and volume, and fluid to be injected;
    (3) EPA contact person; and
    (4) A statement that opportunity to comment will be announced after 
EPA prepares a draft permit. This requirement may be waived by the 
Regional Administrator when he determines that individual notice to all 
land owners and tenants would be impractical.



                          Subpart H_Connecticut



Sec.  147.350  State-administered program.

    The UIC program for all classes of wells in the State of 
Connecticut, except those wells on Indian lands, is the program 
administered by the Connecticut Department of Environmental Protection 
approved by EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the FR on March 26, 1984 (49 FR 11179); the 
effective date of this program is March 26, 1984. This program consists 
of the following elements, as submitted to EPA in the State's program 
application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made part of the applicable UIC program 
under the SDWA for the State of Connecticut. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and CFR part 51. Copies may be obtained at the State of 
Connecticut, Department of Environmental Protection, State Office 
Building, 165 Capitol Avenue, Hartford, Connecticut, 06106. Copies may 
be inspected at the Environmental Protection Agency, Region I, 5 Post 
Office Square--Suite 100, Boston, MA 02109-3912, or at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Connecticut General Statutes Annotated, title 22a (Environmental 
Protection), chapter 439, sections 22a-1 through 22a-27 (1985 and Cumm. 
Supp. 1990);
    (2) Connecticut General Statutes Annotated, Title 22a (Environmental 
Protection), Chapter 446K (1985 and Cumm. Supp. 1990).
    (b) Memorandum of Agreement. The Memorandum of Agreement between EPA 
Region I and the Connecticut Department of Environmental Protection, 
signed by the EPA Regional Administrator on August 9, 1983.
    (c) Statement of legal authority. (1) Statement from the Attorney 
General of the State of Connecticut, signed by the Attorney General on 
May 8, 1981;
    (2) Addendum to the Statement from the Attorney General of the State 
of Connecticut, signed by the Attorney General on May 10, 1983.
    (d) Program Description. The Program Description and any other 
materials submitted as part of the application or as supplements 
thereto.

[56 FR 9413, Mar. 6, 1991, as amended at 76 FR 49673, Aug. 11, 2011]



Sec. Sec.  147.351-147.352  [Reserved]



Sec.  147.353  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in Connecticut is administered by EPA. This program consists of 
the UIC program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Connecticut is November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9413, Mar. 6, 1991]

[[Page 952]]



Sec. Sec.  147.354-147.359  [Reserved]



                           Subpart I_Delaware



Sec.  147.400  State-administered program.

    The UIC program for all classes of wells in the State of Delaware, 
except those wells on Indian lands, is the program administered by the 
Delaware Department of Natural Resources and Environmental Control 
approved by EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the FR on April 5, 1984 (49 FR 13525); the 
effective date of this program is May 7, 1984. This program consists of 
the following elements, as submitted to EPA in the State's program 
application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Delaware. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and 1 CFR part 5l. Copies may be obtained at the Delaware 
Department of Natural Resources and Environmental Control, 89 Kings 
Highway, P.O. Box 1401, Dover, Delaware, 19903. Copies may be inspected 
at the Environmental Protection Agency, Region III, 841 Chestnut Street, 
Philadelphia, Pennsylvania, 19107, or at the National Archives and 
Records Administration (NARA). For information on the availability of 
this material at NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Delaware Environmental Protection Act, (Environmental Control) 7 
Delaware Code Annotated, Chapter 60, Sections 6001-6060 (Revised 1974 
and Cumm. Supp. 1988);
    (2) State of Delaware Regulations Governing Underground Injection 
Control, parts 122, 124 and 146 (Department of Natural Resources and 
Environmental Control), effective August 15, 1983.
    (b) Memorandum of agreement. The Memorandum of Agreement between EPA 
Region III and the Delaware Department of Natural Resources and 
Environmental Control, signed by the EPA Regional Administrator on March 
28, 1984.
    (c) Statement of legal authority. Statement of the Delaware Attorney 
General for the Underground Injection Control Program, signed by the 
Attorney General on January 26, 1984.
    (d) Program Description. The Program Description and any other 
materials submitted as part of the application (August 10, 1983), or as 
supplements thereto (October 14, 1983).

[56 FR 9413, Mar. 6, 1991]



Sec. Sec.  147.401-147.402  [Reserved]



Sec.  147.403  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in Delaware is administered by EPA. This program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Delaware is November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9413, Mar. 6, 1991]



Sec. Sec.  147.404-147.449  [Reserved]



                     Subpart J_District of Columbia



Sec.  147.450  State-administered program. [Reserved]



Sec.  147.451  EPA-administered program.

    (a) Contents. The UIC program for the District of Columbia, 
including any Indian lands in the District, is administered by EPA. This 
program consists of the UIC program requirements of 40 CFR parts 124, 
144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in the District of Columbia is November 25, 1988. The effective 
date for the UIC

[[Page 953]]

program in the rest of the District is June 25, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9413, Mar. 6, 1991]



Sec.  147.452  Aquifer exemptions. [Reserved]



                            Subpart K_Florida



Sec.  147.500  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Florida, except for those on Indian lands is administered by the Florida 
Department of Environmental Regulations, approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on February 7, 1983 (48 FR 5556); the effective date of 
this program is March 9, 1983. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Florida. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Florida Air and Water Pollution Control Act, Florida Statutes 
Annotated sections 403.011 through 403.90 (1973 and Supp. 1983);
    (2) Chapter 17-28, Underground Injection Control, Florida 
Administrative Code (April 27, 1989).
    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Administrative Procedures Act, Florida Statutes Chapter 120;
    (2) Florida Administrative Code, Chapter 17-1 (1982) (Administrative 
Procedures Act);
    (3) Florida Administrative Code, Chapter 17-3 (1982) (Water Quality 
Standards);
    (4) Florida Administrative Code, Chapter 17-4 (1982) (Permits);
    (5) Florida Administrative Code, Chapter 28-5 (1982) (Decisions 
Determining Substantial Interests);
    (6) Florida Administrative Code, Chapter 28-6 (1982) (Licensing);
    (c) The Memorandum of Agreement between EPA Region IV and the 
Florida Department of Environmental Regulation, signed by the EPA 
Regional Administrator on March 31, 1983.
    (d) Statement of legal authority. (1) ``Statement of Legal Authority 
for Implementation of Underground Injection Control Program'' and 
accompanying certifications, signed by General Counsel for the Florida 
Department of Environmental Regulation, January 14, 1982;
    (2) ``Addendum to Statement of Legal Authority for Implementation of 
Underground Injection Control Program'' and accompanying certifications, 
signed by Acting General Counsel for the Florida Department of 
Environmental Regulation, September 20, 1982.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43087, Oct. 25, 1988; 56 
FR 9414, Mar. 6, 1991]



Sec.  147.501  EPA-administered program--Class II wells and Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands and for Class II wells on non-Indian lands in the State of Florida 
is administered by EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date of the UIC program for 
Indian lands in Florida is November 25, 1988. The effective date for 
Class II wells on non-Indian lands is December 30, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9414, Mar. 6, 1991]

[[Page 954]]



Sec.  147.502  Aquifer exemptions. [Reserved]



Sec.  147.503  Existing Class II (except enhanced recovery 
and hydrocarbon storage) wells authorized by rule.

    Maximum injection pressure. To meet the operating requirements of 
Sec.  144.28(f)(3)(i) of this chapter, the owner or operator shall use 
an injection pressure at the well head no greater than the pressure 
calculated using the following formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.

[49 FR 45306, Nov. 15, 1984]



Sec.  147.504  Existing Class II enhanced recovery 
and hydrocarbon storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressure greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may grant such a request after notice, opportunity for 
comment, and opportunity for a public hearing, according to the 
provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressure based on data provided pursuant to 
paragraph (a)(2)(ii) of this section the owner or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within 1 year of the effective date of this 
program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall, when required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) Comply with other requirements which the Regional Administrator 
may specify either in addition to or in lieu

[[Page 955]]

of the requirements set forth in paragraphs (b)(1) through (3) of this 
section as needed to protect USDWs.
    (c) Area of review. Notwithstanding the alternatives presented in 
Sec.  146.06 of this chapter, the area of review shall be a minimum 
fixed radius as described in Sec.  146.06(b) of this chapter.

(The information collection requirements contained in paragraph 
(a)(2)(ii) were appoved by the Office of Management and Budget under 
control number 2040-0042)

[49 FR 45306, Nov. 15, 1984]



                            Subpart L_Georgia



Sec.  147.550  State-administered program.

    The UIC program for all classes of wells in the State of Georgia, 
except those wells on Indian lands, is the program administered by the 
Georgia Department of Natural Resources, Environmental Protection 
Division approved by EPA pursuant to section 1422 of the SDWA. Notice of 
this approval was published in the Federal Register on April 19, 1984 
(49 FR 15553); the effective date of this program is May 21, 1984. This 
program consists of the following elements, as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Georgia. This incorporation by reference 
was approved by the Director of the OFR in accordance with 5 U.S.C. 
552(a) and 1 CFR part 51. Copies may be obtained at the Georgia 
Department of Natural Resources, Environmental Protection Division, 270 
Washington Street, SW., Atlanta, Georgia, 30334. Copies may be inspected 
at the Environmental Protection Agency, Region IV, 345 Courtland Street, 
NE., Atlanta, Georgia, 30365, or at the National Archives and Records 
Administration (NARA). For information on the availability of this 
material at NARA, call 202-741-6030, or go to: http://www.archives.gov/
federal_register/code_of_federal_regulations/ibr_locations.html.
    (1) Oil and Gas and Deep Drilling Act of 1975, Official Code of 
Georgia Annotated (O.C.G.A.) Sec. Sec.  12-4-40 through 12-4-53 (1988);
    (2) Ground Water Use Act of 1972, O.C.G.A. Sec. Sec.  12-5-90 
through 12-5-107 (1988);
    (3) Water Well Standards Act of 1985, O.C.G.A. Sec. Sec.  12-5-120, 
through 12-5-138 (1988);
    (4) Georgia Administrative Procedure Act, O.C.G.A. Sec. Sec.  50-13-
1 through 50-13-22 (Reprinted from the O.C.G.A. and 1988 Cumm. Supp.);
    (5) Georgia Water Quality Control Act, O.C.G.A. Sec. Sec.  12-5-20 
through 12-5-53 (1988);
    (6) Georgia Hazardous Waste Management Act, O.C.G.A. Sec. Sec.  12-
8-60 through 12-8-83 (1988);
    (7) Georgia Safe Drinking Water Act of 1977, O.C.G.A. Sec. Sec.  12-
5-170 through 12-5-193 (1988);
    (8) Rules of Georgia Department of Natural Resources, Environmental 
Protection Division, Water Quality Control, GA. COMP. R. & REGS. Chapter 
391-3-6-.13 (Revised July 28, 1988).
    (b) Memorandum of Agreement. The Memorandum of Agreement between EPA 
Region IV and the State of Georgia, signed March 1, 1984.
    (c) Statement of legal authority. (1) Unofficial Opinion of the 
Georgia Attorney General, Op. Atty. Gen. 080-24, June 12, 1980;
    (2) Underground Injection Control Program, Attorney General's 
Statement, February 4, 1982;
    (3) Amended Attorney General's Statement Relating to Authority of 
the State of Georgia to Implement an Underground Injection Control 
Program, April 22, 1983;
    (4) Letter to EPA Office of General Counsel from Senior Assistant 
Attorney General ``Re: State UIC Program'', July 13, 1983.
    (d) Program Description. The Program Description and any other 
materials submitted as part of the application or as supplements 
thereto.

[56 FR 9414, Mar. 6, 1991; 56 FR 14150, Apr. 5, 1991]

[[Page 956]]



Sec. Sec.  147.551-147.552  [Reserved]



Sec.  147.553  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Georgia is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Georgia is November 25, 1988.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9414, Mar. 6, 1991]



Sec. Sec.  147.554-147.559  [Reserved]



                            Subpart M_Hawaii



Sec.  147.600  State-administered program. [Reserved]



Sec.  147.601  EPA-administered program.

    (a) Contents. The UIC program for the State of Hawaii, including all 
Indian lands, is administered by EPA. This program consists of the UIC 
program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Hawaii is November 25, 1988. The effective date for the UIC 
program for all other lands in Hawaii is December 30, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9414, Mar. 6, 1991]



                             Subpart N_Idaho



Sec.  147.650  State-administrative program--Class I, II, III, IV, and V wells.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Idaho, other than those on Indian lands, is the program administered 
by the Idaho Department of Water Resources, approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on June 7, 1985; the effective date of this program is 
July 22, 1985. This program consists of the following elements, as 
submitted to EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Idaho. This incorporation by reference 
was approved by the Director of the Federal Register effective July 22, 
1985.
    (1) Public Writings, Title 9, Chapter 3, Idaho Code, sections 9-301 
through 9-302 (Bobbs-Merrill 1979);
    (2) Crimes and Punishments, Title 18, Chapter 1, Idaho Code, 
sections 18-113 through 18-114 (Bobbs-Merrill 1979 and Supp. 1984);
    (3) Department of Health and Welfare, Title 39, Chapter 1, Idaho 
Code, Chapter 39-108 (Bobbs-Merrill 1977);
    (4) Drainage-Water Rights and Reclamation, Title 42, Chapter 2, 
Idaho Code sections 42-237(e); section 42-238 (Bobbs-Merrill 1977 and 
Supp. 1984);
    (5) Department of Water Resources-Water Resources Board, Title 42, 
Chapter 17, Idaho Code, sections 42-1701, 42-1703, 42-1735 (Bobbs-
Merrill 1977, section 42-1701A (Supp. 1984);
    (6) Director of Department of Water Resources, Title 42, Chapter 18, 
Idaho Code, sections 42-1801 through 42-1805 (Bobbs-Merrill 1977);
    (7) Waste Disposal and Injection Wells, Title 42, Chapter 39, Idaho 
Code, sections 42-3901 through 42-3914 (Bobbs-Merrill 1977), sections 
42-3915 through 42-3919 (Supp. 1984);
    (8) Idaho Trade Secrets Act, Title 48, Chapter 8, Idaho Code, 
sections 48-801 through 48-807 (Bobbs-Merrill 1977 and Supp. 1984);
    (9) Administrative Procedure, Title 67, Chapter 52, Idaho Code, 
sections

67-5201 through 67-5218 (Bobbs-Merrill 1980 and Supp. 1984);
    (10) Idaho Radiation Control Regulations (IRCR section 1-9002.70; 
sections 1-9100 through 1-9110, Department of Health and Welfare (May 
1981);
    (11) Rules and Regulations: Construction and Use of Injection Wells, 
Idaho

[[Page 957]]

Department of Water Resources, Rules 1 through 14 (August 1984);
    (12) Rules and Regulations: Practice and Procedures, Idaho 
Department of Water Resources, Rules 1 through 14 (October 1983).
    (b) The Memorandum of Agreement between EPA and Region X and the 
Idaho Department of Water Resources signed by the EPA Regional 
Administrator on February 11, 1985.
    (c) Statement of legal authority. (1) The Idaho Attorney General's 
Statement for the Underground Injection Control Program, October 31, 
1984.
    (2) Letter from David J. Barber, Deputy Attorney General, Idaho 
Department of Water Resources to Harold Scott, EPA, Region 10, revising 
the Attorney General's Statement, February 14, 1985.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[50 FR 23957, June 7, 1985]



Sec.  147.651  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Idaho is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date of the UIC program for 
Indian lands in Idaho is June 11, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9414, Mar. 6, 1991]



Sec.  147.652  Aquifer exemptions. [Reserved]



                           Subpart O_Illinois



Sec.  147.700  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Illinois, except those on Indian lands, is the program administered by 
the Illinois Environmental Protection Agency, approved by EPA pursuant 
to section 1422 of the SDWA. Notice of the approval was published in the 
Federal Register on February 1, 1984 (49 FR 3991); the effective date of 
this program is March 3, 1984. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
state statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Illinois. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Illinois Environmental Protection Act, Illinois ch. 111\1/2\, 
sections 1001 to 1051 (Smith-Hurd 1977 Revised Statutes and Supp. 1983), 
as amended by Public Act No. 83-431, 1983 Illinois Legislative Service, 
pages 2910 to 2916 (West);
    (2) Illinois Pollution Control Board Rules and Regulations at Title 
35, Illinois Administrative Code, Chapter I, Part 700, Outline of Waste 
Disposal Regulations; Part 702, RCRA and UIC Permit Programs; Part 704, 
UIC Permit Program; Part 705, Procedures for Permit Issuance and Part 
730, Underground Injection Control Operating Requirements as amended by 
IPCB Order No. R-83039 on December 15, 1983.
    (b) The Memorandum of Agreement between EPA Region V and the 
Illinois Environmental Protection Agency, signed by the EPA Regional 
Administrator on March 22, 1984.
    (c) Statement of legal authority. Letter from Illinois Attorney 
General to Regional Administrator, EPA Region V, and attached statement, 
December 16, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43087, Oct. 25, 1988]



Sec.  147.701  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Illinois, except 
those on Indian lands, is the program administered by the Illinois 
Environmental Protection Agency, approved by EPA pursuant to section 
1425 of the SDWA.

[[Page 958]]

Notice of the approval was published in the Federal Register on February 
1, 1984 (49 FR 3990); the effective date of this program is March 3, 
1984. This program consists of the following elements, as submitted to 
EPA in the state's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State Statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Illinois. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Conservation of Oil and Gas, etc., Illinois Revised Statutes ch. 
96\1/2\, sections 5401 to 5457 (Smith-Hurd 1979 and Supp. 1983), as 
amended by Public Act No. 83-1074 1983 Illinois Legislative Service 
pages 7183 to 7185 (West);
    (2) Illinois Environmental Protection Act, Illinois Revised Statutes 
ch. 111\1/2\, sections 1001-1051 (Smith-Hurd 1977 and Supp. 1983), as 
amended by Public Act No. 83-431, 1983 Illinois Legislative Services 
pages 2910 to 2916 (West);
    (3) Illinois Revised Statutes ch. 100\1/2\, section 26 (Smith-Hurd 
Supp. 1983);
    (4) Illinois Department of Mines and Minerals Regulations for the 
Oil and Gas Division, Rules I, II, IIA, III, V, VII, and IX (1981).
    (b) The Memorandum of Agreement between EPA Region V and the 
Illinois Department of Mines and Minerals, signed by the EPA Regional 
Administrator on March 22, 1984.
    (c) Statement of legal authority. ``Certification of Legal 
Authority,'' signed by State Attorney, Richland County, Illinois, May 5, 
1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43087, Oct. 25, 1988]



Sec.  147.703  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Illinois is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date for the UIC program for 
Indian lands is November 25, 1988.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9414, Mar. 6, 1991]



                            Subpart P_Indiana



Sec.  147.750  State-administered program--Class II wells.

    The UIC program for Class II injection wells in the State of Indiana 
on non-Indian lands is the program administered by the Indiana 
Department of Natural Resources (INDR) approved by the EPA pursuant to 
section 1425 of the SDWA. Notice of this approval was published in the 
FR on August 19, 1991; the effective date of this program is August 19, 
1991. This program consists of the following elements, as submitted to 
EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Indiana. This incorporation by reference 
was approved by the Director of the FR in accordance with 5 U.S.C. 
552(a) and 1 CFR part 51. Copies may be obtained at the Indiana 
Department of Natural Resources, Division of Oil and Gas, 402 West 
Washington Street, room 293, Indianapolis, Indiana, 46204. Copies may be 
inspected at the Environmental Protection Agency, Region V, 77 West 
Jackson Boulevard, Chicago, Illinois, 60604, or at the National Archives 
and Records Administration (NARA). For information on the availability 
of this material at NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Indiana Code, title 4, article 21.5, chapters 1 through 6 
(1988).
    (2) West's Annotated Indiana Code, title 13, article 8, chapters 1 
through 15 (1990 and Cumm. Supp. 1990).

[[Page 959]]

    (3) Indiana Administrative Code, title 310, article 7, rules 1 
through 3 (Cumm. Supp. 1991).
    (b) Memorandum of agreement. The Memorandum of Agreement between EPA 
Region V and the Indiana Department of Natural Resources signed by the 
EPA Regional Administrator on February 18, 1991.
    (c) Statement of legal authority. Statement and Amendment to the 
Statement from the Attorney General of the State of Indiana, signed on 
July 12, 1990, and December 13, 1990, respectively.
    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[56 FR 41072, Aug. 19, 1991, as amended at 62 FR 1834, Jan. 14, 1997]



Sec.  147.751  EPA-administered program.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands, and for Class I, III, IV, and V wells on non-Indian lands in the 
State of Indiana is administered by the EPA. The program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, and 148 and the 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date for the UIC program on 
Indian lands is November 25, 1988. The effective date of the UIC program 
for the rest of Indiana is June 25, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9414, Mar. 6, 1991; 56 
FR 41072, Aug. 19, 1991]



Sec.  147.752  Aquifer exemptions. [Reserved]



Sec.  147.753  Existing Class I and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lessor of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.800-0.433 Sg)d

where:

Pm = injection pressure at the wellhead in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.

[49 FR 20197, May 11, 1984, as amended at 56 FR 41072, Aug. 19, 1991]



                             Subpart Q_Iowa



Sec.  147.800  State-administered program. [Reserved]



Sec.  147.801  EPA-administered program.

    (a) Contents. The UIC program for the State of Iowa, including all 
Indian lands, is administered by EPA. This program consists of the UIC 
program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date for the UIC program for all 
lands in Iowa, including Indian lands, is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9415, Mar. 6, 1991]



Sec.  147.802  Aquifer exemptions. [Reserved]



                            Subpart R_Kansas



Sec.  147.850  State-administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Kansas, except those on Indian lands as described in Sec.  147.860, is 
the program administered by the Kansas Department of Health and 
Environment, approved by EPA pursuant to section 1422 of the SDWA. 
Notice of this approval was published in the Federal Register on 
December 2, 1983 (48 FR 54350); the effective date of this program is 
December 2, 1983. This program consists of the following elements, as 
submitted to EPA in the State's program application.

[[Page 960]]

    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Kansas. This incorporation by reference 
was approved by the Director of the OFR in accordance with 5 U.S.C. 
552(a) and 1 CFR part 51. Copies may be obtained at the Kansas 
Department of Health and Environment, Charles Curtis State Office 
Building, 1000 SW. Jackson, Topeka, Kansas 66612. Copies may be 
inspected at EPA Region 7, 11201 Renner Boulevard, Lenexa, Kansas 66219, 
or at the National Archives and Records Administration (NARA). For 
information on the availability of this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Chapter 28, Article 46, Underground Injection Control 
Regulations, Kansas Administrative Regulations Sec. Sec.  28-46-1 
through 28-46-42 (1986 and Supp. 1987);
    (2) Chapter 28, Article 43, Construction, operation, monitoring and 
abandonment of salt solution mining wells, Kansas Administrative 
Regulations Sec. Sec.  28-43-1 through 28-43-10 (1986);
    (3) Kansas Statutes Annotated Sec. Sec.  65-161, 65-164 through 65-
166a, 65-171d (1980 and Cumm. Supp. 1989).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for the select sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program: Kansas Statutes Annotated Sec. Sec.  65-161 
through 65-171(w), (1980 and Supp. 1983).
    (c) Memorandum of Agreement. (1) The Memorandum of Agreement between 
EPA Region VII and the Kansas Department of Health and Environment, 
signed by the EPA Regional Administrator on July 29, 1983;
    (2) Addendum No. 1 of the Memorandum of Agreement, signed by the EPA 
Regional Administrator on August 29, 1983.
    (d) Statement of legal authority. (1) ``Statement of Attorney 
General'', signed by the Attorney General of the State of Kansas, 
November 25, 1981;
    (2) ``Supplemental Statement of Attorney General'', signed by the 
Attorney General of the State of Kansas, undated (one page).
    (e) Program description. The program description and any other 
materials submitted as part of the application or supplements thereto.

[49 FR 45306, Nov. 15, 1984, as amended at 56 FR 9415, Mar. 6, 1991; 78 
FR 37978, June 25, 2013]



Sec.  147.851  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Kansas, except 
those on Indian lands as described in Sec.  147.860, is the program 
administered by the Kansas Corporation Commission and the Kansas 
Department of Health and Environment, approved by EPA pursuant to 
section 1425 of the SDWA. Notice of this approval was published in the 
Federal Register on February 8, 1984 (49 FR 4735); the effective date of 
this program is February 8, 1984. This program consists of the following 
elements, as submitted to EPA in the State's program application.

[49 FR 45306, Nov. 15, 1984]



Sec. Sec.  147.852-147.859  [Reserved]



Sec.  147.860  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Kansas is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Kansas is December 30, 1984.

[49 FR 45307, Nov. 15, 1984, as amended at 56 FR 9415, Mar. 6, 1991]



                           Subpart S_Kentucky



Sec.  147.900  State-administered program--Class II wells.

    The UIC program for Class II injection wells in the Commonwealth of 
Kentucky, except for those on Indian

[[Page 961]]

lands, is the program administered by the Kentucky Department of Natural 
Resources, Division of Oil and Gas approved by the EPA pursuant to 
section 1425 of the SDWA. Notification of this approval was published in 
the Federal Register on December 28, 2016; the effective date of this 
program is January 27, 2017. Table 1 to paragraph (a) of this section is 
the table of contents of the Kentucky state statutes and regulations 
incorporated as follows by reference. This program consists of the 
following elements, as submitted to the EPA in the state's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
Kentucky State statutes and regulations cited in the binder entitled 
``EPA-Approved Commonwealth of Kentucky Safe Drinking Water Act Sec.  
1425 Underground Injection Control (UIC) Program Statutes and 
Regulations for Class II wells,'' dated August 2016 is hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the Commonwealth of Kentucky. This incorporation by 
reference was approved by the Director of the Federal Register in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the 
Kentucky regulations may be obtained or inspected at the Kentucky 
Department of Natural Resources, Division of Oil and Gas, 3th Floor, 300 
Sower Blvd., Frankfort, Kentucky 40601, (315) 532-0191; at the U.S. 
Environmental Protection Agency, Region 4, 61 Forsyth Street SW., 
Atlanta, Georgia 30303-8960, (404) 562-8190; or at the National Archives 
and Records Administration (NARA). For information on availability of 
this material at NARA, call (202) 741-6030, or go to: http://
www.archives.gov/federal-register/cfr/ibr-locations.html.

 Table 1 to Paragraph (a)--EPA-Approved Kentucky SDWA Sec.   1425 Underground Injection Control Program Statutes
                                       and Regulations for Class II Wells
----------------------------------------------------------------------------------------------------------------
           State citation                   Title/subject          State effective date    EPA approval date \1\
----------------------------------------------------------------------------------------------------------------
Kentucky Revised Statutes Chapter    Kentucky Administrative      June 15, 1994.........  [Insert Federal
 13B.                                 Procedures Act KRS 13B.005                           Register citation].
                                      to 13B.170.
Kentucky Revised Statutes 353.180..  Requirements for plugging    June 24, 2015.........  [Insert Federal
                                      abandoned well--Bids--                               Register citation].
                                      Remedy for possessor of
                                      adjacent land or for
                                      department.
Kentucky Revised Statutes 353.510..  Definition of KRS 353.500    July 15, 2010.........  [Insert Federal
                                      to 353.720.                                          Register citation].
Kentucky Revised Statutes 353.520..  Territorial application of   June 24, 2003.........  [Insert Federal
                                      KRS 353.500 to 353.720--                             Register citation].
                                      Waste of oil and gas
                                      prohibited.
Kentucky Revised Statutes 353.550..  Specific authority over oil  July 15, 1996.........  [Insert Federal
                                      and gas operators.                                   Register citation].
Kentucky Revised Statutes 353.570..  Permit Required--May         July 15, 1998.........  [Insert Federal
                                      authorize operation prior                            Register citation].
                                      to issuance of permit.
Kentucky Revised Statutes 353.590..  Application for permit--     July 15, 2010.........  [Insert Federal
                                      Fees-Plat-Bond to insure                             Register citation].
                                      plugging--Schedule--Blanke
                                      t bonds-Corporate
                                      guarantee--Use of
                                      forfeited funds--Oil and
                                      gas well. plugging fund--
                                      Wells not included in
                                      ``water supply well.''.
Kentucky Revised Statutes 353.591..  Purpose and application of   July 15, 1986.........  [Insert FR citation].
                                      KRS 353.592 and 353.593.
Kentucky Revised Statutes 353.592..  Powers of the department...  June 24, 2015.........  [Insert FR citation].
Kentucky Revised Statutes 353.593..  Appeals....................  July 15, 1996.........  [Insert FR citation].
Kentucky Revised Statutes 353.992..  Penalties..................  July 15, 1986.........  [Insert FR citation].
805 Kentucky Administrative          Providing Protection for     August 9, 2007........  [Insert FR citation].
 Regulations 1:020.                   USDWs.
805 Kentucky Administrative          Well location and as-        October 23, 2009......  [Insert FR citation].
 Regulations 1:030.                   drilled location plat,
                                      preparation, form and
                                      contents.
805 Kentucky Administrative          Plugging wells; non-coal-    June 11, 1975.........  [Insert FR citation].
 Regulations 1:060.                   bearing strata.
805 Administrative Regulations       Plugging wells; coal         October 23, 1975......  [Insert FR citation].
 1:070.                               bearing strata.

[[Page 962]]

 
805 Kentucky Administrative          Underground Injection        April 4, 2008.........  [Insert FR citation].
 Regulations 1:110.                   Control.
----------------------------------------------------------------------------------------------------------------
\1\ In order to determine the EPA effective date for a specific provision listed in this table, consult the
  Federal Register document cited in this column for the particular provision.

    (b) Memorandum of Agreement (MOA). The MOA between EPA Region 4 and 
the Commonwealth of Kentucky Department of Natural Resources signed by 
EPA Regional Administrator on October 20, 2015.
    (c) Statements of Legal Authority. ``Underground Injection Control 
Program, Attorney General's Statement,'' signed by General Counsel of 
Kentucky Energy and Environmental Cabinet on June 7, 2010.
    (d) Program Description. The Program Description submitted as part 
of Kentucky's application, and any other materials submitted as part of 
this application or as a supplement thereto.

[81 FR 95483, Dec. 28, 2016]



Sec.  147.901  EPA-administered program--Class I, III, IV, V, and VI wells 
and Indian lands.

    (a) Contents. The UIC program for Class I, III, IV, V and VI wells 
and all wells on Indian lands in the Commonwealth of Kentucky is 
administered by the EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program on 
Indian lands is November 25, 1988. The effective date for the UIC 
program in the remainder of Kentucky is June 25, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9415, Mar. 6, 1991; 81 
FR 95484, Dec. 28, 2016]



Sec.  147.902  Acquifer exemptions.

    (a) This section identifies any aquifers or their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter. These 
aquifers are not being proposed for exemption under the Commonwealth of 
Kentucky's primacy approval. Rather, the exempted aquifers listed below 
were previously approved while EPA had primary enforcement authority for 
the Class II UIC program in the Commonwealth of Kentucky and are 
included here for reference. Additional information pertinent to these 
exempted aquifers or their portions resides in EPA Region 4.
    (1) The following eight aquifers (underground sources of drinking 
water) in the Commonwealth of Kentucky have been exempted in accordance 
with the provisions of Sec. Sec.  144.7(b) and 146.4 of this chapter for 
Class II injection activities only: A portion of the Tar Springs 
sandstone formation that has a quarter mile radius areal extent (125.6 
acres) that is located at latitude 37.7261 and longitude -86.6914. The 
formation has a true vertical depth from surface of 280 feet.
    (2) A portion of the Tar Springs sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.7294 and longitude -867212. The formation has a true 
vertical depth from surface of 249 feet.
    (3) A portion of the Tar Springs sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.7055 and longitude -86.7177. The formation has a true 
vertical depth from surface of 210 feet.
    (4) A portion of the Pennsylvanian Age sandstone formation that has 
a quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.5402 and longitude -87.2551. The formation has a true 
vertical depth from surface of 1,050 feet.
    (5) A portion of the Tar Springs sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.7301 and longitude -87.6922. The formation has

[[Page 963]]

a true vertical depth from surface of 240 feet.
    (6) A portion of the Caseyville sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.5776 and longitude -87.1321. The formation had a true 
vertical depth from surface of 350 feet.
    (7) A portion of the Caseyville sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.5778 and longitude -87.1379. The formation has a true 
vertical depth from surface of 1,080 feet.
    (8) A portion of the Caseyville sandstone formation that has a 
quarter mile radius areal extent (125.6 acres) that is located at 
latitude 37.5652 and longitude -87.1222. The formation has a true 
vertical depth from surface of 1,060 feet.
    (b) [Reserved]

[81 FR 95484, Dec. 28, 2016]



Sec.  147.903  Existing Class I and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable or;
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.



Sec.  147.904  [Reserved]



Sec.  147.905  Requirements for all wells--area of review.

    Notwithstanding the alternatives presented in Sec.  146.6 of this 
chapter, the area of review shall be a minimum fixed radius as described 
in Sec.  146.6(b) of this chapter.



                           Subpart T_Louisiana



Sec.  147.950  State-administered program.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Louisiana, except those wells on Indian lands, is the program 
administered by the Louisiana Department of Natural Resources approved 
by EPA pursuant to sections 1422 and 1425 of the SDWA. Notice of this 
approval was published in the Federal Register on April 23, 1982 (47 FR 
17487); the effective date of this program is March 23, 1982. This 
program consists of the following elements, as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Louisiana. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Louisiana Revised Statutes Annotated sections 30:1-30:24 (1975 
and Supp. 1982);
    (2) Underground Injection Control Program Regulations for Class I, 
III, IV, and V wells, Statewide Order No. 29-N-1 (February 20, 1982), as 
amended June 1, 1985 and January 20, 1986;
    (3)(i) Statewide Order Governing the Drilling for and Producing of 
Oil and Gas in the State of Louisiana, Statewide Order No. 29-B (August 
26, 1974) (Composite Order Incorporating Amendments through March 1, 
1974);
    (ii) Amendments to Statewide Order No. 29-B (Off-site Disposal of 
Drilling Mud and Salt Water Generated from Drilling and Production of 
Oil and Gas Wells) (effective July 20, 1980);
    (iii) Amendment to Statewide Order No. 29-B (Amendment concerning 
the use of Tables 5A and 6A, etc.) (December 15, 1980, effective January 
1, 1981);
    (iv) Amendment to Statewide Order No. 29-B (Amendment concerning the 
underground injection control of saltwater disposal wells, enhanced 
recovery injection wells, and liquid hydrocarbon storage wells) 
(effective February 20, 1982);
    (v) Amendment to Statewide Order No. 29-B (Amendment concerning the 
offsite disposal of drilling mud and saltwater) (effective May 20, 
1983);

[[Page 964]]

    (vi) Amendment to Statewide Order No. 29-B (Amendment concerning 
disposal of nonhazardous oilfield waste) (March 20, 1984, effective May 
20, 1984);
    (vii) Amendment to Statewide Order No. 29-B (Amendment concerning 
the administrative approval of injectivity tests and pilot projects in 
order to determine the feasibility of proposed enhanced recovery 
projects) (June 20, 1985, effective July 1, 1985).
    (4) (i) Statewide Order adopting rules and regulations pertaining to 
the use of salt dome cavities (i.e., storage chambers) for storage of 
liquid and/or gaseous hydrocarbons, etc., Statewide Order No. 29-M (July 
6, 1977, effective July 20, 1977);
    (ii) Supplement to Statewide Order No. 29-M (October 2, 1978);
    (iii) Second Supplement to Statewide Order No. 29-M (June 8, 1979).
    (b)(1) The Memorandum of Agreement (Class I, III, IV, and V wells) 
between EPA Region VI and the Louisiana Department of Natural Resources, 
Office of Conservation, signed by the EPA Regional Administrator on 
March 17, 1982 and amended by Addendum 1 and Addendum 2 on November 3, 
1989;
    (2) The Memorandum of Agreement (Class II wells) between EPA Region 
VI and the Louisiana Department of Natural Resources, Office of 
Conservation, signed by the EPA Regional Administrator on March 17, 
1982.
    (c) Statement of legal authority. (1) Letter from Attorney General 
of Louisiana to EPA, ``Re: Louisiana Underground Injection Control 
Program Authorization for State of Louisiana'' (Class I, III, IV and V 
Wells), January 13, 1982, (10 pages);
    (2) Letter from Attorney General of Louisiana to EPA, ``Re: 
Louisiana Underground Injection Control Program Authorization for State 
of Louisiana'' (Class II Wells), January 13, 1982 (5 pages).
    (3) Letter from Attorney General of Louisiana to EPA, ``Re: Class I 
Hazardous Waste Injection Well Regulatory Program; Attorney General's 
Statement, October 9, 1989 (9 pages);
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 56 FR 9415, Mar. 6, 1991]



Sec.  147.951  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Louisiana is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date of the UIC program for 
Indian lands in Louisiana is November 25, 1988.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9415, Mar. 6, 1991]



                             Subpart U_Maine



Sec.  147.1000  State-administered program.

    The UIC program for all classes of wells in the State of Maine, 
except those on Indian lands, is the program administered by the Maine 
Department of Environmental Protection approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on August 25, 1983 (48 FR 38641); the effective date of 
this program is September 26, 1983. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made part of the applicable UIC program 
under the SDWA for the State of Maine. This incorporation by reference 
was approved by the Director of the OFR on June 25, 1984.
    (1) Maine Revised Statutes Annotated title 38, sections 361-A, 363-
B, 413, 414, 414-A, 420, and 1317-A (1978);
    (2) Rules to Control the Subsurface Discharge of Pollutants by Well 
Injection, Rules of the Department of Environmental Protection, Chapter 
543

[[Page 965]]

(adopted June 22, 1983, effective July 4, 1983).
    (b) The Memorandum of Agreement between EPA Region I and the Maine 
Department of Environmental Protection, signed by the EPA Regional 
Administrator on May 16, 1983.
    (c) Statement of legal authority. Letter from Attorney General of 
Maine to EPA Regional Administrator, ``Re: Attorney General's Statement: 
Maine Underground Injection Control Program Primacy Application,'' June 
30, 1983.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43088, Oct. 25, 1988; 56 
FR 9415, Mar. 6, 1991]



Sec.  147.1001  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Maine is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date of the UIC program for 
Indian lands in Maine is November 25, 1988.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9416, Mar. 6, 1991]



                           Subpart V_Maryland



Sec.  147.1050  State-administered program--Class I, II, III, IV, and V wells.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Maryland, except those wells on Indian lands, is the program 
administered by the Maryland Department of the Environment approved by 
EPA pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the FR on April 19, 1984 (49 FR 15553); the effective date 
of this program is June 4, 1984. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Maryland. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained at the Maryland 
Department of the Environment, 2500 Broening Highway, Baltimore, 
Maryland, 21224. Copies may be inspected at the Environmental Protection 
Agency, Region III, 841 Chestnut Street, Philadelphia, Pennsylvania, 
19107, or at the National Archives and Records Administration (NARA). 
For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 07 
promulgated and effective as of March 1, 1989;
    (2) Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 01, 
promulgated and effective as of March 1, 1989;
    (3) Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 02, 
promulgated and effective as of March 1, 1989;
    (4) Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 03, 
promulgated and effective as of March 1, 1989;
    (5) Code of Maryland Regulations, Title 26, Subtitle 08, Chapter 04, 
promulgated and effective as of March 1, 1989;
    (6) Code of Maryland Regulations, Title 26, Subtitle 13, Chapter 05, 
section .19, promulgated and effective as of August 1, 1989;
    (7) Code of Maryland Regulations, Title 26, Subtitle 01, Chapter 02, 
promulgated and effective as of March 1, 1989;
    (8) Code of Maryland Regulations, Title 26, Subtitle 01, Chapter 04, 
promulgated and effective as of March 1, 1989.
    (b) Memorandum of Agreement. The Memorandum of Agreement between

[[Page 966]]

EPA Region III and the Maryland Department of the Environment, as 
submitted on August 2, 1983, and revised on February 16, 1984.
    (c) Statement of legal authority. Statement from the Maryland 
Attorney General on the Underground Injection Control Program, as 
submitted on August 2, 1983, and revised on February 16, 1984.
    (d) Program Description. The Program Description and other materials 
submitted as part of the application or as supplements thereto.

[56 FR 9416, Mar. 6, 1991]



Sec. Sec.  147.1051-147.1052  [Reserved]



Sec.  147.1053  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Maryland is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Maryland is November 25, 1988.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9416, Mar. 6, 1991]



Sec. Sec.  147.1054-147.1099  [Reserved]



                         Subpart W_Massachusetts



Sec.  147.1100  State-administered program.

    The UIC program for all classes of wells in the State of 
Massachusetts, except those on Indian lands, is the program administered 
by the Massachusetts Department of Environmental Protection, approved by 
EPA pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on November 23, 1982 (47 FR 52705); 
the effective date of this program is December 23, 1982. This program 
consists of the following elements, as submitted to EPA in the State's 
program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Massachusetts. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Massachusetts General Laws Annotated chapter 21, sections 27, 
43, and 44 (West 1981);
    (2) Code of Massachusetts Regulations, title 310, sections 23.01-
23.11 as amended April 26, 1982.
    (b) The Memorandum of Agreement between EPA Region I and the 
Massachusetts Department of Environmental Quality Engineering, signed by 
the EPA Regional Administrator on August 18, 1982.
    (c) Statement of legal authority. ``Underground Injection Control 
Program--Attorney General's Statement for Class I, II, III, IV and V 
Injection Wells,'' signed by Assistant Attorney General for Attorney 
General of Massachusetts, May 13, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43088, Oct. 25, 1988]



Sec.  147.1101  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Massachusetts is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Massachusetts is November 25, 1988.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9416, Mar. 6, 1991]



                           Subpart X_Michigan



Sec.  147.1150  State-administered program. [Reserved]



Sec.  147.1151  EPA-administered program.

    (a) Contents. The UIC program for the State of Michigan, including 
all Indian

[[Page 967]]

lands, is administered by EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program for all 
lands in Michigan, including Indian lands, is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9416, Mar. 6, 1991]



Sec.  147.1152  Aquifer exemptions. [Reserved]



Sec.  147.1153  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.800-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.



Sec.  147.1154  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regonal 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may grant such a request after notice, opportunity for 
comment, and opportunity for a public hearing, according to the 
provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
field rules for maximum injection pressure based on data provided 
pursuant to paragraph (a)(2)(ii) of this section the owner or operator 
shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within 1 year following the effective date of 
this program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage will may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing

[[Page 968]]

and the well bore to a point 250 feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) of this section, as needed to protect USDWs.



Sec.  147.1155  Requirements for all wells.

    (a) Area of review. Notwithstanding the alternatives presented in 
Sec.  146.6 of this chapter, the area of review for Class II wells shall 
be a fixed radius as described in Sec.  146.6(b) of this chapter.
    (b) Tubing and packer. The owner or operator of an injection well 
injecting salt water for disposal shall inject through tubing and 
packer. The owner of an existing well must comply with this requirement 
within one year of the effective date of this program.



                           Subpart Y_Minnesota



Sec.  147.1200  State-administered program. [Reserved]



Sec.  147.1201  EPA-administered program.

    (a) Contents. The UIC program for the State of Minnesota is 
administered by EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective date. The effective date of the UIC program for 
Minnesota is: June 11, 1984.

[49 FR 20197, May 11, 1984, as amended at 56 FR 9416, Mar. 6, 1991]



Sec.  147.1202  Aquifer exemptions. [Reserved]



Sec.  147.1210  Requirements for Indian lands.

    (a) Purpose and scope. This section sets forth additional 
requirements that apply to injection activities on Indian lands in 
Minnesota.
    (b) Requirements. Notwithstanding the other requirements of this 
subpart, for Indian lands described in paragraph (a) of this section, no 
owner or operator shall construct, operate, maintain, or convert any 
Class I, II, III, or IV well. The UIC program for Class V wells on such 
Indian Lands is administered by EPA, and consists of the applicable 
requirements of 40 CFR parts 124, 144, and 146. In addition, no owner or 
operator shall abandon a well without the approval of the Regional 
Administrator.
    (c) Effective date. The effective date of the UIC program 
requirements for Indian lands in Minnesota is December 30, 1984.

[49 FR 45307, Nov. 15, 1984]



                          Subpart Z_Mississippi



Sec.  147.1250  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Mississippi, except those on Indian lands, is the program administered 
by the Mississippi Department of Natural Resources approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on August 25, 1983 (48 FR 38641); the 
effective date of this program is September 26, 1983. This program 
consists of the following elements, as submitted to EPA in the State's 
program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Mississippi. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.

[[Page 969]]

    (1) Mississippi Air and Water Pollution Control Law, Mississippi 
Code Annotated sections 49-17-1 through 49-17-29 (1972) and Supp. 1983);
    (2) Mississippi Department of Natural Resources, Bureau of Pollution 
Control, Underground Injection Control Program Regulations (adopted 
February 11, 1982);
    (3) Mississippi Department of Natural Resources, Bureau of Pollution 
Control, State of Mississippi Wastewater Permit Regulations for National 
Pollutant Discharge Elimination System (NPDES), Underground Injection 
Control (UIC), and State Operating Permits (adopted May 1, 1974; amended 
February 11, 1982).
    (b) The Memorandum of Agreement between EPA Region IV and the 
Mississippi Department of Natural Resources, signed by the EPA Regional 
Administrator on February 8, 1983.
    (c) Statement of legal authority. (1) Letter from Attorney General 
of Mississippi (by Special Assistant Attorney General) to Executive 
Director, Mississippi Department of Natural Resources, ``Re: Mississippi 
Department of Natural Resources, Bureau of Pollution Control, State 
Underground Injection Control (UIC) Program; Statement of the Attorney 
General of the State of Mississippi,'' December 3, 1981;
    (2) Letter from Attorney General of Mississippi (by Special 
Assistant Attorney General) to Executive Director, Mississippi 
Department of Natural Resources, ``Re: Authority to Regulate and Take 
Samples from Underground Injection Systems,'' October 18, 1982;
    (3) Letter from Attorney General of Mississippi (by Special 
Assistant Attorney General) to Regional Administrator, EPA Region IV, 
``Re: Public Participation in State Enforcement Actions, UIC Program,'' 
June 10, 1983.
    (d) The Program Description and any other materials submitted as 
part of the application or supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43088, Oct. 25, 1988]



Sec.  147.1251  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Mississippi, 
other than those on Indian lands, is the program administered by the 
State Oil and Gas Board of Mississippi approved by EPA pursuant to 
section 1425 of the SDWA. Notice of this approval was published in the 
Federal Register on March 2, 1989; the effective date of this program is 
March 2, 1989. This program consists of the following elements, as 
submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Mississippi. This incorporation by 
reference was approved by the Director of the Federal Register in 
accordance with 5 U.S.C. 552(a).
    (1) Mississippi Code Annotated, section 5-9-9 (Supp. 1988).
    (2) Mississippi Code Annotated, sections 53-1-1 through 53-1-47, 
inclusive and sections 53-1-71 through 53-1-77, inclusive (1972 and 
Supp. 1988).
    (3) Mississippi Code Annotated, sections 53-3-1 through 53-3-165, 
inclusive (1972 and Supp. 1988).
    (4) State Oil and Gas Board Statewide Rules and Regulations, Rules 1 
through 65, inclusive (Aug. 1, 1987, as amended, Sept. 17, 1987).
    (b) The Memorandum of Agreement between EPA Region IV and the State 
Oil and Gas Board of Mississippi signed by the Regional Administrator on 
October 31, 1988.
    (c) Statement of legal authority. Statement from the Attorney 
General signed on October 1, 1987 with amendments to the Statement 
signed August 5, 1988 and September 15, 1988 by the Special Assistant 
Attorney General.
    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[54 FR 8735, Mar. 2, 1989]



Sec.  147.1252  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Mississippi is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners

[[Page 970]]

and operators, and EPA shall comply with these requirements.
    (b) Effective date. The effective date of the UIC program on Indian 
lands is November 25, 1988.

[53 FR 8735, Mar. 2, 1989, as amended at 56 FR 9416, Mar. 6, 1991]



                           Subpart AA_Missouri



Sec.  147.1300  State-administered program.

    The UIC program for all classes of wells in the State of Missouri, 
except those on Indian lands, is administered by the Missouri Department 
of Natural Resources, approved by EPA pursuant to section 1422 and 1425 
of the SDWA. Notice of this approval was published in the Federal 
Register on December 2, 1983 (48 FR 54349); the effective date of this 
program is December 2, 1983). This program consists of the following 
elements, as submitted to EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Missouri. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Vernon's Annotated Missouri Statutes sections 259.010 to 259.240 
(Supp. 1984);
    (2) Missouri Code of State Regulations, title 10, division 50, 
chapters 1 and 2 (June 1984);
    (3) Vernon's Annotated Missouri Statutes chapter 204, Sec. Sec.  
204.006 through 204.470 (1983 and Cumm. Supp. 1990).
    (b) The Memorandum of Agreement between EPA Region VII and the 
Missouri Department of Oil and Gas, signed by the EPA Regional 
Administrator on December 3, 1982.
    (c) Statement of legal authority. (1) Opinion Letter No. 63 and 
attached Memorandum Opinion, signed by Attorney General of Missouri, 
March 16, 1982;
    (2) Addendum to Opinion Letter No. 63 (1982), signed by Attorney 
General of Missouri, October 28, 1982.
    (3) Opinion No. 127-83, signed by Attorney General of Missouri, July 
11, 1983.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43088, Oct. 25, 1988; 56 
FR 9416, Mar. 6, 1991]



Sec.  147.1301  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Missouri, other than those on Indian lands, is the program administered 
by the Missouri Department of Natural Resources, approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on November 2, 1984; the effective 
date of this program is July 31, 1985. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Missouri. This incorporation by 
reference was approved by the Director of the Federal Register effective 
July 31, 1985.
    (1) Revised Statutes of the State of Missouri, Volume 2, sections 
204.016, 204.026, 204.051, 204.056 and Volume V, section 577.155 (1978 
and Cumm. Supp. 1984);
    (2) Missouri Code of State Regulations, title 10, division 20, 
Chapter 6, sections 20-6.010, 20-6.020, 20-6.070, 20-6.080, 20-6.090, 
and title 10, division 20, Chapter 7, section 20-7.031 (1977, amended 
1984).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for select sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program.
    (1) Revised Statutes of the State of Missouri, chapters 204, 260, 
536, 557, 558 and 560; sections 640.130.1 and 1.020 (1978 and Cumm. 
Supp. 1984);
    (2) Rule 52.12 Vernon's Annotated Missouri Rules (1978);

[[Page 971]]

    (3) Missouri Code of State Regulations, title 10, division 20, 
Chapters 1 through 7 (1977, amended 1984).
    (c) The Memorandum of Agreement between EPA Region VII and the 
Missouri Department of Natural Resources, signed by the EPA Regional 
Administrator on October 10, 1984.
    (d) Statement of Legal Authority. Opinion No. 123-84, signed by 
Attorney General of Missouri, September 24, 1984. Amended April 2, 1985.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[50 FR 28942, July 17, 1985]



Sec.  147.1302  Aquifer exemptions. [Reserved]



Sec.  147.1303  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Missouri is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 145, 
146, 148, and any additional requirements set forth in the remainder of 
this subpart. Injection well owners and operators, and EPA shall comply 
with these requirements.
    (b) Effective date. The effective date for the UIC program for 
Indian lands is November 25, 1988.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9417, Mar. 6, 1991]



                           Subpart BB_Montana



Sec.  147.1350  State-administered programs--Class II wells.

    The UIC program for Class II injection wells in the State of 
Montana, except for those in Indian Country, is the program administered 
by the Montana Board of Oil and Gas Conservation (MBOGC) approved by the 
EPA pursuant to Section 1425 of the SDWA. Notice of this approval was 
published in the Federal Register on November 19, 1996; the effective 
date of this program is November 19, 1996. This program consists of the 
following elements as submitted to EPA in the State's program 
application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made part of the applicable UIC program 
under the SDWA for the State of Montana. This incorporation by reference 
was approved by the Director of the FR in accordance with 5 U.S.C. 
552(a) and 1 CFR part 51. Copies may be obtained at the Montana Board of 
Oil and Gas Conservation, 2535 St. Johns Avenue, Billings, Montana, 
59102. Copies may be inspected at the Environmental Protection Agency, 
Region VIII, 999 18th Street, Suite 500, Denver, Colorado, 80202-2466, 
or at the National Archives and Records Administration (NARA). For 
information on the availability of this material at NARA, call 202-741-
6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Montana Statutory Requirements Applicable to the Underground 
Injection Control Program, August, 1996.
    (2) Montana Regulatory Requirements Applicable to the Underground 
Injection Control Program, August, 1996.
    (b) Memorandum of Agreement (MOA). (1) The MOA between EPA Region 
VIII and the MBOGC signed by the Acting EPA Regional Administrator on 
June 9, 1996.
    (2) Letter dated May 24, 1996, from the Administrator of the MBOGC 
and the attached addendum (Addendum No. 1-96) to the MOA between MBOGC 
and EPA Region VIII, signed by the Acting EPA Regional Administrator on 
August 14, 1996.
    (c) Statement of legal authority. (1) Letter from the Montana 
Attorney General to the Regional Administrator dated August 1, 1995.
    (2) MBOGC independent counsel's certification of Montana's UIC 
program for Class II wells dated July 24, 1995.
    (3) Letter dated March 8, 1996, from MBOGC independent counsel to 
USEPA, Region VIII; ``Re: EPA comments of November 29, 1995, on Montana 
Class II primacy application.''
    (4) Letter dated March 8, 1996, from the Administrator of the MBOGC 
and the attached proposed replacement language for the MOA; ``Re: 
Responses to EPA comments on Montana Class II Primacy Application.''

[[Page 972]]

    (d) Program Description. The Program Description and any other 
materials submitted as part of the application or as supplemented 
thereto:
    (1) Application and accompanying materials for approval of Montana's 
UIC program for Class II wells submitted by the Governor of Montana, 
August 3, 1995.
    (2) [Reserved]

[61 FR 58933, Nov. 19, 1996]



Sec.  147.1351  EPA-administered program.

    (a) Contents. The UIC program in the State of Montana for Class I, 
III, IV, and V wells, and for all Classes of wells in Indian country in 
Montana, except for Class II wells on all lands within the exterior 
boundaries of the Fort Peck Indian Reservation, is administered by EPA. 
This program consists of the UIC program requirements of 40 CFR parts 
124, 144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program for 
Class I, III, IV, and V wells for all lands in Montana, including all 
Indian country in Montana, and for Class II wells for all Indian country 
in Montana other than the Fort Peck Indian Reservation, is June 25, 
1984. The effective date for the EPA-approved State-administered UIC 
Class II program for all lands in Montana, except for those in Indian 
country, is provided in Sec.  147.1350.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9417, Mar. 6, 1991; 61 
FR 58933, Nov. 19, 1996; 73 FR 63646, Oct. 27, 2008]



Sec.  147.1352  Aquifer exemptions.

    Those portions of aquifers within one-quarter mile of existing Class 
II wells are exempted for the purpose of Class II injection activities 
only.
    Note: A complete listing of the exemptions and their location is 
available for review in the EPA Regional Office, 1860 Lincoln Street, 
Denver, Colorado. An updated list of exemptions will be maintained in 
the Regional Office.



Sec.  147.1353  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733 - 0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.



Sec.  147.1354  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may grant such a request after notice, opportunity for 
comment, and opportunity for a public hearing, according to the 
provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator established 
rules for maximum injection pressure based on

[[Page 973]]

data provided pursuant to paragraph (ii) below the owner or operator 
shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within 1 year of the effective date of this 
program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall when required by the Regional Administrator:
    (1) Isolate all USDWs by placing cement between the outermost casing 
and the well bore as follows:
    (i) If the injection well is east of the 108th meridian, cement the 
outermost casing from a point 50 feet into a major shale formation 
underlying the uppermost USDW to the surface. For the purpose of this 
paragraph, major shale formations are defined as the Bearpaw, Clagget, 
and Colorado formations.
    (ii) If the injection well is west of the 108th meridian, cement the 
outermost casing to a depth of 1,000 feet, or to the base of the 
lowermost USDW in use as a source of drinking water whichever is deeper. 
The Regional Administrator may allow an owner or operator to cement to a 
lesser depth if he can demonstrate to the satisfaction of the Regional 
Administrator that no USDW will be affected by the injection facilities.
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deteriortion from formation and injection 
fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) of this section, as needed to protect USDWs.



Sec.  147.1355  Requirements for all wells.

    (a) Area of review. Notwithstanding the alternatives presented in 
Sec.  146.6 of this chapter, the area of review shall be a fixed radius 
as described in Sec.  146.06(b) of this chapter.
    (b) The applicant must give separate notice of intent to apply for a 
permit to each owner or tenant of the land within one-quarter mile of 
the site. This requirement may be waived by the Regional Administrator 
where individual notice to all land owners and tenants would be 
impractical. The addresses of those to whom notice is given, and a 
description of how notice was given, shall be submitted with the permit 
application. The notice shall include:
    (1) Name and address of applicant;
    (2) A brief description of the planned injection activities, 
including well location, name and depth of the injection zone, maximum 
injection pressure and volume, and fluid to be injected;
    (3) EPA contact person; and
    (4) A statement that opportunity to comment will be announced after 
EPA prepares a draft permit.
    (c) Owners and operators on or within one-half mile of Indian lands 
shall provide notice as specified in paragraph (b) of this section, 
except that such notice shall be provided within a one-half mile radius 
of the site.



     Sec. Appendix A to Subpart BB of Part 147--State Requirements 
   Incorporated by Reference in Subpart BB of Part 147 of the Code of 
                           Federal Regulations

    The following is an informational listing of state requirements 
incorporated by reference in Subpart BB of part 147 of the Code of 
Federal Regulations:

[[Page 974]]

                           Subpart BB--Montana

    (a) The statutory provisions include:
    (1) Montana Code annotated, 1995, Title 2, Chapter 15:
Section 2-15-121. Allocation for administrative purposes only.
Section 2-15-124. Quasi-judicial boards.
Section 2-15-3303. Board of oil and gas conservation-composition--
allocation--quasi-judicial.
    (2) Montana Code annotated, 1995, Title 82, Chapter 10:
Section 82-10-101. Action for accounting for royalty.
Section 82-10-102. Remedy not exclusive.
Section 82-10-103. Obligation to pay royalties as essence of contract-
interest.
Section 82-10-104. Payment of royalties-form of record required.
Section 82-10-105 through 82-10-109 reserved.
Section 82-10-110. Division order-definition-effect.
Section 82-10-201. Authorization for lease and terms-land not subject to 
leasing.
Section 82-10-202. Acreage pooling.
Section 82-10-203. Interference with normal use of land prohibited.
Section 82-10-204. Lease of acquired oil and gas interests.
Section 82-10-301. Definitions.
Section 82-10-302. Policy.
Section 82-10-303. Use of eminent domain to acquire underground 
reservoirs.
Section 82-10-304. Certificate of board required prior to use of eminent 
domain.
Section 82-10-305. Proceedings.
Section 82-10-401. Notice required before abandonment of well-owner's 
option.
Section 82-10-402. Inventory of abandoned wells and seismic operations-
reclamation procedures.
Section 82-10-501. Purpose-legislative findings.
Section 82-10-502. Definitions.
Section 82-10-503. Notice of drilling operations.
Section 82-10-504. Surface damage and disruption payments-penalty for 
late payment.
Section 82-10-505. Liability for damages to property.
Section 82-10-506. Notification of injury.
Section 82-10-0507. Agreement--offer of settlement.
Section 82-10-508. Rejection--legal action.
Section 82-10-509 and 82-10-510. Reserved.
Section 82-10-511. Remedies cumulative.
    (3) Montana Code annotated, 1995, Title 82, Chapter 11:
Section 82-11-101. Definitions.
Section 82-11-102. Oil or gas wells not public utilities.
Section 82-11-103. Lands subject to law.
Section 82-11-104. Construction-no conflict with board of land 
commissioners' authority.
Section 82-11-105 through 82-11-110 reserved.
Section 82-11-111. Powers and duties of board.
Section 82-11-112. Intergovernmental cooperation.
Section 82-11-113. Role of board in implementation of national gas 
policy.
Section 82-11-114. Appointment of examiners.
Section 82-11-115. Procedure to make determinations.
Section 82-11-116. Public access.
Section 82-11-117. Confidentiality of records.
Section 82-11-118. Fees for processing applications.
Section 82-11-119 through 82-11-120 reserved.
Section 82-11-121. Oil and gas waste prohibited.
Section 82-11-122. Notice of intention to drill or conduct seismic 
operations-notice to surface owner.
Section 82-11-123. Requirements for oil and gas operations.
Section 82-11-124. Requirement relating to waste prevention.
Section 82-11-125. Availability of cores or chips, cuttings, and bottom-
hole temperatures to board.
Section 82-11-126. Availability of facilities to bureau of mines.
Section 82-11-127. Prohibited activity.
Section 82-11-128 through 82-11-130 reserved.
Section 82-11-131. Privilege and license tax.
Section 82-11-132. Statements to treasurer and payment of tax.
Section 82-11-133. Penalty for late payment.
Section 82-11-134. Permit fees.
Section 82-11-135. Money earmarked for board expenses.
Section 82-11-136. Expenditure of funds from bonds for plugging wells.
Section 82-11-137. Class II injection well operating fee.
Section 82-11-138 through 82-11-140 reserved.
Section 82-11-141. Administrative procedure.
Section 82-11-142. Subpoena power-civil actions.
Section 82-11-143. Rehearing.
Section 82-11-144. Court review.
Section 82-11-145. Injunction or restraining order.
Section 82-11-146. Appeal.
Section 82-11-147. Violations.
Section 82-11-148. Criminal penalties.
Section 82-11-149. Civil penalties.
Section 82-11-150. Legal assistance.
Section 82-11-151. Emergencies-notice and hearing.
Section 82-11-152 through 82-11-160 reserved.
Section 82-11-161. Oil and gas production damage mitigation account-
statutory appropriation.
Section 82-11-162. Release of producing oil or gas well from drilling 
bond-fee.
Section 82-11-163. Landowner's bond on noncommercial well.
Section 82-11-164. Lien created.
Section 82-11-165 through 82-11-170 reserved.

[[Page 975]]

Section 82-11-171. Terminated.
Section 82-11-201. Establishment of well spacing units.
Section 82-11-202. Pooling of interest within spacing unit.
Section 82-11-203. Pooling agreements not in violation of antitrust 
laws.
Section 82-11-204. Hearing on operation of pool as unit.
Section 82-11-205. Board order for unit operation-criteria.
Section 82-11-206. Terms and conditions of plan for unit operations.
Section 82-11-207. Approval of plan for unit operations by persons 
paying costs.
Section 82-11-208. Board orders-amendment.
Section 82-11-209. Units established by previous order.
Section 82-11-210. Unit operations-less than whole of pool.
Section 82-11-211. Operations considered as done by all owners in unit.
Section 82-11-212. Property rights and operator's lien.
Section 82-11-213. Contract not terminated by board order.
Section 82-11-214. Title to oil and gas rights not affected by board 
order.
Section 82-11-215. Unit operation not restraint of trade.
Section 82-11-216. No creation of relationship between parties in unit.
Section 82-11-301. Authorization to join interstate compact for 
conservation of oil and gas.
Section 82-11-302. Interstate oil and gas compact.
Section 82-11-303. Extension of expiration date.
Section 82-11-304. Governor as member of Interstate Oil Compact 
Commission.
Section 82-11-305. Limitation on power of representative.
Section 82-11-306. Expenses of representative.
    (b) The regulatory provisions include: Administrative Rules of 
Montana Board of Oil and Gas Conservation, Chapter 22, revised March 
1996:
Rule 36.22.101. Organizational Rule.
Rule 36.22.201. Procedural Rules.
Rule 36.22.202. Environmental Policy Act Procedural Rules.
Rule 36.22.301. Effective Scope of Rules.
Rule 36.22.302. Definitions.
Rule 36.22.303. Classification of Wildcat or Exploratory Wells.
Rule 36 22.304. Inspection of Record, Properties, and Wells.
Rule 36.22.305. Naming of Pools.
Rule 36.22.306. Organization of Reports.
Rule 36.22.307. Adoption of Forms.
Rule 36.22.308. Seal of Board.
Rule 36.22.309. Referral of Administrative Decisions.
Rule 36.22.401. Office and Duties of Petroleum Engineer.
Rule 36.22.402. Office and Duties of Administrator.
Rule 36.22.403. Office and Duties of Geologist.
Rule 36.22.501. Shot Location Limitations.
Rule 36.22.502. Plugging and Abandonment.
Rule 36.22.503. Notification.
Rule 36.22.504. Identification.
Rule 36.22.601. Notice of Intention and Permit to Drill.
Rule 36.22.602. Notice of Intention to Drill and Application for Permit 
to Drill.
Rule 36.22.603. Permit Fees.
Rule 36.22.604. Permit Issuance - Expiration - Extension.
Rule 36.22.605. Transfer of Permits.
Rule 36.22.606. Notice and Eligibility Statement for Drilling or 
Recompletion in Unit Operations.
Rule 36.22.607. Drilling Permits Pending Special Field Rules.
Rule 36.22.701. Spacing Units - General.
Rule 36.22.702. Spacing of Wells.
Rule 36.22.703. Horizontal Wells.
Rule 36.22.1001. Rotary Drilling Procedure.
Rule 36.22.1002. Cable Drilling Procedure.
Rule 36.22.1003. Vertical Drilling Required Deviation.
Rule 36.22.1004. Dual Completion of Wells.
Rule 36.22.1005. Drilling Waste Disposal and Surface Restoration.
Rules 36.22.1006 through 36.22.1010. Reserved.
Rule 36.22.1011. Well Completion and Recompletion Reports.
Rule 36.22.1012. Samples of Cores and Cuttings.
Rule 36.22.1013. Filing of Completion Reports, Well Logs, Analyses, 
Reports, and Surveys.
Rule 36.22.1014. Blowout Prevention and Well Control Equipment.
Rule 36.22.1101. Fire Hazard Prevention.
Rule 36.22.1102. Fire Walls Required.
Rule 36.22.1103. Notification and Report of Emergencies and Undesirable 
Incidents.
Rule 36.22.1104. Control and Cleanup.
Rule 36.22.1105. Solid Waste.
Rule 36.22.1201. Surface Equipment.
Rule 36.22.1202. Identification.
Rule 36.22.1203. Chokes Required.
Rule 36.22.1204. Separators Required.
Rule 36.22.1205. Vacuum Pumps Prohibited.
Rule 36.22.1206. Tubing Required.
Rule 36.22.1207. Earthen Pits and Open Vessels.
Rule 36.22.1208. Producing from Different Pools Through the Same Casing.
Rules 36.22.1209 through 36.22.1212. Reserved.
Rule 36.22.1213. Reservoir or Pool Surveys.
Rule 36.22.1214. Subsurface Pressure Tests.
Rule 36.22.1215. Stabilized Production Test.
Rule 36.22.1216. Gas Oil Ratio Tests.
Rule 36.22.1217. Water Production Report.
Rule 36.22.1218. Gas to be Metered.
Rule 36.22.1219. Gas Waste Prohibited.
Rule 36.22.1220. Associated Gas Flaring Limitation--Application to 
exceed--Board Review and Action.

[[Page 976]]

Rule 36.22.1221. Burning of Waste Gas Required.
Rule 36.22.1222. Hydrogen Sulfide Gas.
Rule 36.22.1223. Fencing, Screening, and Netting of Pits.
Rules 36.22.1224 and 36.22.1425. Reserved.
Rule 36.22.1226. Disposal of Water.
Rule 36.22.1227. Earthen Pits and Ponds.
Rule 36.22.1228. Disposal by Injection.
Rule 36.22.1229. Water Injection and Gas Repressuring.
Rule 36.22.1230. Application Contents and Requirements.
Rule 36.22.1231. Notice of Application Objections.
Rule 36.22.1232. Board Authorization.
Rule 36.22.1233. Notice of Commencement or Discontinuance--Plugging of 
Abandoned Wells.
Rule 36.22.1234. Record Required.
Rules 36.22.1235 through 36.22.1239. Reserved.
Rule 36.22.1240. Report of Well Status Change.
Rule 36.22.1241. Service Company Reports.
Rule 36.22.1242. Reports by Producers.
Rule 36.22.1243. Reports from Transporters, Refiners, and Gasoline or 
Extraction Plants.
Rule 36.22.1244. Producer's Certificate of Compliance.
Rule 36.22.1245. Illegal Production.
Rule 36.22.1301. Notice and Approval of Intention to Abandon Report.
Rule 36.22.1302. Notice of Abandonment.
Rule 36.22.1303. Well Plugging Requirement.
Rule 36.22.1304. Plugging Methods and Procedure.
Rule 36.22.1305. Exception for Fresh Water Wells.
Rule 36.22.1306. Approval for Pulling Casing and Reentering Wells.
Rule 36.22.1307. Restoration of Surface.
Rule 36.22.1308. Plugging and Restoration Bond.
Rule 36.22.1309. Subsequent Report of Abandonment.
Rule 36.22.1401. Definitions.
Rule 36.22.1402. Underground Injection.
Rule 36.22.1403. Application Contents and Requirements Rules.
Rule 36.22.1404 and 36.22.1405. Reserved.
Rule 36.22.1406. Corrective Action.
Rule 36.22.1407. Signing the Application.
Rule 36.22.1408. Financial Responsibility.
Rule 36.22.1409. Hearings.
Rule 36.22.1410. Notice of Application.
Rule 36.22.1411. Board Authorization.
Rules 36.22.1412 and 36.22.1413. Reserved.
Rule 36.22.1414. Notice of Commencement or Discontinuance--Plugging of 
Abandoned Wells.
Rule 36.22.1415. Records Required.
Rule 36.22.1416. Mechanical Integrity.
Rule 36.22.1417. Notification of Tests--Reporting Results.
Rule 36.22.1418. Exempt Aquifers.
Rule 36.22.1419. Tubingless Completions.
Rules 36.22.1420 and 36.22.1421. Reserved.
Rule 36.22.1422. Permit Conditions.
Rule 36.22.1423. Injection Fee--Well Classification.
Rule 36.22.1601. Who May Apply for Determination.
Rule 36.22.1602. Application Requirements and Contents.
Rule 36.22.1603. Documents and Technical Data Supporting Application.
Rule 36.22.1604. Docket Number.
Rule 36.22.1605. List of Applications--Public Access.
Rule 36.22.1606. Objections to Applications.
Rule 36.22.1607. Deadlines for Action Determinations.
Rule 36.22.1608. Deficient Applications.
Rule 36.22.1609. Board Action on Applications.
Rule 36.22.1610. Special Findings and Determinations New Onshore 
Production Wells Under Section 103.
Rule 36.22.1611. Special Findings and Determinations Stripper Well 
Production.

[61 FR 58934, Nov. 19, 1996]



                           Subpart CC_Nebraska



Sec.  147.1400  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Nebraska, except 
those on Indian lands, is the program administered by the Nebraska Oil 
and Gas Conservation Commission, approved by EPA pursuant to section 
1425 of the SDWA.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Nebraska. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Rules and Regulations of the Nebraska Oil and Gas Conservation 
Commission, Rules 1 through 6 (as published by the Commission, May 
1981);
    (2) Revised Statutes of Nebraska, sections 57-903 and 57-906 
(Reissue 1988).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for select sections identified in 
paragraph (a) of this section, are also part of the approved state-
administered program:

[[Page 977]]

    (1) Chapter 57, Oil and Gas Conservation, Revised Statutes of 
Nebraska sections 57-901 through 57-922 (Reissue 1985).
    (c) The Memorandum of Agreement between EPA Region VII and the 
Nebraska Oil and Gas Conservation Commission, signed by the EPA Regional 
Administrator on July 12, 1982.
    (d) Statement of legal authority. (1) ``Nebraska Underground 
Injection Control Program, Attorney General's Statement for Class II 
Wells,'' signed by Assistant Attorney General for Attorney General of 
Nebraska, as submitted with ``State of Nebraska Request for 
Administration of UIC Program,'' January 23, 1982;
    (2) ``Re: Nebraska Underground Injection Control Program, Addendum 
to Attorney General's Statement for Class II Wells,'' signed by 
Assistant Attorney General for Attorney General of Nebraska,'' undated.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 52 FR 17681, May 11, 1987; 56 
FR 9417, Mar. 6, 1991]



Sec.  147.1401  State administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Nebraska, except those on Indian lands, is the program administered by 
the Nebraska Department of Environmental Control, approved by EPA 
pursuant to section 1422 of the SDWA.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Nebraska. This incorporation by 
reference was approved by the Director of the Federal Register effective 
June 26, 1984.
    (1) Nebraska Environmental Protection Act, Revised Statutes of 
Nebraska sections 81-1502, 81-1506, 81-1519, and 81-1520 (Reissue 1987);
    (2) Nebraska Department of Environmental Control, Title 122--Rules 
and Regulations for Underground Injection and Mineral Production Wells, 
Effective Date: February 16, 1982, Amended Dates: November 12, 1983, 
March 22, 1984; as amended by amendment approved by the Governor on 
January 2, 1989.
    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Nebraska Environmental Protection Act, Nebraska Revised Statutes 
sections 81-1502, 81-1506, 81-1519, and 81-1520 (Reissue 1987 and Cumm. 
Supp. 1988);
    (c)(1) The Memorandum of Agreement between EPA Region VII and the 
Nebraska Department of Environmental Control, signed by the EPA Regional 
Administrator on July 12, 1982.
    (2) Addendum to Underground Injection Control Memorandum of 
Agreement signed by the EPA Regional Administrator on July 12, 1982.
    (3) Amendments to the Memorandum of Agreement signed by the EPA 
Regional Administrator on November 22, 1983.
    (d) Statement of legal authority. (1) ``Nebraska Underground 
Injection Control Program, Attorney General's Statement for Class I, 
III, IV, and V Wells'', signed by Assistant Attorney General for 
Attorney General of Nebraska, as submitted with ``State of Nebraska 
Request for Administration of UIC Program, January 28, 1982;
    (2) Letter from Attorney General (of Nebraska), by Assistant 
Attorney General, to Director, (Nebraska) Department of Environmental 
Control, August 7, 1981;
    (3) Letter from Attorney General (of Nebraska), by Assistant 
Attorney General, to Director, (Nebraska) Department of Environmental 
Control, April 29, 1982;
    (4) Letter from Attorney General (of Nebraska), by Assistant 
Attorney General, to Legal Counsel, (Nebraska) Department of 
Environmental Control, October 18, 1983.
    (e) The Program Description and any other materials submitted as 
part of

[[Page 978]]

the original application or as supplements thereto.

(42 U.S.C. 1422)

[49 FR 24134, June 12, 1984, as amended at 52 FR 17681, May 11, 1987; 56 
FR 9417, Mar. 6, 1991]



Sec.  147.1402  Aquifer exemptions. [Reserved]



Sec.  147.1403  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Nebraska is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
Lands in Nebraska is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9417, Mar. 6, 1991]



                            Subpart DD_Nevada



Sec.  147.1450  State-administered program.

    The UIC program for all classes of underground injection wells in 
the State of Nevada, other than those on Indian lands, is the program 
administered by the Nevada Division of Environmental Protection approved 
by EPA pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on February 18, 1988; the effective 
date of this program is October 5, 1988. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Nevada. This incorporation by reference 
was approved by the Director of the Federal Register in accordance with 
5 U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained at the Nevada 
Department of Conservation and Natural Resources, Division of 
Environmental Protection, 201 South Fall Street, Carson City, Nevada 
89710.
    Copies may be inspected at the Environmental Protection Agency, 
Region IX, 215 Fremont Street, San Francisco, California 99105, or at 
the National Archives and Records Administration (NARA). For information 
on the availability of this material at NARA, call 202-741-6030, or go 
to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (1) Nevada Revised Statutes [NRS], Volume 25, Chapters 445.131 
through 445.354, Inclusive. 1987.
    (2) Nevada Revised Statutes [NRS], Volume 29, Chapters 534A.010 
through 534A.090, Inclusive. 1987.
    (3) Nevada Revised Statutes [NRS], Volume 28, Chapters 522.010 
through 522.190, Inclusive. 1987.
    (4) Nevada Administrative Code [NAC], Underground Injection Control 
Regulations, Sections 1 through 96.1, Inclusive. July 22, 1987, revised 
September 3, 1987 (amending NAC Chapter 445).
    (5) Nevada Administrative Code [NAC], Regulations and Rules of 
Practice and Procedure adopted Pursuant to NRS 534A, Sections 1 through 
69, Inclusive. November 12, 1985 (amending NAC Chapter 534A).
    (6) Nevada Administrative Code [NAC], Regulations and Rules of 
Practice and Procedure adopted Pursuant to NRS 522.010 through 522.625, 
Inclusive. July 22, 1987 (amending NAC Chapter 522).
    (b) The Memorandum of Agreement between EPA Region 9 and the Nevada 
Department of Conservation and Natural Resources signed by the EPA 
Regional Administrator on April 6, 1988.
    (c) Statement of Legal Authority. Statement and Amendment to the 
Statement from the Attorney General of the State of Nevada, signed on 
July 22, 1987 and November 6, 1987 respectively, by the Deputy Attorney 
General.
    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[53 FR 39089, Oct. 5, 1988]

[[Page 979]]



Sec.  147.1451  EPA administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Nevada is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective dates. The effective date of the UIC program for 
Indian lands in Nevada is June 25, 1984.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9417, Mar. 6, 1991]



Sec.  147.1452  Aquifer exemptions. [Reserved]



Sec.  147.1453  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the wellhead in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.



Sec.  147.1454  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and (B). The Regional 
Administrator may grant such a request after notice, opportunity for 
comment, and opportunity for public hearing, according to the provisions 
of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
field rules for maximum injection pressure based on data provided 
pursuant to paragraph (a)(2)(ii) of this section the owner or operator 
shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within one year following the effective date 
of this program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and

[[Page 980]]

    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) of this section, as needed to protect USDWs.



                        Subpart EE_New Hampshire



Sec.  147.1500  State-administered program.

    The UIC program for all classes of wells in the State of New 
Hampshire, except those wells on Indian lands, is the program 
administered by the New Hampshire Department of Environmental Services, 
approved by the EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the FR on September 21, 1982 (47 FR 41561); 
the effective date of this program is October 21, 1982. This program 
consists of the following elements:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of New Hampshire. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) New Hampshire Revised Statutes Annotated section 149:8 III(a) 
(1978);
    (2) New Hampshire Code of Administrative Rules, Part Wc 410 
(Protection of Groundwaters of the State, sections Ws 410.1 through Ws 
410.16) (Issue Ws 3-82).
    (b)(1) The Memorandum of Agreement between EPA Region I and the New 
Hampshire Water Supply and Pollution Control Commission, signed by the 
EPA Regional Administrator on August 23, 1982;
    (2) Amendment No. 1 to the Memorandum of Agreement, signed by the 
EPA Regional Administrator on July 16, 1982.
    (c) Statement of legal authority. (1) Letter from Attorney General 
of New Hampshire to Regional Administrator, EPA Region I, ``Re: Attorney 
General's Statement--Underground Injection Control Program,'' March 23, 
1982;
    (2) Letter from Attorney General of New Hampshire to Regional 
Administrator, EPA Region I, ``Re: Attorney General's Statement--
Underground Injection Control Program,'' July 1, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43088, Oct. 25, 1988; 56 
FR 9417, Mar. 6, 1991]



Sec.  147.1501  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of New Hampshire is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in New Hampshire is November 25, 1988.

[53 FR 43088, Oct. 25, 1988, as amended at 56 FR 9417, Mar. 6, 1991]



                          Subpart FF_New Jersey



Sec.  147.1550  State-administered program.

    The UIC program for all classes of wells in the State of New Jersey, 
except those on Indian lands, is the program administered by the New 
Jersey Department of Environmental Protection, approved by EPA pursuant 
to section 1422 of the SDWA. Notice of this approval was published in 
the Federal Register on July 15, 1983 (48 FR 32343); the effective date 
of this program is August 15, 1983. This program consists

[[Page 981]]

of the following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of New Jersey. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Water Pollution Control Act, New Jersey Statutes Annotated 
sections 58:10A-1 through 58:10A-20 (West 1982 and Supp. 1990);
    (2) New Jersey Administrative Code, sections 7:14A-1.1 through 1.9 
(subchapter 1), 7:14A-2.1 through 2.15 (subchapter 2), 7:14A-5.1 through 
5.17, (subchapter 5) (amended March 1988).
    (b)(1) The Memorandum Agreement between EPA Region II and the New 
Jersey Department of Environmental Protection, signed by the EPA 
Regional Administrator on September 9, 1982;
    (2) Letter from Commissioner, New Jersey Department of Environmental 
Protection, to Regional Administrator, EPA Region II, March 21, 1983.
    (c) Statement of legal authority. (1) Letter from Attorney General 
of New Jersey (by Deputy Attorney General) to Commissioner, Department 
of Environmental Protection, ``Re: New Jersey Pollutant Discharge 
Elimination System--Underground Injection Control,'' February 9, 1982;
    (2) Letter from Attorney General of New Jersey (by Deputy Attorney 
General) to Commissioner, Department of Environmental Protection, ``Re: 
New Jersey Pollutant Discharge Elimination System--Underground Injection 
Control,'' April 15, 1983 (six pages);
    (3) Letter from Attorney General of New Jersey (by Assistant 
Attorney General) to Commissioner, Department of Environmental 
Protection, ``Re: New Jersey Pollutant Discharge Elimination System--
Underground Injection Control,'' April 15, 1983 (two pages).
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43089, Oct. 25, 1988; 56 
FR 9417, Mar. 6, 1991]



Sec.  147.1551  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of New Jersey is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in New Jersey is November 25, 1988.

[53 FR 43089, Oct. 25, 1988, as amended at 56 FR 9417, Mar. 6, 1991]



                          Subpart GG_New Mexico



Sec.  147.1600  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of New Mexico, 
except for those on Indian lands, is the program administered by the New 
Mexico Energy and Minerals Department, Oil Conservation Division, 
approved by EPA pursuant to section 1425 of the SDWA. Notice of this 
approval was published in the Federal Register on February 5, 1982 (47 
FR 5412); the effective date of this program is March 7, 1982. This 
program consists of the following elements as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of New Mexico. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Oil and Gas Act, New Mexico Statutes Annotated sections 70-2-1 
through -36 (1978);
    (2) State of New Mexico Energy and Mineral Department, Oil 
Conservation Division--Rules and Regulations (dated 10-

[[Page 982]]

1-78), sections B-3, I-701 through I-708, M-1100 through M-1121.
    (b)(1) The Memorandum of Agreement between EPA Region VI and the New 
Mexico Energy and Minerals Department, Oil Conservation Division, signed 
by the EPA Regional Administrator on December 10, 1981;
    (2) Addendum No. 1 to the Memorandum of Agreement, signed by the EPA 
Regional Administrator on June 28, 1982;
    (3) Addendum No. 2 to the Memorandum of Agreement, signed by the EPA 
Regional Administrator on November 18, 1982;
    (4) Letter from Director, Oil Conservation Division, New Mexico 
Energy and Minerals Department, and Assistant Attorney General of New 
Mexico, to Regional Administrator, EPA Region VI, November 6, 1981.
    (c) Statement of legal authority. ``Statement of Legal Authority of 
the State of New Mexico by and through its Oil Conservation Division of 
the Energy and Mines Department to conduct an Underground Injection 
Control Program,'' signed by Assistant Attorney General and General 
Counsel to the Oil Conservation Division.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43089, Oct. 25, 1988]



Sec.  147.1601  State-administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV and V injection wells in the 
State of New Mexico, except for those on Indian lands, is the program 
administered by the New Mexico Water Quality Control Commission, the 
Environmental Improvement Division, and the Oil Conservation Division, 
approved by EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the Federal Register on July 11, 1983 (48 FR 
31640); the effective date of this program is August 10, 1983. This 
program consists of the following elements, as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of New Mexico. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) New Mexico Water Quality Control Commission Regulations (WQCC 
82-1) sections 1-100 through 5-300 (September 20, 1982).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, are also part of the approved State-
administered UIC program:
    (1) Water Quality Act, New Mexico Statutes Annotated sections 74-6-1 
through 74-6-13 (1978 and Supp. 1982);
    (2) Geothermal Resources Conservation Act, New Mexico Statutes 
Annotated sections 71-5-1 through 71-5-24 (1978 and Supp. 1982);
    (3) Surface Mining Act, New Mexico Statutes Annotated sections 69-
25A-1 through 69-25A-35 (1978 and Supp. 1980).
    (c)(1) The Memorandum of Agreement between EPA Region VI and the New 
Mexico Water Quality Control Commission, the Environmental Improvement 
Division, and the Oil Conservation Division, signed by the EPA Regional 
Administrator on April 13, 1983;
    (2) Letter from the Director, Environmental Improvement Division and 
the Director, Oil Conservation Division, to Regional Administrator, EPA 
Region IV, ``Re: New Mexico Underground Injection Control Program--
Clarification,'' February 10, 1983.
    (d) Statement of legal authority. ``Attorney General's Statement,'' 
signed by the Assistant Attorney General for the Environmental 
Improvement Division, the Assistant Attorney General for Oil 
Conservation Division, and the Deputy Attorney General, Civil Division, 
Counsel for the Mining and Minerals Division, undated, submitted 
December 8, 1982.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43089, Oct. 25, 1988]

[[Page 983]]



Sec.  147.1603  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in New Mexico, except for Class II wells on Navajo Indian lands 
for which EPA has granted the Navajo Nation primacy for the SDWA Class 
II UIC program (as defined in Sec.  147.3400), is administered by EPA. 
The program consists of the requirements set forth at Subpart HHH of 
this part. Injection well owners and operators and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date for the UIC program on Indian 
lands in New Mexico, except for Class II wells on Navajo Indian lands 
for which EPA has granted the Navajo Nation primacy for the SDWA Class 
II UIC program (as defined in Sec.  147.3400), is November 25, 1988.

[53 FR 43089, Oct. 25, 1988, as amended at 73 FR 65565, Nov. 4, 2008]



                           Subpart HH_New York



Sec.  147.1650  State-administered program. [Reserved]



Sec.  147.1651  EPA-administered program.

    (a) Contents. The UIC program for the State of New York, including 
all Indian lands, is administered by EPA. The program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date of the UIC program for New 
York for all injection activities except those on lands of the Seneca 
Indian Tribe is June 25, 1984. The effective date for the UIC program 
for the lands of the Seneca Indian Tribe is November 25, 1988.

[53 FR 43089, Oct. 25, 1988; 54 FR 10616, Mar. 14, 1989, as amended at 
56 FR 9417, Mar. 6, 1991]



Sec.  147.1652  Aquifer exemptions.

    (a) This section identifies any aquifer or their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter at the 
time of program promulgation. EPA may in the future exempt other 
aquifers or portions, according to applicable procedures, without 
codifying such exemptions in this section. An updated list of exemptions 
will be maintained in the Regional office.
    (b) The following portions of aquifers are exempted in accordance 
with the provisions of Sec. Sec.  144.7(b) and 146.4 of this chapter for 
Class II injection activities only:
    (1) The Bradford First, Second, and Third Sand Members and the Kane 
Sand Member in the Bradford Field in Cattaraugus County.
    (2) The Chipmunk Oil field in Cattaraugus County.



Sec.  147.1653  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable; or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.



Sec.  147.1654  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure, or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or

[[Page 984]]

formation in which he is operating provided he submits a request in 
writing to the Regional Administrator, and demonstrates to the 
satisfaction of the Regional Administrator that such injection pressure 
will not violate the requirement of Sec.  144.28(f)(3)(ii) (A) and (B). 
The Regional Administrator may grant such a request after notice, 
opportunity for comment, and opportunity for a public hearing, according 
to the provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressure based on data provided pursuant to 
paragraph (a)(2)(ii) of this section the owner or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within one year of the effective date of this 
program.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (iii) For wells as described in Sec.  146.8(b)(3)(ii), installing a 
smaller diameter pipe inside the existing injection tubing and setting 
it on an appropriate packer; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 50 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) of this section as needed to protect USDWs.



Sec.  147.1655  Requirements for wells authorized by permit.

    (a) The owner or operator of a Class I well authorized by permit 
shall install or shall ensure that the well has:
    (1) Surface casing present;
    (i) Extending from the surface to a depth at least 50 feet below the 
base of the lowermost USDW; and
    (ii) Cemented back to the surface by recirculating the cement; and
    (2) Long string casing and tubing;
    (i) Extending to the injection zone; and
    (ii) Cemented back to 50 feet above the base of the next largest 
casing string.
    (b) The owner or operator of a new Class II well authorized by 
permit shall:
    (1) Install surface casing from the surface to at least 50 feet 
below the base of the lowermost USDW.
    (2) Cement the casing by recirculating to the surface or by using no 
less than 120% of the calculated annular volume.
    (3) For new enhanced recovery wells, install tubing or long string 
casing extending to the injection zone.
    (4) For new salt water disposal wells, install long string casing 
and tubing extending to the injection zone.
    (5) Isolate any injection zone by placing sufficient cement to fill 
the calculated volume to a point 50 feet above the injection zone.

[[Page 985]]

    (c) The Regional Administrator may specify casing and cementing 
requirements other than those listed in paragraphs (a) and (b) of this 
section on a case by case basis as conditions of the permit.



                        Subpart II_North Carolina



Sec.  147.1700  State-administered program.

    The UIC program for all classes of wells in the State of North 
Carolina, except those wells on Indian lands, is the program 
administered by the North Carolina Department of Environment, Health and 
Natural Resources approved by EPA pursuant to section 1422 of the SDWA. 
Notice of this approval was published in the Federal Register on April 
19, 1984 (49 FR 15553); the effective date of this program is April 19, 
1984. This program consists of the following elements, as submitted to 
EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of North Carolina. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained at the North 
Carolina Department of Environment, Health and Natural Resources, P.O. 
Box 27687, Raleigh, North Carolina 27611. Copies may be inspected at the 
Environmental Protection Agency, Region IV, 345 Courtland Street, NE., 
Atlanta, Georgia 30365, or at the National Archives and Records 
Administration (NARA). For information on the availability of this 
material at NARA, call 202-741-6030, or go to: http://www.archives.gov/
federal_register/code_of_federal_regulations/ibr_locations.html.
    (1) Administrative Procedure Act, N.C. GEN. STAT. 150B-1 through 
150B-64 (1987 and Cumm. Supp. 1989);
    (2) North Carolina Well Construction Act, N.C. GEN. STAT. Sec. Sec.  
87-83 through 87-99 (1989 and Cumm. Supp. 1989);
    (3) Water and Air Resources, N.C. GEN. STAT. Sec. Sec.  143-211 
through 143-215.10 (1987 and Cumm. Supp. 1989);
    (4) Solid Waste Management, N.C. GEN. STAT. Sec. Sec.  130A-290 
through 130A-309.03 (1989);
    (5) North Carolina Drinking Water Act, N.C. GEN. STAT. Sec. Sec.  
130A-311 through 130A-332 (1989);
    (6) Sanitary Sewage Systems, N.C. GEN. STAT. Sec. Sec.  130A-333 
through 130A-335 (1989).
    (b) Other laws. The following rules and regulations, although not 
incorporated by reference, are also part of the approved State-
administered program:
    (1) N.C. ADMIN. CODE, Title 15, r. 02L.0100 et seq. Groundwater 
Classification and Standards: General Considerations (September 22, 
1988);
    (2) N.C. ADMIN. CODE, Title 15, r. 02L.0100 et seq. Criteria and 
Standards Applicable to Injection Wells (September 22, 1988).
    (c) Memorandum of Agreement. The Memorandum of Agreement between the 
State of North Carolina and EPA Region IV, signed March 1, 1984.
    (d) Statement of legal authority. (1) Underground Injection Control 
Program, Attorney General's Statement (June 15, 1982);
    (2) Amendment to Underground Injection Control Program, Attorney 
General's Statement (February 9, 1984).
    (e) Program Description. The Program Description and other materials 
submitted as part of the application or as supplements thereto.

[56 FR 9417, Mar. 6, 1991]



Sec. Sec.  147.1701-147.1702  [Reserved]



Sec.  147.1703  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of North Carolina is administered by EPA. This 
program consists of the UIC program requirements of 40 CFR parts 124, 
144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in North Carolina is November 25, 1988.

[53 FR 43089, Oct. 25, 1988, as amended at 56 FR 9418, Mar. 6, 1991]

[[Page 986]]



Sec. Sec.  147.1704-147.1749  [Reserved]



                         Subpart JJ_North Dakota



Sec.  147.1750  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of North Dakota, 
except those on Indian lands, is the program administered by the North 
Dakota Industrial Commission, approved by EPA pursuant to section 1425 
of the SDWA. Notice of this approval was published in the Federal 
Register on August 23, 1983 (48 FR 38237); the effective date of this 
program is September 24, 1983. This program consists of the following 
elements, as submitted to EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of North Dakota. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) North Dakota Century Code, Chapter 38-08 (Control of Gas and Oil 
Resources, 1987 and Supp. 1989);
    (2) North Dakota Administrative Code, Chapter 43-02-05 (Underground 
Injection Control, as published in Statutes and Rules for the 
Conservation of Oil and Gas, North Dakota Industrial Commission, revised 
effective November 1, 1987);
    (3) North Dakota Administrative Code, Chapter 43-02-03 (General 
Rules, as published in Statutes and Rules for the Conservation of Oil 
and Gas, North Dakota Industrial Commission, revised effective November 
1, 1987).
    (b) The Memorandum of Agreement between EPA Region VIII and the 
North Dakota Industrial Commission, Oil and Gas Division, signed by the 
EPA Regional Administrator on June 16, 1983, as amended September 7, 
1989.
    (c) Statement of legal authority. ``Underground Injection Control 
Program Attorney General's Statement,'' as submitted with the North 
Dakota Underground Injection Control Program Primacy Application for 
Class II Injection Wells, transmitted by the Governor on July 15, 1982 
(16 pages).
    (d) The Program Description and other materials submitted as part of 
the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43089, Oct. 25, 1988; 56 
FR 9418, Mar. 6, 1991]



Sec.  147.1751  State-administered program--Class I, III, IV, V and VI wells.

    The UIC program for Class I, III, IV and V wells in the state of 
North Dakota, except those located on Indian lands, is the program 
administered by the North Dakota Department of Health, approved by the 
EPA pursuant to SDWA section 1422. Notification of this approval was 
published in the Federal Register on September 21, 1984; the effective 
date of this program is October 5, 1984. The UIC Program for Class VI 
wells in the state of North Dakota, except those located on Indian 
lands, is the program administered by the North Dakota Industrial 
Commission, approved by the EPA pursuant to SDWA section 1422. 
Notification of this approval was published in the Federal Register on 
April 24, 2018; the effective date of this program is April 24, 2018. 
This program consists of the following elements, as submitted to the EPA 
in the state's program revision application.
    (a) The requirements set forth in the state statutes and regulations 
cited in the binder entitled ``EPA-Approved North Dakota SDWA Sec.  1422 
Underground Injection Control Program Statutes and Regulations for Well 
Classes I, III, IV, V and VI,'' dated December 2013, and listed in Table 
1 to paragraph (a) of this section, are incorporated by reference and 
made a part of the applicable UIC program under SDWA for the state of 
North Dakota. The Director of the Federal Register approves this 
incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR 
part 51. Copies of the North Dakota regulations that are incorporated by 
reference in paragraph (a) of this section may be inspected at the U.S. 
Environmental Protection Agency, Region 8, Library 2nd Floor, 1595 
Wynkoop Street, Denver, Colorado 80202; Water Docket, EPA Docket Center 
(EPA/DC) EPA West, Room 3334,

[[Page 987]]

1301 Constitution Ave. NW, Washington, DC 20460; and the National 
Archives and Records Administration (NARA). If you wish to obtain 
materials from the EPA Regional Office, please call (303) 312-1226; for 
materials from a docket in the EPA Headquarters Library, please call the 
Water Docket at (202) 566-2426. For information on the availability of 
this material at NARA, call (202) 741-6030, or go to http://
www.archives.gov/federal-register/cfr/ibr-locations.html.

    Table 1 to Paragraph (a) EPA-Approved North Dakota SDWA Sec.   1422 Underground Injection Control Program
                         Statutes and Regulations for Well Classes I, III, IV, V and VI
----------------------------------------------------------------------------------------------------------------
                                                                           State
             State citation                      Title/subject           effective       EPA approval date \1\
                                                                           date
----------------------------------------------------------------------------------------------------------------
North Dakota Century Code Sections 38-12- Regulation, Development               1980  September 21, 1984, 49 FR
 01--38-12-03.                             and Production of                           37066.
                                           Subsurface Minerals.
North Dakota Century Code Sections 61-28- Control, Prevention and               1989  March 6, 1991, 56 FR 9418.
 02 and 61-28-06.                          Abatement of Pollution of
                                           Surface Waters.
North Dakota Administrative Code          Underground Injection                 1983  September 21, 1984, 49 FR
 Sections 33-25-01-01--33-25-01-18.        Control Program.                            37066.
North Dakota Administrative Code          Subsurface Mineral                    1986  March 6, 1991, 56 FR 9418.
 Sections 43-02-02-01-43-02-02-50.         Exploration and
                                           Development.
North Dakota Administrative Code          Underground Injection                 1984  September 21, 1984, 49 FR
 Sections 43-02-02.1-01--43-02-02.2-19.    Control Program.                            37066.
North Dakota Century Code Sections 38-22- Carbon Dioxide Underground            2009  April 24, 2018, 83 FR
 01--38-22-23.                             Storage.                                    17761.
North Dakota Administrative Code          Control of Oil and Gas                2013  April 24, 2018, 83 FR
 Sections 38-08-16--38-08-17.              Resources.                                  17761.
North Dakota Administrative Code          Geologic Storage of Carbon            2013  April 24, 2018, 83 FR
 Sections 43-05-01-01--43-05-01-20.        Dioxide.                                    17761.
----------------------------------------------------------------------------------------------------------------
\1\ In order to determine the EPA effective date for a specific provision listed in this table, consult the
  Federal Register notice cited in this column for the particular provision.

    (b) The following statutes and regulations, although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) North Dakota Environmental Law Enforcement Act of 1975, North 
Dakota Century Code Sections 32-40-01 to 32-40-11 (1976);
    (2) North Dakota Century Code, Ch. 38-12 (Regulation, Development, 
and Production of Subsurface Minerals) (1979);
    (3) North Dakota Century Code Chapter 61-28 (Control, Prevention and 
Abatement of Pollution of Surface Waters) (1989);
    (4) North Dakota Administrative Code Article 33-22 (Practice and 
Procedure) (1983).
    (c) The Memorandum of Agreement between EPA Region VIII and the 
North Dakota Department of Health, signed by the EPA Regional 
Administrator on May 18, 1984.
    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.
    (e) The Memorandum of Agreement between EPA Region VIII and the 
North Dakota Industrial Commission, signed by the EPA Regional 
Administrator on October 28, 2013.
    (f) The Memorandum of Understanding between the North Dakota 
Industrial Commission, Department of Mineral Resources, Oil and Gas 
Division and the North Dakota Department of Health, Water Quality 
Division, Related to the Underground Injection Control Program signed on 
June 19, 2013.
    (g) The statement of legal authority, ``Class VI Underground 
Injection Control Program, Attorney General's Statement,'' signed by the 
Attorney General of North Dakota on January 22, 2013.
    (h) The Class VI Program Description and any other materials 
submitted as

[[Page 988]]

part of the program revision or as supplements thereto.

[49 FR 37066, Sept. 21, 1984, as amended at 56 FR 9418, Mar. 6, 1991; 83 
FR 17761, Apr. 24, 2018]



Sec.  147.1752  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of North Dakota is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in North Dakota is November 25, 1988.

[53 FR 43089, Oct. 25, 1988, as amended at 56 FR 9418, Mar. 6, 1991]



                             Subpart KK_Ohio



Sec.  147.1800  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Ohio, except for 
those on Indian lands, is the program administered by the Ohio 
Department of Natural Resources, approved by EPA pursuant to section 
1425 of the SDWA. Notice of this approval was published in the Federal 
Register on August 23, 1983 (48 FR 38238); the effective date of this 
program is September 22, 1983. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Ohio. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Ohio Revised Code Annotated, sections 1509.01 through 1509.22 
(Page 1978 and Supp. 1982);
    (2) Rules of the Division of Oil and Gas, Ohio Administrative Code 
sections 1501:91-01, through 1501: 9-11-13 (1983).
    (b) The Memorandum of Agreement between EPA Region V and the Ohio 
Department of Natural Resources.
    (c) Statement of legal authority. ``Underground Injection Control 
Program--Attorney General's Statement,'' signed by the Assistant 
Attorney General, Chief, Environmental Law Section, for the Attorney 
General of Ohio, September 30, 1982.
    (d) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43089, Oct. 25, 1988]



Sec.  147.1801  State-administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Ohio, other than those on Indian lands, is the program administered by 
the Ohio Department of Natural Resources and the Ohio Environmental 
Protection Agency, approved by EPA pursuant to section 1422 of the SDWA. 
Notice of this approval was published in the Federal Register on 
November 29, 1984; the effective date of this program is January 14, 
1985. This program consists of the following elements, as submitted to 
EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Ohio. This incorporation by reference 
was approved by the Director of the Federal Register effective January 
14, 1985.
    (1) Ohio Revised Code Annotated, sections 1509.01, 1509.03, 1509.221 
(Supp. 1983);
    (2) Rules of the Division of Oil and Gas, Ohio Administrative Code, 
sections 1501:9-7-01 through 7-14 (1984);
    (3) Ohio Revised Code Annotated, sections 6111.04, 6111.043, 
6111.044 (Supp. 1983);
    (4) Rules of the Ohio Environmental Protection Agency, Ohio 
Administrative Code, sections 3745-34-01 through 34-41; 3745-9-01 
through 9-11 (Director Ohio EPA Order, June 18, 1984).

[[Page 989]]

    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Ohio Revised Code, Chapter 119 (1978 Replacement Part);
    (2) Ohio Code Supplement, sections 6111.041, 6111.042, 6111.045 
(Supp. 1982).
    (c) (1) The Memorandum of Agreement between EPA Region V and the 
Ohio Department of Natural Resources, signed by the EPA Regional 
Administrator on March 30, 1984;
    (2) Memorandum of Agreement between the Ohio Department of Natural 
Resources and the Ohio Environmental Protection Agency, Related to the 
Underground Injection Control Program for the State of Ohio, signed 
August 1, 1984.
    (d) Statement of legal authority. Statement from Attorney General of 
the State of Ohio, by Senior Assistant Attorney General, ``Underground 
Injection Control Program--Attorney General's Statement,'' July 25, 
1984.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 46897, Nov. 29, 1984]



Sec.  147.1802  Aquifer exemptions. [Reserved]



Sec.  147.1803  Existing Class I and III wells authorized 
by rule--maximum injection pressure.

    The owner or operator shall limit injection pressure to the lesser 
of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3)(i); or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.8 - 0.433 Sg) d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.

[49 FR 45308, Nov. 15, 1984]



Sec.  147.1805  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Ohio is administered by EPA. This program consists 
of the UIC program requirements of 40 CFR parts 124, 144, 146, 148, and 
any additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Ohio is November 25, 1988.

[53 FR 43089, Oct. 25, 1988, as amended at 56 FR 9418, Mar. 6, 1991]



                           Subpart LL_Oklahoma



Sec.  147.1850  State-administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Oklahoma, except those on Indian lands, is the program administered by 
the Oklahoma State Department of Health, approved by EPA pursuant to 
SDWA section 1422. Notice of this approval was published in the Federal 
Register on June 24, 1982 (47 FR 27273). The effective date of this 
program is July 24, 1982. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Oklahoma. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Oklahoma Statutes title 63 sections 1-901, 1-903 (1981);
    (2) Oklahoma Controlled Industrial Waste Disposal Act, Oklahoma 
Statute Annotated title 63 sections 1-2002, 1-2014 (West Supp. 1983-
1984);
    (3) Regulations. [Reserved]
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for select sections identified in 
paragraph (a) of

[[Page 990]]

this section, are also part of the approved State-administered UIC 
program:
    (1) Oklahoma Open Meeting Act, Oklahoma Statutes title 25 sections 
301 through 314 (Supp. 1978);
    (2) Oklahoma Statutes Annotated title 63 sections 1-101 to 1-114, 1-
901 to 1-911, 1-1601 et seq., 1-1701, 1-2001 to 1-2014 (West 1973 and 
Supp. 1982);
    (3) Oklahoma Statutes Annotated title 75 sections 301 to 327 (West 
1976 and Supp. 1982).
    (c) (1) The Memorandum of Agreement between EPA Region VI and the 
Oklahoma State Department of Health, signed by the EPA Regional 
Administrator on April 13, 1982;
    (2) Memorandum of Understanding between the Oklahoma State 
Department of Health and the Oklahoma Corporation Commission (OCC), 
signed by members of the OCC on February 12, 1982;
    (3) Memorandum of Understanding between the Oklahoma State 
Department of Health and the Oklahoma Department of Mines (ODM), signed 
by the Deputy Chief Mine Inspector, ODM, on February 15, 1982.
    (d) Statement of legal authority. Letter from Attorney General of 
Oklahoma to Commissioner of Health, Oklahoma State Department of Health, 
``Re: Statement and Memorandum of Law Concerning the Authority for the 
Oklahoma State Department of Health's Underground Injection Control 
Program,'' February 12, 1982.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43090, Oct. 25, 1988]



Sec.  147.1851  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Oklahoma, 
including the lands of the Five Civilized Tribes, but not including 
those on other Indian lands, is the program administered by the Oklahoma 
Corporation Commission approved by EPA pursuant to SDWA section 1425. 
Notice of this approval was published in the Federal Register on 
December 2, 1981 (46 FR 58588). This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. [Reserved]
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, are also part of the approved State-
administered UIC program:
    (1) Oklahoma Statutes, title 17 sections 51-53; title 52 sections 
86.1-86.5, 139-153, 243, 307-318.1 (1971).
    (2) OCC-OGR Rules No. 1-101-3-303.
    (c) (1) The Memorandum of Agreement between EPA Region VI and the 
Oklahoma Corporation Commission, signed by the EPA Regional 
Administrator on April 13, 1981;
    (2) Letter from the Manager, Underground Injection Control, Oklahoma 
Corporation Commission, to EPA, June 18, 1981.
    (d) Statement of legal authority. ``Statement of Legal Authority of 
the Oklahoma Corporation Commission to Conduct an Underground Injection 
Control Program,'' (Part IV, pages 30-41 of ``State of Oklahoma Primacy 
Application for Authority to Regulate Class II Injection Wells,'' 
submitted April 14, 1981), signed by the Conservation Attorney, Counsel 
to the Director and the Oklahoma Corporation Commission.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43090, Oct. 25, 1988]



Sec.  147.1852  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all wells on Indian lands in 
Oklahoma, except Class II wells on the lands of the Five Civilized 
Tribes, is administered by EPA. The UIC program for Class II wells on 
the Osage Mineral Reserve consists of the requirements set forth in 
subpart GGG of this part. The UIC program for all other wells on Indian 
lands consists of the requirements set forth in subpart III of this 
part. Injection well owners and operators and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date for UIC program for Class II 
wells on

[[Page 991]]

the Osage Mineral Reserve is December 30, 1984. The effective date for 
the UIC program for all other wells on Indian lands is November 25, 
1988.

[53 FR 43090, Oct. 25, 1988]



                            Subpart MM_Oregon



Sec.  147.1900  State-administered program.

    The UIC program for all classes of wells in the State of Oregon, 
except those on Indian lands, is administered by the Oregon Department 
of Environmental Quality, approved by EPA pursuant to section 1422 and 
section 1425 of the SDWA. Notice of this approval was published in the 
Federal Register on September 25, 1984; the effective date of this 
program is October 9, 1984. This program consists of the following 
elements, as submitted to EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Oregon. This incorporation by reference 
was approved by the Director of the Federal Register effective October 
9, 1984.
    (1) Oregon Revised Statutes, Title 16, chapter 164, section 164.785; 
Title 36, chapter 468, sections 468.005, 468.065 to 468.070, 468.700 to 
468.815; Title 43, chapter 520 sections 520.005, 520.095, 520.155-
520.330 (1983);
    (2) Oregon Administrative Rules, Chapter 340, Division 44, sections 
340-44-005 through 340-44-055 (October 1983); Chapter 340, Division 45, 
sections 340-45-005 through 340-45-075 (January 1990); Chapter 632, 
Division 10, sections 632-10-002 through 632-10-235 (May 1986); Chapter 
632, Division 20, sections 632-20-005 through 632-20-180 (May 1984).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Oregon Revised Statutes, Chapter 183 (1987); 192.420, 192.500, 
459.460(3), 468.005 through 468.605, and 468.780 through 468.997; 
Chapters 516 and 522 (1983);
    (2) Oregon Administrative Rules, chapter 137, Div. 3 (July 1982); 
chapter 340, Div. 11 (April 1988); chapter 340, Div. 12 (March 1989); 
chapter 340, Div. 14 (November 1983); chapter 340, Div. 52 (November 
1983); chapter 632, Div. 1 (June 1980); chapter 632, Div. 20 (January 
1981).
    (c)(1) The Memorandum of Agreement between EPA Region X and the 
Oregon Department of Environmental Quality, signed by the EPA Regional 
Administrator on May 3, 1984.
    (d) Statement of legal authority. (1) ``Underground Injection 
Control Program Legal Counsel's Statement,'' October 1983, signed by the 
Assistant Attorney General, Oregon;
    (2) Opinion of the Attorney General, Oregon, 35 Op. Attorney General 
1042 (1972).
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 37594, Sept. 25, 1984, as amended at 53 FR 43090, Oct. 25, 1988; 
56 FR 9418, Mar. 6, 1991]



Sec.  147.1901  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Oregon is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Oregon is November 25, 1988.

[53 FR 43090, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991]



                         Subpart NN_Pennsylvania



Sec.  147.1950  State-administered program. [Reserved]



Sec.  147.1951  EPA-administered program.

    (a) Contents. The UIC program for the State of Pennsylvania, 
including all Indian lands, is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124,

[[Page 992]]

144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program on 
Indian lands is November 25, 1988. The effective date for the UIC 
program for the rest of Pennsylvania is June 25, 1984.

[53 FR 43090, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991]



Sec.  147.1952  Aquifer exemptions.

    (a) This section identifies any aquifers or their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter at the 
time of program promulgation. EPA may in the future exempt other 
aquifers or portions, according to applicable procedures, without 
codifying such exemptions in this section. An updated list of exemptions 
will be maintained in the Regional office.
    (b) Those portions of the following oil bearing aquifers, which 
would otherwise meet the definition of a USDW, are exempted in 
accordance with the provisions of Sec. Sec.  144.7(b) and 146.4 of this 
chapter for Class II enhanced recovery injection activities only.
    (1) The Sugar Run and Bradford series of oil producing sands of the 
Bradford Field, in McKean County; including the Bradford, West Branch, 
Stack, Bennett Brook, Marilla Brook, Brooder Hollow, Cyclone, Minard 
Run, Minard Run School, and Sugar Run (or Watsonville) Pools.
    (2) The Bradford Third oil producing sand of the Guffey Field in 
McKean County.
    (3) The Bradford series of oil producing sands of the Lewis Run 
Field in McKean County.
    (4) The Bradford series of oil producing sands of the Windfall Field 
and Kings Run Pool in McKean County.
    (5) The Red Valley member of the Second Sand formation of the 
Venango Group of oil producing sands in the Foster-Reno Field in Venango 
County; including the Foster, Bully Hill, Victory, Bredinsburg, Egypt 
Corners, Reno, Monarch Park and Seneca Pools.
    (6) The Glade and Clarendon oil producing sands of the Morrison Run 
Field and Elk Run Pool in Warren County.
    (7) The Clarendon and Glade oil producing sands of the Clarendon 
Field in Warren County.
    (8) The Bradford Third oil producing sand in the Shinglehouse Field, 
including the Kings Run, Janders Run and Ceres Pools in Potter and 
McKean Counties.



Sec.  147.1953  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.733 - 0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of injection fluid (unitless)
d = injection depth in feet.



Sec.  147.1954  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at pressures greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and demonstrates to the satisfaction of the Regional 
Administrator that such injection pressure will not violate the 
requirement of Sec.  144.28(f)(3)(ii) (A) and

[[Page 993]]

(B). The Regional Administrator may grant such a request after notice, 
opportunity for comment, and opportunity for a public hearing, according 
to the provisions of part 124, subpart A of this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressure based on data provided pursuant to 
paragraph (a)(2)(ii) of this section the owner or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The information shall be 
submitted to the Regional Administrator within one year of the effective 
date of this regulation.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirements of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall comply with paragraphs (b) (1) through (4) of this section, when 
required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (iii) For wells as described in Sec.  146.8(b)(3)(ii), installing a 
smaller diameter pipe inside the existing injection tubing and setting 
it on an appropriate packer; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 50 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.
    (4) The Regional Administrator may specify other requirements in 
addition to or in lieu of the requirements set forth in paragraphs (b) 
(1) through (3) of this section as needed to protect USDWs.



Sec.  147.1955  Requirements for wells authorized by permit.

    (a) The owner or operator of a Class I well authorized by permit 
shall install or shall ensure that the well has:
    (1) Surface casing present;
    (i) Extending from the surface to a depth at least 50 feet below the 
base of the lowermost USDW; and
    (ii) Cemented back to the surface by recirculating the cement; and
    (2) Long string casing and tubing;
    (i) Extending to the injection zone; and
    (ii) Cemented back to 50 feet above the base of the next largest 
casing string.
    (b) The owner or operator of a new Class II well authorized by 
permit shall:
    (1) Install surface casing from the surface to at least 50 feet 
below the base of the lowermost USDW.
    (2) Cement the casing by recirculating to the surface or by using no 
less than 120% of the calculated annular volume.
    (3) For new enhanced recovery wells, install tubing or long string 
casing extending to the injection zone.
    (4) For new salt water disposal wells, install long string casing 
and tubing extending to the injection zone.
    (5) Isolate any injection zone by placing sufficient cement to fill 
the calculated volume to a point 50 feet above the injection zone.
    (c) The Regional Administrator may specify casing and cementing 
requirements other than those listed in paragraphs (a) and (b) of this 
section on a case by case basis as conditions of the permit.

[[Page 994]]



                         Subpart OO_Rhode Island



Sec.  147.2000  State-administered program--Class I, II, III, IV, and V wells.

    The UIC program for all classes of wells in Rhode Island, except 
those on Indian lands, is the program administered by the Rhode Island 
Department of Environmental Management, approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on August 1, 1984; the effective date of this program 
is August 15, 1984. This program consists of the following elements, as 
submitted to EPA in the State's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Rhode Island. This incorporation by 
reference was approved by the Director of the Federal Register effective 
August 15, 1984.
    (1) Rhode Island Gen. Laws sections 46-12-1, 46-12-5, and 46-12-28 
(Supp. 1983);
    (2) ``Underground Injection Control Program Rules and Regulations.'' 
State of Rhode Island and Providence Plantations Department of 
Environmental Management. Division of Water Resources (as received by 
the Secretary of State, May 21, 1984).
    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Rhode Island General Laws, Section 10-20-1 et seq., entitled 
``State Environmental Rights'';
    (2) Rhode Island General Laws, Section 23-19.1-1 et seq., entitled 
``Hazardous Waste Management'';
    (3) Rhode Island General Laws, Section 42-17.1 et seq., entitled 
``Department of Environmental Management'';
    (4) Rhode Island General Laws, Section 42-35-1 et seq., entitled 
``Administrative Procedures'';
    (5) Rhode Island General Laws, Section 46-12-1 et seq., entitled 
``Water Pollution'';
    (6) Hazardous Waste Management Facility Operating Permit Rules and 
Regulations--Landfills, at last amended November 2, 1981 (hereinafter 
referred to as the ``Hazardous Waste Regulation'');
    (7) Water Quality Regulations for Water Pollution Control, effective 
November 19, 1981; and
    (8) Administrative Rules of Practices and Procedure for Department 
of Environmental Management, effective November 12, 1980.
    (c) (1) The Memorandum of Agreement between EPA Region I and the 
Rhode Island Department of Environmental Management, signed by the EPA 
Regional Administrator on March 29, 1984;
    (2) Letter from Director, Rhode Island Department of Environmental 
Management, to Regional Administrator, EPA Region I, amending Section 
III, C of the Memorandum of Agreement, April 25, 1984.
    (d) Statement of legal authority. Letter from Attorney General, 
State of Rhode Island and Providence Plantations, to Regional 
Administrator, EPA Region 1, ``Re: Attorney General's Statement, 
Underground Injection Control Program,'' January 17, 1984.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 30699, Aug. 1, 1984, as amended at 53 FR 43090, Oct. 25, 1988]



Sec.  147.2001  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Rhode Island is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in Rhode Island is November 25, 1988.

[53 FR 43090, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991]

[[Page 995]]



                        Subpart PP_South Carolina



Sec.  147.2050  State-administered program.

    The UIC program for all classes of wells in the State of South 
Carolina, except for those on Indian lands, is the program administered 
by the South Carolina Department of Health and Environmental Control, 
approved by EPA pursuant to section 1422 of the SDWA. Notice of this 
approval was published in the Federal Register on July 10, 1984; the 
effective date of this program is July 24, 1984. This program consists 
of the following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of South Carolina. This incorporation by 
reference was approved by the Director of the Federal Register effective 
July 24, 1984.
    (1) Pollution Control Act, S.C. Code Ann. Sections 48-1-10, 48-1-90, 
48-1-100, 48-1-110 (Law. Co-op. 1976 and Supp. 1983).
    (2) South Carolina Department of Health and Environmental Control, 
Ground-Water Protection Division, Underground Injection Control 
Regulations, R-61-87, Effective Date: June 24, 1983 Published in South 
Carolina State Register, Volume 7, Issue 6; Amended Date: March 23, 
1984, as amended by notice in South Carolina State Register, Volume 8, 
Issue 3.
    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
Administered program:
    (1) Pollution Control Act, S.C. Code Ann. Sections 48-1-10 to 48-1-
350 (Law. Co-op. 1976 and Supp. 1983).
    (2) State Safe Drinking Water Act, S.C. Code Ann. Sections 44-55-10 
to 44-55-100 (Law. Co-op. 1976 and Supp. 1983).
    (3) Administrative Procedures Act, S.C. Code Ann. Sections 1-23-10 
et seq., and 1-23-310 to 1-23-400 (Law. Co-op. 1976 and Supp. 1983).
    (4) S.C. Code Ann. Sections 15-5-20, 15-5-200 (Law. Co-op. 1976 and 
Supp. 1983).
    (c)(1) The Memorandum of Agreement between EPA Region IV and the 
South Carolina Department of Health and Environmental Control signed by 
the EPA Regional Administrator on May 29, 1984.
    (d) Statement of legal authority. (1) ``Underground Injection 
Control Program, Attorney General's Statement for Class I, II, III, IV 
and VA and VB Wells,'' signed by the Attorney General of South Carolina 
on April 27, 1984.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 28058, July 10, 1984, as amended at 53 FR 43090, Oct. 25, 1988]



Sec.  147.2051  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Rhode Island is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands in South Carolina is November 25, 1988.

[53 FR 43090, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991]



                         Subpart QQ_South Dakota



Sec.  147.2100  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of South Dakota, 
except those on Indian lands, is the program administered by the South 
Dakota Department of Water and Natural Resources, approved by EPA 
pursuant to section 1425 of the SDWA. Notice of this approval was 
published in the Federal Register on October 24, 1984; the effective 
date of this program is December 7, 1984. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.

[[Page 996]]

    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of South Dakota. This incorporation by 
reference was approved by the Director of the Federal Register effective 
December 7, 1984.
    (1) South Dakota Codified Laws, sections 45-9-2, 45-9-4, 45-9-11, 
45-9-13, 45-9-14, 45-9-15 (1983).
    (2) Administrative Rules of South Dakota, sections 74:10:02 through 
74:10:07, 74:10:09, and 74:10:11 published by the South Dakota Code 
Commission, as revised through October 4, 1987.
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) South Dakota Codified Laws, Chapter 45-9 (sections not cited 
above) (1983); 1-26 (1981).
    (c)(1) The Memorandum of Agreement between EPA Region VIII and the 
South Dakota Department of Water and Natural Resources, signed by the 
EPA Regional Administrator on July 18, 1984.
    (d) Statement of legal authority. (1) ``Underground Injection 
Control Program for Class II Wells: Attorney General's Statement,'' 
signed by Mark V. Meierhery, Attorney General, South Dakota, on January 
16, 1984.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[50 FR 7061, Feb. 20, 1985, as amended at 56 FR 9419, Mar. 6, 1991]



Sec.  147.2101  EPA-administered program--Class I, III, IV and V wells 
and all wells on Indian lands.

    (a) Contents. The UIC program for all Class I, III, IV, and V wells, 
including those on Indian lands, and for Class II wells on Indian lands 
in the state of South Dakota is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Class 
I, III, IV and V wells on all lands in South Dakota, including Indian 
lands, and for Class II wells on Indian lands only, is December 30, 
1984.

[52 FR 17682, May 11, 1987, as amended at 56 FR 9419, Mar. 6, 1991]



Sec.  147.2102  Aquifer exemptions.

    (a) This section identifies any aquifers or their portions exempted 
in accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter at the 
time of program promulgation. EPA may in the future exempt other 
aquifers or their portions, according to applicable procedures, without 
codifying such exemptions in this section. An updated list of exemptions 
will be maintained in the Regional office.
    (b) Those portions of all aquifers located on Indian Lands, which 
meet the definition of USDW and into which existing Class II wells are 
injecting, are exempted within a \1/4\ mile radius of the well for the 
purpose of Class II injection activities only.

[49 FR 45308, Nov. 15, 1984]



Sec.  147.2103  Existing Class II enhanced recovery and hydrocarbon 
storage wells authorized by rule.

    (a) Maximum injection pressure. (1) To meet the operating 
requirements of Sec.  144.28(f)(3)(ii) (A) and (B) of this chapter, the 
owner or operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comments, and 
opportunity for a public hearings, according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure; or
    (ii) May inject at a pressure greater than those specified in 
paragraph (a)(1)(i) of this section for the field or formation in which 
he is operating provided he submits a request in writing to the Regional 
Administrator, and

[[Page 997]]

demonstrates to the satisfaction of the Regional Administrator that such 
injection pressure will not violate the requirement of Sec.  
144.28(f)(3)(ii)(A) and (B). The Regional Administrator may grant such a 
request after notice, opportunity for comment, and opportunity for a 
public hearing, according to the provisions of part 124, subpart A of 
this chapter.
    (2) Prior to such time as the Regional Administrator establishes 
field rules for maximum injection pressure based on data provided 
pursuant to paragraph (a)(2)(ii) of this section the owner or operator 
shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit to the Regional Administrator data acceptable to the 
Regional administrator which defines the fracture pressure of the 
formation in which injection is taking place. A single test may be 
submitted on behalf of two or more operators conducting operations in 
the same formation, if the Regional Administrator approves such 
submission.
    (b) Casing and cementing. Where the Regional Administrator 
determines that the owner or operator of an existing enhanced recovery 
or hydrocarbon storage well may not be in compliance with the 
requirement of Sec. Sec.  144.28(e) and 146.22, the owner or operator 
shall when required by the Regional Administrator:
    (1) Protect USDWs by:
    (i) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (ii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operation pressure;
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone; and/or
    (4) Comply with other requirements which the Regional Administrator 
may specify in addition to or in lieu of the requirements set forth in 
paragraphs (b) (1) through (3) of this section as needed to protect 
USDWs.

[49 FR 45308, Nov. 15, 1984]



Sec.  147.2104  Requirements for all wells.

    (a) The owner or operator converting an existing well to an 
injection well shall check the condition of the casing with one of the 
following logging tools;
    (1) A pipe analysis log; or
    (2) A caliper log.
    (b) The owner or operator of a new injection well cased with plastic 
(PVC, ABS, or others) casings shall:
    (1) Not construct a well deeper than 500 feet;
    (2) Use cement and additives compatible with such casing material; 
and
    (3) Cement the annular space above the injection intermal from the 
bottom of the blank casing to the surface.
    (c) The owner or operator of a newly drilled well shall install 
centralizers as directed by the Regional Administrator.
    (d) The owner or operator shall as required by the Regional 
Administrator:
    (1) Protect USDWs by:
    (i) Setting surface casing 50 feet below the lowermost USDW;
    (ii) Cementing surface casing by recirculating the cement to the 
surface from a point 50 feet below the lowermost USDW; or
    (iii) Isolating all USDWs by placing cement between the outermost 
casing and the well bore; and
    (2) Isolate any injection zones by placing sufficient cement to fill 
the calculated space between the casing and the well bore to a point 250 
feet above the injection zone; and
    (3) Use cement:
    (i) Of sufficient quantity and quality to withstand the maximum 
operating pressure; and
    (ii) Which is resistant to deterioration from formation and 
injection fluids; and
    (iii) In a quantity no less than 120% of the calculated volume 
necessary to cement off a zone.

[[Page 998]]

    (4) The Regional Administrator may approve alternate casing and 
cementing practices provided that the owner or operator demonstrates 
that such practices will adequately protect USDWs.
    (e) Area of review. Notwithstanding the alternatives presented in 
Sec.  146.6 of this chapter, the area of review shall be a fixed radius 
as described in Sec.  146.6(b) of this chapter.
    (f) The applicant must give separate notice of intent to apply for a 
permit to each owner of record of the land within one-quarter mile of 
the site. The addresses of those to whom notice is given and the 
description of how notice was given shall be submitted with the permit 
application. The notice shall include:
    (1) The name and address of applicant;
    (2) A brief description of the planned injection activities, 
including well location, name and depth of the injection zone, maximum 
injection pressure and volume, and fluid to be injected;
    (3) The EPA contact person; and
    (4) A statement that opportunity to comment will be announced after 
EPA prepares a draft permit.

This requirement may be waived by the Regional Administrator if he 
determines that individual notice to all land owners of record would be 
impractical.

[49 FR 45308, Nov. 15, 1984]



                          Subpart RR_Tennessee



Sec.  147.2150  State-administered program--Class I, II, III, IV, and V wells.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Tennessee, except for those on any Indian lands, is the program 
administered by the Tennessee Department of Environment and 
Conservation, approved by EPA pursuant to section 1422 of the SDWA. 
Notice of this approval was published in the Federal Register on April 
6, 2015; the effective date of this program is July 6, 2015. This 
program consists of the following elements, as submitted to EPA in the 
state's program application.
    (a) Incorporation by reference. The requirements set forth in the 
Tennessee State statutes and regulations cited in the binder (Volumes 1 
and 2) entitled ``EPA-Approved State of Tennessee Safe Drinking Water 
Act section 1422 Underground Injection Control (UIC) Program Statutes 
and Regulations for Well Classes I, II, III, IV, and V,'' dated 
September 2013 and Table 1 to paragraph (a) of this section are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Tennessee. This incorporation by 
reference was approved by the Director of the Federal Register in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the 
Tennessee regulations may be obtained or inspected at Tennessee 
Department of Environment and Conservation, 6th Floor, 401 Church 
Street, Nashville, Tennessee 32743, (315) 532-0191, at the Environmental 
Protection Agency, Region 4, 61 Forsyth Street, SW., Atlanta, Georgia 
30303-8960, (404) 562-8190 or at the National Archives and Records 
Administration (NARA). For information on availability of this material 
at NARA, call (202) 741-6030, or go to: http://www.archives.gov/
locations/.

Table 1 to Paragraph (a) EPA-Approved Tennessee SDWA Section 1422 Underground Injection Control Program Statutes
                             and Regulations for Well Classes I, II, III, IV, and V
----------------------------------------------------------------------------------------------------------------
                                                         State effective
         State citation              Title/subject             date                 EPA approval date \1\
----------------------------------------------------------------------------------------------------------------
Tennessee Code Annotated, Title   Uniform              August 5, 2011.....  4/6/15, 80 FR 18318.
 4, Chapter 5.                     Administrative
                                   Procedures Act.
Tennessee Code Annotated, Title   Subsurface Sewage    August 5, 2011.....  4/6/15, 80 FR 18318.
 68, Chapter 221, Part 4.          Disposal Systems.
Tennessee Code Annotated, Title   Tennessee Safe       July 9, 2012.......  4/6/15, 80 FR 18318.
 68, Chapter 221, Part 7.          Drinking Water Act
                                   of 1983.
Tennessee Code Annotated, Title   Hazardous Waste      July 9, 2012.......  4/6/15, 80 FR 18318.
 68, Chapter 212, Section 101 et   Management Act of
 seq.                              1977.

[[Page 999]]

 
Tennessee Code Annotated, Title   Hazardous Waste      July 9, 2012.......  4/6/15, 80 FR 18318.
 68, Chapter 212, Section 201 et   Management Act of
 seq.                              1983.
Tennessee Code Annotated, Title   Tennessee            May 10, 2012.......  4/6/15, 80 FR 18318.
 68, Chapter 203.                  Environmental
                                   Protection Fund.
Tennessee Code Annotated, Title   Tennessee Solid      June 25, 2009......  4/6/15, 80 FR 18318.
 68, Chapter 211, Part 1.          Waste Disposal Act.
Tennessee Code Annotated, Title   Tennessee Petroleum  June 29, 2009......  4/6/15, 80 FR 18318.
 68, Chapter 215, Part 1.          Underground
                                   Storage Tank Act.
Tennessee Code Annotated, Title   Water Quality        October 1, 2012....  4/6/15, 80 FR 18318.
 69, Chapter 3, Part 1.            Control Act.
Official Compilation Rules &      Underground          December 11, 2012..  4/6/15, 80 FR 18318.
 Regulations of the State of       Injection Control.
 Tennessee Chapter 0400-45-06.
Official Compilation Rules &      Public Water         December 11, 2012..  4/6/15, 80 FR 18318.
 Regulations of the State of       Systems.
 Tennessee Chapter 0400-45-01.
Compilation Rules & Regulations   Regulations to       November 24, 2009..  4/6/15, 80 FR 18318.
 of the State of Tennessee         Govern Subsurface
 Chapter 1200-1-6.                 Sewage Disposal
                                   Systems.
Official Compilation Rules &      Hazardous Waste      September 20, 2012.  4/6/15, 80 FR 18318.
 Regulations of the State of       Management.
 Tennessee Chapter 0400-12-01-
 .02(1)(c).
Official Compilation Rules &      Standards For        May 22, 2012.......  4/6/15, 80 FR 18318.
 Regulations of the State of       Protection Against
 Tennessee Chapter 0400-20-05-     Radiation.
 .161.
----------------------------------------------------------------------------------------------------------------
\1\ In order to determine the EPA effective date for a specific provision listed in this table, consult the
  Federal Register document cited in this column for the particular provision.

    (b) Memorandum of Agreement (MOA). The MOA between EPA Region 4 and 
the Tennessee Department of Environment and Conservation signed by EPA 
Regional Administrator on October 20, 2004.
    (c) Statements of legal authority. ``Underground Injection Control 
Program, Attorney General's Statement,'' signed by Attorney General of 
Tennessee on July 26, 2005 and ``Updating the Attorney General's 
Statement on UIC Program Authority,'' signed by General Counsel of the 
Tennessee Department of Environment and Conservation on November 10, 
2011.
    (d) Program description. The Program Description submitted as part 
of Tennessee's application, and any other materials submitted as part of 
this application or as a supplement thereto.

[80 FR 18318, Apr. 6, 2015]



Sec.  147.2151  EPA-administered program Class IV and Indian lands.

    (a) Contents. The UIC program for Class VI wells and all wells on 
Indian lands in the State of Tennessee is administered by EPA. This 
program consists of the UIC program requirements of 40 CFR parts 124, 
144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective dates. Effective date for the UIC program on Indian 
lands is November 25, 1988. The effective date for the UIC program for 
the rest of Tennessee is June 25, 1984.

[53 FR 43090, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991; 80 
FR 18319, Apr. 6, 2015]

[[Page 1000]]



Sec.  147.2152  Aquifer exemptions. [Reserved]



Sec.  147.2153  Existing Class I, II (except enhanced recovery 
and hydrocarbon storage) and III wells authorized by rule.

    Maximum injection pressure. The owner or operator shall limit 
injection pressure to the lesser of:
    (a) A value which will not exceed the operating requirements of 
Sec.  144.28(f)(3) (i) or (ii) as applicable or
    (b) A value for well head pressure calculated by using the following 
formula:

Pm = (0.600-0.433 Sg)d

where:

Pm = injection pressure at the well head in pounds per square inch
Sg = specific gravity of inject fluid (unitless)
d = injection depth in feet.



                            Subpart SS_Texas



Sec.  147.2200  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Texas, except for those wells on Indian lands, Class III brine mining 
wells, and certain Class V wells, is the program administered by the 
Texas Commission on Environmental Quality approved by EPA pursuant to 
section 1422 of the Safe Drinking Water Act (SDWA). Notice of the 
original approval for Class I, III, IV, and V wells was published in the 
Federal Register on January 6, 1982 and became effective February 7, 
1982. Class V geothermal wells and wells for the in situ combustion of 
coal are regulated by the Rail Road Commission of Texas under a separate 
UIC program approved by EPA and published in the Federal Register on 
April 23, 1982. A subsequent program revision application for Class I, 
III, IV, and V wells, not including Class III brine mining wells, was 
approved by the EPA pursuant to section 1422 of SDWA. Notice of this 
approval was published in the Federal Register on February 25, 2004; the 
effective date of these programs is March 26, 2004. The program for 
Class I, III, IV, and V wells, not including Class III brine mining 
wells, consists of the following elements as submitted to the EPA in the 
State's revised program applications. The UIC program for Class III 
brine mining wells in the State of Texas, except for those wells on 
Indian lands, is the program administered by the Railroad Commission of 
Texas. A program revision application for Class III brine mining wells 
was submitted by Texas and approved by EPA. Notice of that approval was 
published in the Federal Register on February 26, 2004; the effective 
date of this program is March 29, 2004.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made part of the applicable UIC program 
under SDWA for the State of Texas. This incorporation by reference was 
approved by the Director of the Federal Register in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies of the materials that are 
incorporated by reference in this paragraph are available at EPA Region 
VI, 1445 Ross Avenue, Dallas, TX 75202 or from the National Archives and 
Records Administration (NARA). For information on the availability of 
this material at NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Texas Statutory and Regulatory Requirements Applicable to the 
Underground Injection Control Program for Class I, III, IV, and V Wells, 
except for Class III Brine Mining Wells, March 2002.
    (2) Texas Statutory and Regulatory Requirements Applicable to the 
Underground Injection Control Program for Class III Brine Mining Wells, 
March 2002.
    (b) Other laws. The following statutes and regulations, as effective 
on March 31, 2002, although not incorporated by reference except for any 
provisions identified in paragraph (a) of this section, are also part of 
the approved State-administered UIC program.
    (1) Class I, III, IV, and V wells. (i) Title 30 of the Texas 
Administrative Code Chapters 39, 50, 55, 80, and 281.
    (ii) Vernon's Texas Codes Annotated, Water Code, Chapters 5, 7, 26, 
and 32, Health and Safety Code Section 361, Government Code (ORA) 
Chapter 552

[[Page 1001]]

and Government Code (APA) Chapter 2001.
    (2) Class III brine mining wells. (i) Vernon's Texas Codes 
Annotated, Natural Resources Code, Chapters 91, 2001, and 331;
    (ii) Vernon's Texas Codes Annotated, Government Code Title 10, 
Chapters 2001, 552, and 311.
    (iii) General Rules of Practice and Procedure before the Railroad 
Commission of Texas.
    (c) Memorandum of Agreement--(1) Class I, III, IV, and V wells. The 
Memorandum of Agreement between EPA Region VI and the Texas Natural 
Resource Conservation Commission a predecessor to the Texas Commission 
on Environmental Quality (TCEQ), revised March 23, 1999, and signed by 
the EPA Regional Administrator on October 23, 2001.
    (2) Class III brine mining wells. The Memorandum of Agreement 
between EPA Region VI and the Railroad Commission of Texas signed by the 
EPA Regional Administrator on October 23, 2001.
    (d) Statement of legal authority--(1) Class I, III, IV, and V wells. 
``State of Texas Office of Attorney General Statement for Class I, III, 
IV, and V Underground Injections Wells,'' signed by the Attorney General 
of Texas, June 30, 1998.
    (2) Class III brine mining wells. State of Texas ``Attorney 
General's Statement'' for Class III Brine Mining Injection Wells, signed 
by the Attorney General of Texas, February 2, 1992 and the ``Supplement 
to Attorney General's Statement of February 19, 1992,'' signed by the 
Attorney General of Texas, June 2, 1998.
    (e) Program Description--(1) Class I, III, IV, and V wells. The 
Program Description and any other materials submitted as part of the 
revision application or as supplements thereto.
    (2) Class III brine mining wells. The Program Description and any 
other materials submitted as part of the revision application or as 
supplements thereto.

[69 FR 8568, Feb. 25, 2004, as amended at 69 FR 8828, Feb. 26, 2004]



Sec.  147.2201  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Texas, except for 
those wells on Indian lands, is the program administered by the Railroad 
Commission of Texas, approved by EPA pursuant to section 1425 of the 
SDWA. Notice of this approval was published in the Federal Register on 
April 23, 1982 (47 FR 17488). The effective date of this program was May 
23, 1982. This program consists of the following elements, as submitted 
to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Texas. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Injection Well Act, Texas Water Code Annotated sections 27.031 
and 27.033 (Vernon Supp. 1984);
    (2) Texas Natural Resources Code Annotated sections 85.041, 85.045, 
85.046 and 85.052 (Vernon 1978 and Supp. 1982);
    (3) Rules Having Statewide General Application to Oil, Gas, and 
Geothermal Resource Operations, sections .051.02.02.000 to 
.051.02.02.080 (Railroad Commission of Texas, Oil and Gas Division, 
Revised 12-22-81), amended as follows:
    (i) Amendment to 16 TAC section 3.9 (section .051.02.02.009) issued 
December 21, 1981, effective April 1, 1982;
    (ii) Amendment to 16 TAC section 3.46 (section .051.02.02.046) 
issued December 21, 1981, effective April 1, 1982.
    (iii) Amendment to 16 TAC section 3.71 (section .051.02.02.074) 
issued December 21, 1981, effective April 1, 1982.
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference, are also part of the approved State-
administered UIC program:
    (1) Texas Water Code, Chapters 26, 27 and 29 (Vernon 1972 and Supp. 
1982);
    (2) Texas Natural Resources Code, Chapters 81, 85-89, 91 and 141 
(Vernon 1978 and Supp. 1982);
    (3) General Rules of Practice and Procedure, Subchapters A-J 
(Railroad

[[Page 1002]]

Commission of Texas, adopted November 24, 1975, revised December 1980).
    (c)(1) The Memorandum of Agreement between EPA Region VI and the 
Railroad Commission of Texas, signed by the EPA Regional Administrator 
on March 24, 1982.
    (2) Letter from Director of Underground Injection Control, Railroad 
Commission of Texas, to Chief, Ground Water Protection Section, EPA 
Region VI, ``Re: Letter of Clarification--UIC Program Application,'' 
March 21, 1982.
    (d) Statement of legal authority. ``Statement of Legal Authority of 
the Railroad Commission of Texas to conduct the Underground Injection 
Control Program,'' signed by Special Counsel, Railroad Commission of 
Texas, as submitted with ``State of Texas Underground Injection Control 
Program Application for Primacy Enforcement Authority,'' prepared by the 
Railroad Commission of Texas, January 15, 1982.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43091, Oct. 25, 1988]



Sec.  147.2205  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Texas is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date for the Indian lands program 
for the State of Texas is November 25, 1988.

[53 FR 43091, Oct. 25, 1988, as amended at 56 FR 9419, Mar. 6, 1991]



                             Subpart TT_Utah



Sec.  147.2250  State-administered program--Class I, III, IV, and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
Utah, except those on Indian lands, is administered by the Utah 
Department of Health, Division of Environmental Health, approved by EPA 
pursuant to Section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on January 9, 1983 (47 FR 2321). The 
effective date of this program is February 10, 1983. Changes to Utah's 
regulations for Class I wells were made on May 15, 1990, in response to 
modification of national rules as promulgated by 53 FR 28188, July 26, 
1988. Utah's rules were effective July 20, 1990. The revised rules, 
Program Description, Attorney General's statement, and Memorandum of 
Agreement were approved as a minor program modification on October 3, 
1990. This program consists of the following elements as submitted to 
EPA:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Utah. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Utah Water Pollution Control Act, Utah Code Annotated, Title 26, 
Chapter 11, Sections 2, 8, and 10 (1989);
    (2) Underground Injection Control Regulations; Utah Administrative 
Code, Section R448-7 (effective as of January 2, 1990);
    (3) Underground Injection Control Program (adopted January 20, 1982 
and revised effective July 20, 1990) (Officially submitted to EPA by the 
Executive Secretary of Utah Water Pollution Control Committee on August 
16, 1990).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for selected sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program:
    (1) Utah Pollution Control Act, Utah Code Annotated, Sections 26-11-
1 through -20 (Supp. 1990);
    (c)(1) The revised Memorandum of Agreement between EPA, Region VIII 
and the Utah Department of Health, Division of Environmental Health, 
signed by the Regional Administrator on October 3, 1990.
    (2) Letter from Director, Utah Department of Health, Division of 
Environmental Health, Bureau of Water

[[Page 1003]]

Pollution Control, to EPA Region VIII, Re: Underground Injection Control 
Program--Utah, March 15, 1982;
    (3) Letter from the Executive Secretary of the Utah Water Pollution 
Control Committee to EPA Region VIII, ``Re: Utah UIC Class I Well 
Program Changes,'' August 16, 1990;
    (d) Statement of legal authority. (1) ``Underground Injection 
Control Program--Attorney General's statement,'' signed by Attorney 
General, State of Utah, January, 1982;
    (2) Letter from Assistant Attorney General of Utah to Chief, 
Drinking Water Branch, EPA Region VIII, June 18, 1982;
    (3) Addendum to Underground Injection Control Program, Attorney 
General's Statement signed by Attorney General of Utah, August 10, 1990.
    (e) The Program Description (revised June 19, 1990) and any other 
materials submitted as part of the application or supplements thereto.

[56 FR 9419, Mar. 6, 1991]



Sec.  147.2251  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Utah, except 
those on Indian lands, is the program administered by the Utah 
Department of Natural Resources, Division of Oil, Gas, and Mining, 
approved by EPA pursuant to section 1425 of the SDWA. Notice of this 
approval was published in the Federal Register on October 8, 1982 (47 FR 
44561); the effective date of this program is November 7, 1982. This 
program consists of the following elements, as submitted to EPA in the 
State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Utah. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Utah Code Annotated, 1953, section 40-6-1 through 40-6-18, as 
amended 1988 and Cumm. Supp. 1990;
    (2) The Oil and Gas Conservation General Rules, adopted under the 
authority of the Oil and Gas Conservation Act, 40-6-1 et seq., Utah Code 
Annotated, as amended 1988 (revised March 1989), rules R615-1 through 
R615-4, and R615-8 through R615-10.
    (b) Other laws. [Reserved]
    (c)(1) The Memorandum of Agreement between EPA, Region VIII and the 
Utah Department of Natural Resources, Division of Oil, Gas, and Mining 
and the Board of Oil, Gas and Mining, signed by the EPA Regional 
Administrator on July 19, 1983;
    (2) Letter from Director, Division of Oil, Gas and Mining, Utah 
Department of Natural Resources and Energy, to Regional Administrator, 
EPA Region VIII, ``Re: Aquifer Exemption Process,'' June 16, 1982;
    (3) ``Memorandum of Understanding'' between Utah Department of 
Health and Utah Department of Natural Resources, dated March 5, 1981;
    (4) ``Second Addition to Agreement between the Department of Health 
and the Department of Natural Resources and Energy,'' dated December 15, 
1981.
    (d) Statement of legal authority. (1) Part III of ``Primacy 
Application--Class II Underground Injection Wells,'' consisting of 
``Synopsis of Pertinent Statutes and Regulations,'' ``Statement of Legal 
Authority,'' and ``Certification by the Attorney General,'' by Assistant 
Attorney General, Department of Natural Resources and Energy, dated 
December 18, 1981;
    (2) Letter from Assistant Attorney General, State of Utah, to EPA 
Region VIII, undated, received in the EPA Office of Regional Counsel 
June 10, 1982.
    (3) Memorandum to Director, Division of Oil, Gas and Mining from 
Assistant Attorney General regarding Underground Injection Control 
Program, January 8, 1985.
    (e) The Program Description and any other materials submitted as 
part of the application or amendments thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43091, Oct. 25, 1988; 56 
FR 9420, Mar. 6, 1991]



Sec.  147.2253  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Utah, except for Class II wells on Navajo Indian 
lands for which EPA

[[Page 1004]]

has granted the Navajo Nation primacy for the SDWA Class II UIC program 
(as defined in Sec.  147.3400), is administered by EPA. The program for 
wells on Navajo Indian lands, except for Class II wells on Navajo Indian 
lands for which EPA has granted the Navajo Nation primacy for the SDWA 
Class II UIC program, and for Ute Mountain Ute consists of the 
requirements set forth at subpart HHH of this part. The program for all 
other wells on Indian lands consists of the UIC program requirements of 
40 CFR parts 124, 144, 146, 148, and any additional requirements set 
forth in the remainder of this subpart. Injection well owners and 
operators, and EPA shall comply with these requirements.
    (b) Effective date. The effective date for this program for all 
other Indian lands in Utah, except for Class II wells on Navajo Indian 
lands for which EPA has granted the Navajo Nation primacy for the SDWA 
Class II UIC program (as defined in Sec.  147.3400), is November 25, 
1988.

[53 FR 40391, Oct. 25, 1988, as amended at 56 FR 9420, Mar. 6, 1991; 73 
FR 65565, Nov. 4, 2008]



                           Subpart UU_Vermont



Sec.  147.2300  State-administered program.

    The UIC program for all classes of wells in the State of Vermont, 
except those wells on Indian lands, is the program administered by the 
Vermont Department of Environmental Conservation, approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the FR on June 22, 1984; the effective date of this program 
is July 6, 1984. This program consists of the following elements:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Vermont. This incorporation by reference 
was approved by the Director of the Federal Register July 6, 1984.
    (1) Vt. Stat. Ann. tit. 10, sections 1251, 1259, 1263 (1973 and 
Supp. 1981), Effective date: July 1, 1982.
    (2) Vermont Department of Water Resources and Environmental 
Engineering, Chapter 13 Water Pollution Control Regulations, Subchapter 
13.UIC--Underground Injection Control, Discharges to Injection Wells, 
Effective Date: June 21, 1984.
    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Vt. Stat. Ann. tit. 10, sections 1251 through 1283 (1973 and 
Supp. 1981).
    (2) Vt. Stat. Ann. tit. 10, sections 901 through 911 (1973 and Supp. 
1981).
    (3) Vt. Stat. Ann. tit. 3, sections 801 through 847 (1973 and Supp. 
1981).
    (c)(1) The Memorandum of Agreement between EPA Region I and the 
Vermont Agency of Environmental Conservation signed by the EPA Regional 
Administrator on January 16, 1984.
    (d) Statement of legal authority. (1) ``Vermont Attorney General's 
Statement for Classes I, II, III, IV and V Injection Wells,'' signed by 
Attorney General John J. Easton, Jr., as submitted with Vermont 
Application for Primary Enforcement Responsibility to Administer the 
Underground Water Source Protection Program Pursuant to the Safe 
Drinking Water Act and 40 CFR 145.21 through 145.24 (December 20, 1983).
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

(42 U.S.C. 300)

[49 FR 25634, June 22, 1984, as amended at 53 FR 43091, Oct. 25, 1988; 
56 FR 9420, Mar. 6, 1991]



Sec. Sec.  147.2301-147.2302  [Reserved]



Sec.  147.2303  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Vermont is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.

[[Page 1005]]

    (b) Effective date. The effective date of the UIC program for Indian 
lands in Vermont is November 25, 1988.

[53 FR 43091, Oct. 25, 1988, as amended at 56 FR 9420, Mar. 6, 1991]



Sec. Sec.  147.2304-147.2349  [Reserved]



                           Subpart VV_Virginia



Sec.  147.2350  State-administered program. [Reserved]



Sec.  147.2351  EPA-administered program.

    (a) Contents. The UIC program for the State of Virginia, including 
all Indian lands, is administered by EPA. This program consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date for the UIC program on 
Indian lands is November 25, 1988. The effective date for the UIC 
program for the remainder of Virginia is June 25, 1984. (53 FR 43091, 
October 25, 1988).

[56 FR 9420, Mar. 6, 1991]



Sec.  147.2352  Aquifer exemptions. [Reserved]



                          Subpart WW_Washington



Sec.  147.2400  State-administered program--Class I, II, III, IV, and V wells.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Washington other than those on Indian lands, is the program 
administered by the Washington Department of Ecology, approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on August 9, 1984; the effective date 
of this program is September 24, 1984. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
state statutes and regulations cited in the binder entitled ``EPA-
Approved Washington SDWA section 1422 Underground Injection Control 
Program Statutes and Regulations for Well Classes I, II, III, IV, and 
V,'' dated January 2014, and Table 1 to paragraph (a) of this section 
are hereby incorporated by reference and made a part of the applicable 
UIC program under the SDWA for the State of Washington. The Director of 
the Federal Register approves this incorporation by reference in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the State 
of Washington regulations that are incorporated by reference in 
paragraph (a) of this section may be inspected at the U.S. Environmental 
Protection Agency, Region 10, Library, 10th Floor, 1200 Sixth Avenue, 
Seattle, Washington 98101; Water Docket, EPA Docket Center (EPA/DC) EPA 
West, Room 3334, 1301 Constitution Ave. NW., Washington, DC 20460; and 
the National Archives and Records Administration (NARA). If you wish to 
obtain materials from the EPA Regional Office, please call (206) 553-
1289; for materials from a docket in the EPA Headquarters Library, 
please call the Water Docket at (202) 566-2426. For information on the 
availability of this material at NARA, call (202) 741-6030, or go to 
http://www.archives.gov/locations/.

[[Page 1006]]



    Table 1 to Paragraph (a) EPA-Approved Washington SDWA Section 1422 Underground Injection Control Program
                         Statutes and Regulations for Well Classes I, II, III, IV, and V
----------------------------------------------------------------------------------------------------------------
                                                            State effective
         State citation               Title/subject              date                EPA approval date \1\
----------------------------------------------------------------------------------------------------------------
Revised Code of Washington       Water Pollution Control  February 3, 2006..  4/6/15 [Insert Federal Register
 Sections 90.48.010--90.48.906.                                                Citation]
Revised Code of Washington       Departments authorized   February 3, 2006..  [Insert the date of publication in
 Section 43.21A.445.              to participate in and                        the Federal Register] [Insert
                                  administer federal                           Federal Register Citation]
                                  Safe Drinking Water
                                  Act--Agreements with
                                  other departments.
Washington Administrative Code   Underground Injection    June 19, 2008.....  4/6/15 [Insert Federal Register
 Sections 173-218-010--173-218-   Control Program.                             Citation]
 130.
Washington Administrative Code   Oil and Gas              June 29, 1988.....  4/6/15 [Insert Federal Register
 Sections 344-12-001--344-12-     Conservation                                 Citation]
 295.                             Committee, General
                                  Rules.
Washington Administrative Code   Minimum Standards for    December 19, 2008.  4/6/15 [Insert Federal Register
 Sections 173-160-010--173-160-   Construction and                             Citation]
 990.                             Maintenance of Wells.
----------------------------------------------------------------------------------------------------------------
\1\ In order to determine the EPA effective date for a specific provision listed in this table, consult the
  Federal Register document cited in this column for the particular provision.


[[Page 1007]]

    (b) Other laws. The following statutes and regulations although not 
incorporated by reference, also are part of the approved State-
administered program:
    (1) Revised Code of Washington, chapter 34.04 (Bureau of National 
Affairs, 1981 Laws), entitled ``Administrative Procedure act'';
    (2) Revised Code of Washington, chapter 43.21A (Bureau of National 
Affairs, 1980 Laws), entitled ``Department of Ecology,'' as amended by 
1983 Washington Laws, Chapter 270;
    (3) Revised Code of Washington, chapter 70.105 (Bureau of National 
Affairs, 1983 Laws), entitled ``Hazardous Waste Disposal'';
    (4) Revised Code of Washington, chapter 78.52 (Bureau of National 
Affairs, 1983 Laws), entitled ``Oil and Gas Conservation'';
    (5) Revised Code of Washington, chapter 90.48 (Bureau of National 
Affairs, 1986 Laws), entitled ``Water Pollution Control.''
    (c)(1) The Memorandum of Agreement between EPA Region X and the 
Washington Department of Ecology, signed by the EPA Regional 
Administrator on February 15, 2011.
    (2) Memorandum of Agreement between the Washington Department of 
Ecology and Oil and Gas Conservation Committee, Related to the 
Underground Injection Control Program for the State of Washington, 
signed March 23, 1984;
    (3) Memorandum of Agreement between the Washington Department of 
Ecology and Washington Department of Natural Resources, Related to the 
Underground Injection Control Program for the State of Washington, 
signed March 23, 1984;
    (4) Memorandum of Agreement between the Washington Department of 
Ecology and Department of Social and Health Services, Related to the 
Underground Injection Control Program for the State of Washington, 
signed March 23, 1984;
    (5) Memorandum of Agreement between the Washington Department of 
Ecology and the Energy Facility Site Evaluation Council, Related to the 
Underground Injection Control Program for the State of Washington, 
signed March 19, 2009.
    (d) Statement of legal authority. Letter from Attorney General of 
the State of Washington, by Senior Assistant Attorney General, to 
Director, Washington State Department of Ecology, ``Re: Underground 
Injection Control Regulatory Program--Attorney General's Statement,'' 
February 28, 1984.
    (e) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[49 FR 31876, Aug. 9, 1984, as amended at 56 FR 9420, Mar. 6, 1991; 80 
FR 18322, Apr. 6, 2015]



Sec.  147.2403  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Washington is administered by EPA. This program, 
for all Indian lands except those of the Colville Tribe, consists of the 
UIC program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date for the UIC program for 
Indian lands in Washington is November 25, 1988.

[53 FR 43091, Oct. 25, 1988, as amended at 56 FR 9420, Mar. 6, 1991]



Sec.  147.2404  EPA-administered program--Colville Reservation.

    (a) The UIC program for the Colville Indian Reservation consists of 
a prohibition of all Class I, II, III and IV injection wells and of a 
program administered by EPA for Class V wells. This program consists of 
the UIC program requirements of 40 CFR part 124, 144 and 146 and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and EPA shall comply with these requirements. The 
prohibition on Class I-IV wells is effective November 25, 1988. No owner 
or operator shall construct, operate, maintain, convert, or conduct any 
other injection activity thereafter using Class I-IV wells.
    (b) Owners and operators of Class I, II, III or IV wells in 
existence on the effective date of the program shall cease injection 
immediately. Within 60 days of the effective date of the program,

[[Page 1008]]

the owner or operator shall submit a plan and schedule for plugging and 
abandoning the well for the Director's approval. The owner or operator 
shall plug and abandon the well according to the approved plan and 
schedule.

[53 FR 43091, Oct. 25, 1988]



                        Subpart XX_West Virginia



Sec. Sec.  147.2450-147.2452  [Reserved]



Sec.  147.2453  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of West Virginia is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date for the UIC program on Indian 
lands in West Virginia is November 25, 1988.

[53 FR 43092, Oct. 25, 1988, as amended at 56 FR 9420, Mar. 6, 1991]



Sec. Sec.  147.2454-147.2499  [Reserved]



                          Subpart YY_Wisconsin



Sec.  147.2500  State-administered program.

    The UIC program for Class I, II, III, IV, and V wells in the State 
of Wisconsin, other than those on Indian lands as described in Sec.  
147.2510, is the program administered by the Wisconsin Department of 
Natural Resources, approved by EPA pursuant to SDWA section 1422. Notice 
of this approval was published in the Federal Register on September 30, 
1983 (48 FR 44783); the effective date of this program is November 30, 
1983. This program consists of a prohibition of all injection wells 
except heat pump return flow injection wells and may be found in the 
following elements, as submitted to EPA in the State's program 
application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Wisconsin. This incorporation by 
reference was approved by the Director of the OFR in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained at the Wisconsin 
Department of Natural Resources, Box 7921, Madison, Wisconsin, 53707. 
Copies may be inspected at the Environmental Protection Agency, Region 
V, 77 West Jackson Boulevard, Chicago, Illinois, 60604, or at the 
National Archives and Records Administration (NARA). For information on 
the availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Wisconsin Statutes Annotated Sec. Sec.  147.015, 147.02 and 
147.04 (West 1974 and Supp. 1983);
    (2) Chapter NR 112, Well Construction and Pump Installation, 
Wisconsin Administrative Code Sec. Sec.  NR 112.03 and 112.20 (October 
1981), as amended by Natural Resources Board Order No. WQ-25-82, 
approved by the Natural Resources Board on August 25, 1982;
    (3) Chapter NR 113, Servicing Septic Tanks, Seepage Pits, Grease 
Traps or Privies, Wisconsin Administrative Code Sec. Sec.  NR 113.07-
113.08 (1979), as amended by Natural Resources Board Order No. WQ-25-82, 
approved by the Wisconsin Natural Resources Board on August 25, 1982;
    (4) Chapter NR 181, Hazardous Waste Management, Wisconsin 
Administrative Code Sec. Sec.  NR 181.04-181.415 (1981), as amended June 
1985;
    (5) Chapter NR 210, Sewage Treatment Works, Wisconsin Administrative 
Code Sec.  210.05 Natural Resources Board Order No. WQ-25-82, approved 
by the Wisconsin Natural Resources Board on August 25, 1982;
    (6) Chapter NR 214, Land Application and Disposal of Liquid 
Industrial Wastes and By-Products, Wisconsin Administrative Code 
Sec. Sec.  214.03 and 214.08 (1983).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for select sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program:

[[Page 1009]]

    (1) Chapter 144, Water, Sewage, Refuse, Mining and Air Pollution, 
Wisconsin Statutes Annotated (West 1974 and Supp. 1983);
    (2) Chapter 147, Pollution Discharge Elimination, Wisconsin Statutes 
Annotated (West 1974 and Supp. 1983);
    (3) Chapter 162, Pure Drinking Water, Wisconsin Statutes Annotated 
(West 1974 and Supp. 1983);
    (4) Laws of 1981, Chapter 20, Sec.  2038 (Re: heat pump injection);
    (5) Wisconsin Statutes 803.09(1) (West 1977) (intervention as of 
right in civil actions).
    (c) Memorandum of Agreement. The Memorandum of Agreement between EPA 
Region V and the Wisconsin Department of Natural Resources, signed by 
the Regional Administrator on December 6, 1983.
    (d) Statement of legal authority. (1) ``Attorney General's 
Statement,'' signed by Attorney General, State of Wisconsin;
    (2) Letter from Assistant Attorney General, State of Wisconsin, to 
EPA Region, ``Re: Amendments to Attorney General's Statement-UIC,'' June 
30, 1983.
    (e) Program Description. The Program Description and other materials 
submitted as part of the application or as supplements thereto.

[49 FR 45309, Nov. 15, 1984, as amended at 56 FR 9420, Mar. 6, 1991; 56 
FR 14150, Apr. 5, 1991; 62 FR 1834, Jan. 14, 1997]



Sec.  147.2510  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for Indian lands in the State of 
Wisconsin is administered by EPA. This program consists of 40 CFR parts 
144 and 146 and additional requirements set forth in this section. 
Injection well owners and operators, and EPA, shall comply with these 
requirements.
    (b) Requirements. Notwithstanding the requirements of paragraph (a) 
of this section for Indian lands in Wisconsin no owner or operator shall 
construct, operate, maintain, or convert any Class I, II, III, IV or V 
injection well.
    (c) Effective date. The effective date of the UIC program 
requirements for Indian lands in Wisconsin is December 30, 1984.

[49 FR 45309, Nov. 15, 1984]



                           Subpart ZZ_Wyoming



Sec.  147.2550  State-administered program--Class I, III, IV and V wells.

    The UIC program for Class I, III, IV and V wells in the State of 
Wyoming, except those on Indian lands is the program administered by the 
Wyoming Department of Environmental Quality approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on July 15, 1983 (48 FR 32344); the effective date of 
this program is August 17, 1983. The program consists of the following 
elements as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Wyoming. This incorporation by reference 
was approved by the Director of the Federal Register on June 25, 1984.
    (1) Wyoming Environmental Quality Act, Wyoming Statutes sections 35-
11-101 through 35-11-115, and 35-11-301 through 35-11-305 (1977 
Republished Edition and 1989 Cumm. Supp.);
    (2) Water Quality Rules and Regulations, Wyoming Department of 
Environmental Quality, Chapter III: Regulations for Permit to Construct, 
Install or Modify Public Facilities Capable or, (sic) Causing or 
Contributing to Pollution (certified copy, signed December 21, 1983);
    (3) Water Quality Rules and Regulations, Wyoming Department of 
Environmental Quality, Chapter VIII: Quality Standards for Groundwaters 
of Wyoming (certified copy, signed April 9, 1980);
    (4) Water Quality Rules and Regulations, Wyoming Department of 
Environmental Quality, Chapter IX: Wyoming Groundwater Pollution Control 
Permit (certified copy, signed April 9, 1980);

[[Page 1010]]

    (5) Water Quality Rules and Regulations, Wyoming Department of 
Environmental Quality, Chapter XIII: Prohibitions of Permits for New 
Hazardous Waste Injection Wells (certified copy, signed August 25, 
1989);
    (6) Land Quality Rules and Regulations, Wyoming Department of 
Environmental Quality, Chapter XXI: In Situ Mining (effective March 26, 
1981).
    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for select sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program:
    (1) Article 9, Underground Water, Wyoming Statutes sections 41-3-901 
through 41-3-938 (September 1982);
    (2) Wyoming Administrative Procedure Act, Wyoming Statutes sections 
9-4-101 through 9-4-115 (1988);
    (3) Department of Environmental Quality Rules of Practice and 
Procedure (1982).
    (c)(1) The Memorandum of Agreement between EPA, Region VIII and the 
Wyoming Department of Environmental Quality, signed by the EPA Regional 
Administrator on April 26, 1983.
    (2) Letter from Regional Administrator, EPA Region VIII, to Governor 
of Wyoming, May 21, 1982, with Attachment (regarding aquifer 
exemptions);
    (3) Letter from Governor of Wyoming to Regional Administrator, EPA 
Region VIII, ``Re: Underground Injection Control (UIC) Program--Aquifer 
Exemption Issues,'' June 7, 1982;
    (4) Letter from Regional Administrator, EPA Region VIII to Governor 
of Wyoming, ``Re: Underground Injection Control (UIC) Program--Aquifer 
Exemption Issues,'' June 25, 1982;
    (5) Letter from Director, Wyoming Department of Environmental 
Quality, to Acting Director, Water Management Division, EPA Region VIII, 
December 1, 1982.
    (d) Statement of legal authority. (1) ``Attorney General's 
Statement--Wyoming Statutory and Regulatory Authority for Assumption of 
the Underground Injection Control Program Pursuant to the Federal Safe 
Drinking Water Act,'' signed by Attorney General and Assistant Attorney 
General for the State of Wyoming, September 22, 1982;
    (2) Letter from Attorney General for the State of Wyoming to Acting 
Regional Counsel, EPA Region VIII, ``Re: Wyoming Assumption of the UIC 
Program--$36, Chapter IX, Wyoming Water Quality Rules and Regulations,'' 
November 24, 1982.
    (e) The Program Description and any other materials submitted as 
part of the application or amendment thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43092, Oct. 25, 1988; 56 
FR 9421, Mar. 6, 1991]



Sec.  147.2551  State-administered program--Class II wells.

    The UIC program for Class II wells in the State of Wyoming, except 
those on Indian lands, is the program administered by the Wyoming Oil 
and Gas Conservation Commission approved by EPA pursuant to section 1425 
of the SDWA. Notice of this approval was published in the FR on November 
23, 1982 (47 FR 52434); the effective date of this program is December 
23, 1982. This program consists of the following elements as submitted 
to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Wyoming. This incorporation by reference 
was approved by the Director of the OFR in accordance with 5 U.S.C. 
552(a) and 1 CFR Part 51. Copies may be obtained at the Wyoming Oil and 
Gas Conservation Commission, Office of the State Oil and Gas Supervisor, 
P.O. Box 2640, 77 West First Street, Casper, Wyoming, 82602. Copies may 
be inspected at the Environmental Protection Agency, Region VIII, 999 
18th Street, Suite 500, Denver, Colorado, 80202-2405, or at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Rules and Regulations of the Wyoming Oil and Gas Conservation 
Commission, including Rules of Practice

[[Page 1011]]

and Procedure, as published by the Wyoming Oil and Gas Conservation 
Commission, August 7, 1990;
    (2) Title 30, Chapter 5, Wyoming Statutes, sections 30-5-101 through 
30-5-126 (June 1983 and Wyoming Statutes Annotated, July 1990 Supp.).
    (b) Memorandum of Agreement. (1) The initial Memorandum of Agreement 
between EPA, Region VIII and Wyoming Oil and Gas Conservation 
Commission, signed by the EPA Regional Administrator and the Oil Field 
Supervisor of the Commission on June 2, 1982;
    (2) Amendment No. 1 to the Memorandum of Agreement, dated December 
22, 1982;
    (3) Amendment No. 2 to the Memorandum of Agreement, dated January 
25, 1990;
    (4) Letter from State Oil and Gas Supervisor, Wyoming Oil and Gas 
Conservation Commission, to the Acting Director, Water Management 
Division, EPA Region VIII, ``Re: Application for Primacy in the 
Regulation of Class II Injection Wells,'' March 8, 1982;
    (5) Letter from State Oil and Gas Supervisor, Wyoming Oil and Gas 
Conservation Commission, to EPA Region VIII, ``Re: Regulation of Liquid 
Hydrocarbon Storage Wells Under the UIC Program,'' July 1, 1982;
    (6) Memorandum of Agreement Between the Wyoming State Board of 
Control, State Engineer, Oil and Gas Conservation Commission, and the 
Department of Environmental Quality, dated October 14, 1981.
    (c) Statement of legal authority. (1) ``Statement of Legal 
Authority'' and ``State Review of Regulations and Statutes Relevant to 
the UIC Program-Class II Wells,'' signed by Special Assistant Attorney 
General for the State of Wyoming, as submitted with ``Wyoming Oil and 
Gas Conservation Commission, Application for Primacy in the Regulation 
of Class II Injection Wells under Section 1425 of the Safe Drinking 
Water Act,'' November 1981;
    (2) Letter from special Assistant Attorney General for the State of 
Wyoming to Assistant Regional Counsel, EPA Region VIII, May 13, 1982;
    (3) Letter from special Assistant Attorney General for the State of 
Wyoming to Assistant Regional Counsel, EPA Region VIII, July 1, 1982.
    (d) Program Description. The Program Description and other material 
submitted as part of the application or amendments thereto, including 
the memorandum to the National UIC Branch reporting on Improvement to 
the Wyoming Oil and Gas 1425 program, dated April 28, 1989.

[56 FR 9421, Mar. 6, 1991]



Sec.  147.2553  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the State of Wyoming is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date for the UIC program on Indian 
lands in Wyoming is November 25, 1988.

[53 FR 43092, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



Sec.  147.2554  Aquifer exemptions.

    In accordance with Sec. Sec.  144.7(b) and 146.4 of this chapter, 
those portions of aquifers currently being used for injection in 
connection with Class II (oil and gas) injection operations on the Wind 
River Reservation, which are described below, are hereby exempted for 
the purpose of Class II injection activity. This exemption applies only 
to the aquifers tabulated below, and includes those portions of the 
aquifers defined on the surface by an outer boundary of those quarter-
quarter sections dissected by a line drawn parallel to, but one-quarter 
mile outside, the field boundary, and is restricted to extend no further 
than one-quarter mile outside the Reservation boundary. Maps showing the 
exact boundaries of the field may be consulted at the EPA's Region 8 
Office, and at the EPA Headquarters in Washington, DC.

[[Page 1012]]



            Areas To Be Exempted for the Purpose of Class II Injection on the Wind River Reservation
----------------------------------------------------------------------------------------------------------------
                                                   Approximate
                   Formation                          depth                          Location
----------------------------------------------------------------------------------------------------------------
Steamboat Butte Field
    Phosphoria.................................     6,500-7,100  T3N, R1W--W/2 Sec. 4, Sec. 5, E/2 Sec. 6, NE/4
                                                                  Sec. 8, W/2 Sec. 9.
                                                                 T4N, R1W--W/2 Sec. 29, E/2 Sec. 30, E/2 Sec.
                                                                  31, Sec. 32.
    Tensleep...................................     6,900-7,500  T3N, R1W--W/2 Sec. 4, Sec. 5, E/2 Sec. 6, NE/4
                                                                  Sec. 8, W/2 Sec. 9.
                                                                 T4N, R1W--W/2 Sec. 29, E/2 Sec. 30, E/2 Sec.
                                                                  31, Sec. 32.
Winkleman Dome Field
    Tensleep...................................     2,800-3,300  T2N, R1W--SW/4 Sec. 17, Sections 18, 19, 20,
                                                                  29, NE/4 Sec. 30.
                                                                 T2N, R2W--E/2 Sec. 13, NE/4 Sec. 24.
    Phosphoria.................................     2,800-3,600  T2N, R1W--SW/4 Sec. 17, Sections 18, 19, 20,
                                                                  29, NE/4 Sec. 30.
                                                                 T2N, R2W--E/2 Sec. 13, NE/4 Sec. 24.
    Nugget.....................................     1,100-1,500  T2N, R1W--SW/4 Sec. 17, Sections 18, 19, 20,
                                                                  29, NE/4 Sec. 30.
                                                                 T2N, R2W--E/2 Sec. 13, NE/4 Sec. 24.
Lander Field
    Phosphoria.................................     1,100-3,800  T2S, R1E--Sections 12 and 13, E/2 Sec. 24, NE/4
                                                                  Sec. 25.
                                                                 T2S, R2E--W/2 Sec. 18, W/2 Sec. 19, Sec. 30.
                                                                 T33N, R99W--Sec. 4.
NW Sheldon Field
    Crow Mountain and Cloverly.................     3,400-3,600  T6N, R3W--SE/4 Sec. 35, SW/4 Sec. 36.
                                                                 T5N, R3W--N/2 Sec. 1.
Circle Ridge Field
    Tensleep...................................     1,500-1,800  T6N, R2W--Sec. 6, N/2 Sec. 7.
                                                                 T7N, R3W--SE/4 Sec. 36.
                                                                 T7N, R2W--SW/4 Sec. 31.
                                                                 T6N, R3W--E/2 Sec. 1.
    Phosphoria.................................       800-1,800  T7N, R3W--S/2 Sec. 36.
                                                                 T6N, R3W--NE/4 Sec. 1.
    Amsden.....................................       700-l,200  T6N, R3W--Sec. 6.
Rolff Lake Field
    Crow Mountain..............................     3,500-3,700  T6N, R3W--SW/4 Sec. 26, NW/4 Sec. 27.
----------------------------------------------------------------------------------------------------------------


[53 FR 43092, Oct. 25, 1988]

[[Page 1013]]



Sec.  147.2555  Aquifer exemptions since January 1, 1999.

    In accordance with Sec.  144.7(b) and Sec.  146.4 of this chapter, 
the aquifers described in the following table are hereby exempted from 
the definition of an underground source of drinking water, as defined in 
40 CFR 144.3:

                Aquifer Exemptions Since January 1, 1999
------------------------------------------------------------------------
                                Approximate depth
           Formation               (feet below            Location
                                 ground surface)
------------------------------------------------------------------------
Powder River Basin, only        3,800-6,800......  Two cylindrical
 approximately 0.4 square                           volumes with centers
 miles of the Lance Formation                       in the wells COGEMA
 which is less than 0.005% of                       DW No. 1 and 18-3
 the Basin at indicated depths                      Christensen
 and location..                                     respectively, and
                                                    radius of 1,320
                                                    feet. Both wells are
                                                    located in the
                                                    Christensen Ranch,
                                                    in Johnson County,
                                                    WY. The COGEMA DW
                                                    No. 1 well is
                                                    located at
                                                    approximately 450
                                                    feet West of N/S
                                                    line and 100 feet
                                                    North of E/W line of
                                                    SE/4, NW/4, Section
                                                    7, T44N, R76W. The
                                                    18-3 Christensen
                                                    well is located
                                                    approximately 600
                                                    feet West of N/S
                                                    line and 550 South
                                                    of E/W line of NE/4,
                                                    NW/4, Section 18,
                                                    T44N, R76W.
Lance Formation at indicated    3,800-6,500......  Two cylindrical
 depths and locations.                              volumes with centers
                                                    in the wells COGEMA
                                                    DW No. 2 and COGEMA
                                                    DW No. 3
                                                    respectively, and
                                                    radius of 1320 feet.
                                                    Both wells are
                                                    located in the
                                                    Christensen Ranch,
                                                    in Johnson County
                                                    WY. The COGEMA DW
                                                    No. 2 is located at
                                                    approximately 2,290
                                                    feet from the North
                                                    line and 1130 feet
                                                    from the East line
                                                    SW1/4 SE1/4 NE1/4 of
                                                    Section 7, Township
                                                    44 North, Range 76
                                                    West. The COGEMA DW
                                                    No. 3 is located
                                                    approximately 3300
                                                    feet from the North
                                                    line and 1340 feet
                                                    from the West line
                                                    center of SW1/4 of
                                                    Section 5, Township
                                                    44 North, Range 76
                                                    West.
------------------------------------------------------------------------


[64 FR 14803, Mar. 26, 1999, as amended at 67 FR 47726, July 22, 2002]



                            Subpart AAA_Guam



Sec.  147.2600  State-administered program.

    The UIC program for all classes of wells in the territory of Guam, 
except those on Indian lands, is the program administered by the Guam 
Environmental Protection Agency, approved by EPA pursuant to SDWA 
section 1422. Notice of this approval was published in the Federal 
Register on May 2, 1983 (47 FR 19717); the effective date of this 
program is June 1, 1983. This program consists of the following 
elements, as submitted to EPA in the State's program application:
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the territory of Guam. This incorporation by 
reference was approved by the Director of the Federal Register on June 
25, 1984.
    (1) Water Resources Conservation Act, Government Code of Guam 
sections 57021-57025, Public Law 9-31 (March 9, 1967), as amended by 
Public Law 9-76 (July 29, 1967), as amended by Public Law 12-191 
(December 30, 1974);
    (2) Water Pollution Control Act, Government Code of Guam sections 
57042 and 57045, Public Law 9-76 (July 29, 1967), as amended by Public 
Law 9-212 (August 5, 1968), as amended by Public Law 10-31 (March 10, 
1969), as amended by Public Law 12-191 (December 30, 1974);
    (3) Guam Environmental Protection Agency, Underground Injection 
Control Regulations, Chapters 1-9, as revised by amendments adopted 
September 24, 1982;
    (4) Guam Environmental Protection Agency, Water Quality Standards, 
Section I-IV (approved September 25, 1981, effective November 16, 1981).

[[Page 1014]]

    (b) Other laws. The following statutes and regulations, although not 
incorporated by reference except for specific sections identified in 
paragraph (a) of this section, are also part of the approved State-
administered program:
    (1) Government Code of Guam, Title XXV, Chapters I-III (sections 
24000-24207);
    (2) Government Code of Guam, Title LXI, Chapters I-III (sections 
57000-57051);
    (3) Government Code of Guam, Title LXI, Chapters VI (sections 57120-
57142);
    (4) Government Code of Guam, Title LXI, Chapters VIII (sections 
57170-57188);
    (5) Government Code of Guam, Title LXI, Chapters XII (sections 
57285-57299);
    (c) The Memorandum of Agreement between EPA, Region IX and the Guam 
Environmental Protection Agency signed by the Regional Administrator on 
January 14, 1983.
    (d) Statement of legal authority. (1) Letter from Attorney General 
of Guam to Regional Administrator, Region IX, ``Re: Attorney General's 
Statement for Underground Injection Control Program (UIC), Ground Water 
Program Guidance 16'' May 12, 1982;
    (2) Letter from Attorney General of Guam to Regional Administrator, 
Region IX, ``Re: Additional comments to be incorporated into the May 12, 
1982, Attorney General's Statement for Underground Injection Control 
Program,'' September 2, 1982.
    (e) The Program Description and any other materials submitted as 
part of the application or amendments thereto.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43092, Oct. 25, 1988]



Sec.  147.2601  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for Indian lands in the territory of 
Guam is administered by EPA. This program consists of the UIC program 
requirements of 40 CFR parts 124, 144, 146, 148, and any additional 
requirements set forth in the remainder of this subpart. Injection well 
owners and operators, and EPA shall comply with these requirements.
    (b) Effective date. The effective date for the UIC program on Indian 
lands in the territory of Guam is November 25, 1988.

[53 FR 43093, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



                         Subpart BBB_Puerto Rico



Sec.  147.2650  State-administered program--Class I, II, III, IV, and V wells.

    The Underground Injection Control Program for all classes of wells 
in the Commonwealth of Puerto Rico, other than those on Indian lands, is 
the program administered by Puerto Rico's Environmental Quality Board 
(EQB), approved by the EPA pursuant to the Safe Drinking Water Act 
(SDWA) section 1422. This program consists of the following elements, as 
submitted to EPA in the Commonwealth's program application.
    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the Commonwealth of Puerto Rico. This incorporation 
by reference was approved by the Director of the Federal Register in 
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be 
obtained or inspected at the following locations: EPA, Region II, 26 
Federal Plaza, room 845, New York, NY 10278; EPA, Headquarters, 401 M 
St., SW., room E1101A, Washington, DC 20460; or the National Archives 
and Records Administration (NARA). For information on the availability 
of this material at NARA, call 202-741-6030, or go to: http://
www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (1) Underground Injection Control Regulations of the Commonwealth of 
Puerto Rico, Parts I through V and appendices A and B, adopted September 
14, 1983 (Amended July 20, 1988).
    (2) Puerto Rico Public Policy Environmental Act (PRPPE), Title 12 
Laws of Puerto Rico Annotated (LPRA) Chapters 121 and 131, 1977 edition, 
as amended 1988 edition, and Chapter 122, 1988 edition.

[[Page 1015]]

    (b) Memorandum of Agreement. The Memorandum of Agreement between EPA 
Region II and the Commonwealth of Puerto Rico's EQB signed by the 
Regional Administrator on August 23, 1991.
    (c) Statement of legal authority. (1) Attorney General's statement 
on the Commonwealth of Puerto Rico's Authority to apply for, assume and 
carry out the UIC Program, dated June 26, 1987. (2) Letter from the 
Governor of the Commonwealth of Puerto Rico requesting the program, 
dated July 16, 1987.
    (d) Program description. The Description of the Commonwealth of 
Puerto Rico's Underground Injection Control Program, dated with the 
effective date October 30, 1986.

[57 FR 33446, July 29, 1992]



Sec.  147.2651  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in the Commonwealth of Puerto Rico is administered by EPA. This 
program consists of the UIC program requirements of 40 CFR parts 124, 
144, 146, 148 and any additional requirements set forth in the remainder 
of this subpart. Injection well owners and operators and EPA shall 
comply with the requirements.
    (b) Effective date. The effective date for the UIC program on Indian 
Lands in the Commonwealth of Puerto Rico is November 25, 1988.

[57 FR 33446, July 29, 1992]



                       Subpart CCC_Virgin Islands



Sec.  147.2700  State-administered program. [Reserved]



Sec.  147.2701  EPA-administered program.

    (a) Contents. The UIC program for the Virgin Islands, including all 
Indian lands, is administered by EPA. This program consists of the UIC 
program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date of the UIC program for non-
Indian lands in the Virgin Islands is December 30, 1984. The effective 
date for Indian lands in the Virgin Islands is November 25, 1988.

[53 FR 43093, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



                       Subpart DDD_American Samoa



Sec.  147.2750  State-administered program. [Reserved]



Sec.  147.2751  EPA-administered program.

    (a) Contents. The UIC program for American Samoa, including all 
Indian lands, is administered by EPA. This program consists of the UIC 
program requirements of 40 CFR parts 124, 144, 146, 148, and any 
additional requirements set forth in the remainder of this subpart. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective dates. The effective date for the UIC program on non-
Indian lands is June 25, 1984. The effective date of the UIC program on 
Indian lands is November 25, 1988.

[53 FR 43093, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



Sec.  147.2752  Aquifer exemptions. [Reserved]



        Subpart EEE_Commonwealth of the Northern Mariana Islands



Sec.  147.2800  State-administered program--Class I, II, III, IV, and V wells.

    The UIC program for Class I, II, III, IV, and V wells in the 
Commonwealth of the Northern Mariana Islands, other than those on Indian 
lands, is the program administered by the Commonwealth of the Northern 
Mariana Islands Division of Environmental Quality approved by EPA 
pursuant to Section 1422 of the SDWA. Notice of this approval was 
published in the Federal Register on January 18, 1985; the effective 
date of this program is August 30, 1985. This program consists of the 
following elements, as submitted to EPA in the State's program 
application.

[[Page 1016]]

    (a) Incorporation by reference. The requirements set forth in the 
State statutes and regulations cited in this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the Commonwealth of the Northern Mariana Islands. 
This incorporation by reference was approved by the Director of the 
Federal Register effective July 31, 1985.
    (1) CNMI Environmental Protection Act, 2 CMC sections 3101, et seq. 
(1984);
    (2) CNMI Coastal Resources Management Act, 2 CMC sections 1501, et 
seq. (1984);
    (3) CNMI Drinking Water Regulations, Commonwealth Register, Volume 
4, Number 4 (August 15, 1982);
    (4) CNMI Underground Injection Control Regulations, Commonwealth 
Register, Volume 6, Number 5 (May 15, 1984, amended November 15, 1984, 
January 15, 1985);
    (5) CNMI Coastal Resources Management Regulations, Commonwealth 
Register, Volume 6, Number 12, December 17, 1984.
    (b)(1) The Memorandum of Agreement between EPA Region IX and the 
Commonwealth of the Northern Mariana Islands Division of Environmental 
Quality, signed by the EPA Regional Administrator on May 3, 1985;
    (c) Statement of legal authority. Statement from Attorney General 
Commonwealth of the Northern Mariana Islands, ``Underground Injection 
Control Program--Attorney General's Statement,'' signed on October 10, 
1984.
    (d) The Program Description and any other materials submitted as 
part of the original application or as supplements thereto.

[50 FR 28943, July 17, 1985]



Sec.  147.2801  EPA-administered program.

    (a) Contents. The UIC program for Indian lands in the Commonwealth 
of the Northern Mariana Islands is administered by EPA. This program 
consists of the UIC program requirements of 40 CFR parts 124, 144, 146, 
148, and any additional requirements set forth in the remainder of this 
subpart. Injection well owners and operators, and EPA shall comply with 
these requirements.
    (b) Effective date. The effective date of the UIC program for Indian 
lands is November 25, 1988.

[53 FR 43093, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



Sec.  147.2802  Aquifer exemptions. [Reserved]



           Subpart FFF_Trust Territory of the Pacific Islands



Sec.  147.2850  State-administered program. [Reserved]



Sec.  147.2851  EPA-administered program.

    (a) Contents. The UIC program for Trust Territory of the Pacific 
Islands, including all Indian lands, is administered by EPA. This 
program consists of the UIC program requirements of 40 CFR parts 124, 
144, 146, 148, and any additional requirements set forth in the 
remainder of this subpart. Injection well owners and operators, and EPA 
shall comply with these requirements.
    (b) Effective dates. The effective date of the UIC program for non-
Indian lands of the Trust Territory of the Pacific Islands is June 25, 
1984. The effective date for the Indian lands is November 25, 1988.

[53 FR 43093, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



Sec.  147.2852  Aquifer exemptions. [Reserved]



            Subpart GGG_Osage Mineral Reserve_Class II Wells

    Authority: Safe Drinking Water Act, 42 U.S.C. 300h.

    Source: 49 FR 45309, Nov. 15, 1984, unless otherwise noted.



Sec.  147.2901  Applicability and scope.

    This subpart sets forth the rules and permitting requirements for 
the Osage Mineral Reserve, Osage County, Oklahoma, Underground Injection 
Control Program. The regulations apply to owners and operators of Class 
II injection wells located on the Reserve, and to EPA.

[[Page 1017]]



Sec.  147.2902  Definitions.

    Most of the following terms are defined in Sec.  144.3, and have 
simply been reproduced here for the convenience of the reader. This 
section also includes definitions of some terms unique to the Osage 
program. Terms used in this subpart are defined as follows:
    Administrator--the Administrator of the United States Environmental 
Protection Agency, or an authorized representative.
    Aquifer--a geologic formation, group of formations, or part of a 
formation that is capable of yielding a significant amount of water to a 
well or spring.
    BIA--The ``Bureau of Indian Affairs,'' United States Department of 
Interior.
    Casing--a pipe or tubing of varying diameter and weight, lowered 
into a borehole during or after drilling in order to support the sides 
of the hole and, thus, prevent the walls from caving, to prevent loss of 
drilling mud into porous ground, or to prevent water, gas, or other 
fluid from entering the hole.
    Cementing--the operation whereby a cement slurry is pumped into a 
drilled hole and/or forced behind the casing.
    Class II Wells--wells which inject fluids:
    (a) Which are brought to the surface in connection with conventional 
oil or natural gas production and may be commingled with waste waters 
from gas plants which are an integral part of production operations, 
unless those waters would be classified as a hazardous waste at the time 
of injection;
    (b) For enhanced recovery of oil or natural gas; and
    (c) For storage of hydrocarbons which are liquid at standard 
temperature and pressure.
    Existing Class II Wells--wells that were authorized by BIA and 
constructed and completed before the effective date of this program.
    New Class II Wells--wells constructed or converted after the 
effective date of this program, or which are under construction on the 
effective date of this program.
    Confining bed--a body of impermeable or distinctly less permeable 
material stratigraphically adjacent to one or more aquifers.
    Confining zone--a geologic formation, group of formations, or part 
of a formation that is capable of limiting fluid movement above an 
injection zone.
    Contaminant--any physical, chemical, biological, or radiological 
substance or matter in water.
    Disposal well--a well used for the disposal of waste into a 
subsurface stratum.
    EPA--The United States Environmental Protection Agency.
    Fault--a surface or zone of rock fracture along which there has been 
displacement.
    Fluid--material or substance which moves or flows whether in a 
semisolid, liquid, sludge, gas or any other form or state.
    Formation--a body of rock characterized by a degree of lithologic 
homogeneity which is prevailingly, but not necessarily, tabular and is 
mappable on the earth's surface or traceable in the subsurface.
    Freshwater--``Underground source of drinking water.''
    Ground water--water below the land surface in a zone of saturation.
    Injection well--a well into which fluids are being injected.
    Injection zone--a geological formation, group of formations, or part 
of a formation receiving fluids through a well.
    Lithology--the description of rocks on the basis of their physical 
and chemical characteristics.
    Owner/operator--the owner or operator of any facility or activity 
subject to regulation under the Osage UIC program.
    Packer--a device lowered into a well to produce a fluid-tight seal 
within the casing.
    Permit--an authorization issued by EPA to implement UIC program 
requirements. Permit does not include the UIC authorization by rule or 
any permit which has not yet been the subject of final Agency action.
    Plugging--the act or process of stopping the flow of water, oil or 
gas into or out of a formation through a borehole or well penetrating 
that formation.
    Pressure--the total load or force per unit area acting on a surface.

[[Page 1018]]

    Regional Administrator--the Regional Administrator of Region 6 of 
the United States Environmental Protection Agency, or an authorized 
representative.
    Subsidence-- the lowering of the natural land surface in response 
to: Earth movements; lowering of fluid pressure; removal of underlying 
supporting material by mining or solution solids, either artificially or 
from natural causes; compaction due to wetting (hydrocompaction); 
oxidation of organic matter in soils; or added load on the land surface.
    Underground source of drinking water-- an aquifer or its portion:
    (a)(1) Which supplies any public water system; or
    (2) Which contains a sufficient quantity of ground water to supply a 
public water system; and
    (i) Currently supplies drinking water for human consumption; or
    (ii) Contains fewer than 10,000 mg/1 total dissolved solids; and
    (b) Which is not an exempted aquifer.
    USDW--underground source of drinking water.
    Well--a bored, drilled, or driven shaft, or a dug hole whose depth 
is greater than the largest surface dimension.
    Well injection--the subsurfac emplacement of fluids through a bored, 
drilled, or driven well; or through a dug well, where the depth of the 
dug well is greater than the largest surface dimension.
    Well workover--any reentry of an injection well; including, but not 
limited to, the pulling of tubular goods, cementing or casing repairs; 
and excluding any routine maintenance (e.g. re-seating the packer at the 
same depth, or repairs to surface equipment).



Sec.  147.2903  Prohibition of unauthorized injection.

    (a) Any underground injection, except as authorized by permit or 
rule issued under the UIC program, is prohibited. The construction or 
operation of any well required to have a permit is prohibited until the 
permit has been issued.
    (b) No owner or operator shall construct, operate, maintain, 
convert, plug, or abandon any injection well, or conduct any other 
injection activity, in a manner that allows the movement of fluid 
containing any contaminant into underground sources of drinking water, 
if the presence of that contaminant may cause the violation of any 
primary drinking water regulation under 40 CFR part 142 or may otherwise 
adversely affect the health of persons. The applicant for a permit shall 
have the burden of showing that the requirements of this paragraph are 
met.
    (c) Injection between the outermost casing protecting underground 
sources of drinking water and the well bore is prohibited.



Sec.  147.2904  Area of review.

    (a) The area of review for an injection well or project will be a 
fixed radius of one-forth of a mile from the well, field or project.
    (b) The zone of endangering influence is the lateral area around the 
injection well or project in which the injection zone pressures may 
cause movement of fluid into an underground source of drinking water 
(USDW) if there are improperly sealed, completed or abandoned wells 
present. A zone of endangering influence may be determined by EPA 
through the use of an appropriate formula that addresses the relevant 
geologic, hydrologic, engineering and operational features of the well, 
field, or project.



Sec.  147.2905  Plugging and abandonment.

    The owner/operator shall notify the Osage UIC office within 30 days 
of the date injection has terminated. The well must be plugged within 1 
year after termination of injection. The Regional Administrator may 
extend the time to plug, but only if no fluid movement into a USDW will 
occur, and the operator has presented a viable plan for utilizing the 
well within a reasonable time.
    (a) Until an injection well has been properly plugged and abandoned, 
annual reports to the Regional Administrator on well status, and 
mechanical integrity tests as outlined in Sec. Sec.  147.2912 and 
147.2920 will be required, whether or not injection has ceased.
    (b) All wells shall be plugged to prevent movement of fluid into an 
USDW.
    (c) The owner/operator shall notify the Osage UIC office by 
certified mail

[[Page 1019]]

at least 5 days prior to the commencement of plugging operations. The 
Osage UIC office may waive or reduce the 5-day notice requirement when a 
qualified EPA representative is available to witness the plugging 
operation. The following information must be submitted as part of the 
notification:
    (1) Type and number of plugs to be used;
    (2) Elevation of top and bottom of each plug;
    (3) Method of plug placement; and
    (4) Type, grade and quantity of cement to be used.
    (d) The well shall be kept full of mud as casing is removed. No 
surface casing shall be removed without written approval from the 
Regional Administrator.
    (e)(1) If surface casing is adequately set and cemented through all 
freshwater zones (set to at least 50 feet below the base of freshwater), 
a plug shall be set at least 50 feet below the shoe of the casing and 
extending at least 50 feet above the shoe of the casing, or
    (2) If the surface casing and cementing is inadequate, the well bore 
shall be filled with cement from a point 50 feet below the base of fresh 
water to a point 50 feet above the shoe of the surface casing, and any 
additional plugs as required by the Osage UIC office and/or the Osage 
Agency.
    (3) In all cases, the top 20 feet of the well bore below 3 feet of 
ground surface shall be filled with cement. Surface casing shall be cut 
off 3 feet below ground surface and covered with a secure steel cap on 
top of the surface pipe. The remaining 3 feet shall be filled with dirt.
    (f)(1) Except as provided in paragraph (f)(2) of this section, each 
producing or receiving formation shall be sealed off with a 50-foot 
cement plug placed at the base of the formation and a 50-foot cement 
plug placed at the top of the formation.
    (2) The requirement in paragraph (f)(1) of this section does not 
apply if the producing/receiving formation is already sealed off from 
the well bore with adequate casing and cementing behind casing, and 
casing is not to be removed, or the only openings from the producing/
receiving formation into the well bore are perforations in the casing, 
and the annulus between the casing and the outer walls of the well is 
filled with cement for a distance of 50 feet below the base of the 
formation and 50 feet above the top of the formation. When such 
conditions exist, a bridge plug capped with 10 feet of cement set at the 
top of the producing formation may be used.
    (g) When specified by the Osage UIC office, any uncased hole below 
the shoe of any casing to be left in the well shall be filled with 
cement to a depth of at least 50 feet below the casing shoe, or the 
bottom of the hole, and the casing above the shoe shall be filled with 
cement to at least 50 feet above the shoe of the casing. If the well has 
a screen or liner which is not to be removed, the well bore shall be 
filled with cement from the base of the screen or liner to at least 50 
feet above the top of the screen or liner.
    (h) All intervals between cement plugs in the well bore shall be 
filled with mud.
    (i) A report containing copies of the cementing tickets shall be 
submitted to BIA within 10 days of plugging completion.
    (j) A surety bond must be on file with the Bureau of Indian Affairs 
(BIA), and shall not be released until the well has been properly 
plugged and the Regional Administrator has agreed to the release of the 
bond.



Sec.  147.2906  Emergency permits.

    (a) An emergency permit may be issued if:
    (1) There will be an imminent health hazard unless an emergency 
permit is issued; or
    (2) There will be a substantial and irretrievable loss of oil and 
gas resources, timely application for a permit could not practicably 
have been made, and injection will not result in movement of fluid into 
an USDW; or
    (3) There will be a substantial delay in oil or gas production, and 
injection will not result in movement of fluid into an USDW.
    (b) Requirements--(1) Permit duration. (i) Emergency permits issued 
to avoid an imminent health threat may last no longer than the time 
necessary to prevent the hazard.

[[Page 1020]]

    (ii) Emergency permits issued to prevent a substantial and 
irretrievable loss of oil or gas resources shall be for no longer than 
90 days, unless a complete permit application has been submitted during 
that time; in which case the emergency permit may be extended until a 
final decision on the permit application has been made.
    (iii) Emergency permits to avoid a substantial delay in oil or gas 
production shall be issued only after a complete permit application has 
been submitted and shall be effective until a final decision on the 
permit application is made.
    (2) Notice of the emergency permit will be given by the Regional 
Administrator according to the notice procedure for a draft permit 
within 10 days after issuance.
    (3) An emergency permit may be oral or written. If oral, a written 
emergency permit must be issued within five calendar days.



Sec.  147.2907  Confidentiality of information.

    (a) The following information cannot be claimed confidential by the 
submitter:
    (1) Name and address of permit applicant or permittee.
    (2) Information concerning the existence, absence or level of 
contaminants in drinking water.
    (b) Other information claimed as confidential will be processed in 
accordance with 40 CFR part 2.



Sec.  147.2908  Aquifer exemptions.

    (a) After notice and opportunity for a public hearing, the 
Administrator may designate any aquifer or part of an aquifer as an 
exempted aquifer.
    (b) An aquifer or its portion that meets the definition of a USDW 
may be exempted by EPA from USDW status if the following conditions are 
met:
    (1) It does not currently serve as a source of drinking water, and
    (2) It cannot now and will not in the future serve as a source of 
drinking water because:
    (i) It is hydrocarbon producing, or can be demonstrated by a permit 
applicant as a part of a permit application for a Class II operation to 
contain hydrocarbons that are expected to be commercially producible 
(based on historical production or geologic information); or
    (ii) It is situated at a depth or location which makes recovery of 
water for drinking water purposes economically or technologically 
impractical; or
    (iii) It is so contaminated that it would be economically or 
technologically impractical to render that water fit for human 
consumption; or
    (3) The Total Dissolved Solids content of the groundwater is more 
than 3,000 and less than 10,000 mg/1 and it is not reasonably expected 
to supply a public water system.



Sec.  147.2909  Authorization of existing wells by rule.

    All existing Class II injection wells (wells authorized by BIA and 
constructed or completed on or before the effective date of the Osage 
UIC program) are hereby authorized. Owners or operators of wells 
authorized by rule must comply with the provisions of Sec. Sec.  
147.2903, 147.2905, 147.2907, and 147.2910 through 147.2915.



Sec.  147.2910  Duration of authorization by rule.

    Existing Class II injuction wells are authorized for the life of the 
well, subject to the obligation to obtain a permit if specifically 
required by the Regional Administrator pursuant to Sec.  147.2915.



Sec.  147.2911  Construction requirements for wells authorized by rule.

    All Class II wells shall be cased and cemented to prevent movement 
of fluids into USDWs. The Regional Administrator shall review inventory 
information, data submitted in permit applications, and other records, 
to determine the adequacy of construction (completion) or existing 
injection wells. At the Regional Administrator's discretion, well casing 
and cementing may be considered adequate if it meets the BIA 
requirements that were in effect at the time of construction 
(completion) and will not result in movement of fluid into an USDW. If 
the Regional Administrator determines that the construction of a well 
authorized by rule is inadequate, he shall require a permit, or he shall 
notify the owner/

[[Page 1021]]

operator and the owner/operator shall correct the problem according to 
instructions from the Regional Administrator. All corrections must be 
completed within one year of owner/operator notification of 
inadequacies.



Sec.  147.2912  Operating requirements for wells authorized by rule.

    (a) Each well authorized by rule must have mechanical integrity. 
Mechanical integrity must be demonstrated within five years of program 
adoption. The Regional Administrator will notify the well owner/operator 
three months before proof of mechanical integrity must be submitted to 
EPA. The owner/operator must contact the Osage UIC office at least five 
days prior to testing. The owner/operator may perform the mechanical 
integrity test prior to receiving notice from the Regional 
Administrator, provided the Osage UIC office is notified at least five 
days in advance. Conditions of both paragraphs (a)(1) and (a)(2) of this 
section must be met.
    (1) There is no significant leak in the casing, tubing or packer. 
This may be shown by the following:
    (i) Performance of a pressure test of the casing/tubing annulus to 
at least 200 psi, or the pressure specified by the Regional 
Administrator, to be repeated thereafter, at five year intervals, for 
the life of the well (pressure tests conducted during well operation 
shall maintain an injection/annulus pressure differential of at least 
100 psi through the tubing length); or
    (ii) Maintaining a positive gauge pressure on the casing/tubing 
annulus (filled with liquid) and monitoring the pressure monthly and 
reporting of the pressure information annually; or
    (iii) Radioactive tracer survey; or
    (iv) For enhanced recovery wells, records of monitoring showing the 
absence of significant changes in the relationship between injection 
pressure and injection flow rate at the well head, following an initial 
pressure test as described by paragraph (a)(1)(i) or (v) of this 
section; or
    (v) Testing or monitoring programs approved by the Regional 
Administrator on a case-by-case basis, and
    (2) There is no significant fluid movement into a USDW through 
vertical channels adjacent to the well bore. This may be shown by any of 
the following:
    (i) Cementing records (need not be reviewed every five years);
    (ii) Tracer survey (in appropriate hydrogeologic settings; must be 
used in conjunction with at least one of the other alternatives);
    (iii) Temperature log;
    (iv) Noise log; or
    (v) Other tests deemed acceptable by the Regional Administrator.
    (b) Injection pressure at the wellhead shall be limited so that it 
does not initiate new fractures or propagate existing fractures in the 
confining zone adjacent to any UDSW.
    (1) For existing Class II salt water disposal wells, The owner/
operator shall, except during well stimulation, use an injection 
pressure at the wellhead no greater than the pressure calculated by 
using the following formula:

Pm = (0.75-0.433Sg)d

where:

Pm = injection pressure at the wellhead in pounds per square inch
Sg = specific gravity of injected fluid (unitless)
d = injection depth in feet.


Owner/operator of wells shall comply with the above injection pressure 
limits no later than one year after the effective date of this 
regulation.
    (2) For existing Class II enhanced recovery wells, the owner or 
operator:
    (i) Shall use an injection pressure no greater than the pressure 
established by the Regional Administrator for the field or formation in 
which the well is located. The Regional Administrator shall establish 
such a maximum pressure after notice, opportunity for comment, and 
opportunity for a public hearing according to the provisions of part 
124, subpart A of this chapter, and will inform owners and operators in 
writing of the applicable maximum pressure.
    (ii) Prior to such time as the Regional Administrator establishes 
rules for maximum injection pressures based on data provided pursuant to 
paragraph (b)(2)(ii)(B) of this section the owner/operator shall:

[[Page 1022]]

    (A) Limit injection pressure at the wellhead to a value which will 
not initiate new fractures or propagate existing fractures in the 
confining zone adjacent to any USDW; and
    (B) Submit data acceptable to the Regional Administrator which 
defines the fracture pressure of the formation in which injection is 
taking place. A single test may be submitted on behalf of two or more 
operators conducting operations in the same formation, if the Regional 
Administrator approves such submission. The data shall be submitted to 
the Regional Administrator within one year of the effective date of this 
program.
    (c) Injection wells or projects which have exhibited failure to 
confine injected fluids to the authorized injection zone or zones may be 
subject to restriction of injection volume and pressure, or shut-down, 
until the failure has been identified and corrected.

(The information collection requirements contained in paragraphs (a)(1) 
(ii) through (v) and (a)(2) (i) through (v) were approved by the Office 
of Management and Budget under control number 2040-0042)



Sec.  147.2913  Monitoring and reporting requirements for wells 
authorized by rule.

    (a) The owner/operator has the duty to submit inventory information 
to the Regional Administrator upon request. Such request may be a 
general request to all operators in the County (e.g., public notice, or 
mailout requesting verification of information).
    (b) The operator shall monitor the injection pressure (psi) and rate 
(bb1/day) at least monthly, with the results reported annually. The 
annual report shall specify the types of methods used to generate the 
monitoring data.
    (c) The owner/operator shall notify the Osage UIC office within 30 
days of any mechanical failure or down-hole problems involving well 
integrity, well workovers, or any noncompliance. As required, operators 
must apply for and obtain a workover permit from the Bureau of Indian 
Affairs Osage Agency before reentering an injection well. If the 
condition may endanger an USDW, the owner/operator shall notify the 
Osage UIC office orally within 24 hours, with written notice including 
plans for testing and/or repair to be submitted within five days. If all 
the information is not available within five days, a followup report 
must be submitted within 30 days.
    (d) The owner/operator shall determine the nature of injected fluids 
initially, when the nature of injected fluids is changed or when new 
constituents are added. The records should reflect the source of 
character of the new fluid and the date changes were made.
    (e) The owner/operator shall retain all monitoring records for three 
years, unless an enforcement action is pending, and then until three 
years after the enforcement action has been resolved.

(Approved by the Office of Management and Budget under control number 
2040-0042)



Sec.  147.2914  Corrective action for wells authorized by rule.

    Based on the Regional Administrator's discretion, corrective action 
to prevent movement of fluid into an USDW may be required for improperly 
sealed, completed or abandoned wells (i.e., wells or well bores which 
may provide and avenue for fluid migration into a USDW) within the zone 
of endangering influence (as defined in Sec.  147.2904, Area of Review) 
of an injection well authorized by rule.
    (a) EPA will notify the operator when corrective action is required. 
Corrective action may include:
    (1) Well modifications:
    (i) Recementing;
    (ii) Workover;
    (iii) Reconditioning;
    (iv) Plugging or replugging;
    (2) Limitations on injection pressure to prevent movement of fluid 
into an USDW;
    (3) A more stringent monitoring program; and/or
    (4) Periodic testing of other wells to determine if significant 
movement of fluid has occurred.
    (b) If the monitoring discussed in paragraph (a) (3) or (4) of this 
section indicate the potential endangerment of an USDW, then action as 
described in paragraph (a) (1) or (2) of this section must be taken.

[[Page 1023]]



Sec.  147.2915  Requiring a permit for wells authorized by rule.

    (a) The Regional Administrator may require the owner or operator of 
any well authorized by rule to apply for an individual or area permit. 
The Regional Administrator shall notify the owner/operator in writing 
that a permit application is required. The notice shall contain:
    (1) Explanation of need for application;
    (2) Application form and, if appropriate, a list of additional 
information to be submitted; and
    (3) Deadline for application submission.
    (b) Cases in which the Regional Administrator may require a permit 
include:
    (1) The owner or operator is not in compliance with provisions of 
the rule;
    (2) Injection well is no longer within the category of wells 
authorized by rule;
    (3) Protection of USDWs requires that the injection operation be 
regulated by requirements which are not contained in the rule; or
    (4) Discretion of Regional Administrator.
    (c) Injection is no longer authorized by rule upon the effective 
date of a permit or permit denial, or upon failure of the owner/operator 
to submit an application in a timely manner as specified in the notice 
described in paragraph (a) of this section.
    (d) Any owner/operator authorized by rule may request to be excluded 
from the coverage of the rules by applying for an individual or area UIC 
permit.



Sec.  147.2916  Coverage of permitting requirements.

    The owner or operator of a new Class II injection well or any other 
Class II well required to have a permit in the Osage Mineral Reserve 
shall comply with the requirements of Sec. Sec.  147.2903, 147.2907, 
147.2918, through 147.2928.



Sec.  147.2917  Duration of permits.

    Unless otherwise specified in the permit, the permits will be in 
effect until the well is plugged and abandoned or the permit terminated. 
The Regional Administrator will review each issued permit at least once 
every five years to determine whether it should be modified or 
terminated.



Sec.  147.2918  Permit application information.

    (a) The owner/operator must submit the original and three copies of 
the permit application, with two complete sets of attachments, to the 
Osage UIC office. The application should be signed by the owner/operator 
or a duly authorized representative. The application should also include 
appropriate forms (i.e., BIA's Application for Operation or Report on 
Wells and EPA's permit application). The applicant has the burden of 
proof to show that the proposed injection activities will not endanger 
USDWs.
    (b) The application shall include the information listed below. 
Information required by paragraphs (b) (5), (7), or (9) of this section 
that is contained in EPA or BIA files may be included in the application 
by reference.
    (1) Map using township-range sections showing the area of review and 
identifying all wells of public record penetrating the injection 
interval.
    (2) Tabulation of data on the wells identified in paragraph (b)(1) 
of this section, including location, depth, date drilled, and record of 
plugging and/or completion.
    (3) Operating data:
    (i) Maximum and average injection rate;
    (ii) Maximum and average injection pressure;
    (iii) Whether operation is on cyclic or continuous operation basis; 
and
    (iv) Source and appropriate analysis of injected fluids, including 
total dissolved solids, chlorides, and additives.
    (4) Geologic data on the injection and confining zones, including 
faults, geological name, thickness permeability, depth and lithologic 
description.
    (5) Depth to base of fresh water.
    (6) Schematic drawings of the surface and subsurface details of the 
well, showing:
    (i) Total depth or plug-back depth;
    (ii) Depth to top and bottom of injection interval;
    (iii) Depths to tops and bottoms of casing and cemented intervals, 
and amount of cement to be used;

[[Page 1024]]

    (iv) Size of casing and tubing, and depth of packer; and
    (v) Hole diameter.
    (7) Proof that surety bond has been filed with the BIA 
Superintendent in accordance with 25 CFR 226.6. A surety bond must be 
maintained until the well has been properly plugged.
    (8) Verification of public notice, consisting of a list showing the 
names, addresses, and date that notice of permit application was given 
or sent to:
    (i) The surface land owner;
    (ii) Tenants on land where injection well is located or proposed to 
be located; and
    (iii) Each operator of a producing lease within one-half mile of the 
well location.
    (9) All available logging and testing data on the well (for existing 
wells, i.e., wells to be converted or wells previously authorized by 
rule).

(Approved by the Office of Management and Budget under control number 
2040-0042)



Sec.  147.2919  Construction requirements for wells authorized by permit.

    (a) All Class II wells shall be sited so that they inject into a 
formation that is separated from any USDW by a confining zone free of 
known open faults or fractures within the area of review.
    (b) All Class II wells shall be cased and cemented to prevent 
movement of fluids into or between USDWs. Requirements shall be based on 
the depth to base of fresh water, and the depth to the injection zone. 
Newly drilled Class II wells must have surface casing set and cemented 
to at least 50 feet below the base of fresh water, or the equivalent 
(e.g., long string cemented to surface). At the Regional Administrator's 
discretion, the casing and cementing of wells to be converted may be 
considered adequate if they meet the BIA requirements that were in 
effect at the time of construction (completion), and will not result in 
movement of fluid into a USDW.
    (c) Owner/operators shall provide a standard female fitting with 
cut-off valves, connected to the tubing and the tubing/casing annulus so 
that the injection pressure and annulus pressure may be measured by an 
EPA representative by attaching a gauge having a standard male fitting.
    (d) No owner or operator may begin construction of a new well until 
a permit authorizing such construction has been issued, unless such 
construction is otherwise authorized by an area permit.



Sec.  147.2920  Operating requirements for wells authorized by permit.

    (a) For new Class II wells, injection shall be through adequate 
tubing and packer. Packer shall be run on the tubing and set inside the 
casing within 75 feet of the top of the injection interval. For existing 
Class II, wells, injection shall be through adequate tubing and packer, 
or according to alternative operating requirements approved by the 
Regional Administrator, as necessary to prevent the movement of fluid 
into a USDW.
    (b) Each well must have mechanical integrity. Mechanical integrity 
of the injection well must be shown prior to operation. The owner/
operator must notify the Osage UIC office at least five days prior to 
mechanical integrity testing. Conditions of both paragraphs (b) (1) and 
(2) of this section must be met.
    (1) There is no significant leak in the casing, tubing or packer. 
This may be shown by the following:
    (i) Performance of a pressure test of the casing/tubing annulus to 
at least 200 psi, or the pressure specified by the Regional 
Administrator, to be repeated thereafter, at five year intervals, for 
the life of the well (Pressure tests conducted during well operation 
shall maintain an injection/annulus pressure differential of at least 
100 psi throughout the tubing length); or
    (ii) Maintaining a positive gauge pressure on the casing/tubing 
annulus (filled with liquid) and monitoring the pressure monthly and 
reporting of the pressure information annually; or
    (iii) Radioactive tracer survey; or
    (iv) For enhanced recovery wells, record of monitoring showing the 
absence of significant changes in the relationship between injection 
pressure and injection flow rate at the wellhead, following an initial 
pressure test as described by paragraph (b)(1) (i) or (v) of this 
section; or

[[Page 1025]]

    (v) Testing or monitoring programs approved by the Administrator on 
a case-by-case basis, and
    (2) There is no significant fluid movement into a USDW through 
vertical channels adjacent to the well bore. This may be shown by any of 
the following:
    (i) Cementing records (need not be reviewed every five years);
    (ii) Tracer survey (in appropriate hydrogelogic settings; must be 
used in conjunction with at least one of the other alternatives);
    (iii) Temperature log;
    (iv) Noise log; or
    (v) Other tests deemed acceptable by the Administrator.
    (c) Injection pressure at the wellhead shall be limited so that it 
does not initiate new fractures or propagate existing fractures in the 
confining zone adjacent to any UDSW.
    (d) Injection wells or projects which have exhibited failure to 
confine injected fluids to the authorized injection zone or zones may be 
subject to restriction of injected volume and pressure or shut-in, until 
the failure has been identified and corrected.
    (e) Operation shall not commence until proof has been submitted to 
the Regional Administrator, or an EPA representative has witnessed that 
any corrective action specified in the permit has been completed.



Sec.  147.2921  Schedule of compliance.

    The permit may, when appropriate, specify a schedule of compliance 
leading to compliance with the Safe Drinking Water Act and the Osage UIC 
regulations.
    (a) Any schedule of compliance shall require compliance as soon as 
possible, and in no case later than three years after the effective date 
of the permit.
    (b) If a permit establishes a schedule of compliance which exceeds 
one year from the date of permit issuance, the schedule shall set forth 
interim requirements and the dates for their achievement.
    (1) The time between interim dates shall not exceed one year.
    (2) If the time necessary for completion of any interim requirement 
is more than 1 year and is not readily divisible into stages for 
completion, the permit shall specify interim dates for the submission of 
reports of progress toward completion of the interim requirements and 
indicate a projected completion date.
    (c) The permit shall be written to require that if a schedule of 
compliance is applicable, progress reports be submitted no later than 30 
days following each interim date and the final date of compliance.



Sec.  147.2922  Monitoring and reporting requirements for wells 
authorized by permit.

    (a) The owner/operator shall notify the Osage UIC office within 30 
days of the date on which injection commenced.
    (b) The operator shall monitor the injection pressure (psi) and rate 
(bbl/day) at least monthly, with the results reported annually. The 
annual reports shall specify the types or methods used to generate the 
monitoring data.
    (c) The owner/operator shall notify the Osage UIC office within 30 
days of any mechanical failure or down-hole problems involving well 
integrity, well workovers, or any noncompliance. (Operators should note 
the obligation to apply for and obtain a workover permit from the Bureau 
of Indian Affairs Osage Agency before reentering an injection well.) If 
the condition may endanger an USDW, the owner/operator shall notify the 
Osage UIC officer orally within 24 hours, with written notice including 
plans for testing and/or repair to be submitted within five days. If all 
the information is not available within five days, a followup report 
must be submitted within 30 days.
    (d) The owner/operator shall retain all monitoring records for three 
years, unless an enforcement action is pending, and then until three 
years after the enforcement action has been resolved.
    (e) The owner/operator shall notify the Osage UIC office in writing 
of a transfer of ownership at least 10 days prior to such transfer.

(Approved by the Office of Management and Budget under control number 
2040-0042)

[[Page 1026]]



Sec.  147.2923  Corrective action for wells authorized by permit.

    All improperly sealed, completed or abandoned wells (i.e., wells or 
well bores which may provide an avenue for movement of fluid into an 
UDSW) within the zone of endangering influence (as defined in Sec.  
147.2904, Area of Review) that penetrate the injection zone of a Class 
II well, must have corrective action taken to prevent movement of fluid 
into a USDW.
    (a) EPA will review completion and plugging records of wells within 
the zone of endangering influence that penetrate the injection zone and 
will notify the operator when corrective action is required. Corrective 
action may include:
    (1) Well modifications, including:
    (i) Recementing;
    (ii) Workover;
    (iii) Reconditioning; and/or
    (iv) Plugging or replugging;
    (2) Permit conditions to limit injection pressure so as to prevent 
movement of fluid into a USDW;
    (3) A more stringent monitoring program; and/or
    (4) Periodic testing of other wells within the area of review to 
determine if significant movement of fluid has occurred. If the 
monitoring discussed in paragraph (a)(3) or (a)(4) of this section 
indicates the potential endangerment of a USDW, then action as described 
in paragraph (a)(1) or (a)(2) of this section must be taken.
    (b) If the Regional Administrator has demonstrable knowledge that 
wells within the zone of endangering influence will not serve as 
conduits for fluid movement into a USDW, the permit may be approved 
without requiring corrective action. However, additional monitoring 
shall be required to confirm that no significant migration will occur.



Sec.  147.2924  Area permits.

    (a) Area permits may be issued for more than one injection well if 
the following conditions are met:
    (1) All existing wells are described and located in the permit 
application;
    (2) All wells are within the same well field, project, reservoir or 
similar unit;
    (3) All wells are of similar construction; and
    (4) All wells are operated by the same owner/operator.
    (b) Area permits shall specify:
    (1) The area within which injection is authorized; and
    (2) The requirements for construction, monitoring, reporting, 
operation and abandonment for all wells authorized by the permit.
    (c) Area permits can authorize the construction and operation of new 
wells within the permit area, if:
    (1) The permittee notifies the Regional Administrator in the annual 
report of when and where any new wells have or will be drilled;
    (2) The new wells meet the criteria outlined in paragraphs (a) and 
(b) of this section; and
    (3) The effects of the new wells were addressed in the permit 
application and approved by the Regional Administrator.



Sec.  147.2925  Standard permit conditions.

    (a) The permittee must comply with all permit conditions, except as 
authorized by an emergency permit (described in Sec.  147.2906). 
Noncompliance is grounds for permit modification, permit termination or 
enforcement action.
    (b) The permittee has a duty to halt or reduce activity in order to 
maintain compliance with permit conditions.
    (c) The permittee shall take all reasonable steps to mitigate any 
adverse environmental impact resulting from noncompliance.
    (d) The permittee shall properly operate and maintain all facilities 
installed or used to meet permit conditions. Proper operation and 
maintenance also includes adequate operator staffing and training, 
adequate funding, and adequate engineering capability available.
    (e) This permit may be modified or terminated for cause (see 
Sec. Sec.  147.2927 and 147.2928). The filing of a request by the 
permittee for a permit modification or termination, or a notification of 
planned changes or anticipated noncompliance, does not stay any permit 
condition.
    (f) This permit does not convey any property rights, or any 
exclusive privilege.
    (g) The permittee shall furnish, within a reasonable time, 
information that

[[Page 1027]]

the Regional Administrator requests, for determination of permit 
compliance, or if cause exists, for permit modification or termination.
    (h) The permittee shall allow EPA representatives, upon presentation 
of appropriate credentials or other documentation, to:
    (1) Enter permittee's premises where a regulated activity is 
conducted or located, or where records required by this permit are kept;
    (2) Have access to and copy records required by this permit;
    (3) Inspect any facilities, equipment, practices or operations 
regulated or required by this permit; and
    (4) Sample or monitor any substances or parameters at any location 
for purpose of assuring compliance with this permit or the SDWA.
    (i) Monitoring and records. (1) Samples and monitoring data shall be 
representative of injection activity.
    (2) Permittee shall retain monitoring records for three years.
    (3) Monitoring records shall include:
    (i) Date, exact place and time of sampling or measurement;
    (ii) Individual(s) who preformed the measurements;
    (iii) Date(s) analyses were performed;
    (iv) Individual(s) who performed the analyses;
    (v) Analytical techniques or methods used, including quality 
assurance techniques employed to insure the generation of reliable data; 
and
    (vi) Results of analyses.
    (j) Signatory requirements. All applications, reports or information 
submitted to the Regional Administrator or the Osage UIC office must be 
signed by the injection facility owner/operator or his duly authorized 
representative. The person signing these documents must make the 
following certification:

    ``I certify under penalty of law that I have personally examined and 
am familiar with the information submitted in this document and all 
attachments and that, based on my inquiry of those individuals 
immediately responsible for obtaining the information, I believe that 
the information is true, accurate, and complete. I am aware that there 
are significant penalties for submitting false information, including 
the possibility of fine and imprisonment.''

    (k) Reporting requirements. (1) The permittee shall notify the 
Regional Administrator as soon as possible of any planned changes to the 
facility.
    (2) The permittee shall give advance notice to the Regional 
Administrator of any planned changes which may result in noncompliance.
    (3) This permit is not transferable to any person except after 
notice to the Regional Administrator in accordance with Sec.  147.2926.
    (l) A new injection well shall not commence injection until 
construction is complete and the Regional Administrator has been 
notified of completion of construction and has given his approval to 
commence injection.

(The information collection requirements contained in paragraphs (g) and 
(i) were approved by the Office of Management and Budget under control 
number 2040-0042)



Sec.  147.2926  Permit transfers.

    (a) Permits may be transferred to another permittee:
    (1) If the current permittee notifies the Regional Administrator at 
least 10 days before the proposed transfer date; and
    (2) If the notice includes a written agreement between the existing 
and new permittees containing:
    (i) A specific date for transfer of permit responsibility, coverage 
and liability; and
    (ii) Assurance that the new permittee has a surety bond on file with 
BIA; and
    (3) If the Regional Administrator does not respond with a notice to 
the existing permittee that the permit will be modified.
    (b) If the conditions in paragraph (a) of this section are met, the 
transfer is effective on the date specified in paragraph (a)(2)(i) of 
this section.



Sec.  147.2927  Permit modification.

    (a) Permits may be modified for the following causes only (with the 
exceptions listed in paragraph (b) of this section regarding minor 
modifications):
    (1) There are substantial changes to the facility or activity which 
occurred after permit issuance that justify revised or additional permit 
conditions.
    (2) The Regional Administrator has received information (e.g., from 
monitoring reports, inspections) which warrants a modified permit.

[[Page 1028]]

    (3) The regulations or standards on which the permit was based have 
changed.
    (4) The Regional Administrator has received notice of a proposed 
permit transfer.
    (5) An interested person requests in writing that a permit be 
modified, and the Regional Administrator determines that cause for 
modification exists.
    (6) Cause exists for termination under Sec.  147.2928, but the 
Regional Administrator determines that permit modification is 
appropriate.
    (b) Minor modifications. (1) Minor modifications do not require that 
the procedures listed in paragraph (c) of this section be followed.
    (2) Minor modifications consist of:
    (i) Correcting typographical errors;
    (ii) Requiring more frequent monitoring or reporting;
    (iii) Changing ownership or operational control (see Sec.  147.2926, 
Permit Transfers); or
    (iv) Changing quantities or types of injected fluids, provided:
    (A) The facility can operate within conditions of permit;
    (B) The facility classification would not change.
    (c) Modification procedures. (1) A draft permit shall be prepared 
with proposed modifications.
    (2) The draft permit shall follow the general permitting procedures 
(i.e., public comment period, etc.) before a final decision is made.
    (3) Only the changed conditions shall be addressed in the draft 
permit or public review.



Sec.  147.2928  Permit termination.

    (a) Permits may be terminated for the following causes only:
    (1) Noncompliance with any permit condition.
    (2) Misrepresentation or failure to fully disclose any relevant 
facts.
    (3) Determination that the permitted activity endangers human health 
or the environment.
    (4) Interested person requests in writing that a permit be 
terminated and the Regional Administrator determines that request is 
valid.
    (b) Termination procedures. (1) The Regional Administrator shall 
issue notice of intent to terminate (which is a type of draft permit).
    (2) Notice of intent to terminate shall follow the general 
permitting procedures (i.e., public comment period, etc.) before a final 
decision is made.



Sec.  147.2929  Administrative permitting procedures.

    (a) Completeness review. (1) The Regional Administrator shall review 
each permit application for completeness with the application 
requirements in Sec.  147.2918. The review will be completed in 10 days, 
and the Regional Administrator shall notify the applicant whether or not 
the application is complete.
    (2) If the application is incomplete, the Regional Administrator 
shall:
    (i) List the additional information needed;
    (ii) Specify a date by which the information must be submitted; and
    (iii) Notify the applicant when the application is complete.
    (3) After an application is determined complete, the Regional 
Administrator may request additional information to clarify previously 
submitted information. The application will still be considered 
complete.
    (4) If an applicant fails or refuses to correct deficiencies in the 
application, the permit may be denied and appropriate enforcement 
actions taken.
    (b) Draft permits. (1) After an application is deemed complete, the 
Regional Administrator shall either prepare a draft permit or notice of 
intent to deny the permit (which is a type of draft permit). If the 
Regional Administrator later decides the tentative decision to deny was 
wrong, he shall withdraw the notice of intent to deny and prepare a 
draft permit.
    (2) A draft permit shall contain at least the following information:
    (i) The standard permit conditions in Sec.  147.2925;
    (ii) Any monitoring and reporting requirements;
    (iii) The construction and operation requirements; and
    (iv) Plugging and abandonment requirements.

[[Page 1029]]

    (c) Statement of basis. (1) The Regional Administrator shall prepare 
a statement of basis for every draft permit.
    (2) The statement of basis shall briefly describe the draft permit 
conditions and the reasons for them. In the case of a notice of intent 
to deny or terminate, the statement of basis shall give reasons to 
support the tentative decision.
    (3) The statement of basis shall be sent to the applicant, and to 
any other person who requests a copy.
    (d) Public notice. (1)(i) The Regional Administrator shall give 
public notice when:
    (A) A permit application has been tentatively denied;
    (B) A draft permit has been prepared;
    (C) A hearing has been scheduled; or
    (D) An appeal has been granted.
    (ii) The applicant shall give public notice that he is submitting a 
permit application.
    (iii) Public notice is not required when a request for permit 
modification or termination is denied. However, written notice will be 
given to the permittee and the requester.
    (iv) Public notices may include more than one permit or action.
    (2)(i) Public notice of a draft permit (including notice of intent 
to deny) shall allow at least 15 days for public comment.
    (ii) Public notice of a hearing shall be given at least 30 days 
before the hearing.
    (3)(i) Public notice given by the Regional Administrator for the 
reasons listed in paragraph (d)(1)(i) of this section shall be mailed to 
the applicant, and published in a daily or weekly paper of general 
circulation in the affected area.
    (ii) Notice of application submission required by paragraph 
(d)(1)(ii) of this section shall be given to the surface landowner, 
tenants on the land where an injection well is located or is proposed to 
be located, and to each operator of a producing lease within one-half 
mile of the well location prior to submitting the application to the 
Regional Administrator.
    (4) The notice of application submission in paragraphs (d)(1)(ii) 
and (d)(3)(ii) of this section shall contain:
    (i) The applicant's name and address;
    (ii) The legal location of the injection well;
    (iii) Nature of activity;
    (iv) A statement that EPA will be preparing a draft permit and that 
there will be an opportunity for public comment; and
    (v) The name and phone number of EPA contact person.
    (5) All other notices shall contain:
    (i) The name, address, and phone number of the Osage UIC office and 
contact person for additional information and copies of the draft 
permit;
    (ii) Name and address of permit applicant or permittee;
    (iii) Brief description of nature of activity;
    (iv) Brief description of comment period and comment procedures;
    (v) Location of the information available for public review; and
    (vi) In the case of a notice for a hearing the notice shall also 
include:
    (A) Date, time, and location of hearing;
    (B) Reference to date of previous notices of the same permit; and
    (C) Brief description of the purpose of the hearing, including rules 
and procedures.
    (e) Public comments. (1) During the public comment period, any 
person may submit written comments on the draft permit, and may request 
a public hearing. A request for hearing shall be in writing and state 
the issues proposed to be raised in the hearing.
    (2) The Regional Administrator shall consider all comments when 
making the final decision, and shall respond to comments after the 
decision is made. The response shall:
    (i) Specify if any changes were made from the draft permit to the 
final permit decision, and why;
    (ii) Briefly describe and respond to all significant comments on the 
draft permit made during the comment period, or hearing, if held; and
    (iii) Be made available to the public.
    (f) Public hearings. (1) The Regional Administrator shall hold a 
public hearing whenever he finds a significant amount of public interest 
in a draft permit, based on the requests submitted, or at his 
discretion.

[[Page 1030]]

    (2) Any person may submit oral or written statements and data 
concerning the draft permit. The public comment period shall be 
automatically extended to the close of any public hearing held, or may 
be extended by the hearing officer at the hearing.
    (3) A tape recording or written transcript of the hearing shall be 
made available to the public.
    (g) Reopening of the comment period. (1) If any of the information 
submitted during the public comment period raises substantial new 
questions about a permit, the Regional Administrator may:
    (i) Prepare a new draft permit;
    (ii) Prepare a revised statement of basis; or
    (iii) Reopen the comment period.
    (2) Comments submitted during a reopened comment period shall be 
limited to the substantial new questions that caused its reopening.
    (3) Public notice about any of the above actions shall be given and 
shall define the scope of the new questions raised.
    (h) Issuance and effective date of a permit. (1) After the close of 
the comment period on a draft permit, the Regional Administrator shall 
make a final permit decision. The Regional Administrator shall notify 
the applicant and each person who commented or requested to receive 
notice. The notice shall include reference to the procedures for 
appealing a permit decision.
    (2) A final permit decision shall become effective 30 days after 
giving notice of the decision unless:
    (i) A later date is specified in the notice;
    (ii) Review is requested under Sec.  147.2929(j); or
    (iii) No comments requested a change in the draft permit, in which 
case the permit is effective immediately upon issuance.
    (i) Stays of contested permit conditions. If a request for review of 
a final UIC permit Sec.  147.2929(j) is granted, the effect of the 
contested permit conditions shall be stayed and shall not be subject to 
judicial review pending final agency action. If the permit involves a 
new injection well or project, the applicant shall be without a permit 
for the proposed well pending final agency action. Uncontested 
provisions which are not severable from those contested provisions shall 
be stayed with the contested provisions.
    (j) Appeal of permits. (1) Any person who filed comments on the 
draft permit or participated in the public hearing may petition the 
Administrator to review any condition of the permit decision. Any person 
who failed to file comments or participate in the hearing may petition 
for administrative review only to the extent of the changes from the 
preliminary permit to the final permit decision.
    (2) A person may request review of a final permit decision within 30 
days after a final permit decision has been issued. The 30-day period 
within which a person may request review begins with the service of 
notice of the Regional Administrator's final permit decision unless a 
later date is specified in that notice.
    (3) The petition requesting review shall include:
    (i) A demonstration that the petition is eligible under the 
requirements of paragraph (j)(1) of this section; and, when appropriate,
    (ii) A showing that the condition in question is based on:
    (A) A finding of fact or conclusion of law that is clearly 
erroneous; or
    (B) An exercise of discretion or important policy consideration 
which the Administrator, in his discretion, should review.
    (4) The Administrator may also decide, on his initiative, to review 
any condition of any UIC permit issued under these requirements. The 
Administrator must act under this paragraph within 30 days of the date 
notice was given of the Regional Administrator's action.
    (5) Within a reasonable time following the filing of the petition 
for review, the Administrator shall issue an order either granting or 
denying the request. To the extent that review is denied, the conditions 
of the final permit decision become final agency action.
    (6) Public notice shall be given by the Regional Administrator of 
any grant of a review petition by the Administrator. Notice shall be 
sent to the applicant,

[[Page 1031]]

the person requesting the review, appropriate persons on the Osage 
County mailing list and to newspapers of general circulation in the 
county. Included in the notice shall be a briefing schedule for the 
appeal and a statement that any interested person may file an amicus 
brief. Notice of denial of the review petition will be sent only to the 
person(s) requesting the review.
    (7) A petition to the Administrator, under paragraphs (j) (1) and 
(2) of this section is a prerequisite to the seeking of judicial review 
of the final agency action. For purposes of judicial review, final 
agency action occurs when a final UIC permit is issued or denied by the 
Regional Administrator and agency review procedures are exhausted. A 
final permit decision shall be issued by the Regional Administrator:
    (i) When the Administrator issues notice to the parties involved 
that review has been denied;
    (ii) When the Administrator issues a decision on the merits of the 
appeal and the decision does not include a remand of the proceedings; or
    (iii) Upon the completion of the remand proceedings if the 
proceedings are remanded, unless the Administrator's remand order 
specifically provides that the appeal of the remand decision will be 
required to exhaust the administrative remedies.



  Subpart HHH_Lands of the Navajo, Ute Mountain Ute, and All Other New 
                              Mexico Tribes

    Source: 53 FR 43104, Oct. 25, 1988, unless otherwise noted.



Sec.  147.3000  EPA-administered program.

    (a) Contents. The UIC program for Navajo Indian lands, except for 
Class II wells on Navajo Indian lands for which EPA has granted the 
Navajo Nation primacy for the SDWA Class II UIC program (as defined in 
Sec.  147.3400), the Ute Mountain Ute (Class II wells only on Ute 
Mountain Ute lands in Colorado and all wells on Ute Mountain Ute lands 
in Utah and New Mexico), and all wells on other Indian lands in New 
Mexico is administered by EPA. (The term ``Indian lands'' is defined at 
40 CFR 144.3.) The Navajo Indian lands are in the States of Arizona, New 
Mexico, and Utah; and the Ute Mountain Ute lands are in Colorado, New 
Mexico and Utah. This program consists of the UIC program requirements 
of 40 CFR parts 124, 144, 146, 148, and additional requirements set 
forth in the remainder of this subpart. The additions and modifications 
of this subpart apply only to the Indian lands described above. 
Injection well owners and operators, and EPA shall comply with these 
requirements.
    (b) Effective date. The effective date for the UIC program on these 
lands, except for Class II wells on Navajo Indian lands for which EPA 
has granted the Navajo Nation primacy for the SDWA Class II UIC program 
(as defined in Sec.  147.3400), is November 25, 1988.

[53 FR 43104, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991; 73 
FR 65565, Nov. 4, 2008]



Sec.  147.3001  Definition.

    Area of review. For the purposes of this subpart, area of review 
means the area surrounding an injection well or project area described 
according to the criteria set forth in Sec.  147.3009 of this subpart.



Sec.  147.3002  Public notice of permit actions.

    An applicant shall give public notice of his intention to apply for 
a permit as follows:
    (a) Prior to submitting an application to the Director, the 
applicant shall give notice to each landowner, tenant, and operator of a 
producing lease within one-half mile of the well and to the affected 
Tribal Government. The notice shall include:
    (1) Name and address of applicant;
    (2) A brief description of the planned injection activities 
including well location, name and depth of the injection zone, maximum 
injection pressure and volume, and source and description of the fluid 
to be injected;
    (3) Name, address, and phone number of the EPA contact person; and
    (4) A statement that opportunity to comment will be announced to the 
public after EPA prepares a draft permit.
    (b) In addition to the requirements of Sec.  144.31(e) of this 
chapter, a permit applicant shall submit a description of the way the 
notice was given and the

[[Page 1032]]

names and addresses of those to whom it was given.
    (c) Upon written request and supporting documentation, the Director 
may waive the requirement in paragraph (a) of this section to give 
individual notice of intent to apply for permits in an area where it 
would be impractical. However, notice to the affected Tribal government 
shall not be waived.
    (d) The Director shall also provide to the affected Tribal 
government all notices given to State governments under Sec.  124.10(c) 
of this chapter.



Sec.  147.3003  Aquifer exemptions.

    (a) Aquifer exemptions in connection with Class II wells. In 
accordance with Sec.  144.7(b) and Sec.  146.4 of this chapter, the 
portions of authorized injection zones into which existing Class II 
wells are currently injecting which are described in appendix A are 
hereby exempted. The exempted aquifers are defined by a one-quarter mile 
radius from the existing injection well. The exemption includes the 
intended injection zone only and is solely for the purpose of Class II 
injection.
    (b) Class III wells. In addition to the requirements of Sec.  
144.7(c)(1) of this chapter, an applicant for a uranium mining permit 
which necessitates an aquifer exemption shall submit a plugging and 
abandonment plan containing an aquifer cleanup plan, acceptable to the 
Director, describing the methods or techniques that will be used to meet 
the standards of Sec.  147.3011. The cleanup plan shall include an 
analysis of pre-injection water quality for the constituents required by 
the Director. The Director shall consider the cleanup plan in addition 
to the other information required for permit applications under 
Sec. Sec.  144.31(e) and 146.34 of this chapter.



Sec.  147.3004  Duration of rule authorization for existing Class I 
and III wells.

    Notwithstanding Sec.  144.21(a)(3)(i)(B) of this chapter, 
authorization by rule for existing Class I and III wells will expire 90 
days after the effective date of this UIC program unless a complete 
permit application has been submitted to the Director.



Sec.  147.3005  Radioactive waste injection wells.

    Notwithstanding Sec. Sec.  144.24 and 146.51(b) of this chapter, 
owners and operators of wells used to dispose of radioactive waste (as 
defined in 10 CFR part 20, appendix B, table II, but not including high 
level and transuranic waste and spent nuclear fuel covered by 40 CFR 
part 191) shall comply with the permitting requirements pertaining to 
Class I wells in parts 124, 144 and 146 of this chapter, as modified and 
supplemented by this subpart.



Sec.  147.3006  Injection pressure for existing Class II wells 
authorized by rule.

    (a) Rule-authorized Class II saltwater disposal wells. In addition 
to the requirements of Sec.  144.28(f)(3)(ii) of this chapter, the owner 
or operator shall, except during well stimulation, use an injection 
pressure measured at the wellhead that is not greater than the pressure 
calculated by using the following formula:

Pm = 0.2d

where:

Pm = injection pressure at the wellhead in pounds per square inch
d = depth in feet to the top of the injection zone.


Owners and operators shall comply with this requirement no later than 
one year after the effective date of this program.
    (b) Rule-authorized Class II enhanced recovery and hydrocarbon 
storage wells. (1) In addition to the requirements of Sec.  
144.28(f)(3)(ii) of this chapter, owners and operators shall use an 
injection pressure no greater than the pressure established by the 
Director for the field or formation in which the well is located. The 
Director shall establish such maximum pressure after notice (including 
notice to the affected Tribe), opportunity for comment, and opportunity 
for public hearing according to the provisions of part 124, subpart A, 
of this chapter, and shall inform owners and operators and the affected 
Tribe in writing of the applicable maximum pressure; or
    (2) An owner or operator may inject at a pressure greater than that 
specified in paragraph (b)(1) of this section

[[Page 1033]]

for the field or formation in which he is operating after demonstrating 
in writing to the satisfaction of the Director that such injection 
pressure will not violate the requirements of Sec.  144.28(f)(3)(ii) of 
this chapter. The Director may grant such a request after notice 
(including notice to the affected Tribe), opportunity for comment and 
opportunity for a public hearing according to the provisions of part 
124, subpart A of this chapter.
    (3) Prior to the time that the Director establishes rules for 
maximum injection pressure under paragraph (b)(1) of this section the 
owner or operator shall:
    (i) Limit injection pressure to a value which will not exceed the 
operating requirements of Sec.  144.28(f)(3)(ii); and
    (ii) Submit data acceptable to the Director which defines the 
fracture pressure of the formation in which injection is taking place. A 
single submission may be made on behalf of two or more operators 
conducting operations in the same field and formation, if the Director 
approves. The data shall be submitted to the Director within one year of 
the effective date of this program.



Sec.  147.3007  Application for a permit.

    (a) Notwithstanding the requirements of Sec.  144.31(c)(1) of this 
chapter, the owner or operator of an existing Class I or III well shall 
submit a complete permit application no later than 90 days after the 
effective date of the program.
    (b) The topographic map (or other map if a topographic map is 
unavailable) required by Sec.  144.31(e)(7) of this chapter, shall 
extend two miles from Class II wells, and 2\1/2\ miles from Class I and 
III wells. These maps will show all the information listed in paragraph 
144.31(e)(7) within \1/2\ mile for Class II wells and 2\1/2\ miles for 
Class I and III wells.



Sec.  147.3008  Criteria for aquifer exemptions.

    The aquifer exemption criterion in Sec.  146.4(c) of this chapter 
shall not be available for this program.



Sec.  147.3009  Area of review.

    The area of review shall be defined as follows:
    (a) Class II wells. The area of review for Class II permits and area 
permits shall be defined by a fixed radius as described in Sec.  
146.6(b) (1) and (2) of this chapter except that the radius shall be 
one-half mile.
    (b) Class I and III wells. The area of review for Class I and III 
wells are well fields which may be either:
    (1) An area defined by a radius two and one-half miles from the well 
or well field; or
    (2) An area one-quarter mile from the well or well field where the 
well field production at the times exceeds injection to produce a net 
withdrawal; or
    (3) A suitable distance, not less than one-quarter mile, proposed by 
the owner or operator and approved by the Director based upon a 
mathematical calculation such as that found in Sec.  146.6(a)(2) of this 
chapter.



Sec.  147.3010  Mechanical integrity tests.

    The monitoring of annulus pressure listed in Sec.  146.8(b)(1) of 
this chapter will only be acceptable if preceded by a pressure test, 
using liquid or gas that clearly demonstrates that mechanical integrity 
exists at the time of the pressure test.



Sec.  147.3011  Plugging and abandonment of Class III wells.

    To meet the requirements of Sec.  146.10(d) of this chapter, owners 
and operators of Class III uranium projects underlying or in aquifers 
containing up to 5,000 mg/l TDS which have been exempted under Sec.  
146.4 of this chapter shall:
    (a) Include in the required plugging and abandonment plan a plan for 
aquifer clean-up and monitoring which demonstrates adequate protection 
of surrounding USDWs.
    (1) The Director shall include in each such permit for a Class III 
uranium project the concentrations of contaminants to which aquifers 
must be cleaned up in order to protect surrounding USDWs.
    (2) The concentrations will be set as close as is feasible to the 
original conditions.

[[Page 1034]]

    (b) When requesting permission to plug a well, owners and operators 
shall submit for the Director's approval a schedule for the proposed 
aquifer cleanup, in addition to the information required by Sec.  
146.34(c).
    (c) Cleanup and monitoring shall be continued until the owner or 
operator certifies that no constituent listed in the permit exceeds the 
concentrations required by the permit, and the Director notifies the 
permittee in writing that cleanup activity may be terminated.



Sec.  147.3012  Construction requirements for Class I wells.

    In addition to the cementing requirement of Sec.  146.12(b) of this 
chapter, owners and operators of Class I wells shall, through 
circulation, cement all casing to the surface.



Sec.  147.3013  Information to be considered for Class I wells.

    (a) In addition to the information listed in Sec.  146.14(a) of this 
chapter, the Director shall consider the following prior to issuing any 
Class I permit:
    (1) Expected pressure changes, native fluid displacement, and 
direction of movement of the injected fluid; and
    (2) Methods to be used for sampling, and for measurement and 
calculation of flow.
    (b) In addition to the information listed in Sec.  146.14(b) of this 
chapter, the Director shall consider any information required under 
Sec.  146.14(a) of this chapter (as supplemented by this subpart) that 
has been gathered during construction.



Sec.  147.3014  Construction requirements for Class III wells.

    (a) In addition to the requirements of Sec.  146.32(c)(3) of this 
chapter, radiological characteristics of the formation fluids shall be 
provided to the Director.
    (b) In addition to the requirements of Sec.  146.32(e) of this 
chapter, the Director may require monitoring wells to be completed into 
USDWs below the injection zone if those USDWs may be affected by mining 
operations.



Sec.  147.3015  Information to be considered for Class III wells.

    (a) In addition to the requirements of Sec.  146.34(a) of this 
chapter, the following information shall be considered by the Director:
    (1) Proposed construction procedures, including a cementing and 
casing program, logging procedures, deviation checks, and a drilling, 
testing and coring program.
    (2) Depth to the proposed injection zone, and a chemical, physical 
and radiological analysis of the ground water in the proposed injection 
zone sufficient to define pre-injection water quality as required for 
aquifer cleanup by Sec.  147.3011 of this subpart.
    (3) An aquifer cleanup plan if required by Sec.  147.3003(b) of this 
subpart.
    (4) Any additional information that may be necessary to demonstrate 
that cleanup will reduce the level of contaminants in the surrounding 
USDWs as close as feasible to the original conditions.
    (b) In addition to the requirements of Sec.  146.34(b) of this 
chapter, the Director shall consider any information required under 
Sec.  146.34(a) of this chapter (as supplemented by this subpart) that 
has been gathered during construction.



Sec.  147.3016  Criteria and standards applicable to Class V wells.

    In addition to the criteria and standards applicable to Class V 
wells set forth in subpart F of part 146 of this chapter, owners and 
operators of wells that do not fall within the Class IV category but 
that are used to dispose of radioactive wastes (as defined in 10 CFR 
part 20, appendix B, table II, column 2, but not including high level 
and transuranic wastes and spent nuclear fuel covered by 40 CFR part 
191) shall comply with all of the requirements applicable to Class I 
injection wells in 40 CFR parts 124, 144 and 146 as supplemented by this 
subpart.



  Sec. Appendix A to Subpart HHH of Part 147--Exempted Aquifers in New 
                                 Mexico

    The areas described by a one-quarter mile radius around the 
following Class II wells in the listed formations are exempted for the 
purpose of Class II injection.

[[Page 1035]]



----------------------------------------------------------------------------------------------------------------
                                                                                                           Well
                                                   Sec.                                                    No.
----------------------------------------------------------------------------------------------------------------
                     Arco Oil & Gas Co.--Operator/Horseshoe Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
SE/NE..........................................        5            T30N R16W     1650'FNL      330'FEL      134
NW/NW..........................................       30            T31N R16W      660'FNL      703'FWL        8
SE/SW..........................................       28            T31N R16W      790'FSL     2150'FWL      167
NW/SE..........................................       33            T31N R16W     1710'FSL     2310'FEL      199
SE/NW..........................................       35            T31N R16W     2105'FNL     2105'FWL      196
NW/NW..........................................        4            T30N R16W      455'FNL     4435'FEL      219
NW/SW..........................................       33            T31N R16W     1980'FSL      386'FWL       65
NW/SE..........................................       27            T31N R16W     1980'FSL     2080'FEL      164
SE/SE..........................................       30            T31N R16W      660'FSL      660'FEL        5
NW/NW..........................................       34            T31N R16W      730'FNL      515'FWL      180
NW/NE..........................................       34            T31N R16W      813'FNL     2036'FEL      182
NW/NE..........................................        2            T30N R16W      720'FNL     2040'FEL      229
NW/NW..........................................       29            T31N R16W      660'FNL      660'FWL       24
NW/SW..........................................       13            T31N R17W     1975'FSL      670'FWL       77
NW/SE..........................................       29            T31N R16W     1980'FSL     1980'FEL       22
SE/SW..........................................       27            T31N R16W      660'FSL     1980'FWL      171
NW/SW..........................................       35            T31N R16W     1980'FSL      660'FWL      205
SE/NW..........................................       30            T31N R16W     1980'FNL     2061'FWL        7
NW/NE..........................................       31            T31N R16W      660'FNL     1980'FEL       17
NW/NE..........................................        4            T30N R16W      330'FNL     2160'FEL      221
NW/NE..........................................       29            T31N R16W      660'FNL     1980'FEL       26
SE/NE..........................................       34            T31N R16W     1990'FNL      645'FEL      194
SE/SE..........................................       31            T31N R16W      640'FSL      660'FEL       27
NE/SW..........................................       14            T31N R17W     2250'FSL     2630'FWL       94
NE/NW..........................................       14            T31N R17W      625'FNL    1995'FWI,       69
SE/NW..........................................       10            T30N R16W     1900'FNL     2080'FWL      271
SE/SE..........................................       29            T31N R16W      560'FSL  ...........       21
SE/NE..........................................       30            T31N R16W     1980'FNL      660'FEL       10
SE/NW..........................................       29            T31N R16W     2080'FNL     1980'FWL       23
NW/SE..........................................       25            T31N R17W     1980'FSL     1980'FEL      122
SE/SW..........................................       32            T31N R16W      660'FSL     1980'FWL       14
NW/SW..........................................       30            T31N R16W     2021'FSL      742'FWL       19
SE/SW..........................................       13            T31N R17W      660'FSL     1980'FWL       82
NW/NW..........................................       27            T31N R16W      520'FNL      660'FWL      150
SE/SE..........................................       28            T31N R16W      660'FSL      660'FEL      169
NW/SW..........................................       29            T31N R16W     1980'FSL      660'FWL       11
SE/NW..........................................       34            T31N R16W     2310'FNL     1650'FWL      192
SE/NW..........................................       29            T31N R16W      660'FSL     1980'FWL       12
NW/SW..........................................       27            T31N R16W     1650'FSL      330'FWL      162
NE/SE..........................................       23            T31N R17W     1880'FSL      340'FEL       96
NW/SW..........................................       24            T31N R17W     2050'FSL      990'FWL       97
SE/NW..........................................        4            T30N R16W     2060'FNL     1710'FWL      232
NW/NW..........................................       31            T31N R16W      620'FNL      701'FWL       30
NW/SE..........................................       35            T31N R16W     1980'FSL     1980'FEL      207
SE/NE..........................................       32            T31N R16W     1980'FNL      417'FEL       20
NE/NW..........................................       28            T31N R16W     1980'FNL     1980'FEL      152
NE/NW..........................................       34            T31N R16W     2140'FSL      735'FWL      201
SE/NW..........................................        3            T30N R16W     2310'FNL     1640'FWL      236
SE/SW..........................................       34            T31N R16W      660'FSL     1980'FWL      213
NW/NE..........................................       30            T31N R16W      660'FNL     1980'FFL        9
SE/SW..........................................       26            T31N R16W      660'FSL     1980'FWL      175
NW/SE..........................................       30            T31N R16W     1980'FSL     1980'FEL        6
SE/NW..........................................        9            T30N R16W     1650'FNL     2131'FWL      264
NW/SW..........................................        4            T30N R16W     2310'FSL     4390'FEL      242
NW/SW..........................................        2            T30N R16W     1980'FSL      660'FWL      250
NW/NW..........................................       33            T31N R16W      660'FNL      386'FWL       66
NE/NE..........................................       15            T31N R17W      660'FNL      660'FEL       67
NW/NE..........................................       33            T31N R16W      660'FNL     1980'FEL      178
NW/SE..........................................       24            T31N R17W     1875'FSL     1900'FEL       99
NW/NE..........................................       28            T31N R16W      660'FNL     1980'FEL      148
NW/NW..........................................       19            T31N R16W      680'FNL      682'FWL       89
NW/SE..........................................        4            T30N R16W     1820'FSL     2130'FEL      244
SE/SW..........................................       20            T31N R16W      660'FSL     1980'FWL      115
NW/NE..........................................       25            T31N R17W      660'FNL     1980'FEL      118
SE/SW..........................................        4            T30N R16W      660'FSL     3300'FEL      253
NW/SW..........................................       19            T31N R16W     1980'FSL      706'FWL      101
NW/SE..........................................       32            T31N R16W     1950'FSL     1980'FEL       22
NW/NW..........................................       35            T31N R16W      605'FNL      690'FWL      184
SE/NE..........................................       29            T31N R16W     1980'FNL      417'FEL       25
SE/NW..........................................       19            T31N R16W     1980'FNL     2023'FWL       95
NW/NW..........................................       32            T31N R16W      660'FNL      660'FWL        4

[[Page 1036]]

 
SE/SW..........................................       24            T31N R17W      660'FSL     3300'FEL      107
SE/NE..........................................       28            T31N R16W     2105'FNL      940'FEL      154
NW/NE..........................................       35            T31N R16W      610'FNL     2000'FEL      186
SE/SW..........................................        5            T31N R16W      990'FSL     2310'FWL      139
NW/SE..........................................       28            T31N R16W     1980'FSL     1980'FEL      160
SE/SE..........................................       33            T31N R16W      330'FSL      990'FEL      211
NW/NE..........................................        5            T30N R16W      330'FNL     1650'FEL      128
SE/NW..........................................       27            T31N R16W     1900'FNL     2050'FWL      156
SE/SW..........................................       35            T31N R16W      660'FSL     1980'FWL      217
NW/NW..........................................       10            T30N R16W      526'FNL      330'FWL      265
NE/SW..........................................       21            T31N R16W     1880'FSL     1980'FWL      143
NW/NE..........................................       24            T31N R17W      409'FNL     1914'FEL       87
NW/SW..........................................       32            T31N R16W     1980'FSL      660'FWL       15
SE/SE..........................................       34            T31N R16W      960'FSL      910'FEL      215
SW/SE..........................................       21            T31N R16W      820'FSL     1820'FEL      145
SE/SE..........................................       27            T31N R16W      610'FSL      640'FEL      173
NW/SW..........................................        3            T30N R16W     1920'FSL      350'FWL      246
SE/SW..........................................       19            T31N R16W      601'FSL     2002'FWL      111
SW/SE..........................................       14            T31N R17W      330'FSL     1900'FEL       79
NW/NW..........................................       27            T31N R16W      520'FNL      660'FWL      150
SE/NW..........................................       31            T31N R16W     1724'FNL     2067'FWL       29
NW/NE..........................................       32            T31N R16W      660'FNL     1980'FEL       13
SE/NE..........................................       24            T31N R17W     1998'FNL      702'FEL       93
NW/NW..........................................        5            T30N R16W      660'FNL      660'FWL      126
NW/SW..........................................       28            T31N R16W     1740'FSL      590'FWL      158
SE/NE..........................................       31            T31N R16W     1980'FNL      660'FEL       16
NW/NW..........................................       24            T31N R17W      660'FNL      760'FWL       85
----------------------------------------------------------------------------------------------------------------
                 Energy Reserve Backup Inc.--Operator/Horseshoe Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
SE/SE..........................................        5            T31N R17W      660'FSL      660'FEL        4
NE/SW..........................................       10            T30N R16W     1970'FSL     2210'FWL       31
SE/NW..........................................       11            T30N R16W     2090'FNL     2190'FWI       29
SE/SE..........................................       10            T30N R16W      700'FSL      500'FEL       37
----------------------------------------------------------------------------------------------------------------
                        Solar Petroelum Inc.--Operator/Horseshoe--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
SW/SE..........................................       11            T31N R17W      736'FSL     2045'FEL      205
SE/NE..........................................        9            T31N R17W     1980'FNL      660'FEL      122
NW/SE..........................................        4            T31N R17W     1980'FSL     1980'FFL      127
NE/NE..........................................       10            T31N R17W      660'FNL      660'FEL      136
SE/SW..........................................        4            T31N R17W      660'FSL     1980'FWL      125
SW/NW..........................................       11            T31N R17W     2300'FNL      660'FWL      206
NW/SW..........................................        4            T31N R17W     1980'FSL      660'FWL      103
SE/NW..........................................        4            T31N R17W     1989'FNL     1980'FWL      128
NW/NW..........................................        4            T31N R17W      660'FNL      660'FWL      101
SW/NE..........................................       10            T31N R17W     1980'FNL     1980'FEL      117
SW/NW..........................................       10            T31N R17W     1980'FNL      660'FWL      108
SW/SW..........................................       10            T31N R17W      660'FSL      660'FWL      114
SW/SE..........................................        3            T31N R17W      330'FSL     2310'FEL      143
SE/NE..........................................        5            T31N R17W     1980'FNL      660'FEL      302
NE/NE..........................................        5            T31N R17W     1950'FNL     1050'FEL      307
SE/SE..........................................        9            T31N R17W      990'FSL      850'FEL      140
NE/NW..........................................       10            T31N R17W      660'FNL     1980'FWL      118
SW/SW..........................................       11            T31N R17W      660'FSL      660'FWL      204
NW/SE..........................................        9            T31N R17W     1980'FSL     1980'FEL      115
SW/SE..........................................       10            T31N R17W      990'FSL     1980'FEL      144
NW/NE..........................................        9            T31N R17W      660'FNL     1980'FEL      123
NE/SW..........................................       10            T31N R17W     1980'FSL     1980'FWL      109
NE/SW..........................................       11            T31N R17W     1980'FSL     1980'FWL      203
SE/NW..........................................        9            T31N R17W     1980'FNL     1980'FWL      134
NW/SW..........................................        3            T31N R17W     1980'FSL      660'FWL      132
SW/SW..........................................        3            T31N R17W      560'FSL      660'FWL      110
NW/NW..........................................        9            T31N R16W      660'FNL      660'FWL      133
SE/SE..........................................        4            T31N R17W      660'FSL      660'FEL      124
----------------------------------------------------------------------------------------------------------------
                         WTR Oil Co.--Operator/Horseshoe Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
NE/SW..........................................       33            T32N R17W     1980'FSL     1989'FWL        2
----------------------------------------------------------------------------------------------------------------
                     Arco Oil & Gas Co.--Operator/Many Rocks Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
NW/NW..........................................        7            T31N R16W      898'FNL      500'FWL        2
SW/NE..........................................       17            T31N R16W     1673'FNL     1789'FEL       21

[[Page 1037]]

 
NW/SE..........................................       17            T31N R16W     1890'FSL     2150'FEL       23
SW/NE..........................................        7            T31N R16W     2310'FNL     2310'FEL        6
NE/SW..........................................        8            T31N R16W     1650'FSL     1650'FWL       12
NE/NW..........................................       17            T31N R16W      660'FNL     2030'FWL       18
NE/NE..........................................       18            T31N R16W      360'FNL      855'FEL       16
SE/SW..........................................        7            T31N R16W      716'FSL     2185'FWL       13
SE/SE..........................................       17            T31N R16W      660'FSL      660'FEL       26
NE/SW..........................................       17            T31N R16W     2040'FSL     2070'FWL       22
SW/SW..........................................        6            T31N R16W      330'FSL      330'FWL        1
SW/NW..........................................       17            T31N R16W     2073'FNL      641'FWL       19
NW/SW..........................................       17            T31N R16W     1967'FSL      981'FWL        8
----------------------------------------------------------------------------------------------------------------
                      James P. Woosley--Operator/Many Rocks Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
NW/NE..........................................       20            T32N R17W      330'FNL     2310'FEL       13
SW/SW..........................................       27            T32N R17W      660'FSL      990'FWL        1
SW/NW..........................................       17            T32N R17W     2310'FWL      330'FWL        4
SW/NW..........................................       27            T32N R17W      260'FWL     1360'FNL       11
NE/SW..........................................       27            T32N R17W     1980'FSL     1980'FWL        6
NE/SE..........................................       18            T32N R17W     2474'FSL      133'FEL       18
SW/SE..........................................       27            T32N R17W      625'FNL     2000'FEL        3
NE/SE..........................................       28            T32N R17W     1980'FSL      330'FEL       12
----------------------------------------------------------------------------------------------------------------
                    Solar Petroleum Inc.--Operator/Many Rocks Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
SE/NW..........................................        1            T31N R17W     1980'FNL     1980'FWL      216
NW/NE..........................................        2            T31N R17W      805'FNL      940'FEL      215
SE/NE..........................................        2            T31N R17W     1980'FNL      660'FEL      218
NW/SW..........................................        1            T31N R17W     2310'FSL      990'FNL      223
SE/NE..........................................       12            T31N R17W     1820'FNL      500'FEL      217
----------------------------------------------------------------------------------------------------------------
                        WTR Oil Co.--Operator/Many Rocks Gallup--Field/Gallup--Formation
----------------------------------------------------------------------------------------------------------------
NW/NW..........................................       35            T32N R17W      810'FNL      510'FWL       11
SE/SE..........................................       35            T32N R17W      660'FSL      660'FEL        6
SE/NE..........................................       34            T32N R17W      775'FEL     1980'FNL        8
SE/NW..........................................       35            T32N R16W     1980'FNL     1980'FWL        9
NW/SE..........................................       35            T32N R17W     1980'FSL     1980'FEL        7
----------------------------------------------------------------------------------------------------------------
                       Chaco Oil Co.--Operator/Red Mtn Meseverde--Field/Menefee--Formation
----------------------------------------------------------------------------------------------------------------
NE/NE..........................................       29             T20N R9W      395'FNL     1265'FEL        6
SE/SW..........................................       20             T20N R9W      442'FSL     2430'FWL       17
----------------------------------------------------------------------------------------------------------------
                   Geo Engineering Inc.--Operator/Red Mtn Meseverde--Field/Menefee--Formation
----------------------------------------------------------------------------------------------------------------
NW/NE..........................................       29             T20N R9W      160'FNL     2135'FEL       35
NE/NE..........................................       29             T20N R9W      225'FNL     1265'FEL        7
SE/NW..........................................       29             T20N R9W     1344'FNL     2555'FWL       20
NW/NE..........................................       29             T20N R9W      615'FNL     1920'FEL        5
NE/NW..........................................       29             T20N R9W      834'FNL     2113'FWL       21
SW/SE..........................................       20             T20N R9W      265'FSL     2150'FEL       36
NE/NE..........................................       29             T20N R9W        5'FNL     1130'FEL        8
SE/SE..........................................       20             T20N R9W      450'FSL     1145'FEL       24
SE/SE..........................................       20             T20N R9W      990'FSL     1280'FEL       10
NW/NE..........................................       29             T20N R9W     1115'FNL     2325'FEL       22
SE/SE..........................................       20             T20N R9W     1085'FSL      860'FEL       12
----------------------------------------------------------------------------------------------------------------
                  Tesoro Petroleum Co.--Operator/S. Hospah Lower Sand--Field/Hospah--Formation
----------------------------------------------------------------------------------------------------------------
NW/SE..........................................        6             T17N R8W     2310'FSL     2310'FEL       28
SW/SE..........................................        6             T17N R8W      990'FSL     2310'FFL       34
SW/SW..........................................        6             T17N R8W        5'FSL       20'FWL       18
SE/SW..........................................        6             T17N R8W        5'FSL     2635'FWL       20
----------------------------------------------------------------------------------------------------------------


[[Page 1038]]



           Subpart III_Lands of Certain Oklahoma Indian Tribes

    Source: 53 FR 43109, Oct. 25, 1988, unless otherwise noted.



Sec.  147.3100  EPA-administered program.

    (a) Contents. The UIC program for the Indian lands in Oklahoma, 
except for that covering the Class II wells of the Five Civilized 
Tribes, is administered by EPA. The UIC program for all wells on Indian 
lands in Oklahoma, except Class II wells on the Osage Mineral Reserve 
(found at 40 CFR part 147, Subpart GGG) and the Class II program for the 
Five Civilized Tribes, consists of the UIC program requirements of 40 
CFR parts 124, 144, 146, 148, and additional requirements set forth in 
the remainder of this subpart. Injection well owners and operators, and 
EPA shall comply with these requirements.
    (b) Effective date. The effective date for the UIC program for all 
wells on Indian lands except Class II wells on the Osage Mineral Reserve 
and Class II wells on the lands of the Five Civilized Tribes is November 
25, 1988.

[53 FR 43109, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



Sec.  147.3101  Public notice of permit actions.

    (a) In addition to the notice requirements of Sec.  124.10 of this 
chapter, the Director shall provide to the affected Tribal government 
all notices given to an affected State government under Sec.  124.10(c) 
of this chapter.
    (b) Class I and III wells. In addition to the notice requirements of 
Sec.  124.10 of this chapter:
    (1) Owners and operators of Class I and III wells shall notify the 
affected Tribal government prior to submitting an application for a 
permit, shall publish such notice in at least two newspapers of general 
circulation in the area of the proposed well, and shall broadcast notice 
over at least one local radio station.
    (2) The Director shall publish a notice of availability of a draft 
permit in at least two newspapers of general circulation in the area of 
the proposed well, and broadcast notice over at least one local radio 
station. The public notice shall allow at least 45 days for public 
comment.
    (c) Class II wells. In addition to the notice requirements of Sec.  
124.10 of this chapter:
    (1) Owners and operators of Class II wells shall give notice of 
application for a permit to the affected Tribal government prior to 
submitting the application to the Director.
    (2) In addition to the public notice required for each action listed 
in Sec.  124.10(a) of this chapter, the Director shall also publish 
notice in a daily or weekly newspaper of general circulation in the 
affected area for actions concerning Class II wells.



Sec.  147.3102  Plugging and abandonment plans.

    In lieu of the requirements of Sec.  144.28(c)(1) and (2) (i)-(iii) 
of this chapter, owners and operators of Class II wells shall comply 
with the plugging and abandonment provisions of Sec.  147.3108 of this 
subpart.



Sec.  147.3103  Fluid seals.

    Notwithstanding Sec. Sec.  144.28(f)(2) and 146.12(c) of this 
chapter, owners and operators shall not use a fluid seal as an 
alternative to a packer.



Sec.  147.3104  Notice of abandonment.

    (a) In addition to the notice required by Sec.  144.28(j)(2) of this 
chapter, the owner or operator shall at the same time submit plugging 
information in conformance with Sec.  147.3108 of this subpart 
including:
    (1) Type and number of plugs;
    (2) Elevation of top and bottom of each plug;
    (3) Method of plug placement; and
    (4) Type, grade and quantity of cement to be used.
    (b) In addition to the permit conditions specified in Sec. Sec.  
144.51 and 144.52 of this chapter, each owner and operator shall submit 
and each permit shall contain the following information (in conformance 
with Sec.  146.3108 of this subpart):
    (1) Type and number of plugs;
    (2) Elevation of top and bottom of each plug;
    (3) Method of plug placement; and
    (4) Type, grade and quantity of cement to be used.

[[Page 1039]]



Sec.  147.3105  Plugging and abandonment report.

    (a) In lieu of the time periods for submitting a plugging report in 
Sec.  144.28(k) of this chapter, owners and operators of Class I and III 
wells shall submit the report within 15 days of plugging the well and 
owners or operators of Class II wells within 30 days of plugging, or at 
the time of the next required operational report (whichever is less.) If 
the required operational report is due less than 15 days following 
completion of plugging, then the plugging report shall be submitted 
within 30 days for Class II wells and 15 days for Class I and III wells.
    (b) In addition to the requirement of Sec.  144.28(k)(1) of this 
chapter, owners and operators of Class II wells shall include a 
statement that the well was plugged in accordance with Sec.  146.10 of 
this chapter and Sec.  147.3109 of this subpart, and, if the actual 
plugging differed, specify the actual procedures used.
    (c) The schedule upon which reports of plugging must be submitted 
are changed from those in Sec.  144.51(o) to those specified in 
paragraph (a) of this section.



Sec.  147.3106  Area of review.

    (a) When determining the area of review under Sec.  146.6(b) of this 
chapter, the fixed radius shall be no less than one mile for Class I 
wells and one-half mile for Class II and III wells. In the case of an 
application for an area permit, determination of the area of review 
under Sec.  146.6(b) shall be a fixed width of not less than one mile 
for the circumscribing area of Class I projects and one-half mile for 
the circumscribing area of Class II and III projects.
    (b) However, in lieu of Sec.  146.6(c) of this chapter, if the area 
of review is determined by a mathematical model pursuant to paragraph 
Sec.  146.6(a) of this chapter, the permissible radius is the result of 
such calculation even if it is less than one mile for Class I wells and 
one-half for Class II and III wells.



Sec.  147.3107  Mechanical integrity.

    (a) Monitoring of annulus pressure conducted pursuant to Sec.  
146.8(b)(1) shall be preceded by an initial pressure test. A positive 
gauge pressure on the casing/tubing annulus (filled with liquid) shall 
be maintained continuously. The pressure shall be monitored monthly.
    (b) Pressure tests conducted pursuant to Sec.  146.8(b)(2) of this 
chapter shall be performed with a pressure on the casing/tubing annulus 
of at least 200 p.s.i. unless otherwise specified by the Director. In 
addition, pressure tests conducted during well operation shall maintain 
an injection/annulus pressure differential of at least 100 p.s.i. 
throughout the tubing length.
    (c) Monitoring of enhanced recovery wells conducted pursuant to 
Sec.  146.8(b)(3), must be preceded by an initial pressure test that was 
conducted no more than 90 days prior to the commencement of monitoring.



Sec.  147.3108  Plugging Class I, II, and III wells.

    In addition to the requirements of Sec.  146.10 of this chapter, 
owners and operators shall comply with the following when plugging a 
well:
    (a) For Class I and III wells:
    (1) The well shall be filled with mud from the bottom of the well to 
a point one hundred (100) feet below the top of the highest disposal or 
injection zone and then with a cement plug from there to at least one 
hundred (100) feet above the top of the disposal or injection zone.
    (2) A cement plug shall also be set from a point at least fifty (50) 
feet below the shoe of the surface casing to a point at least five (5) 
feet above the top of the lowest USDW.
    (3) A final cement plug shall extend from a point at least thirty 
feet below the ground surface to a point five (5) feet below the ground 
surface.
    (4) All intervals between plugs shall be filled with mud.
    (5) The top plug shall clearly show by permanent markings inscribed 
in the cement or on a steel plate embedded in the cement the well permit 
number and date of plugging.
    (b) For Class II wells:
    (1) The well shall be kept full of mud as casing is removed. No 
surface casing shall be removed without written approval from the 
Director.
    (2) If surface casing is adequately set and cemented through all 
USDWs (set to at least 50 feet below the base of the USDW), a plug shall 
be set at least 50

[[Page 1040]]

feet below the shoe of the casing and extending at least 50 feet above 
the shoe of the casing; or
    (3) If the surface casing and cementing is inadequate, the well bore 
shall be filled with cement from a point at least 50 feet below the base 
of the USDW to a point at least 50 feet above the shoe of the surface 
casing, and any additional plugs as required by the Director.
    (4) In all cases, the top 20 feet of the well bore below 3 feet of 
ground surface shall be filled with cement. Surface casing shall be cut 
off 3 feet below ground surface and covered with a secure steel cap on 
top of the surface pipe. The remaining 3 feet shall be filled with dirt.
    (5) Except as provided in sub-paragraph (b)(6) of this section, each 
producing or receiving formation shall be sealed off with at least a 50-
foot cement plug placed at the base of the formation and at least a 50-
foot cement plug placed at the top of the formation.
    (6) The requirement in sub-paragraph (b)(5) of this section does not 
apply if the producing/receiving formation is already sealed off from 
the well bore with adequate casing and cementing behind casing, and 
casing is not to be removed, or the only openings from the producing/
receiving formation into the well bore are perforations in the casing, 
and the annulus between the casing and the outer walls of the well is 
filled with cement for a distance of 50 feet above the top of the 
formation. When such conditions exist, a bridge plug capped with at 
least 10 feet of cement set at the top of the producing formation may be 
used.
    (7) When specified by the Director, any uncased hole below the shoe 
of any casing to be left in the well shall be filled with cement to a 
depth of at least 50 feet below the casing shoe, or the bottom of the 
hole, and the casing above the shoe shall be filled with cement to at 
least 50 feet above the shoe of the casing. If the well has a screen or 
liner which is not to be removed, the well bore shall be filled with 
cement from the base of the screen or liner to at least 50 feet above 
the top of the screen or liner.
    (8) All intervals between cement plugs in the well bore must be 
filled with mud.
    (c) For the purposes of this section mud shall be defined as: mud of 
not less than thirty-six (36) viscosity (API Full Funnel Method) and a 
weight of not less than nine (9) pounds per gallon.



Sec.  147.3109  Timing of mechanical integrity test.

    The demonstrations of mechanical integrity required by Sec.  
146.14(b)(2) of this chapter prior to approval for the operation of a 
Class I well shall, for an existing well, be conducted no more than 90 
days prior to application for the permit and the results included in the 
permit application. The owner or operator shall notify the Director at 
least seven days in advance of the time and date of the test so that EPA 
observers may be present.



                Subpart JJJ_Assiniboine and Sioux Tribes



Sec.  147.3200  Fort Peck Indian Reservation: Assiniboine & Sioux Tribes--
Class II wells.

    The UIC program for Class II injection wells on all lands within the 
exterior boundaries of the Fort Peck Indian Reservation is the program 
administered by the Assiniboine and Sioux (Fort Peck) Tribes approved by 
EPA pursuant to section 1425 of the SDWA. Notice of this approval was 
published in the Federal Register on October 27, 2008; the effective 
date of this program is November 26, 2008. This program consists of the 
following elements as submitted to EPA in the Fort Peck Tribes' program 
application:
    (a) Incorporation by reference. The requirements set forth in the 
Fort Peck Tribes' Statutes, Regulations, and Resolutions notebook, dated 
June 2008, are hereby incorporated by reference and made part of the 
applicable UIC program under the SDWA for the Fort Peck Indian 
Reservation. This incorporation by reference was approved by the 
Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 
1 CFR part 51. Copies may be obtained or

[[Page 1041]]

inspected at the Fort Peck Tribal Offices, 605 Indian Avenue, Poplar, 
Montana 59255, (406) 768-5155, at the Environmental Protection Agency, 
Region 8, 1595 Wynkoop Street, Denver, Colorado 80202-1129, (800) 227-
8917, or at the National Archives and Records Administration (NARA). For 
information on the availability of this material at NARA, call (202) 
741-6030, or go to: http://www.archives.gov/federal_register/
code_of_federal_regulations/ibr_locations.html.
    (b) Memorandum of Agreement (MOA). The MOA between EPA and the Fort 
Peck Tribes signed by EPA on July 31, 2007.
    (c) Statements of legal authority. Letters to EPA from Sonosky, 
Chambers, Sachse, Endreson & Perry, dated September 4, 2003 (attaching a 
June 17, 2002 letter), March 27, 2001, July 19, 1999, March 13, 1995, 
March 16, 1994, November 4, 1992, July 14, 1989, and April 13, 1989, and 
letters submitted as part of the Fort Peck Tribes' application.
    (d) Program Description. The Program Description submitted as part 
of the Fort Peck Tribes' application, and any other materials submitted 
as part of the application or as a supplement to it.

[73 FR 63646, Oct. 27, 2008]

Subpart KKK [Reserved]



                     Subpart LLL_Navajo Indian Lands



Sec.  147.3400  Navajo Indian lands--Class II wells.

    The UIC program for Class II injection wells located: Within the 
exterior boundaries of the formal Navajo Reservation, including the 
three satellite reservations (Alamo, Canoncito and Ramah), but excluding 
the former Bennett Freeze Area, the Four Corners Power Plant and the 
Navajo Generating Station; and on Navajo Nation tribal trust lands and 
trust allotments outside those exterior boundaries (collectively 
referred to as ``Navajo Indian lands for which EPA has granted the 
Navajo Nation primacy for the SDWA Class II UIC program''), is the 
program administered by the Navajo Nation approved by EPA pursuant to 
section 1425 of the SDWA. Notice of this approval was published in the 
Federal Register on November 4, 2008; the effective date of this program 
is December 4, 2008. This program consists of the following elements as 
submitted to EPA in the Navajo Nation's program application:
    (a) Incorporation by reference. The requirements set forth in the 
Navajo Nation Statutes, Regulations and Resolution notebook, dated 
October 2008, are hereby incorporated by reference and made part of the 
applicable UIC program under the SDWA for Class II injection wells on 
Navajo Indian lands for which EPA has granted the Navajo Nation primacy 
for the SDWA Class II UIC program (as defined in this section). This 
incorporation by reference was approved by the Director of the Federal 
Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies 
may be obtained or inspected at the Navajo Nation Environmental 
Protection Agency UIC Office, Old NAPA Auto Parts Building (Tribal Bldg. 
S009-080), Highway 64, Shiprock, New Mexico 87420 (505-368-1040), at 
the Environmental Protection Agency, Region 9, 75 Hawthorne Street, San 
Francisco, California 94105-3920 (415-972-3533), or at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call (202) 741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/
ibr_locations.html.
    (b) Memorandum of Agreement (MOA). The MOA between EPA Region 9 and 
the Navajo Nation, signed by the EPA Regional Administrator on August 
21, 2001. The Criminal Enforcement MOA between EPA Region 9 and the 
Navajo Nation, signed by EPA on October 30, 2006.
    (c) Statement of legal authority. (1) ``Statement of the Attorney 
General of the Navajo Nation Pursuant to 40 CFR 145.24'', August 27, 
2001.
    (2) ``Statement of the Attorney General of the Navajo Nation 
Regarding the Regulatory Authority and Jurisdiction of the Navajo Nation 
with Respect To Its Underground Injection Control Program'', July 3, 
2002.
    (3) ``Supplemental Statement of the Navajo Nation Attorney General 
Regarding the Regulatory Authority and

[[Page 1042]]

Jurisdiction of the Navajo Nation to Operate an Underground Injection 
Control Program under the Safe Drinking Water Act'', October 11, 2006.
    (d) Program Description. The Program Description submitted as part 
of the Navajo Nation's application, and any other materials submitted as 
part of this application or as a supplement thereto.

[73 FR 65565, Nov. 4, 2008]



PART 148_HAZARDOUS WASTE INJECTION RESTRICTIONS--Table of Contents



                            Subpart A_General

Sec.
148.1 Purpose, scope and applicability.
148.2 Definitions.
148.3 Dilution prohibited as a substitute for treatment.
148.4 Procedures for case-by-case extensions to an effective date.
148.5 Waste analysis.

                   Subpart B_Prohibitions on Injection

148.10 Waste specific prohibitions--solvent wastes.
148.11 Waste specific prohibitions--dioxin-containing wastes.
148.12 Waste specific prohibitions--California list wastes.
148.14 Waste specific prohibitions--first third wastes.
148.15 Waste specific prohibitions--second third wastes.
148.16 Waste specific prohibitions--third third wastes.
148.17 Waste specific prohibitions; newly listed wastes.
148.18 Waste specific prohibitions-newly listed and identified wastes.

               Subpart C_Petition Standards and Procedures

148.20 Petitions to allow injection of a waste prohibited under subpart 
          B.
148.21 Information to be submitted in support of petitions.
148.22 Requirements for petition submission, review and approval or 
          denial.
148.23 Review of exemptions granted pursuant to a petition.
148.24 Termination of approved petition.

    Authority: Secs. 3004, Resource Conservation and Recovery Act, 42 
U.S.C. 6901 et seq.

    Source: 53 FR 28154, July 26, 1988, unless otherwise noted.



                            Subpart A_General



Sec.  148.1  Purpose, scope and applicability.

    (a) This part identifies wastes that are restricted from disposal 
into Class I wells and defines those circumstances under which a waste, 
otherwise prohibited from injection, may be injected.
    (b) The requirements of this part apply to owners or operators of 
Class I hazardous waste injection wells used to inject hazardous waste.
    (c) Wastes otherwise prohibited from injection may continue to be 
injected:
    (1) If an extension from the effective date of a prohibition has 
been granted pursuant to Sec.  148.4 with respect to such wastes; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition filed under Sec.  148.20 to allow injection of restricted 
wastes with respect to those wastes and wells covered by the exemption; 
or
    (3) If the waste is generated by a conditionally exempt small 
quantity generator, as defined in Sec.  261.5; or
    (d) Wastes that are hazardous only because they exhibit a hazardous 
characteristic, and which are otherwise prohibited under this part, or 
part 268 of this chapter, are not prohibited if the wastes:
    (1) Are disposed into a nonhazardous or hazardous injection well as 
defined under 40 CFR Sec.  146.6(a); and
    (2) Do not exhibit any prohibited characteristic of hazardous waste 
identified in 40 CFR part 261, subpart C at the point of injection.

[53 FR 28154, July 26, 1988, as amended at 55 FR 22683, June 1, 1990; 57 
FR 8088, Mar. 6, 1992; 57 FR 31763, July 20, 1992; 60 FR 33932, June 29, 
1995; 61 FR 15596, Apr. 8, 1996; 61 FR 33682, June 28, 1996]



Sec.  148.2  Definitions.

    Injection interval means that part of the injection zone in which 
the well is screened, or in which the waste is otherwise directly 
emplaced.
    Transmissive fault or fracture is a fault or fracture that has 
sufficient permeability and vertical extent to allow fluids to move 
between formations.

[[Page 1043]]



Sec.  148.3  Dilution prohibited as a substitute for treatment.

    The prohibition of Sec.  268.3 shall apply to owners or operators of 
Class I hazardous waste injection wells.



Sec.  148.4  Procedures for case-by-case extensions to an effective date.

    The owner or operator of a Class I hazardous waste injection well 
may submit an application to the Administrator for an extension of the 
effective date of any applicable prohibition established under subpart B 
of this part according to the procedures of Sec.  268.5.



Sec.  148.5  Waste analysis.

    Generators of hazardous wastes that are disposed of into Class I 
injection wells must comply with the applicable requirements of Sec.  
268.7 (a) and (b). Owners or operators of Class I hazardous waste 
injection wells must comply with the applicable requirements of Sec.  
268.7(c).



                   Subpart B_Prohibitions on Injection



Sec.  148.10  Waste specific prohibitions--solvent wastes.

    (a) Effective August 8, 1988, the spent solvent wastes specified in 
Sec.  261.31 as EPA Hazardous Waste Nos. F001, F002, F003, F004, and 
F005 are prohibited from underground injection unless the solvent waste 
is a solvent-water mixture or solvent-containing sludge containing less 
than 1 percent total F001-F005 solvent constituents listed in Table A of 
this section.
    (b) Effective August 8, 1990, all spent F001-F005 solvent wastes 
containing less than 1 percent total F001-F005 solvent constituents 
listed in Table A of this section are prohibited from injection.
    (c) Effective August 8, 1990, all spent F002 and F005 wastes 
containing solvent constituents listed in Table B of this section are 
prohibited from underground injection at off-site injection facilities.
    (d) Effective November 8, 1990, the wastes specified in paragraph 
(c) of this section are prohibited from underground injection at on-site 
injection facilities.
    (e) The requirements of paragraphs (a) and (b) of this section do 
not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

                                 Table A

Acetone
n-Butyl alcohol
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Cresols and cresylic acid
Cyclohexanone
1,2-dichlorobenzene
Ethyl acetate
Ethyl benzene
Ethyl ether
Isobutanol
Methanol
Methylene chloride
Methylene chloride (from the pharmaceutical industry)
Methyl ethyl ketone
Methyl isobutyl ketone
Nitrobenzene
Pyridine
Tetrachloroethylene
Toulene
1,1,1-Trichloroethane
1,2,2-Trichloro-1,2,2-trifluoroethane
Trichloroethylene
Trichlorofluoromethane
Xylene

                                 Table B

Benzene
2-Ethoxyethanol
2-Nitropropane
1,1,2-Trichloroethane

[53 FR 28154, July 26, 1988, as amended at 54 FR 25422, June 14, 1989; 
56 FR 3876, Jan. 31, 1991; 57 FR 8088, Mar. 6, 1992]



Sec.  148.11  Waste specific prohibitions--dioxin-containing wastes.

    (a) Effective August 8, 1988, the dioxin-containing wastes specified 
in Sec.  261.31 as EPA Hazardous Waste Nos. F020, F021, F022, F023, 
F026, F027, and F028, and prohibited from underground injection.
    (b) The requirements of paragraph (a) of this section do not apply:

[[Page 1044]]

    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

[53 FR 28154, July 26, 1988, as amended at 54 FR 25422, June 14, 1989]



Sec.  148.12  Waste specific prohibitions--California list wastes.

    (a) Effective August 8, 1988, the hazardous wastes listed in 40 CFR 
268.32 containing polychlorinated biphenyls at concentrations greater 
than or equal to 50 ppm or halogenated organic compounds at 
concentrations greater than or equal to 10,000 mg/kg are prohibited from 
underground injection.
    (b) Effective August 8, 1990, the following hazardous wastes are 
prohibited from underground injection:
    (1) Liquid hazardous wastes, including free liquids associated with 
any solid or sludge, containing free cyanides at concentrations greater 
than or equal to 1,000 mg/l;
    (2) Liquid hazardous wastes, including free liquids associated with 
any solid or sludge, containing the following metals (or elements) or 
compounds of these metals (or elements) at concentrations greater than 
or equal to those specified below:
    (i) Arsenic and/or compounds (as As) 500 mg/l;
    (ii) Cadmium and/or compounds (as Cd) 100 mg/l;
    (iii) Chromium (VI) and/or compounds (as Cr VI) 500 mg/l;
    (iv) Lead and/or compounds (as Pb) 500 mg/l;
    (v) Mercury and/or compounds (as Hg) 20 mg/l;
    (vi) Nickel and/or compounds (as Ni) 134 mg/l;
    (vii) Selenium and/or compounds (as Se) 100 mg/l; and
    (viii) Thallium and/or compounds (as Tl) 130 mg/l;
    (3) Liquid hazardous waste having a pH less than or equal to two 
(2.0); and
    (4) Hazardous wastes containing halogenated organic compounds in 
total concentration less than 10,000 mg/kg but greater than or equal to 
1,000 mg/kg.
    (c) The requirements of paragraphs (a) and (b) of this section do 
not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension is granted under Sec.  148.4 of this part.

[53 FR 30918, Aug. 16, 1988, as amended at 53 FR 41602, Oct. 24, 1988]



Sec.  148.14  Waste specific prohibitions--first third wastes.

    (a) Effective June 7, 1989, the wastes specified in 40 CFR 261.31 as 
EPA Hazardous Waste numbers F006 (nonwastewaters) and the wastes 
specified in 40 CFR 261.32 as EPA Hazardous Waste numbers K001, K015 
(wastewaters), K016 (at concentrations greater than or equal to 1%), 
K018, K019, K020, K021 (nonwastewaters generated by the process 
described in the waste listing description and disposed after August 17, 
1988, and not generated in the course of treating wastewater forms of 
these wastes), K022 (nonwastewaters), K024, K030, K036 (nonwastewaters 
generated by the process described in the waste listing description and 
disposed after August 17, 1988, and not generated in the course of 
treating wastewater forms of these wastes), K037, K044, K045, 
nonexplosive K046 (nonwastewaters), K047, K048, K060 (nonwastewaters 
generated by the process described in the waste listing description and 
disposed after August 17, 1988, and not generated in the course of 
treating wastewater forms of these wastes), K061 (nonwastewaters), 
noncalcium sulfate K069 (nonwastewaters generated by the process 
described in the waste listing description and disposed after August 17, 
1988, and not generated in the course of treating wastewater forms of 
these wastes), K086 solvent washes, K087, K099, K101 (all wastewaters 
and less than 1% total arsenic nonwastewaters), K102 (all wastewaters

[[Page 1045]]

and less than 1% total arsenic nonwastewaters), and K103 are prohibited 
from underground injection.
    (b) Effective June 8, 1989, the waste specified in 40 CFR 261.32 as 
EPA Hazardous Waste number K036 (wastewaters); and the wastes specified 
in 40 CFR 261.33 as P030, P039, P041, P063, P071, P089, P094, P097, 
U221, and U223 are prohibited from underground injection.
    (c) Effective July 8, 1989, the wastes specified in 40 CFR 261.31 as 
EPA Hazardous Waste numbers F008 and F009 are prohibited from 
underground injection.
    (d) Effective August 8, 1990, the wastes specified in 40 CFR 261.31 
as EPA Hazardous Waste Number F006 (wastewaters) and F019; the wastes 
specified in 40 CFR 261.32 as EPA Hazardous Waste Numbers K004, K008, 
K015 (nonwastewaters), K017, K021 (wastewaters), K022 (wastewaters), 
K031, K035, K046 (reactive nonwastewaters and all wastewaters), K060 
(wastewaters), K061 (wastewaters), K069 (calcium sulfate nonwastewaters 
and all wastewaters), K073, K083, K084, K085, K086 (all but solvent 
washes), K101 (high arsenic nonwastewaters), K102 (high arsenic 
nonwastewaters), and K106; and the wastes specified in 40 CFR part 
261.33 as EPA Hazardous Waste Numbers P001, P004, P005, P010, P011, 
P012, P015, P016, P018, P020, P036, P037, P048, P050, P058, P059, P068, 
P069, P070, P081, P082, P084, P087, P092, P102, P105, P108, P110, P115, 
P120, P122, P123, U007, U009, U010, U012, U016, U018, U019, U022, U029, 
U031, U036, U037, U041, U043, U044, U046, U050, U051, U053, U061, U063, 
U064, U066, U067, U074, U077, U078, U086, U089, U103, U105, U108, U115, 
U122, U124, U129, U130, U133, U134, U137, U151, U154, U155, U157, U158, 
U159, U171, U177, U180, U185, U188, U192, U200, U209, U210, U211, U219, 
U220, U226, U227, U228, U237, U238, U248, and U249 are prohibited from 
underground injection at off-site injection facilities.
    (e) Effective August 8, 1990, the wastes specified in 40 CFR 261.32 
as EPA Hazardous Waste numbers K049, K050, K051, K052, K062, K071, and 
K104 are prohibited from underground injection.
    (f) Effective November 8, 1990, the wastes specified in paragraph 
(d) of this section are prohibited from underground injection at on-site 
injection facilities.
    (g) Effective June 7, 1991, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste numbers K016 (at concentrations less than 1%) are 
prohibited from underground injection.
    (h) Effective June 8, 1991, the waste specified in 40 CFR 261.31 as 
EPA Hazardous Waste number F007; and the wastes specified in 40 CFR 
261.32 as K011 (nonwastewaters) and K013 (nonwastewaters) are prohibited 
from underground injection.
    (i) Effective May 8, 1992, the wastes specified in 40 CFR 261.32 and 
261.33 as EPA Hazardous Waste Numbers K011 (wastewaters), K013 
(wastewaters), and K014 are prohibited from underground injection.
    (j) The requirements of paragraphs (a) through (i) of this section 
do not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

[54 FR 25423, June 14, 1989, as amended at 54 FR 26647, June 23, 1989; 
54 FR 35328, Aug. 25, 1989; 55 FR 22683, June 1, 1990]



Sec.  148.15  Waste specific prohibitions--second third wastes.

    (a) Effective June 7, 1989, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste numbers K025 (nonwastewaters generated by the 
process described in the waste listing description and disposed after 
August 17, 1988, and not generated in the course of treating wastewater 
forms of these wastes) are prohibited from underground injection.
    (b) Effective June 8, 1989, the wastes specified in 40 CFR 261.31 as 
EPA Hazardous Waste numbers F010, F024; the wastes specified in 40 CFR 
261.32 as K009 (nonwastewaters), K010, K027, K028, K029 
(nonwastewaters), K038, K039, K040, K043, K095 (nonwastewaters), K096

[[Page 1046]]

(nonwastewaters), K113, K114, K115, K116; and wastes specified in 40 CFR 
261.33 as P029, P040, P043, P044, P062, P074, P085, P098, P104, P106, 
P111, U028, U058, U107, and U235 are prohibited from underground 
injection.
    (c) Effective July 8, 1989, and continuing until December 8, 1989, 
the wastes specified in 40 CFR 261.31 as EPA Hazardous Waste numbers 
F011 and F012 are prohibited from underground injection pursuant to the 
treatment standards specified in Sec. Sec.  268.41 and 268.43 applicable 
to F007, F008, and F009 wastewaters and nonwastewaters. Effective 
December 8, 1989, F011 (nonwastewaters) and F012 (nonwastewaters) are 
prohibited pursuant to the treatment standards specified in Sec. Sec.  
268.41 and 268.43 applicable to F011 and F012 wastewaters and 
nonwastewaters.
    (d) Effective August 8, 1990, the wastes specified in 40 CFR 261.32 
as EPA Hazardous Waste Number K025 (wastewaters), K029 (wastewaters), 
K041, K042, K095 (wastewaters), K096 (wastewaters), K097, K098, and 
K105; and the wastes specified in 40 CFR part 261.33 as P002, P003, 
P007, P008, P014, P026, P027, P049, P054, P057, P060, P066, P067, P072, 
P107, P112, P113, P114, U002, U003, U005, U008, U011, U014, U015, U020, 
U021, U023, U025, U026, U032, U035, U047, U049, U057, U059, U060, U062, 
U070, U073, U080, U083, U092, U093, U094, U095, U097, U098, U099, U101, 
U106, U109, U110, U111, U114, U116, U119, U127, U128, U131, U135, U138, 
U140, U142, U143, U144, U146, U147, U149, U150, U161, U162, U163, U164, 
U165, U168, U169, U170, U172, U173, U174, U176, U178, U179, U189, U193, 
U196, U203, U205, U206, U208, U213, U214, U215, U216, U217, U218, U239, 
and U244 are prohibited from underground injection at off-site injection 
facilities.
    (e) Effective June 8, 1991, the waste specified in 40 CFR 261.32 as 
EPA Hazardous Waste number K009 (wastewaters) is prohibited from 
underground injection.
    (f) Effective November 8, 1990, the wastes specified in paragraph 
(d) of this section are prohibited from underground injection at on-site 
injection facilities.
    (g) The requirements of paragraphs (a) through (f) of this section 
do not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

[54 FR 25423, June 14, 1989, as amended at 54 FR 26647, June 23, 1989; 
55 FR 22683, June 1, 1990]



Sec.  148.16  Waste specific prohibitions--third third wastes.

    (a) Effective June 7, 1989, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste numbers K100 (nonwastewaters generated by the 
process described in the waste listing description and disposed after 
August 17, 1988, and not generated in the course of treating wastewater 
forms of these wastes) are prohibited from underground injection.
    (b) Effective June 8, 1989, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste numbers K005 (nonwastewaters), K007 
(nonwastewaters), K023, K093, K094; and the wastes specified in 40 CFR 
261.33 as P013, P021, P099, P109, P121, U069, U087, U088, U102, and U190 
are prohibited from underground injection.
    (c) Effective August 8, 1990, the wastes identified in 40 CFR 261.31 
as EPA Hazardous Waste Number F039 (nonwastewaters); the wastes 
specified in 40 CFR 261.32 as EPA Hazardous Waste Numbers K002, K003, 
K005 (wastewaters), K006, K007 (wastewaters), K026, K032, K033, K034, 
and K100 (wastewaters); the wastes specified in 40 CFR 261.33 as P006, 
P009, P017, P022, P023, P024, P028, P031, P033, P034, P038, P042, P045, 
P046, P047, P051, P056, P064, P065, P073, P075, P076, P077, P078, P088, 
P093, P095, P096, P101, P103, P116, P118, P119, U001, U004, U006, U017, 
U024, U027, U030, U033, U034, U038, U039, U042, U045, U048, U052, U055, 
U056, U068, U071, U072, U075, U076, U079, U081, U082, U084, U085, U090, 
U091, U096, U112, U113, U117, U118, U120, U121, U123, U125, U126, U132, 
U136, U141, U145, U148, U152, U153, U156, U160, U166, U167, U181, U182, 
U183, U184, U186, U187, U191, U194, U197, U201,

[[Page 1047]]

U202, U204, U207, U222, U225, U234, U236, U240, U243, U246, and U247; 
and the wastes identified in 40 CFR 261.21, 261.23 or 261.24 as 
hazardous based on a characteristic alone, designated as D001, D004, 
D005, D006, D008, D009 (wastewaters), D010, D011, D012, D013, D014, 
D015, D016, D017, and newly listed waste F025 are prohibited from 
underground injection at off-site injection facilities.
    (d) Effective August 8, 1990, mixed radioactive/hazardous waste in 
40 CFR 268.10, 268.11, and 268.12, that are mixed radioactive and 
hazardous wastes, are prohibited from underground injection.
    (e) Effective November 8, 1990, the wastes specified in paragraph 
(c) of this section are prohibited from underground injection at on-site 
injection facilities. These effective dates do not apply to the wastes 
listed in 40 CFR 148.12(b) which are prohibited from underground 
injection on August 8, 1990.
    (f) Effective May 8, 1992, the waste identified in 40 CFR 261.31 as 
EPA Hazardous Waste Number F039 (wastewaters); the wastes identified in 
40 CFR 261.22, 261.23 or 261.24 as hazardous based on a characteristic 
alone, designated as D002 (wastewaters and nonwastewaters), D003 
(wastewaters and nonwastewaters), D007 (wastewaters and nonwastewaters), 
and D009 (nonwastewaters) are prohibited from underground injection. 
These effective dates do not apply to the wastes listed in 40 CFR 
148.12(b) which are prohibited from underground injection on August 8, 
1990.
    (g) The requirements of paragraphs (a) through (f) of this section 
do not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

[54 FR 25423, June 14, 1989, as amended at 54 FR 26647, June 23, 1989; 
55 FR 22683, June 1, 1990; 55 FR 33694, Aug. 17, 1990; 56 FR 3876, Jan. 
31, 1991]



Sec.  148.17  Waste specific prohibitions; newly listed wastes.

    (a) Effective November 9, 1992, the wastes specified in 40 CFR part 
261 as EPA hazardous waste numbers F037, F038, K107, K108, K109, K110, 
K111, K112, K117, K118, K123, K124, K125, K126, K131, K136, U328, U353, 
and U359 are prohibited from underground injection.
    (b) Effective December 19, 1994 the wastes specified in 40 CFR 
261.32 as EPA Hazardous waste numbers K141, K142, K143, K144, K145, 
K147, K148, K149, K150, and K151, are prohibited from underground 
injection.
    (c) [Reserved]
    (d) Effective June 30, 1995, the wastes specified in 40 CFR part 261 
as EPA Hazardous waste numbers K117, K118, K131, and K132 are prohibited 
from underground injection.
    (e) The requirements of paragraphs (a) and (b) of this section do 
not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4 of this part.

[57 FR 37263, Aug. 18, 1992, as amended at 59 FR 48041, Sept. 19, 1994; 
61 FR 15662, Apr. 8, 1996]



Sec.  148.18  Waste specific prohibitions--newly listed and identified wastes.

    (a) Effective August 24, 1998, all newly identified D004-D011 wastes 
and characteristic mineral processing wastes, except those identified in 
paragraph (b) of this section, are prohibited from underground 
injection.
    (b) Effective May 26, 2000, characteristic hazardous wastes from 
titanium dioxide mineral processing, and radioactive wastes mixed with 
newly identified D004-D011 or mixed with newly identified characteristic 
mineral processing wastes, are prohibited from underground injection.
    (c) Effective August 11, 1997, the wastes specified in 40 CFR part 
261 as EPA Hazardous waste numbers F032, F034, F035 are prohibited from 
underground injection.

[[Page 1048]]

    (d) Effective May 12, 1999, the wastes specified in 40 CFR part 261 
as EPA Hazardous waste numbers F032, F034, F035 that are mixed with 
radioactive wastes are prohibited from underground injection.
    (e) On July 8, 1996, the wastes specified in 40 CFR 261.32 as EPA 
Hazardous waste numbers K156-K161, P127, P128, P185, P188-P192, P194, 
P196-P199, P201-P205, U271, U277-U280, U364-U367, U372, U373, U375-U379, 
U381-387, U389-U396, U400-U404, U407, and U409-U411 are prohibited from 
underground injection.
    (f) On January 8, 1997, the wastes specified in 40 CFR 261.32 as EPA 
Hazardous waste number K088 is prohibited from underground injection.
    (g) On April 8, 1998, the wastes specified in 40 CFR part 261 as EPA 
Hazardous waste numbers D018-043, and Mixed TC/Radioactive wastes, are 
prohibited from underground injection.
    (h) [Reserved]
    (i) Effective February 8, 1999, the wastes specified in 40 CFR 
261.32 as EPA Hazardous Waste Numbers K169, K170, K171, and K172 are 
prohibited from underground injection.
    (j) Effective May 8, 2001, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste Numbers K174 and K175 are prohibited from 
underground injection.
    (k) Effective May 20, 2002, the wastes specified in 40 CFR 261.32 as 
EPA Hazardous Waste Numbers K176, K177, and K178 are prohibited from 
underground injection.
    (l) Effective August 23, 2005, the waste specified in 40 CFR 261.32 
as EPA Hazardous Waste Number K181 is prohibited from underground 
injection.
    (m) The requirements of paragraphs (a) through (l) of this section 
do not apply:
    (1) If the wastes meet or are treated to meet the applicable 
standards specified in subpart D of 40 CFR part 268; or
    (2) If an exemption from a prohibition has been granted in response 
to a petition under subpart C of this part; or
    (3) During the period of extension of the applicable effective date, 
if an extension has been granted under Sec.  148.4.

[61 FR 15662, Apr. 8, 1996, as amended at 62 FR 26018, May 12, 1997; 63 
FR 24624, May 4, 1998; 63 FR 28636, May 26, 1998; 63 FR 35149, June 29, 
1998; 63 FR 42184, Aug. 6, 1998; 65 FR 14474, Mar. 17, 2000; 65 FR 
36366, June 8, 2000; 65 FR 67126, Nov. 8, 2000; 66 FR 58297, Nov. 20, 
2001; 70 FR 9174, Feb. 24, 2005]



               Subpart C_Petition Standards and Procedures



Sec.  148.20  Petitions to allow injection of a waste prohibited 
under subpart B.

    (a) Any person seeking an exemption from a prohibition under subpart 
B of this part for the injection of a restricted hazardous waste into an 
injection well or wells shall submit a petition to the Director 
demonstrating that, to a reasonable degree of certainty, there will be 
no migration of hazardous constituents from the injection zone for as 
long as the waste remains hazardous. This demonstration requires a 
showing that:
    (1) The hydrogeological and geochemical conditions at the sites and 
the physiochemical nature of the waste stream(s) are such that reliable 
predictions can be made that:
    (i) Fluid movement conditions are such that the injected fluids will 
not migrate within 10,000 years:
    (A) Vertically upward out of the injection zone; or
    (B) Laterally within the injection zone to a point of discharge or 
interface with an Underground Source of Drinking Water (USDW) as defined 
in 40 CFR part 146; or
    (ii) Before the injected fluids migrate out of the injection zone or 
to a point of discharge or interface with USDW, the fluid will no longer 
be hazardous because of attenuation, transformation, or immobilization 
of hazardous constituents within the injection zone by hydrolysis, 
chemical interactions or other means; and
    (2) For each well the petition has:
    (i) Demonstrated that the injection well's area of review complies 
with the substantive requirements of Sec.  146.63;
    (ii) Located, identified, and ascertained the condition of all wells

[[Page 1049]]

within the injection well's area of review (as specified in Sec.  
146.63) that penetrate the injection zone or the confining zone by use 
of a protocol acceptable to the Director that meets the substantive 
requirements of Sec.  146.64;
    (iii) Submitted a corrective action plan that meets the substantive 
requirements of Sec.  146.64, the implementation of which shall become a 
condition of petition approval; and
    (iv) Submitted the results of pressure and radioactive tracer tests 
performed within one year prior to submission of the petition 
demonstrating the mechanical integrity of the well's long string casing, 
injection tube, annular seal, and bottom hole cement. In cases where the 
petition has not been approved or denied within one year after the 
initial demonstration of mechanical integrity, the Director may require 
the owner or operator to perform the tests again and submit the results 
of the new tests.
    Note: The requirements of Sec.  148.20(a)(2) need not be 
incorporated in a permit at the time of petition approval.
    (b) A demonstration under Sec.  148.20(a)(1)(i) shall identify the 
strata within the injection zone which will confine fluid movement above 
the injection interval and include a showing that this strata is free of 
known transmissive faults of fractures and that there is a confining 
zone above the injection zone.
    (c) A demonstration under Sec.  148.20(a)(1)(ii) shall identify the 
strata within the injection zone where waste transformation will be 
accomplished and include a showing that this strata is free of known 
transmissive faults or fractures and that there is a confining zone 
above the injection zone.
    (d) A demonstration may include a showing that:
    (1) Treatment methods, the implementation of which shall become a 
condition of petition approval, will be utilized that reduce the 
toxicity or mobility of the wastes; or
    (2) A monitoring plan, the implementation of which shall become a 
condition of petition approval, will be utilized to enhance confidence 
in one or more aspects of the demonstration.
    (e) Any person who has been granted an exemption pursuant to this 
section may submit a petition for reissuance of the exemption to include 
an additional restricted waste or wastes or to modify any conditions 
placed on the exemption by the Director. The Director shall reissue the 
petition if the petitioner complies with the requirements of paragraphs 
(a), (b) and (c) of this section.
    (f) Any person who has been granted an exemption pursuant to this 
section may submit a petition to modify an exemption to include an 
additional (hazardous) waste or wastes. The Director may grant the 
modification if he determines, to a reasonable degree of certainty, that 
the additional waste or wastes will behave hydraulically and chemically 
in a manner similar to previously included wastes and that it will not 
interfere with the containment capability of the injection zone.



Sec.  148.21  Information to be submitted in support of petitions.

    (a) Information submitted in support of Sec.  148.20 must meet the 
following criteria:
    (1) All waste analysis and any new testing performed by the 
petitioner shall be accurate and reproducible and performed in 
accordance with quality assurance standards;
    (2) Estimation techniques shall be appropriate, and EPA-certified 
test protocols shall be used where available and appropriate;
    (3) Predictive models shall have been verified and validated, shall 
be appropriate for the specific site, waste streams, and injection 
conditions of the operation, and shall be calibrated for existing sites 
where sufficient data are available;
    (4) An approved quality assurance and quality control plan shall 
address all aspects of the demonstration;
    (5) Reasonably conservative values shall be used whenever values 
taken from the literature or estimated on the basis of known information 
are used instead of site-specific measurements; and
    (6) An analysis shall be performed to identify and assess aspects of 
the demonstration that contribute significantly to uncertainty. The 
petitioner shall conduct a sensitivity analysis to determine the effect 
that significant

[[Page 1050]]

uncertainty may contribute to the demonstration. The demonstration shall 
then be based on conservative assumptions identified in the analysis.
    (b) Any petitioner under Sec.  148.20(a)(1)(i) shall provide 
sufficient site-specific information to support the demonstration, such 
as:
    (1) Thickness, porosity, permeability and extent of the various 
strata in the injection zone;
    (2) Thickness, porosity, permeability, extent, and continuity of the 
confining zone;
    (3) Hydraulic gradient in the injection zone;
    (4) Hydrostatic pressure in the injection zone; and
    (5) Geochemical conditions of the site.
    (c) In addition to the information in Sec.  148.21(b), any 
petitioner under Sec.  148.20(a)(1)(ii) shall provide sufficient waste-
specific information to ensure reasonably reliant predictions about the 
waste transformation. The petitioner shall provide the information 
necessary to support the demonstration, such as:
    (1) Description of the chemical processes or other means that will 
lead to waste transformation; and
    (2) Results of laboratory experiments verifying the waste 
transformation.



Sec.  148.22  Requirements for petition submission, 
review and approval or denial.

    (a) Any petition submitted to the Director pursuant to Sec.  
148.20(a) shall include the following components:
    (1) An identification of the specific waste or wastes and the 
specific injection well or wells for which the demonstration will be 
made;
    (2) A waste analysis to describe fully the chemical and physical 
characteristics of the subject wastes;
    (3) Such additional information as is required by the Director to 
support the petition under Sec. Sec.  148.20 and 148.21; and
    (4) This statement signed by the petitioner or an authorized 
representative:

    I certify under penalty of law that I have personally examined and 
am familiar with the information submitted in this petition and all 
attached documents, and that, based on my inquiry of those individuals 
immediately responsible for obtaining the information, I believe that 
submitted information is true, accurate, and complete. I am aware that 
there are significant penalties for submitting false information, 
including the possibility of fine and imprisonment.

    (b) The Director shall provide public notice and an opportunity for 
public comment in accordance with the procedures in Sec.  124.10 of the 
intent to approve or deny a petition. The final decision on a petition 
will be published in the Federal Register.
    (c) If an exemption is granted it will apply only to the underground 
injection of the specific restricted waste or wastes identified in the 
petition into a Class I hazardous waste injection well or wells 
specifically identified in the petition (unless the exemption is 
modified or reissued pursuant to Sec.  148.20(e) or (f).
    (d) Upon request by any petitioner who obtains an exemption for a 
well under this subpart, the Director shall initiate and reasonably 
expedite the necessary procedures to issue or reissue a permit or 
permits for the hazardous waste well or wells covered by the exemption 
for a term not to exceed ten years.



Sec.  148.23  Review of exemptions granted pursuant to a petition.

    (a) When considering whether to reissue a permit for the operation 
of a Class I hazardous waste injection well, the Director shall review 
any petition filed pursuant to Sec.  148.20 and require a new 
demonstration if information shows that the basis for granting the 
exemption may no longer be valid.
    (b) Whenever the Director determines that the basis for approval of 
a petition may no longer be valid, the Director shall require a new 
demonstration in accordance with Sec.  148.20.



Sec.  148.24  Termination of approved petition.

    (a) The Director may terminate an exemption granted under Sec.  
148.20 for the following causes:
    (1) Noncompliance by the petitioner with any condition of the 
exemption;
    (2) The petitioner's failure in the petition or during the review 
and approval to disclose fully all relevant facts, or the petitioner's 
misrepresentation of any relevant facts at any time; or

[[Page 1051]]

    (3) A determination that new information shows that the basis for 
approval of the petition is no longer valid.
    (b) The Director shall terminate an exemption granted under Sec.  
148.20 for the following causes:
    (1) The petitioner's willful withholding during the review and 
approval of the petition of facts directly and materially relevant to 
the Director's decision on the petition;
    (2) A determination that there has been migration from the injection 
zone or the well that is not in accordance with the terms of the 
exemption, except that the Director may at his discretion decide not to 
terminate where:
    (i) The migration resulted from a mechanical failure of the well 
that can be corrected promptly through a repair to the injection well 
itself or from an undetected well or conduit that can be plugged 
promptly; and
    (ii) The requirements of Sec.  146.67(i) are satisfied.
    (c) The Director shall follow the procedures in Sec.  124.5 in 
terminating any exemption under this section.



PART 149_SOLE SOURCE AQUIFERS--Table of Contents



  Subpart A_Criteria for Identifying Critical Aquifer Protection Areas

Sec.
149.1 Purpose.
149.2 Definitions.
149.3 Critical Aquifer Protection Areas.

     Subpart B_Review of Projects Affecting the Edwards Underground 
 Reservoir, A Designated Sole Source Aquifer in the San Antonio, Texas 
                                  Area

149.100 Applicability.
149.101 Definitions.
149.102 Project review authority.
149.103 Public information.
149.104 Submission of petitions.
149.105 Decision to review.
149.106 Notice of review.
149.107 Request for information.
149.108 Public hearing.
149.109 Decision under section 1424(e).
149.110 Resubmittal of redesigned projects.
149.111 Funding to redesigned projects.

    Authority: Sec. 1424(e), Safe Drinking Water Act (42 U.S.C. 300h-
3(e); sec. 1427 of the Safe Drinking Water Act, (42 U.S.C. 300h-6).



  Subpart A_Criteria for Identifying Critical Aquifer Protection Areas

    Source: 52 FR 23986, June 26, 1987, unless otherwise noted.



Sec.  149.1  Purpose.

    The purpose of this subpart is to provide criteria for identifying 
critical aquifer protection areas, pursuant to section 1427 of the Safe 
Drinking Water Act (SDWA).



Sec.  149.2  Definitions.

    (a) Aquifer means a geological formation, group of formations, or 
part of a formation that is capable of yielding a significant amount of 
water to a well or spring.
    (b) Recharge means a process, natural or artificial, by which water 
is added to the saturated zone of an aquifer.
    (c) Recharge Area means an area in which water reaches the zone of 
saturation (ground water) by surface infiltration; in addition, a major 
recharge area is an area where a major part of the recharge to an 
aquifer occurs.
    (d) Sole or Principal Source Aquifer (SSA) means an aquifer which is 
designated as an SSA under section 1424(e) of the SDWA.

[54 FR 6843, Feb. 14, 1989]



Sec.  149.3  Critical Aquifer Protection Areas.

    A Critical Aquifer Protection Area is either:
    (a) All or part of an area which was designated as a sole or 
principal source aquifer prior to June 19, 1986, and for which an 
areawide ground-water quality protection plan was approved, under 
section 208 of the Clean Water Act, prior to that date; or
    (b) All or part of a major recharge area of a sole or principal 
source aquifer, designated before June 19, 1988, for which:
    (1) The sole or principal source aquifer is particularly vulnerable 
to contamination due to the hydrogeologic characteristics of the 
unsaturated or saturated zone within the suggested critical aquifer 
protection area; and
    (2) Contamination of the sole or principal source aquifer is 
reasonably likely to occur, unless a program to reduce

[[Page 1052]]

or prevent such contamination is implemented; and
    (3) In the absence of any program to reduce or prevent 
contamination, reasonably foreseeable contamination would result in 
significant cost, taking into account:
    (i) The cost of replacing the drinking water supply from the sole or 
principal source aquifer, and
    (ii) Other economic costs and environmental and social costs 
resulting from such contamination.

[54 FR 6843, Feb. 14, 1989]



     Subpart B_Review of Projects Affecting the Edwards Underground 
 Reservoir, A Designated Sole Source Aquifer in the San Antonio, Texas 
                                  Area

    Source: 42 FR 51574, Sept. 29, 1977, unless otherwise noted. 
Redesignated at 52 FR 23986, June 26, 1987.



Sec.  149.100  Applicability.

    This subpart sets forth, pursuant to sections 1424(e) and 1450 of 
the Public Health Service Act, as amended by the Safe Drinking Water 
Act, Pub. L. 93-523, regulations relating the Edwards Underground 
Reservoir which is the sole or principal drinking water source for the 
San Antonio area and which, if contaminated, would create a significant 
hazard to public health.

[42 FR 51574, Sept. 29, 1977. Redesignated and amended at 52 FR 23986, 
June 26, 1987]



Sec.  149.101  Definitions.

    As used in this subpart and except as otherwise specifically 
provided, the term(s):
    (a) Act means the Public Health Service Act, as amended by the Safe 
Drinking Water Act, Public Law 93-523.
    (b) Contaminant means any physical, chemical, biological, or 
radiological substance or matter in water.
    (c) Recharge zone means the area through which water enters the 
Edwards Underground Reservoir as defined in the December 16, 1975, 
Notice of Determination.
    (d) Administrator (Regional Administrator) means the Administrator 
(Regional Administrator) of the United States Environmental Protection 
Agency.
    (e) Person means an individual, corporation, company, association, 
partnership, State, or municipality.
    (f) Project means a program or action for which an application for 
Federal financial assistance has been made.
    (g) Federal financial assistance means any financial benefits 
provided directly as aid to a project by a department, agency, or 
instrumentality of the Federal government in any form including 
contracts, grants, and loan guarantees. Actions or programs carried out 
by the Federal government itself such as dredging performed by the Army 
Corps of Engineers do not involve Federal financial assistance. Actions 
performed for the Federal government by contractors, such as 
construction of roads on Federal lands by a contractor under the 
supervision of the Bureau of Land Management, should be distinguished 
from contracts entered into specifically for the purpose of providing 
financial assistance, and will not be considered programs or actions 
receiving Federal financial assistance. Federal financial assistance is 
limited to benefits earmarked for a specific program or action and 
directly awarded to the program or action. Indirect assistance, e.g., in 
the form of a loan to a developer by a lending institution which in turn 
receives Federal assistance not specifically related to the project in 
question is not Federal financial assistance under section 1424(e).
    (h) Commitment of Federal financial assistance means a written 
agreement entered into by a department, agency, or instrumentality of 
the Federal Government to provide financial assistance as defined in 
paragraph (g) of this section. Renewal of a commitment which the issuing 
agency determines has lapsed shall not constitute a new commitment 
unless the Regional Administrator determines that the project's impact 
on the aquifer has not been previously reviewed under section 1424(e). 
The determination of a Federal agency that a certain written agreement 
constitutes a commitment shall be conclusive with respect to the 
existence of such a commitment.
    (i) Streamflow source zone means the upstream headwaters area which 
drains

[[Page 1053]]

into the recharge zone as defined in the December 16, 1975, Notice of 
Determination.
    (j) Significant hazard to public health means any level of 
contaminant which causes or may cause the aquifer to exceed any maximum 
contaminant level set forth in any promulgated National Primary Drinking 
Water Standard at any point where the water may be used for drinking 
purposes or which may otherwise adversely affect the health of persons, 
or which may require a public water system to install additional 
treatment to prevent such adverse effect.
    (k) Aquifer means the Edwards Underground Reservoir.

[42 FR 51574, Sept. 29, 1977. Redesignated and amended at 52 FR 23986, 
June 26, 1987]



Sec.  149.102  Project review authority.

    (a) Once an area is designated, no subsequent commitments of Federal 
financial assistance may be made to projects which the Administrator 
determines may contaminate the aquifer so as to create a significant 
hazard to public health.
    (b) The Regional Administrator is hereby delegated the authority and 
assigned responsibility for carrying out the project review process 
assigned to the Administrator under section 1424(e) of the Act, except 
the final determination that a project may contaminate the aquifer 
through its recharge zone so as to create a significant hazard to public 
health.
    (c) The Regional Administrator may review any project which he 
considers may potentially contaminate the aquifer through its recharge 
zone so as to create a significant hazard to public health.



Sec.  149.103  Public information.

    After the area is designated under section 1424(e), Federal 
agencies, for projects, located in the recharge zone and streamflow 
source zones, are required to:
    (a) Maintain a list of projects for which environmental impact 
statements will be prepared in accordance with the National 
Environmental Policy Act (NEPA);
    (b) Revise the list at regular intervals and submit to EPA; and
    (c) Make the list available to the public upon request.



Sec.  149.104  Submission of petitions.

    Any person may submit a petition requesting the Regional 
Administrator to review a project to determine if such project may 
contaminate the aquifer through its recharge zone so as to create a 
significant hazard to public health. Any such petition shall identify:
    (a) The name, address, and telephone number of the individual, 
organization, or other entity submitting the petition;
    (b) A brief statement of the requesting person's interest in the 
Regional Administrator's determination;
    (c) The name of the project and Federal agency involved;

In addition, the petitioner is requested to submit to EPA available 
information on:
    (d) Applicable action already taken by State and local agencies 
including establishment of regulations to prevent contamination of the 
aquifer and why, in the petitioner's judgment, the action was 
inadequate.
    (e) Any actions taken under the National Environmental Policy Act 
and why, in the petitioner's judgment, that action was inadequate in 
regard to evaluation of potential effect on the aquifer.
    (f) The potential contaminants involved;
    (g) The means by which the contaminant might enter the aquifer; and
    (h) The potential impact of the proposed project.



Sec.  149.105  Decision to review.

    (a) The Regional Administrator shall review under section 1424(e) 
all projects located in the recharge or streamflow source zone of the 
aquifer for which a draft or final EIS is submitted which may have an 
impact on ground water quality and which involve Federal financial 
assistance as defined in these regulations.
    (b) Upon receipt of a public petition, the Regional Administrator 
shall decide whether the project which is the subject of the petition 
should be reviewed under section 1424(e).

[[Page 1054]]

    (c) The Regional Administrator may decide to review a project upon 
his own motion.
    (d) In determining whether to review a project upon receipt of a 
public petition or upon his own motion, the Regional Administrator shall 
consider whether the project is likely to directly or indirectly cause 
contamination of the aquifer through its recharge zone, taking into 
account any factors he deems relevant, including:
    (1) The location of the project, and
    (2) The nature of the project.
    (e) In determining whether to review a project upon receipt of a 
public petition or upon his own motion, the Regional Administrator may 
consult with, or request information from, the Federal agency to which 
the project application has been made, the applicant seeking Federal 
assistance, appropriate State and local agencies, and other appropriate 
persons or entities.
    (f) In determining whether to review a project which is the subject 
of a public petition, the Regional Administrator may request such 
additional information from the petitioner as he deems necessary.



Sec.  149.106  Notice of review.

    (a) Notice to Federal agency. If the Regional Administrator decides 
upon receipt of a public petition or upon his own motion to review a 
project under section 1424(e), he shall give written notification of the 
decision to the Federal agency from which financial assistance is 
sought. The notification shall include a description and identification 
of the project.
    (b) Notice to public. When the Regional Administrator undertakes to 
review a project pursuant to Sec.  149.13 above, he shall provide public 
notice of project review by such means as he deems appropriate. The 
notice shall set forth the availability for public review of all data 
and information available, and shall solicit comments, data and 
information with respect to the determination of impact under section 
1424(e). The period for public comment shall be 30 days after public 
notice unless the Regional Administrator extends the period at his 
discretion or a public hearing is held under Sec.  149.16.



Sec.  149.107  Request for information.

    In reviewing a project under section 1424(e), the Regional 
Administrator may request any additional information from the funding 
Federal agency which is pertinent to reaching a decision. If full 
evaluation of the groundwater impact of a project has not been submitted 
in accordance with the agency's NEPA procedures, the Regional 
Administrator may specifically request that the Federal agency submit a 
groundwater impact evaluation of whether the proposed project may 
contaminate the aquifer through its recharge zone so as to create a 
significant hazard to public health.



Sec.  149.108  Public hearing.

    If there is significant public interest, the Regional Administrator 
may hold a public hearing with respect to any project or projects to be 
reviewed if he finds that such a hearing is necessary and would be 
helpful in clarifying the issues. Public hearings held under this 
section should be coordinated, if possible, with other Federal public 
hearings held pursuant to applicable laws and regulations. Any such 
hearing shall be conducted by the Regional Administrator or designee in 
an informal, orderly and expeditious manner. Where appropriate, limits 
may be placed upon the time allowed for oral statements, and statements 
may be required to be submitted in writing. The record will be held open 
for further public comment for seven (7) days following the close of the 
public hearing.



Sec.  149.109  Decision under section 1424(e).

    (a) As soon as practicable after the submission of public comments 
under section 1424(e) and information requested by the Environmental 
Protection Agency from the originating Federal agency, on the basis of 
such information as is available to him, the Regional Administrator 
shall review the project taking all relevant factors into account 
including:
    (1) The extent of possible public health hazard presented by the 
project;
    (2) Planning, design, construction, operation, maintenance and 
monitoring measures included in the project

[[Page 1055]]

which would prevent or mitigate the possible health hazard;
    (3) The extent and effectiveness of State or local control over 
possible contaminant releases to the aquifer;
    (4) The cumulative and secondary impacts of the proposed project; 
and
    (5) The expected environmental benefits of the proposed project.
    (b) After reviewing the available information, the Regional 
Administrator shall:
    (1) Determine that the risk of contamination of the aquifer through 
the recharge zone so as to create a significant hazard to public health 
is not sufficiently great so as to prevent commitment of Federal funding 
to the project; or
    (2) Forward the information to the Administrator with his 
recommendation that the project may contaminate the aquifer through the 
recharge zone so as to create a significant hazard to public health.
    (c) After receiving the available information forwarded by the 
Regional Administrator, the Administrator shall:
    (1) Determine that the risk of contamination of the aquifer through 
the recharge zone so as to create a significant hazard to public health 
is not sufficiently great so as to prevent commitment of Federal funding 
to the project; or
    (2) Determine that the project may contaminate the aquifer through 
the recharge zone so as to create a significant hazard to public health.
    (d) Notice of any decisions by the Regional Administrator under 
paragraph (b)(1) of this section or by the Administrator under 
paragraphs (c)(1) and (2) of this section to prevent a commitment of 
Federal funding shall be published in the Federal Register. Such notices 
shall include a description of the propsed project, and a statement of 
decision with an accompanying statement of facts and reasons.



Sec.  149.110  Resubmittal of redesigned projects.

    If a project is redesigned in response to EPA's objections, the 
applicant for Federal financial assistance or the grantor agency may 
file a petition with the Regional Administrator for withdrawal of the 
determination that the project may contaminate the aquifer through the 
recharge zone so as to create a significant hazard to public health. Any 
such petition shall demonstrate how the project has been redesigned so 
as to justify the withdrawal of EPA's objections. If appropriate, the 
Regional Administrator may request public comments or hold an informal 
public hearing to consider the petition. After review of pertinent 
information, the Regional Administrator shall either deny the petition 
or recommend to the Administrator that the initial determination that a 
project may contaminate the aquifer be vacated. Upon receipt of a 
recommendation from the Regional Administrator that a determination be 
vacated, the Administrator shall either deny the petition or order that 
the initial determination be vacated. The final decision regarding a 
petition shall be published in the Federal Register with an accompanying 
statement of reasons.



Sec.  149.111  Funding to redesigned projects.

    After publication of a decision that a proposed project may 
contaminate a sole or principal source aquifer in a designated area 
through its recharge zone so as to create a significant hazard to public 
health, a commitment for Federal financial assistance may be entered 
into, if authorized under another provision of law, to plan or redesign 
such project to assure that it will not so contaminate the aquifer.

[[Page 1057]]



                              FINDING AIDS




  --------------------------------------------------------------------

  A list of CFR titles, subtitles, chapters, subchapters and parts and 
an alphabetical list of agencies publishing in the CFR are included in 
the CFR Index and Finding Aids volume to the Code of Federal Regulations 
which is published separately and revised annually.

  Table of CFR Titles and Chapters
  Alphabetical List of Agencies Appearing in the CFR
  List of CFR Sections Affected

[[Page 1059]]



                    Table of CFR Titles and Chapters




                      (Revised as of July 1, 2018)

                      Title 1--General Provisions

         I  Administrative Committee of the Federal Register 
                (Parts 1--49)
        II  Office of the Federal Register (Parts 50--299)
       III  Administrative Conference of the United States (Parts 
                300--399)
        IV  Miscellaneous Agencies (Parts 400--599)
        VI  National Capital Planning Commission (Parts 600--699)

                    Title 2--Grants and Agreements

            Subtitle A--Office of Management and Budget Guidance 
                for Grants and Agreements
         I  Office of Management and Budget Governmentwide 
                Guidance for Grants and Agreements (Parts 2--199)
        II  Office of Management and Budget Guidance (Parts 200--
                299)
            Subtitle B--Federal Agency Regulations for Grants and 
                Agreements
       III  Department of Health and Human Services (Parts 300--
                399)
        IV  Department of Agriculture (Parts 400--499)
        VI  Department of State (Parts 600--699)
       VII  Agency for International Development (Parts 700--799)
      VIII  Department of Veterans Affairs (Parts 800--899)
        IX  Department of Energy (Parts 900--999)
         X  Department of the Treasury (Parts 1000--1099)
        XI  Department of Defense (Parts 1100--1199)
       XII  Department of Transportation (Parts 1200--1299)
      XIII  Department of Commerce (Parts 1300--1399)
       XIV  Department of the Interior (Parts 1400--1499)
        XV  Environmental Protection Agency (Parts 1500--1599)
     XVIII  National Aeronautics and Space Administration (Parts 
                1800--1899)
        XX  United States Nuclear Regulatory Commission (Parts 
                2000--2099)
      XXII  Corporation for National and Community Service (Parts 
                2200--2299)
     XXIII  Social Security Administration (Parts 2300--2399)
      XXIV  Department of Housing and Urban Development (Parts 
                2400--2499)
       XXV  National Science Foundation (Parts 2500--2599)
      XXVI  National Archives and Records Administration (Parts 
                2600--2699)

[[Page 1060]]

     XXVII  Small Business Administration (Parts 2700--2799)
    XXVIII  Department of Justice (Parts 2800--2899)
      XXIX  Department of Labor (Parts 2900--2999)
       XXX  Department of Homeland Security (Parts 3000--3099)
      XXXI  Institute of Museum and Library Services (Parts 3100--
                3199)
     XXXII  National Endowment for the Arts (Parts 3200--3299)
    XXXIII  National Endowment for the Humanities (Parts 3300--
                3399)
     XXXIV  Department of Education (Parts 3400--3499)
      XXXV  Export-Import Bank of the United States (Parts 3500--
                3599)
     XXXVI  Office of National Drug Control Policy, Executive 
                Office of the President (Parts 3600--3699)
    XXXVII  Peace Corps (Parts 3700--3799)
     LVIII  Election Assistance Commission (Parts 5800--5899)
       LIX  Gulf Coast Ecosystem Restoration Council (Parts 5900--
                5999)

                        Title 3--The President

         I  Executive Office of the President (Parts 100--199)

                           Title 4--Accounts

         I  Government Accountability Office (Parts 1--199)

                   Title 5--Administrative Personnel

         I  Office of Personnel Management (Parts 1--1199)
        II  Merit Systems Protection Board (Parts 1200--1299)
       III  Office of Management and Budget (Parts 1300--1399)
        IV  Office of Personnel Management and Office of the 
                Director of National Intelligence (Parts 1400--
                1499)
         V  The International Organizations Employees Loyalty 
                Board (Parts 1500--1599)
        VI  Federal Retirement Thrift Investment Board (Parts 
                1600--1699)
      VIII  Office of Special Counsel (Parts 1800--1899)
        IX  Appalachian Regional Commission (Parts 1900--1999)
        XI  Armed Forces Retirement Home (Parts 2100--2199)
       XIV  Federal Labor Relations Authority, General Counsel of 
                the Federal Labor Relations Authority and Federal 
                Service Impasses Panel (Parts 2400--2499)
       XVI  Office of Government Ethics (Parts 2600--2699)
       XXI  Department of the Treasury (Parts 3100--3199)
      XXII  Federal Deposit Insurance Corporation (Parts 3200--
                3299)
     XXIII  Department of Energy (Parts 3300--3399)
      XXIV  Federal Energy Regulatory Commission (Parts 3400--
                3499)
       XXV  Department of the Interior (Parts 3500--3599)
      XXVI  Department of Defense (Parts 3600--3699)

[[Page 1061]]

    XXVIII  Department of Justice (Parts 3800--3899)
      XXIX  Federal Communications Commission (Parts 3900--3999)
       XXX  Farm Credit System Insurance Corporation (Parts 4000--
                4099)
      XXXI  Farm Credit Administration (Parts 4100--4199)
    XXXIII  Overseas Private Investment Corporation (Parts 4300--
                4399)
     XXXIV  Securities and Exchange Commission (Parts 4400--4499)
      XXXV  Office of Personnel Management (Parts 4500--4599)
     XXXVI  Department of Homeland Security (Parts 4600--4699)
    XXXVII  Federal Election Commission (Parts 4700--4799)
        XL  Interstate Commerce Commission (Parts 5000--5099)
       XLI  Commodity Futures Trading Commission (Parts 5100--
                5199)
      XLII  Department of Labor (Parts 5200--5299)
     XLIII  National Science Foundation (Parts 5300--5399)
       XLV  Department of Health and Human Services (Parts 5500--
                5599)
      XLVI  Postal Rate Commission (Parts 5600--5699)
     XLVII  Federal Trade Commission (Parts 5700--5799)
    XLVIII  Nuclear Regulatory Commission (Parts 5800--5899)
      XLIX  Federal Labor Relations Authority (Parts 5900--5999)
         L  Department of Transportation (Parts 6000--6099)
       LII  Export-Import Bank of the United States (Parts 6200--
                6299)
      LIII  Department of Education (Parts 6300--6399)
       LIV  Environmental Protection Agency (Parts 6400--6499)
        LV  National Endowment for the Arts (Parts 6500--6599)
       LVI  National Endowment for the Humanities (Parts 6600--
                6699)
      LVII  General Services Administration (Parts 6700--6799)
     LVIII  Board of Governors of the Federal Reserve System 
                (Parts 6800--6899)
       LIX  National Aeronautics and Space Administration (Parts 
                6900--6999)
        LX  United States Postal Service (Parts 7000--7099)
       LXI  National Labor Relations Board (Parts 7100--7199)
      LXII  Equal Employment Opportunity Commission (Parts 7200--
                7299)
     LXIII  Inter-American Foundation (Parts 7300--7399)
      LXIV  Merit Systems Protection Board (Parts 7400--7499)
       LXV  Department of Housing and Urban Development (Parts 
                7500--7599)
      LXVI  National Archives and Records Administration (Parts 
                7600--7699)
     LXVII  Institute of Museum and Library Services (Parts 7700--
                7799)
    LXVIII  Commission on Civil Rights (Parts 7800--7899)
      LXIX  Tennessee Valley Authority (Parts 7900--7999)
       LXX  Court Services and Offender Supervision Agency for the 
                District of Columbia (Parts 8000--8099)
      LXXI  Consumer Product Safety Commission (Parts 8100--8199)
    LXXIII  Department of Agriculture (Parts 8300--8399)

[[Page 1062]]

     LXXIV  Federal Mine Safety and Health Review Commission 
                (Parts 8400--8499)
     LXXVI  Federal Retirement Thrift Investment Board (Parts 
                8600--8699)
    LXXVII  Office of Management and Budget (Parts 8700--8799)
      LXXX  Federal Housing Finance Agency (Parts 9000--9099)
   LXXXIII  Special Inspector General for Afghanistan 
                Reconstruction (Parts 9300--9399)
    LXXXIV  Bureau of Consumer Financial Protection (Parts 9400--
                9499)
    LXXXVI  National Credit Union Administration (Parts 9600--
                9699)
     XCVII  Department of Homeland Security Human Resources 
                Management System (Department of Homeland 
                Security--Office of Personnel Management) (Parts 
                9700--9799)
    XCVIII  Council of the Inspectors General on Integrity and 
                Efficiency (Parts 9800--9899)
      XCIX  Military Compensation and Retirement Modernization 
                Commission (Parts 9900--9999)
         C  National Council on Disability (Parts 10000--10049)

                      Title 6--Domestic Security

         I  Department of Homeland Security, Office of the 
                Secretary (Parts 1--199)
         X  Privacy and Civil Liberties Oversight Board (Parts 
                1000--1099)

                         Title 7--Agriculture

            Subtitle A--Office of the Secretary of Agriculture 
                (Parts 0--26)
            Subtitle B--Regulations of the Department of 
                Agriculture
         I  Agricultural Marketing Service (Standards, 
                Inspections, Marketing Practices), Department of 
                Agriculture (Parts 27--209)
        II  Food and Nutrition Service, Department of Agriculture 
                (Parts 210--299)
       III  Animal and Plant Health Inspection Service, Department 
                of Agriculture (Parts 300--399)
        IV  Federal Crop Insurance Corporation, Department of 
                Agriculture (Parts 400--499)
         V  Agricultural Research Service, Department of 
                Agriculture (Parts 500--599)
        VI  Natural Resources Conservation Service, Department of 
                Agriculture (Parts 600--699)
       VII  Farm Service Agency, Department of Agriculture (Parts 
                700--799)
      VIII  Grain Inspection, Packers and Stockyards 
                Administration (Federal Grain Inspection Service), 
                Department of Agriculture (Parts 800--899)
        IX  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Fruits, Vegetables, Nuts), Department 
                of Agriculture (Parts 900--999)

[[Page 1063]]

         X  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Milk), Department of Agriculture 
                (Parts 1000--1199)
        XI  Agricultural Marketing Service (Marketing Agreements 
                and Orders; Miscellaneous Commodities), Department 
                of Agriculture (Parts 1200--1299)
       XIV  Commodity Credit Corporation, Department of 
                Agriculture (Parts 1400--1499)
        XV  Foreign Agricultural Service, Department of 
                Agriculture (Parts 1500--1599)
       XVI  Rural Telephone Bank, Department of Agriculture (Parts 
                1600--1699)
      XVII  Rural Utilities Service, Department of Agriculture 
                (Parts 1700--1799)
     XVIII  Rural Housing Service, Rural Business-Cooperative 
                Service, Rural Utilities Service, and Farm Service 
                Agency, Department of Agriculture (Parts 1800--
                2099)
        XX  Local Television Loan Guarantee Board (Parts 2200--
                2299)
       XXV  Office of Advocacy and Outreach, Department of 
                Agriculture (Parts 2500--2599)
      XXVI  Office of Inspector General, Department of Agriculture 
                (Parts 2600--2699)
     XXVII  Office of Information Resources Management, Department 
                of Agriculture (Parts 2700--2799)
    XXVIII  Office of Operations, Department of Agriculture (Parts 
                2800--2899)
      XXIX  Office of Energy Policy and New Uses, Department of 
                Agriculture (Parts 2900--2999)
       XXX  Office of the Chief Financial Officer, Department of 
                Agriculture (Parts 3000--3099)
      XXXI  Office of Environmental Quality, Department of 
                Agriculture (Parts 3100--3199)
     XXXII  Office of Procurement and Property Management, 
                Department of Agriculture (Parts 3200--3299)
    XXXIII  Office of Transportation, Department of Agriculture 
                (Parts 3300--3399)
     XXXIV  National Institute of Food and Agriculture (Parts 
                3400--3499)
      XXXV  Rural Housing Service, Department of Agriculture 
                (Parts 3500--3599)
     XXXVI  National Agricultural Statistics Service, Department 
                of Agriculture (Parts 3600--3699)
    XXXVII  Economic Research Service, Department of Agriculture 
                (Parts 3700--3799)
   XXXVIII  World Agricultural Outlook Board, Department of 
                Agriculture (Parts 3800--3899)
       XLI  [Reserved]
      XLII  Rural Business-Cooperative Service and Rural Utilities 
                Service, Department of Agriculture (Parts 4200--
                4299)

[[Page 1064]]

                    Title 8--Aliens and Nationality

         I  Department of Homeland Security (Immigration and 
                Naturalization) (Parts 1--499)
         V  Executive Office for Immigration Review, Department of 
                Justice (Parts 1000--1399)

                 Title 9--Animals and Animal Products

         I  Animal and Plant Health Inspection Service, Department 
                of Agriculture (Parts 1--199)
        II  Grain Inspection, Packers and Stockyards 
                Administration (Packers and Stockyards Programs), 
                Department of Agriculture (Parts 200--299)
       III  Food Safety and Inspection Service, Department of 
                Agriculture (Parts 300--599)

                           Title 10--Energy

         I  Nuclear Regulatory Commission (Parts 0--199)
        II  Department of Energy (Parts 200--699)
       III  Department of Energy (Parts 700--999)
         X  Department of Energy (General Provisions) (Parts 
                1000--1099)
      XIII  Nuclear Waste Technical Review Board (Parts 1300--
                1399)
      XVII  Defense Nuclear Facilities Safety Board (Parts 1700--
                1799)
     XVIII  Northeast Interstate Low-Level Radioactive Waste 
                Commission (Parts 1800--1899)

                      Title 11--Federal Elections

         I  Federal Election Commission (Parts 1--9099)
        II  Election Assistance Commission (Parts 9400--9499)

                      Title 12--Banks and Banking

         I  Comptroller of the Currency, Department of the 
                Treasury (Parts 1--199)
        II  Federal Reserve System (Parts 200--299)
       III  Federal Deposit Insurance Corporation (Parts 300--399)
        IV  Export-Import Bank of the United States (Parts 400--
                499)
         V  Office of Thrift Supervision, Department of the 
                Treasury (Parts 500--599)
        VI  Farm Credit Administration (Parts 600--699)
       VII  National Credit Union Administration (Parts 700--799)
      VIII  Federal Financing Bank (Parts 800--899)
        IX  Federal Housing Finance Board (Parts 900--999)
         X  Bureau of Consumer Financial Protection (Parts 1000--
                1099)
        XI  Federal Financial Institutions Examination Council 
                (Parts 1100--1199)
       XII  Federal Housing Finance Agency (Parts 1200--1299)

[[Page 1065]]

      XIII  Financial Stability Oversight Council (Parts 1300--
                1399)
       XIV  Farm Credit System Insurance Corporation (Parts 1400--
                1499)
        XV  Department of the Treasury (Parts 1500--1599)
       XVI  Office of Financial Research (Parts 1600--1699)
      XVII  Office of Federal Housing Enterprise Oversight, 
                Department of Housing and Urban Development (Parts 
                1700--1799)
     XVIII  Community Development Financial Institutions Fund, 
                Department of the Treasury (Parts 1800--1899)

               Title 13--Business Credit and Assistance

         I  Small Business Administration (Parts 1--199)
       III  Economic Development Administration, Department of 
                Commerce (Parts 300--399)
        IV  Emergency Steel Guarantee Loan Board (Parts 400--499)
         V  Emergency Oil and Gas Guaranteed Loan Board (Parts 
                500--599)

                    Title 14--Aeronautics and Space

         I  Federal Aviation Administration, Department of 
                Transportation (Parts 1--199)
        II  Office of the Secretary, Department of Transportation 
                (Aviation Proceedings) (Parts 200--399)
       III  Commercial Space Transportation, Federal Aviation 
                Administration, Department of Transportation 
                (Parts 400--1199)
         V  National Aeronautics and Space Administration (Parts 
                1200--1299)
        VI  Air Transportation System Stabilization (Parts 1300--
                1399)

                 Title 15--Commerce and Foreign Trade

            Subtitle A--Office of the Secretary of Commerce (Parts 
                0--29)
            Subtitle B--Regulations Relating to Commerce and 
                Foreign Trade
         I  Bureau of the Census, Department of Commerce (Parts 
                30--199)
        II  National Institute of Standards and Technology, 
                Department of Commerce (Parts 200--299)
       III  International Trade Administration, Department of 
                Commerce (Parts 300--399)
        IV  Foreign-Trade Zones Board, Department of Commerce 
                (Parts 400--499)
       VII  Bureau of Industry and Security, Department of 
                Commerce (Parts 700--799)
      VIII  Bureau of Economic Analysis, Department of Commerce 
                (Parts 800--899)
        IX  National Oceanic and Atmospheric Administration, 
                Department of Commerce (Parts 900--999)

[[Page 1066]]

        XI  National Technical Information Service, Department of 
                Commerce (Parts 1100--1199)
      XIII  East-West Foreign Trade Board (Parts 1300--1399)
       XIV  Minority Business Development Agency (Parts 1400--
                1499)
            Subtitle C--Regulations Relating to Foreign Trade 
                Agreements
        XX  Office of the United States Trade Representative 
                (Parts 2000--2099)
            Subtitle D--Regulations Relating to Telecommunications 
                and Information
     XXIII  National Telecommunications and Information 
                Administration, Department of Commerce (Parts 
                2300--2399) [Reserved]

                    Title 16--Commercial Practices

         I  Federal Trade Commission (Parts 0--999)
        II  Consumer Product Safety Commission (Parts 1000--1799)

             Title 17--Commodity and Securities Exchanges

         I  Commodity Futures Trading Commission (Parts 1--199)
        II  Securities and Exchange Commission (Parts 200--399)
        IV  Department of the Treasury (Parts 400--499)

          Title 18--Conservation of Power and Water Resources

         I  Federal Energy Regulatory Commission, Department of 
                Energy (Parts 1--399)
       III  Delaware River Basin Commission (Parts 400--499)
        VI  Water Resources Council (Parts 700--799)
      VIII  Susquehanna River Basin Commission (Parts 800--899)
      XIII  Tennessee Valley Authority (Parts 1300--1399)

                       Title 19--Customs Duties

         I  U.S. Customs and Border Protection, Department of 
                Homeland Security; Department of the Treasury 
                (Parts 0--199)
        II  United States International Trade Commission (Parts 
                200--299)
       III  International Trade Administration, Department of 
                Commerce (Parts 300--399)
        IV  U.S. Immigration and Customs Enforcement, Department 
                of Homeland Security (Parts 400--599) [Reserved]

                     Title 20--Employees' Benefits

         I  Office of Workers' Compensation Programs, Department 
                of Labor (Parts 1--199)
        II  Railroad Retirement Board (Parts 200--399)

[[Page 1067]]

       III  Social Security Administration (Parts 400--499)
        IV  Employees' Compensation Appeals Board, Department of 
                Labor (Parts 500--599)
         V  Employment and Training Administration, Department of 
                Labor (Parts 600--699)
        VI  Office of Workers' Compensation Programs, Department 
                of Labor (Parts 700--799)
       VII  Benefits Review Board, Department of Labor (Parts 
                800--899)
      VIII  Joint Board for the Enrollment of Actuaries (Parts 
                900--999)
        IX  Office of the Assistant Secretary for Veterans' 
                Employment and Training Service, Department of 
                Labor (Parts 1000--1099)

                       Title 21--Food and Drugs

         I  Food and Drug Administration, Department of Health and 
                Human Services (Parts 1--1299)
        II  Drug Enforcement Administration, Department of Justice 
                (Parts 1300--1399)
       III  Office of National Drug Control Policy (Parts 1400--
                1499)

                      Title 22--Foreign Relations

         I  Department of State (Parts 1--199)
        II  Agency for International Development (Parts 200--299)
       III  Peace Corps (Parts 300--399)
        IV  International Joint Commission, United States and 
                Canada (Parts 400--499)
         V  Broadcasting Board of Governors (Parts 500--599)
       VII  Overseas Private Investment Corporation (Parts 700--
                799)
        IX  Foreign Service Grievance Board (Parts 900--999)
         X  Inter-American Foundation (Parts 1000--1099)
        XI  International Boundary and Water Commission, United 
                States and Mexico, United States Section (Parts 
                1100--1199)
       XII  United States International Development Cooperation 
                Agency (Parts 1200--1299)
      XIII  Millennium Challenge Corporation (Parts 1300--1399)
       XIV  Foreign Service Labor Relations Board; Federal Labor 
                Relations Authority; General Counsel of the 
                Federal Labor Relations Authority; and the Foreign 
                Service Impasse Disputes Panel (Parts 1400--1499)
        XV  African Development Foundation (Parts 1500--1599)
       XVI  Japan-United States Friendship Commission (Parts 
                1600--1699)
      XVII  United States Institute of Peace (Parts 1700--1799)

                          Title 23--Highways

         I  Federal Highway Administration, Department of 
                Transportation (Parts 1--999)

[[Page 1068]]

        II  National Highway Traffic Safety Administration and 
                Federal Highway Administration, Department of 
                Transportation (Parts 1200--1299)
       III  National Highway Traffic Safety Administration, 
                Department of Transportation (Parts 1300--1399)

                Title 24--Housing and Urban Development

            Subtitle A--Office of the Secretary, Department of 
                Housing and Urban Development (Parts 0--99)
            Subtitle B--Regulations Relating to Housing and Urban 
                Development
         I  Office of Assistant Secretary for Equal Opportunity, 
                Department of Housing and Urban Development (Parts 
                100--199)
        II  Office of Assistant Secretary for Housing-Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Parts 200--299)
       III  Government National Mortgage Association, Department 
                of Housing and Urban Development (Parts 300--399)
        IV  Office of Housing and Office of Multifamily Housing 
                Assistance Restructuring, Department of Housing 
                and Urban Development (Parts 400--499)
         V  Office of Assistant Secretary for Community Planning 
                and Development, Department of Housing and Urban 
                Development (Parts 500--599)
        VI  Office of Assistant Secretary for Community Planning 
                and Development, Department of Housing and Urban 
                Development (Parts 600--699) [Reserved]
       VII  Office of the Secretary, Department of Housing and 
                Urban Development (Housing Assistance Programs and 
                Public and Indian Housing Programs) (Parts 700--
                799)
      VIII  Office of the Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Section 8 Housing Assistance 
                Programs, Section 202 Direct Loan Program, Section 
                202 Supportive Housing for the Elderly Program and 
                Section 811 Supportive Housing for Persons With 
                Disabilities Program) (Parts 800--899)
        IX  Office of Assistant Secretary for Public and Indian 
                Housing, Department of Housing and Urban 
                Development (Parts 900--1699)
         X  Office of Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Interstate Land Sales 
                Registration Program) (Parts 1700--1799)
       XII  Office of Inspector General, Department of Housing and 
                Urban Development (Parts 2000--2099)
        XV  Emergency Mortgage Insurance and Loan Programs, 
                Department of Housing and Urban Development (Parts 
                2700--2799) [Reserved]
        XX  Office of Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Parts 3200--3899)

[[Page 1069]]

      XXIV  Board of Directors of the HOPE for Homeowners Program 
                (Parts 4000--4099) [Reserved]
       XXV  Neighborhood Reinvestment Corporation (Parts 4100--
                4199)

                           Title 25--Indians

         I  Bureau of Indian Affairs, Department of the Interior 
                (Parts 1--299)
        II  Indian Arts and Crafts Board, Department of the 
                Interior (Parts 300--399)
       III  National Indian Gaming Commission, Department of the 
                Interior (Parts 500--599)
        IV  Office of Navajo and Hopi Indian Relocation (Parts 
                700--899)
         V  Bureau of Indian Affairs, Department of the Interior, 
                and Indian Health Service, Department of Health 
                and Human Services (Parts 900--999)
        VI  Office of the Assistant Secretary, Indian Affairs, 
                Department of the Interior (Parts 1000--1199)
       VII  Office of the Special Trustee for American Indians, 
                Department of the Interior (Parts 1200--1299)

                      Title 26--Internal Revenue

         I  Internal Revenue Service, Department of the Treasury 
                (Parts 1--End)

           Title 27--Alcohol, Tobacco Products and Firearms

         I  Alcohol and Tobacco Tax and Trade Bureau, Department 
                of the Treasury (Parts 1--399)
        II  Bureau of Alcohol, Tobacco, Firearms, and Explosives, 
                Department of Justice (Parts 400--699)

                   Title 28--Judicial Administration

         I  Department of Justice (Parts 0--299)
       III  Federal Prison Industries, Inc., Department of Justice 
                (Parts 300--399)
         V  Bureau of Prisons, Department of Justice (Parts 500--
                599)
        VI  Offices of Independent Counsel, Department of Justice 
                (Parts 600--699)
       VII  Office of Independent Counsel (Parts 700--799)
      VIII  Court Services and Offender Supervision Agency for the 
                District of Columbia (Parts 800--899)
        IX  National Crime Prevention and Privacy Compact Council 
                (Parts 900--999)
        XI  Department of Justice and Department of State (Parts 
                1100--1199)

[[Page 1070]]

                            Title 29--Labor

            Subtitle A--Office of the Secretary of Labor (Parts 
                0--99)
            Subtitle B--Regulations Relating to Labor
         I  National Labor Relations Board (Parts 100--199)
        II  Office of Labor-Management Standards, Department of 
                Labor (Parts 200--299)
       III  National Railroad Adjustment Board (Parts 300--399)
        IV  Office of Labor-Management Standards, Department of 
                Labor (Parts 400--499)
         V  Wage and Hour Division, Department of Labor (Parts 
                500--899)
        IX  Construction Industry Collective Bargaining Commission 
                (Parts 900--999)
         X  National Mediation Board (Parts 1200--1299)
       XII  Federal Mediation and Conciliation Service (Parts 
                1400--1499)
       XIV  Equal Employment Opportunity Commission (Parts 1600--
                1699)
      XVII  Occupational Safety and Health Administration, 
                Department of Labor (Parts 1900--1999)
        XX  Occupational Safety and Health Review Commission 
                (Parts 2200--2499)
       XXV  Employee Benefits Security Administration, Department 
                of Labor (Parts 2500--2599)
     XXVII  Federal Mine Safety and Health Review Commission 
                (Parts 2700--2799)
        XL  Pension Benefit Guaranty Corporation (Parts 4000--
                4999)

                      Title 30--Mineral Resources

         I  Mine Safety and Health Administration, Department of 
                Labor (Parts 1--199)
        II  Bureau of Safety and Environmental Enforcement, 
                Department of the Interior (Parts 200--299)
        IV  Geological Survey, Department of the Interior (Parts 
                400--499)
         V  Bureau of Ocean Energy Management, Department of the 
                Interior (Parts 500--599)
       VII  Office of Surface Mining Reclamation and Enforcement, 
                Department of the Interior (Parts 700--999)
       XII  Office of Natural Resources Revenue, Department of the 
                Interior (Parts 1200--1299)

                 Title 31--Money and Finance: Treasury

            Subtitle A--Office of the Secretary of the Treasury 
                (Parts 0--50)
            Subtitle B--Regulations Relating to Money and Finance
         I  Monetary Offices, Department of the Treasury (Parts 
                51--199)
        II  Fiscal Service, Department of the Treasury (Parts 
                200--399)
        IV  Secret Service, Department of the Treasury (Parts 
                400--499)
         V  Office of Foreign Assets Control, Department of the 
                Treasury (Parts 500--599)

[[Page 1071]]

        VI  Bureau of Engraving and Printing, Department of the 
                Treasury (Parts 600--699)
       VII  Federal Law Enforcement Training Center, Department of 
                the Treasury (Parts 700--799)
      VIII  Office of Investment Security, Department of the 
                Treasury (Parts 800--899)
        IX  Federal Claims Collection Standards (Department of the 
                Treasury--Department of Justice) (Parts 900--999)
         X  Financial Crimes Enforcement Network, Department of 
                the Treasury (Parts 1000--1099)

                      Title 32--National Defense

            Subtitle A--Department of Defense
         I  Office of the Secretary of Defense (Parts 1--399)
         V  Department of the Army (Parts 400--699)
        VI  Department of the Navy (Parts 700--799)
       VII  Department of the Air Force (Parts 800--1099)
            Subtitle B--Other Regulations Relating to National 
                Defense
       XII  Defense Logistics Agency (Parts 1200--1299)
       XVI  Selective Service System (Parts 1600--1699)
      XVII  Office of the Director of National Intelligence (Parts 
                1700--1799)
     XVIII  National Counterintelligence Center (Parts 1800--1899)
       XIX  Central Intelligence Agency (Parts 1900--1999)
        XX  Information Security Oversight Office, National 
                Archives and Records Administration (Parts 2000--
                2099)
       XXI  National Security Council (Parts 2100--2199)
      XXIV  Office of Science and Technology Policy (Parts 2400--
                2499)
     XXVII  Office for Micronesian Status Negotiations (Parts 
                2700--2799)
    XXVIII  Office of the Vice President of the United States 
                (Parts 2800--2899)

               Title 33--Navigation and Navigable Waters

         I  Coast Guard, Department of Homeland Security (Parts 
                1--199)
        II  Corps of Engineers, Department of the Army, Department 
                of Defense (Parts 200--399)
        IV  Saint Lawrence Seaway Development Corporation, 
                Department of Transportation (Parts 400--499)

                          Title 34--Education

            Subtitle A--Office of the Secretary, Department of 
                Education (Parts 1--99)
            Subtitle B--Regulations of the Offices of the 
                Department of Education
         I  Office for Civil Rights, Department of Education 
                (Parts 100--199)

[[Page 1072]]

        II  Office of Elementary and Secondary Education, 
                Department of Education (Parts 200--299)
       III  Office of Special Education and Rehabilitative 
                Services, Department of Education (Parts 300--399)
        IV  Office of Career, Technical and Adult Education, 
                Department of Education (Parts 400--499)
         V  Office of Bilingual Education and Minority Languages 
                Affairs, Department of Education (Parts 500--599) 
                [Reserved]
        VI  Office of Postsecondary Education, Department of 
                Education (Parts 600--699)
       VII  Office of Educational Research and Improvement, 
                Department of Education (Parts 700--799) 
                [Reserved]
            Subtitle C--Regulations Relating to Education
        XI  (Parts 1100--1199) [Reserved]
       XII  National Council on Disability (Parts 1200--1299)

                          Title 35 [Reserved]

             Title 36--Parks, Forests, and Public Property

         I  National Park Service, Department of the Interior 
                (Parts 1--199)
        II  Forest Service, Department of Agriculture (Parts 200--
                299)
       III  Corps of Engineers, Department of the Army (Parts 
                300--399)
        IV  American Battle Monuments Commission (Parts 400--499)
         V  Smithsonian Institution (Parts 500--599)
        VI  [Reserved]
       VII  Library of Congress (Parts 700--799)
      VIII  Advisory Council on Historic Preservation (Parts 800--
                899)
        IX  Pennsylvania Avenue Development Corporation (Parts 
                900--999)
         X  Presidio Trust (Parts 1000--1099)
        XI  Architectural and Transportation Barriers Compliance 
                Board (Parts 1100--1199)
       XII  National Archives and Records Administration (Parts 
                1200--1299)
        XV  Oklahoma City National Memorial Trust (Parts 1500--
                1599)
       XVI  Morris K. Udall Scholarship and Excellence in National 
                Environmental Policy Foundation (Parts 1600--1699)

             Title 37--Patents, Trademarks, and Copyrights

         I  United States Patent and Trademark Office, Department 
                of Commerce (Parts 1--199)
        II  U.S. Copyright Office, Library of Congress (Parts 
                200--299)
       III  Copyright Royalty Board, Library of Congress (Parts 
                300--399)
        IV  National Institute of Standards and Technology, 
                Department of Commerce (Parts 400--599)

[[Page 1073]]

           Title 38--Pensions, Bonuses, and Veterans' Relief

         I  Department of Veterans Affairs (Parts 0--199)
        II  Armed Forces Retirement Home (Parts 200--299)

                       Title 39--Postal Service

         I  United States Postal Service (Parts 1--999)
       III  Postal Regulatory Commission (Parts 3000--3099)

                  Title 40--Protection of Environment

         I  Environmental Protection Agency (Parts 1--1099)
        IV  Environmental Protection Agency and Department of 
                Justice (Parts 1400--1499)
         V  Council on Environmental Quality (Parts 1500--1599)
        VI  Chemical Safety and Hazard Investigation Board (Parts 
                1600--1699)
       VII  Environmental Protection Agency and Department of 
                Defense; Uniform National Discharge Standards for 
                Vessels of the Armed Forces (Parts 1700--1799)
      VIII  Gulf Coast Ecosystem Restoration Council (Parts 1800--
                1899)

          Title 41--Public Contracts and Property Management

            Subtitle A--Federal Procurement Regulations System 
                [Note]
            Subtitle B--Other Provisions Relating to Public 
                Contracts
        50  Public Contracts, Department of Labor (Parts 50-1--50-
                999)
        51  Committee for Purchase From People Who Are Blind or 
                Severely Disabled (Parts 51-1--51-99)
        60  Office of Federal Contract Compliance Programs, Equal 
                Employment Opportunity, Department of Labor (Parts 
                60-1--60-999)
        61  Office of the Assistant Secretary for Veterans' 
                Employment and Training Service, Department of 
                Labor (Parts 61-1--61-999)
   62--100  [Reserved]
            Subtitle C--Federal Property Management Regulations 
                System
       101  Federal Property Management Regulations (Parts 101-1--
                101-99)
       102  Federal Management Regulation (Parts 102-1--102-299)
  103--104  [Reserved]
       105  General Services Administration (Parts 105-1--105-999)
       109  Department of Energy Property Management Regulations 
                (Parts 109-1--109-99)
       114  Department of the Interior (Parts 114-1--114-99)
       115  Environmental Protection Agency (Parts 115-1--115-99)
       128  Department of Justice (Parts 128-1--128-99)
  129--200  [Reserved]
            Subtitle D--Other Provisions Relating to Property 
                Management [Reserved]

[[Page 1074]]

            Subtitle E--Federal Information Resources Management 
                Regulations System [Reserved]
            Subtitle F--Federal Travel Regulation System
       300  General (Parts 300-1--300-99)
       301  Temporary Duty (TDY) Travel Allowances (Parts 301-1--
                301-99)
       302  Relocation Allowances (Parts 302-1--302-99)
       303  Payment of Expenses Connected with the Death of 
                Certain Employees (Part 303-1--303-99)
       304  Payment of Travel Expenses from a Non-Federal Source 
                (Parts 304-1--304-99)

                        Title 42--Public Health

         I  Public Health Service, Department of Health and Human 
                Services (Parts 1--199)
   II--III  [Reserved]
        IV  Centers for Medicare & Medicaid Services, Department 
                of Health and Human Services (Parts 400--699)
         V  Office of Inspector General-Health Care, Department of 
                Health and Human Services (Parts 1000--1099)

                   Title 43--Public Lands: Interior

            Subtitle A--Office of the Secretary of the Interior 
                (Parts 1--199)
            Subtitle B--Regulations Relating to Public Lands
         I  Bureau of Reclamation, Department of the Interior 
                (Parts 400--999)
        II  Bureau of Land Management, Department of the Interior 
                (Parts 1000--9999)
       III  Utah Reclamation Mitigation and Conservation 
                Commission (Parts 10000--10099)

             Title 44--Emergency Management and Assistance

         I  Federal Emergency Management Agency, Department of 
                Homeland Security (Parts 0--399)
        IV  Department of Commerce and Department of 
                Transportation (Parts 400--499)

                       Title 45--Public Welfare

            Subtitle A--Department of Health and Human Services 
                (Parts 1--199)
            Subtitle B--Regulations Relating to Public Welfare
        II  Office of Family Assistance (Assistance Programs), 
                Administration for Children and Families, 
                Department of Health and Human Services (Parts 
                200--299)

[[Page 1075]]

       III  Office of Child Support Enforcement (Child Support 
                Enforcement Program), Administration for Children 
                and Families, Department of Health and Human 
                Services (Parts 300--399)
        IV  Office of Refugee Resettlement, Administration for 
                Children and Families, Department of Health and 
                Human Services (Parts 400--499)
         V  Foreign Claims Settlement Commission of the United 
                States, Department of Justice (Parts 500--599)
        VI  National Science Foundation (Parts 600--699)
       VII  Commission on Civil Rights (Parts 700--799)
      VIII  Office of Personnel Management (Parts 800--899)
        IX  Denali Commission (Parts 900--999)
         X  Office of Community Services, Administration for 
                Children and Families, Department of Health and 
                Human Services (Parts 1000--1099)
        XI  National Foundation on the Arts and the Humanities 
                (Parts 1100--1199)
       XII  Corporation for National and Community Service (Parts 
                1200--1299)
      XIII  Administration for Children and Families, Department 
                of Health and Human Services (Parts 1300--1399)
       XVI  Legal Services Corporation (Parts 1600--1699)
      XVII  National Commission on Libraries and Information 
                Science (Parts 1700--1799)
     XVIII  Harry S. Truman Scholarship Foundation (Parts 1800--
                1899)
       XXI  Commission of Fine Arts (Parts 2100--2199)
     XXIII  Arctic Research Commission (Parts 2300--2399)
      XXIV  James Madison Memorial Fellowship Foundation (Parts 
                2400--2499)
       XXV  Corporation for National and Community Service (Parts 
                2500--2599)

                          Title 46--Shipping

         I  Coast Guard, Department of Homeland Security (Parts 
                1--199)
        II  Maritime Administration, Department of Transportation 
                (Parts 200--399)
       III  Coast Guard (Great Lakes Pilotage), Department of 
                Homeland Security (Parts 400--499)
        IV  Federal Maritime Commission (Parts 500--599)

                      Title 47--Telecommunication

         I  Federal Communications Commission (Parts 0--199)
        II  Office of Science and Technology Policy and National 
                Security Council (Parts 200--299)
       III  National Telecommunications and Information 
                Administration, Department of Commerce (Parts 
                300--399)

[[Page 1076]]

        IV  National Telecommunications and Information 
                Administration, Department of Commerce, and 
                National Highway Traffic Safety Administration, 
                Department of Transportation (Parts 400--499)
         V  The First Responder Network Authority (Parts 500--599)

           Title 48--Federal Acquisition Regulations System

         1  Federal Acquisition Regulation (Parts 1--99)
         2  Defense Acquisition Regulations System, Department of 
                Defense (Parts 200--299)
         3  Department of Health and Human Services (Parts 300--
                399)
         4  Department of Agriculture (Parts 400--499)
         5  General Services Administration (Parts 500--599)
         6  Department of State (Parts 600--699)
         7  Agency for International Development (Parts 700--799)
         8  Department of Veterans Affairs (Parts 800--899)
         9  Department of Energy (Parts 900--999)
        10  Department of the Treasury (Parts 1000--1099)
        12  Department of Transportation (Parts 1200--1299)
        13  Department of Commerce (Parts 1300--1399)
        14  Department of the Interior (Parts 1400--1499)
        15  Environmental Protection Agency (Parts 1500--1599)
        16  Office of Personnel Management, Federal Employees 
                Health Benefits Acquisition Regulation (Parts 
                1600--1699)
        17  Office of Personnel Management (Parts 1700--1799)
        18  National Aeronautics and Space Administration (Parts 
                1800--1899)
        19  Broadcasting Board of Governors (Parts 1900--1999)
        20  Nuclear Regulatory Commission (Parts 2000--2099)
        21  Office of Personnel Management, Federal Employees 
                Group Life Insurance Federal Acquisition 
                Regulation (Parts 2100--2199)
        23  Social Security Administration (Parts 2300--2399)
        24  Department of Housing and Urban Development (Parts 
                2400--2499)
        25  National Science Foundation (Parts 2500--2599)
        28  Department of Justice (Parts 2800--2899)
        29  Department of Labor (Parts 2900--2999)
        30  Department of Homeland Security, Homeland Security 
                Acquisition Regulation (HSAR) (Parts 3000--3099)
        34  Department of Education Acquisition Regulation (Parts 
                3400--3499)
        51  Department of the Army Acquisition Regulations (Parts 
                5100--5199)
        52  Department of the Navy Acquisition Regulations (Parts 
                5200--5299)
        53  Department of the Air Force Federal Acquisition 
                Regulation Supplement (Parts 5300--5399) 
                [Reserved]

[[Page 1077]]

        54  Defense Logistics Agency, Department of Defense (Parts 
                5400--5499)
        57  African Development Foundation (Parts 5700--5799)
        61  Civilian Board of Contract Appeals, General Services 
                Administration (Parts 6100--6199)
        99  Cost Accounting Standards Board, Office of Federal 
                Procurement Policy, Office of Management and 
                Budget (Parts 9900--9999)

                       Title 49--Transportation

            Subtitle A--Office of the Secretary of Transportation 
                (Parts 1--99)
            Subtitle B--Other Regulations Relating to 
                Transportation
         I  Pipeline and Hazardous Materials Safety 
                Administration, Department of Transportation 
                (Parts 100--199)
        II  Federal Railroad Administration, Department of 
                Transportation (Parts 200--299)
       III  Federal Motor Carrier Safety Administration, 
                Department of Transportation (Parts 300--399)
        IV  Coast Guard, Department of Homeland Security (Parts 
                400--499)
         V  National Highway Traffic Safety Administration, 
                Department of Transportation (Parts 500--599)
        VI  Federal Transit Administration, Department of 
                Transportation (Parts 600--699)
       VII  National Railroad Passenger Corporation (AMTRAK) 
                (Parts 700--799)
      VIII  National Transportation Safety Board (Parts 800--999)
         X  Surface Transportation Board (Parts 1000--1399)
        XI  Research and Innovative Technology Administration, 
                Department of Transportation (Parts 1400--1499) 
                [Reserved]
       XII  Transportation Security Administration, Department of 
                Homeland Security (Parts 1500--1699)

                   Title 50--Wildlife and Fisheries

         I  United States Fish and Wildlife Service, Department of 
                the Interior (Parts 1--199)
        II  National Marine Fisheries Service, National Oceanic 
                and Atmospheric Administration, Department of 
                Commerce (Parts 200--299)
       III  International Fishing and Related Activities (Parts 
                300--399)
        IV  Joint Regulations (United States Fish and Wildlife 
                Service, Department of the Interior and National 
                Marine Fisheries Service, National Oceanic and 
                Atmospheric Administration, Department of 
                Commerce); Endangered Species Committee 
                Regulations (Parts 400--499)
         V  Marine Mammal Commission (Parts 500--599)

[[Page 1078]]

        VI  Fishery Conservation and Management, National Oceanic 
                and Atmospheric Administration, Department of 
                Commerce (Parts 600--699)

[[Page 1079]]





           Alphabetical List of Agencies Appearing in the CFR




                      (Revised as of July 1, 2018)

                                                  CFR Title, Subtitle or 
                     Agency                               Chapter

Administrative Committee of the Federal Register  1, I
Administrative Conference of the United States    1, III
Advisory Council on Historic Preservation         36, VIII
Advocacy and Outreach, Office of                  7, XXV
Afghanistan Reconstruction, Special Inspector     5, LXXXIII
     General for
African Development Foundation                    22, XV
  Federal Acquisition Regulation                  48, 57
Agency for International Development              2, VII; 22, II
  Federal Acquisition Regulation                  48, 7
Agricultural Marketing Service                    7, I, IX, X, XI
Agricultural Research Service                     7, V
Agriculture, Department of                        2, IV; 5, LXXIII
  Advocacy and Outreach, Office of                7, XXV
  Agricultural Marketing Service                  7, I, IX, X, XI
  Agricultural Research Service                   7, V
  Animal and Plant Health Inspection Service      7, III; 9, I
  Chief Financial Officer, Office of              7, XXX
  Commodity Credit Corporation                    7, XIV
  Economic Research Service                       7, XXXVII
  Energy Policy and New Uses, Office of           2, IX; 7, XXIX
  Environmental Quality, Office of                7, XXXI
  Farm Service Agency                             7, VII, XVIII
  Federal Acquisition Regulation                  48, 4
  Federal Crop Insurance Corporation              7, IV
  Food and Nutrition Service                      7, II
  Food Safety and Inspection Service              9, III
  Foreign Agricultural Service                    7, XV
  Forest Service                                  36, II
  Grain Inspection, Packers and Stockyards        7, VIII; 9, II
       Administration
  Information Resources Management, Office of     7, XXVII
  Inspector General, Office of                    7, XXVI
  National Agricultural Library                   7, XLI
  National Agricultural Statistics Service        7, XXXVI
  National Institute of Food and Agriculture      7, XXXIV
  Natural Resources Conservation Service          7, VI
  Operations, Office of                           7, XXVIII
  Procurement and Property Management, Office of  7, XXXII
  Rural Business-Cooperative Service              7, XVIII, XLII
  Rural Development Administration                7, XLII
  Rural Housing Service                           7, XVIII, XXXV
  Rural Telephone Bank                            7, XVI
  Rural Utilities Service                         7, XVII, XVIII, XLII
  Secretary of Agriculture, Office of             7, Subtitle A
  Transportation, Office of                       7, XXXIII
  World Agricultural Outlook Board                7, XXXVIII
Air Force, Department of                          32, VII
  Federal Acquisition Regulation Supplement       48, 53
Air Transportation Stabilization Board            14, VI
Alcohol and Tobacco Tax and Trade Bureau          27, I
Alcohol, Tobacco, Firearms, and Explosives,       27, II
     Bureau of
AMTRAK                                            49, VII
American Battle Monuments Commission              36, IV
American Indians, Office of the Special Trustee   25, VII

[[Page 1080]]

Animal and Plant Health Inspection Service        7, III; 9, I
Appalachian Regional Commission                   5, IX
Architectural and Transportation Barriers         36, XI
     Compliance Board
Arctic Research Commission                        45, XXIII
Armed Forces Retirement Home                      5, XI
Army, Department of                               32, V
  Engineers, Corps of                             33, II; 36, III
  Federal Acquisition Regulation                  48, 51
Bilingual Education and Minority Languages        34, V
     Affairs, Office of
Blind or Severely Disabled, Committee for         41, 51
     Purchase from People Who Are
Broadcasting Board of Governors                   22, V
  Federal Acquisition Regulation                  48, 19
Career, Technical, and Adult Education, Office    34, IV
     of
Census Bureau                                     15, I
Centers for Medicare & Medicaid Services          42, IV
Central Intelligence Agency                       32, XIX
Chemical Safety and Hazardous Investigation       40, VI
     Board
Chief Financial Officer, Office of                7, XXX
Child Support Enforcement, Office of              45, III
Children and Families, Administration for         45, II, III, IV, X, XIII
Civil Rights, Commission on                       5, LXVIII; 45, VII
Civil Rights, Office for                          34, I
Council of the Inspectors General on Integrity    5, XCVIII
     and Efficiency
Court Services and Offender Supervision Agency    5, LXX
     for the District of Columbia
Coast Guard                                       33, I; 46, I; 49, IV
Coast Guard (Great Lakes Pilotage)                46, III
Commerce, Department of                           2, XIII; 44, IV; 50, VI
  Census Bureau                                   15, I
  Economic Analysis, Bureau of                    15, VIII
  Economic Development Administration             13, III
  Emergency Management and Assistance             44, IV
  Federal Acquisition Regulation                  48, 13
  Foreign-Trade Zones Board                       15, IV
  Industry and Security, Bureau of                15, VII
  International Trade Administration              15, III; 19, III
  National Institute of Standards and Technology  15, XI; 37, IV
  National Marine Fisheries Service               50, II, IV
  National Oceanic and Atmospheric                15, IX; 50, II, III, IV, 
       Administration                             VI
  National Technical Information Service          15, XI
  National Telecommunications and Information     15, XXIII; 47, III, IV
       Administration
  National Weather Service                        15, IX
  Patent and Trademark Office, United States      37, I
  Secretary of Commerce, Office of                15, Subtitle A
Commercial Space Transportation                   14, III
Commodity Credit Corporation                      7, XIV
Commodity Futures Trading Commission              5, XLI; 17, I
Community Planning and Development, Office of     24, V, VI
     Assistant Secretary for
Community Services, Office of                     45, X
Comptroller of the Currency                       12, I
Construction Industry Collective Bargaining       29, IX
     Commission
Consumer Financial Protection Bureau              5, LXXXIV; 12, X
Consumer Product Safety Commission                5, LXXI; 16, II
Copyright Royalty Board                           37, III
Corporation for National and Community Service    2, XXII; 45, XII, XXV
Cost Accounting Standards Board                   48, 99
Council on Environmental Quality                  40, V
Court Services and Offender Supervision Agency    5, LXX; 28, VIII
     for the District of Columbia
Customs and Border Protection                     19, I
Defense Contract Audit Agency                     32, I
Defense, Department of                            2, XI; 5, XXVI; 32, 
                                                  Subtitle A; 40, VII
  Advanced Research Projects Agency               32, I

[[Page 1081]]

  Air Force Department                            32, VII
  Army Department                                 32, V; 33, II; 36, III; 
                                                  48, 51
  Defense Acquisition Regulations System          48, 2
  Defense Intelligence Agency                     32, I
  Defense Logistics Agency                        32, I, XII; 48, 54
  Engineers, Corps of                             33, II; 36, III
  National Imagery and Mapping Agency             32, I
  Navy Department                                 32, VI; 48, 52
  Secretary of Defense, Office of                 2, XI; 32, I
Defense Contract Audit Agency                     32, I
Defense Intelligence Agency                       32, I
Defense Logistics Agency                          32, XII; 48, 54
Defense Nuclear Facilities Safety Board           10, XVII
Delaware River Basin Commission                   18, III
Denali Commission                                 45, IX
Disability, National Council on                   5, C; 34, XII
District of Columbia, Court Services and          5, LXX; 28, VIII
     Offender Supervision Agency for the
Drug Enforcement Administration                   21, II
East-West Foreign Trade Board                     15, XIII
Economic Analysis, Bureau of                      15, VIII
Economic Development Administration               13, III
Economic Research Service                         7, XXXVII
Education, Department of                          2, XXXIV; 5, LIII
  Bilingual Education and Minority Languages      34, V
       Affairs, Office of
  Career, Technical, and Adult Education, Office  34, IV
       of
  Civil Rights, Office for                        34, I
  Educational Research and Improvement, Office    34, VII
       of
  Elementary and Secondary Education, Office of   34, II
  Federal Acquisition Regulation                  48, 34
  Postsecondary Education, Office of              34, VI
  Secretary of Education, Office of               34, Subtitle A
  Special Education and Rehabilitative Services,  34, III
       Office of
Educational Research and Improvement, Office of   34, VII
Election Assistance Commission                    2, LVIII; 11, II
Elementary and Secondary Education, Office of     34, II
Emergency Oil and Gas Guaranteed Loan Board       13, V
Emergency Steel Guarantee Loan Board              13, IV
Employee Benefits Security Administration         29, XXV
Employees' Compensation Appeals Board             20, IV
Employees Loyalty Board                           5, V
Employment and Training Administration            20, V
Employment Policy, National Commission for        1, IV
Employment Standards Administration               20, VI
Endangered Species Committee                      50, IV
Energy, Department of                             2, IX; 5, XXIII; 10, II, 
                                                  III, X
  Federal Acquisition Regulation                  48, 9
  Federal Energy Regulatory Commission            5, XXIV; 18, I
  Property Management Regulations                 41, 109
Energy, Office of                                 7, XXIX
Engineers, Corps of                               33, II; 36, III
Engraving and Printing, Bureau of                 31, VI
Environmental Protection Agency                   2, XV; 5, LIV; 40, I, IV, 
                                                  VII
  Federal Acquisition Regulation                  48, 15
  Property Management Regulations                 41, 115
Environmental Quality, Office of                  7, XXXI
Equal Employment Opportunity Commission           5, LXII; 29, XIV
Equal Opportunity, Office of Assistant Secretary  24, I
     for
Executive Office of the President                 3, I
  Environmental Quality, Council on               40, V
  Management and Budget, Office of                2, Subtitle A; 5, III, 
                                                  LXXVII; 14, VI; 48, 99
  National Drug Control Policy, Office of         2, XXXVI; 21, III

[[Page 1082]]

  National Security Council                       32, XXI; 47, 2
  Presidential Documents                          3
  Science and Technology Policy, Office of        32, XXIV; 47, II
  Trade Representative, Office of the United      15, XX
       States
Export-Import Bank of the United States           2, XXXV; 5, LII; 12, IV
Family Assistance, Office of                      45, II
Farm Credit Administration                        5, XXXI; 12, VI
Farm Credit System Insurance Corporation          5, XXX; 12, XIV
Farm Service Agency                               7, VII, XVIII
Federal Acquisition Regulation                    48, 1
Federal Aviation Administration                   14, I
  Commercial Space Transportation                 14, III
Federal Claims Collection Standards               31, IX
Federal Communications Commission                 5, XXIX; 47, I
Federal Contract Compliance Programs, Office of   41, 60
Federal Crop Insurance Corporation                7, IV
Federal Deposit Insurance Corporation             5, XXII; 12, III
Federal Election Commission                       5, XXXVII; 11, I
Federal Emergency Management Agency               44, I
Federal Employees Group Life Insurance Federal    48, 21
     Acquisition Regulation
Federal Employees Health Benefits Acquisition     48, 16
     Regulation
Federal Energy Regulatory Commission              5, XXIV; 18, I
Federal Financial Institutions Examination        12, XI
     Council
Federal Financing Bank                            12, VIII
Federal Highway Administration                    23, I, II
Federal Home Loan Mortgage Corporation            1, IV
Federal Housing Enterprise Oversight Office       12, XVII
Federal Housing Finance Agency                    5, LXXX; 12, XII
Federal Housing Finance Board                     12, IX
Federal Labor Relations Authority                 5, XIV, XLIX; 22, XIV
Federal Law Enforcement Training Center           31, VII
Federal Management Regulation                     41, 102
Federal Maritime Commission                       46, IV
Federal Mediation and Conciliation Service        29, XII
Federal Mine Safety and Health Review Commission  5, LXXIV; 29, XXVII
Federal Motor Carrier Safety Administration       49, III
Federal Prison Industries, Inc.                   28, III
Federal Procurement Policy Office                 48, 99
Federal Property Management Regulations           41, 101
Federal Railroad Administration                   49, II
Federal Register, Administrative Committee of     1, I
Federal Register, Office of                       1, II
Federal Reserve System                            12, II
  Board of Governors                              5, LVIII
Federal Retirement Thrift Investment Board        5, VI, LXXVI
Federal Service Impasses Panel                    5, XIV
Federal Trade Commission                          5, XLVII; 16, I
Federal Transit Administration                    49, VI
Federal Travel Regulation System                  41, Subtitle F
Financial Crimes Enforcement Network              31, X
Financial Research Office                         12, XVI
Financial Stability Oversight Council             12, XIII
Fine Arts, Commission of                          45, XXI
Fiscal Service                                    31, II
Fish and Wildlife Service, United States          50, I, IV
Food and Drug Administration                      21, I
Food and Nutrition Service                        7, II
Food Safety and Inspection Service                9, III
Foreign Agricultural Service                      7, XV
Foreign Assets Control, Office of                 31, V
Foreign Claims Settlement Commission of the       45, V
     United States
Foreign Service Grievance Board                   22, IX
Foreign Service Impasse Disputes Panel            22, XIV
Foreign Service Labor Relations Board             22, XIV
Foreign-Trade Zones Board                         15, IV
Forest Service                                    36, II

[[Page 1083]]

General Services Administration                   5, LVII; 41, 105
  Contract Appeals, Board of                      48, 61
  Federal Acquisition Regulation                  48, 5
  Federal Management Regulation                   41, 102
  Federal Property Management Regulations         41, 101
  Federal Travel Regulation System                41, Subtitle F
  General                                         41, 300
  Payment From a Non-Federal Source for Travel    41, 304
       Expenses
  Payment of Expenses Connected With the Death    41, 303
       of Certain Employees
  Relocation Allowances                           41, 302
  Temporary Duty (TDY) Travel Allowances          41, 301
Geological Survey                                 30, IV
Government Accountability Office                  4, I
Government Ethics, Office of                      5, XVI
Government National Mortgage Association          24, III
Grain Inspection, Packers and Stockyards          7, VIII; 9, II
     Administration
Gulf Coast Ecosystem Restoration Council          2, LIX; 40, VIII
Harry S. Truman Scholarship Foundation            45, XVIII
Health and Human Services, Department of          2, III; 5, XLV; 45, 
                                                  Subtitle A
  Centers for Medicare & Medicaid Services        42, IV
  Child Support Enforcement, Office of            45, III
  Children and Families, Administration for       45, II, III, IV, X, XIII
  Community Services, Office of                   45, X
  Family Assistance, Office of                    45, II
  Federal Acquisition Regulation                  48, 3
  Food and Drug Administration                    21, I
  Indian Health Service                           25, V
  Inspector General (Health Care), Office of      42, V
  Public Health Service                           42, I
  Refugee Resettlement, Office of                 45, IV
Homeland Security, Department of                  2, XXX; 5, XXXVI; 6, I; 8, 
                                                  I
  Coast Guard                                     33, I; 46, I; 49, IV
  Coast Guard (Great Lakes Pilotage)              46, III
  Customs and Border Protection                   19, I
  Federal Emergency Management Agency             44, I
  Human Resources Management and Labor Relations  5, XCVII
       Systems
  Immigration and Customs Enforcement Bureau      19, IV
  Transportation Security Administration          49, XII
HOPE for Homeowners Program, Board of Directors   24, XXIV
     of
Housing and Urban Development, Department of      2, XXIV; 5, LXV; 24, 
                                                  Subtitle B
  Community Planning and Development, Office of   24, V, VI
       Assistant Secretary for
  Equal Opportunity, Office of Assistant          24, I
       Secretary for
  Federal Acquisition Regulation                  48, 24
  Federal Housing Enterprise Oversight, Office    12, XVII
       of
  Government National Mortgage Association        24, III
  Housing--Federal Housing Commissioner, Office   24, II, VIII, X, XX
       of Assistant Secretary for
  Housing, Office of, and Multifamily Housing     24, IV
       Assistance Restructuring, Office of
  Inspector General, Office of                    24, XII
  Public and Indian Housing, Office of Assistant  24, IX
       Secretary for
  Secretary, Office of                            24, Subtitle A, VII
Housing--Federal Housing Commissioner, Office of  24, II, VIII, X, XX
     Assistant Secretary for
Housing, Office of, and Multifamily Housing       24, IV
     Assistance Restructuring, Office of
Immigration and Customs Enforcement Bureau        19, IV
Immigration Review, Executive Office for          8, V
Independent Counsel, Office of                    28, VII
Independent Counsel, Offices of                   28, VI
Indian Affairs, Bureau of                         25, I, V

[[Page 1084]]

Indian Affairs, Office of the Assistant           25, VI
     Secretary
Indian Arts and Crafts Board                      25, II
Indian Health Service                             25, V
Industry and Security, Bureau of                  15, VII
Information Resources Management, Office of       7, XXVII
Information Security Oversight Office, National   32, XX
     Archives and Records Administration
Inspector General
  Agriculture Department                          7, XXVI
  Health and Human Services Department            42, V
  Housing and Urban Development Department        24, XII, XV
Institute of Peace, United States                 22, XVII
Inter-American Foundation                         5, LXIII; 22, X
Interior, Department of                           2, XIV
  American Indians, Office of the Special         25, VII
       Trustee
  Endangered Species Committee                    50, IV
  Federal Acquisition Regulation                  48, 14
  Federal Property Management Regulations System  41, 114
  Fish and Wildlife Service, United States        50, I, IV
  Geological Survey                               30, IV
  Indian Affairs, Bureau of                       25, I, V
  Indian Affairs, Office of the Assistant         25, VI
       Secretary
  Indian Arts and Crafts Board                    25, II
  Land Management, Bureau of                      43, II
  National Indian Gaming Commission               25, III
  National Park Service                           36, I
  Natural Resource Revenue, Office of             30, XII
  Ocean Energy Management, Bureau of              30, V
  Reclamation, Bureau of                          43, I
  Safety and Enforcement Bureau, Bureau of        30, II
  Secretary of the Interior, Office of            2, XIV; 43, Subtitle A
  Surface Mining Reclamation and Enforcement,     30, VII
       Office of
Internal Revenue Service                          26, I
International Boundary and Water Commission,      22, XI
     United States and Mexico, United States 
     Section
International Development, United States Agency   22, II
     for
  Federal Acquisition Regulation                  48, 7
International Development Cooperation Agency,     22, XII
     United States
International Joint Commission, United States     22, IV
     and Canada
International Organizations Employees Loyalty     5, V
     Board
International Trade Administration                15, III; 19, III
International Trade Commission, United States     19, II
Interstate Commerce Commission                    5, XL
Investment Security, Office of                    31, VIII
James Madison Memorial Fellowship Foundation      45, XXIV
Japan-United States Friendship Commission         22, XVI
Joint Board for the Enrollment of Actuaries       20, VIII
Justice, Department of                            2, XXVIII; 5, XXVIII; 28, 
                                                  I, XI; 40, IV
  Alcohol, Tobacco, Firearms, and Explosives,     27, II
       Bureau of
  Drug Enforcement Administration                 21, II
  Federal Acquisition Regulation                  48, 28
  Federal Claims Collection Standards             31, IX
  Federal Prison Industries, Inc.                 28, III
  Foreign Claims Settlement Commission of the     45, V
       United States
  Immigration Review, Executive Office for        8, V
  Independent Counsel, Offices of                 28, VI
  Prisons, Bureau of                              28, V
  Property Management Regulations                 41, 128
Labor, Department of                              2, XXIX; 5, XLII
  Employee Benefits Security Administration       29, XXV
  Employees' Compensation Appeals Board           20, IV
  Employment and Training Administration          20, V
  Employment Standards Administration             20, VI
  Federal Acquisition Regulation                  48, 29

[[Page 1085]]

  Federal Contract Compliance Programs, Office    41, 60
       of
  Federal Procurement Regulations System          41, 50
  Labor-Management Standards, Office of           29, II, IV
  Mine Safety and Health Administration           30, I
  Occupational Safety and Health Administration   29, XVII
  Public Contracts                                41, 50
  Secretary of Labor, Office of                   29, Subtitle A
  Veterans' Employment and Training Service,      41, 61; 20, IX
       Office of the Assistant Secretary for
  Wage and Hour Division                          29, V
  Workers' Compensation Programs, Office of       20, I, VII
Labor-Management Standards, Office of             29, II, IV
Land Management, Bureau of                        43, II
Legal Services Corporation                        45, XVI
Libraries and Information Science, National       45, XVII
     Commission on
Library of Congress                               36, VII
  Copyright Royalty Board                         37, III
  U.S. Copyright Office                           37, II
Local Television Loan Guarantee Board             7, XX
Management and Budget, Office of                  5, III, LXXVII; 14, VI; 
                                                  48, 99
Marine Mammal Commission                          50, V
Maritime Administration                           46, II
Merit Systems Protection Board                    5, II, LXIV
Micronesian Status Negotiations, Office for       32, XXVII
Military Compensation and Retirement              5, XCIX
     Modernization Commission
Millennium Challenge Corporation                  22, XIII
Mine Safety and Health Administration             30, I
Minority Business Development Agency              15, XIV
Miscellaneous Agencies                            1, IV
Monetary Offices                                  31, I
Morris K. Udall Scholarship and Excellence in     36, XVI
     National Environmental Policy Foundation
Museum and Library Services, Institute of         2, XXXI
National Aeronautics and Space Administration     2, XVIII; 5, LIX; 14, V
  Federal Acquisition Regulation                  48, 18
National Agricultural Library                     7, XLI
National Agricultural Statistics Service          7, XXXVI
National and Community Service, Corporation for   2, XXII; 45, XII, XXV
National Archives and Records Administration      2, XXVI; 5, LXVI; 36, XII
  Information Security Oversight Office           32, XX
National Capital Planning Commission              1, IV, VI
National Counterintelligence Center               32, XVIII
National Credit Union Administration              5, LXXXVI; 12, VII
National Crime Prevention and Privacy Compact     28, IX
     Council
National Drug Control Policy, Office of           2, XXXVI; 21, III
National Endowment for the Arts                   2, XXXII
National Endowment for the Humanities             2, XXXIII
National Foundation on the Arts and the           45, XI
     Humanities
National Geospatial-Intelligence Agency           32, I
National Highway Traffic Safety Administration    23, II, III; 47, VI; 49, V
National Imagery and Mapping Agency               32, I
National Indian Gaming Commission                 25, III
National Institute of Food and Agriculture        7, XXXIV
National Institute of Standards and Technology    15, II; 37, IV
National Intelligence, Office of Director of      5, IV; 32, XVII
National Labor Relations Board                    5, LXI; 29, I
National Marine Fisheries Service                 50, II, IV
National Mediation Board                          29, X
National Oceanic and Atmospheric Administration   15, IX; 50, II, III, IV, 
                                                  VI
National Park Service                             36, I
National Railroad Adjustment Board                29, III
National Railroad Passenger Corporation (AMTRAK)  49, VII
National Science Foundation                       2, XXV; 5, XLIII; 45, VI
  Federal Acquisition Regulation                  48, 25

[[Page 1086]]

National Security Council                         32, XXI
National Security Council and Office of Science   47, II
     and Technology Policy
National Telecommunications and Information       15, XXIII; 47, III, IV, V
     Administration
National Transportation Safety Board              49, VIII
Natural Resources Conservation Service            7, VI
Natural Resource Revenue, Office of               30, XII
Navajo and Hopi Indian Relocation, Office of      25, IV
Navy, Department of                               32, VI
  Federal Acquisition Regulation                  48, 52
Neighborhood Reinvestment Corporation             24, XXV
Northeast Interstate Low-Level Radioactive Waste  10, XVIII
     Commission
Nuclear Regulatory Commission                     2, XX; 5, XLVIII; 10, I
  Federal Acquisition Regulation                  48, 20
Occupational Safety and Health Administration     29, XVII
Occupational Safety and Health Review Commission  29, XX
Ocean Energy Management, Bureau of                30, V
Oklahoma City National Memorial Trust             36, XV
Operations Office                                 7, XXVIII
Overseas Private Investment Corporation           5, XXXIII; 22, VII
Patent and Trademark Office, United States        37, I
Payment From a Non-Federal Source for Travel      41, 304
     Expenses
Payment of Expenses Connected With the Death of   41, 303
     Certain Employees
Peace Corps                                       2, XXXVII; 22, III
Pennsylvania Avenue Development Corporation       36, IX
Pension Benefit Guaranty Corporation              29, XL
Personnel Management, Office of                   5, I, XXXV; 5, IV; 45, 
                                                  VIII
  Human Resources Management and Labor Relations  5, XCVII
       Systems, Department of Homeland Security
  Federal Acquisition Regulation                  48, 17
  Federal Employees Group Life Insurance Federal  48, 21
       Acquisition Regulation
  Federal Employees Health Benefits Acquisition   48, 16
       Regulation
Pipeline and Hazardous Materials Safety           49, I
     Administration
Postal Regulatory Commission                      5, XLVI; 39, III
Postal Service, United States                     5, LX; 39, I
Postsecondary Education, Office of                34, VI
President's Commission on White House             1, IV
     Fellowships
Presidential Documents                            3
Presidio Trust                                    36, X
Prisons, Bureau of                                28, V
Privacy and Civil Liberties Oversight Board       6, X
Procurement and Property Management, Office of    7, XXXII
Public Contracts, Department of Labor             41, 50
Public and Indian Housing, Office of Assistant    24, IX
     Secretary for
Public Health Service                             42, I
Railroad Retirement Board                         20, II
Reclamation, Bureau of                            43, I
Refugee Resettlement, Office of                   45, IV
Relocation Allowances                             41, 302
Research and Innovative Technology                49, XI
     Administration
Rural Business-Cooperative Service                7, XVIII, XLII
Rural Development Administration                  7, XLII
Rural Housing Service                             7, XVIII, XXXV
Rural Telephone Bank                              7, XVI
Rural Utilities Service                           7, XVII, XVIII, XLII
Safety and Environmental Enforcement, Bureau of   30, II
Saint Lawrence Seaway Development Corporation     33, IV
Science and Technology Policy, Office of          32, XXIV
Science and Technology Policy, Office of, and     47, II
     National Security Council
Secret Service                                    31, IV
Securities and Exchange Commission                5, XXXIV; 17, II

[[Page 1087]]

Selective Service System                          32, XVI
Small Business Administration                     2, XXVII; 13, I
Smithsonian Institution                           36, V
Social Security Administration                    2, XXIII; 20, III; 48, 23
Soldiers' and Airmen's Home, United States        5, XI
Special Counsel, Office of                        5, VIII
Special Education and Rehabilitative Services,    34, III
     Office of
State, Department of                              2, VI; 22, I; 28, XI
  Federal Acquisition Regulation                  48, 6
Surface Mining Reclamation and Enforcement,       30, VII
     Office of
Surface Transportation Board                      49, X
Susquehanna River Basin Commission                18, VIII
Tennessee Valley Authority                        5, LXIX; 18, XIII
Thrift Supervision Office, Department of the      12, V
     Treasury
Trade Representative, United States, Office of    15, XX
Transportation, Department of                     2, XII; 5, L
  Commercial Space Transportation                 14, III
  Emergency Management and Assistance             44, IV
  Federal Acquisition Regulation                  48, 12
  Federal Aviation Administration                 14, I
  Federal Highway Administration                  23, I, II
  Federal Motor Carrier Safety Administration     49, III
  Federal Railroad Administration                 49, II
  Federal Transit Administration                  49, VI
  Maritime Administration                         46, II
  National Highway Traffic Safety Administration  23, II, III; 47, IV; 49, V
  Pipeline and Hazardous Materials Safety         49, I
       Administration
  Saint Lawrence Seaway Development Corporation   33, IV
  Secretary of Transportation, Office of          14, II; 49, Subtitle A
  Transportation Statistics Bureau                49, XI
Transportation, Office of                         7, XXXIII
Transportation Security Administration            49, XII
Transportation Statistics Bureau                  49, XI
Travel Allowances, Temporary Duty (TDY)           41, 301
Treasury, Department of                           2, X;5, XXI; 12, XV; 17, 
                                                  IV; 31, IX
  Alcohol and Tobacco Tax and Trade Bureau        27, I
  Community Development Financial Institutions    12, XVIII
       Fund
  Comptroller of the Currency                     12, I
  Customs and Border Protection                   19, I
  Engraving and Printing, Bureau of               31, VI
  Federal Acquisition Regulation                  48, 10
  Federal Claims Collection Standards             31, IX
  Federal Law Enforcement Training Center         31, VII
  Financial Crimes Enforcement Network            31, X
  Fiscal Service                                  31, II
  Foreign Assets Control, Office of               31, V
  Internal Revenue Service                        26, I
  Investment Security, Office of                  31, VIII
  Monetary Offices                                31, I
  Secret Service                                  31, IV
  Secretary of the Treasury, Office of            31, Subtitle A
  Thrift Supervision, Office of                   12, V
Truman, Harry S. Scholarship Foundation           45, XVIII
United States and Canada, International Joint     22, IV
     Commission
United States and Mexico, International Boundary  22, XI
     and Water Commission, United States Section
U.S. Copyright Office                             37, II
Utah Reclamation Mitigation and Conservation      43, III
     Commission
Veterans Affairs, Department of                   2, VIII; 38, I
  Federal Acquisition Regulation                  48, 8
Veterans' Employment and Training Service,        41, 61; 20, IX
     Office of the Assistant Secretary for
Vice President of the United States, Office of    32, XXVIII
Wage and Hour Division                            29, V
Water Resources Council                           18, VI
Workers' Compensation Programs, Office of         20, I, VII

[[Page 1088]]

World Agricultural Outlook Board                  7, XXXVIII

[[Page 1089]]



List of CFR Sections Affected



All changes in this volume of the Code of Federal Regulations (CFR) that 
were made by documents published in the Federal Register since January 
1, 2013 are enumerated in the following list. Entries indicate the 
nature of the changes effected. Page numbers refer to Federal Register 
pages. The user should consult the entries for chapters, parts and 
subparts as well as sections for revisions.
For changes to this volume of the CFR prior to this listing, consult the 
annual edition of the monthly List of CFR Sections Affected (LSA). The 
LSA is available at www.fdsys.gov. For changes to this volume of the CFR 
prior to 2001, see the ``List of CFR Sections Affected, 1949-1963, 1964-
1972, 1973-1985, and 1986-2000'' published in 11 separate volumes. The 
``List of CFR Sections Affected 1986-2000'' is available at 
www.fdsys.gov.

                                  2013

40 CFR
                                                                   78 FR
                                                                    Page
Chapter I
136 Policy statement...............................................14457
141.2 Amended......................................................10346
141.4 Revised......................................................10346
141.21 (h) added...................................................10347
141.21--141.29 (Subpart C) Appendix A amended......................32565
    Appendix A correctly amended...................................37463
141.52 Revised.....................................................10347
141.63 Revised.....................................................10347
141.71 (b)(5) revised..............................................10347
141.74 (b)(6)(i) and (c)(3)(i) revised.............................10347
141.132 (c)(1)(i) revised..........................................10348
141.151--141.155 (Subpart O) Appendix A amended....................10349
141.153 (c)(4), (d)(4)(x) and (h)(7) added; (d)(4)(iv) 
        introductory text, (vii) introductory text and (viii) 
        revised....................................................10348
141.202 (a) Table 1 amended........................................10350
141.203 (b)(2) revised.............................................10350
141.204 (a) Table 1 amended........................................10350
141.201--141.211 (Subpart Q) Appendix A amended....................10350
    Appendix B amended.............................................10351
141.402 (a) revised................................................10353
141.405 (b)(4) revised.............................................10353
141.803 (a)(3) and (5) revised.....................................10354
141.851--141.861 (Subpart Y) Added.................................10354
142.14 (a)(1)(iii) revised; (a)(10) added..........................10363
142.15 (c)(3) added................................................10364
142.16 (q) added...................................................10364
142.63 (b) revised.................................................10365
147.850 (a) introductory text revised..............................37978

                                  2014

40 CFR
                                                                   79 FR
                                                                    Page
Chapter I
136.1 (c) added....................................................49013
141.21--141.29 (Subpart C) Appendix A amended......................35086
    Appendix A corrected...........................................36428
141.201--141.211 (Subpart Q) Appendix A amended....................10669
141.852 (a)(5) table amended.......................................10669
141.855 (d)(2) added...............................................10670
141.861 (b)(1) amended.............................................10670
142.16 (q)(2) introductory text and (ii) revised...................10670

                                  2015

40 CFR
                                                                   80 FR
                                                                    Page
Chapter I
147.2150 Added; eff. 7-6-15........................................18318
147.2151 Heading revised; (a) amended; eff. 7-6-15.................18319
147.2154 Removed; eff. 7-6-15......................................18319

[[Page 1090]]

147.2155 Removed; eff. 7-6-15......................................18319
147.2400 (a) introductory text and (c)(1) revised; (a)(1) through 
        (4) removed; (c)(5) added eff. 7-6-15......................18322

                                  2016

40 CFR
                                                                   81 FR
                                                                    Page
Chapter I
141.21--141.29 (Subpart C) Appendix A amended......................46844
141.35 (b)(1), (2), (c)(1), (2), (3)(i), (ii) and (4) amended; 
        (c)(5)(i), (6) introductory text, (d)(2) and (e) revised 
                                                                   92684
141.40 (a) introductory text, (4)(i), (5)(ii) and (vi) amended; 
        (a)(1), (2)(i)(A), (ii)(A), (C), (3), (4)(i)(B), (C), (ii) 
        introductory text, (5)(v) and (c) revised; (a)(4)(ii)(F) 
        removed; (a)(4)(iii) added.................................92688
147 Authority citation revised..............................74929, 95483
    Regulation at 81 FR 74929 withdrawn............................95484
147.900 Added...............................................74929, 95483
    Regulation at 81 FR 74929 withdrawn............................95484
147.901 Heading revised; (a) amended........................74930, 95484
    Regulation at 81 FR 74930 withdrawn............................95484
147.902 Added...............................................74930, 95484
    Regulation at 81 FR 74930 withdrawn............................95484
147.903 Heading revised.....................................74930, 95484
    Regulation at 81 FR 74930 withdrawn............................95484
147.904 Removed.............................................74930, 95484
    Regulation at 81 FR 74930 withdrawn............................95484

                                  2017

40 CFR
                                                                   82 FR
                                                                    Page
Chapter I
136.1 (a) revised..................................................40846
136.2 (d) and (f) revised..........................................40846
136.3 (b)(19)(vii), (viii), (33), and (34) redesignated as 
        (b)(19)(ix), (x), (35), and (36); (b)(26) through (32) 
        redesignated as (b)(27) through (33); new (b)(19)(vii), 
        (viii), (25)(ii), and (iii) added; (b)(20)(v) removed; (a) 
        introductory text, table IA, table IB, table IC, table ID, 
        table IF, table IG, table IH, (b) introductory text, 
        (8)(v), (xiii), (xv), (10)(viii) through (lviii), (lxi), 
        (lxii), (lxiii), (lxviii), (15)(v), (viii), (ix), (x), 
        (xii), (xiii), (xv), (xvi), (xvii), (xxii), (xxiii), 
        (xxiv), (xxx), (xxxv), (xxxvii), (xxxix), (xlii), (l), 
        (lii), (lv), (lviii), (lix), (lxi), (lxiv), (lxvi), 
        (lxviii), (20)(i) through (iv), (25)(i), new (35), (c), 
        and (e) table II revised...................................40846
136.4 (a) introductory text, (b), and (c) revised..................40874
136.5 (a), (b), (c)(1), and (d) revised............................40875
136.6 (b)(1) and (2) introductory text revised; (b)(4)(xvii) 
        removed; (b)(4)(xviii) through first (xxii) redesignated 
        as (b)(4)(xvii) through (xxi); (c) added...................40875
136 Appendix A amended.............................................40875
    Appendix B revised.............................................40939
141 Subpart C, Appendix A amended..................................34867
147 Regulation at 81 FR 95483 eff. date delayed to 3-21-17..........8499
147.900 Regulation at 81 FR 95483 eff. date delayed to 3-21-17......8499
147.901 Regulation at 81 FR 95484 eff. date delayed to 3-21-17......8499
147.902 Regulation at 81 FR 95484 eff. date delayed to 3-21-17......8499
147.903 Regulation at 81 FR 95484 eff. date delayed to 3-21-17......8499
147.904 Regulation at 81 FR 95484 eff. date delayed to 3-21-17......8499

[[Page 1091]]

                                  2018

   (Regulations published from January 1, 2018, through July 1, 2018)

40 CFR
                                                                   82 FR
                                                                    Page
Chapter I
147.1751 Section heading, introductory text, (a) and (b) 
        introductory text revised; (e) through (h) added...........17761


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