[Title 40 CFR ]
[Code of Federal Regulations (annual edition) - July 1, 1999 Edition]
[From the U.S. Government Printing Office]


          40



          Protection of Environment



[[Page i]]

          PARTS 136 to 149

                         Revised as of July 1, 1999

          CONTAINING
          A CODIFICATION OF DOCUMENTS
          OF GENERAL APPLICABILITY
          AND FUTURE EFFECT

          AS OF JULY 1, 1999
          With Ancillaries
          Published by
          the Office of the Federal Register
          National Archives and Records
          Administration

          as a Special Edition of
          the Federal Register



[[Page ii]]

                                      




                     U.S. GOVERNMENT PRINTING OFFICE
                            WASHINGTON : 1999



               For sale by U.S. Government Printing Office
 Superintendent of Documents, Mail Stop: SSOP, Washington, DC 20402-9328



[[Page iii]]




                            Table of Contents



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

  Title 40:
          Chapter I--Environmental Protection Agency 
          (Continued)                                                3
  Finding Aids:
      Material Approved for Incorporation by Reference........     777
      Table of CFR Titles and Chapters........................     793
      Alphabetical List of Agencies Appearing in the CFR......     811
      List of CFR Sections Affected...........................     821



[[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 
issues of the Federal Register. These two publications must be used 
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    To determine whether a Code volume has been amended since its 
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Sections Affected (LSA),'' which is issued monthly, and the ``Cumulative 
List of Parts Affected,'' which appears in the Reader Aids section of 
the daily Federal Register. These two lists will identify the Federal 
Register page number of the latest amendment of any given rule.

EFFECTIVE AND EXPIRATION DATES

    Each volume of the Code contains amendments published in the Federal 
Register since the last revision of that volume of the Code. Source 
citations for the regulations are referred to by volume number and page 
number of the Federal Register and date of publication. Publication 
dates and effective dates are usually not the same and care must be 
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Code a note has been inserted to reflect the future effective date. In 
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states a date certain for expiration, an appropriate note will be 
inserted following the text.

OMB CONTROL NUMBERS

    The Paperwork Reduction Act of 1980 (Pub. L. 96-511) requires 
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 
amendments to existing regulations in the CFR. These OMB numbers are 
placed as close as possible to the applicable recordkeeping or reporting 
requirements.

OBSOLETE PROVISIONS

    Provisions that become obsolete before the revision date stated on 
the cover of each volume are not carried. Code users may find the text 
of provisions in effect on a given date in the past by using the 
appropriate numerical list of sections affected. For the period before 
January 1, 1986, consult either the List of CFR Sections Affected, 1949-
1963, 1964-1972, or 1973-1985, published in seven separate volumes. For 
the period beginning January 1, 1986, a ``List of CFR Sections 
Affected'' is published at the end of each CFR volume.

INCORPORATION BY REFERENCE

    What is incorporation by reference? Incorporation by reference was 
established by statute and allows Federal agencies to meet the 
requirement to publish regulations in the Federal Register by referring 
to materials already published elsewhere. For an incorporation to be 
valid, the Director of the Federal Register must approve it. The legal 
effect of incorporation by reference is that the material is treated as 
if it were published in full in the Federal Register (5 U.S.C. 552(a)). 
This material, like any other properly issued regulation, has the force 
of law.
    What is a proper incorporation by reference? The Director of the 
Federal Register will approve an incorporation by reference only when 
the requirements of 1 CFR part 51 are met. Some of the elements on which 
approval is based are:
    (a) The incorporation will substantially reduce the volume of 
material published in the Federal Register.
    (b) The matter incorporated is in fact available to the extent 
necessary to afford fairness and uniformity in the administrative 
process.
    (c) The incorporating document is drafted and submitted for 
publication in accordance with 1 CFR part 51.
    Properly approved incorporations by reference in this volume are 
listed in the Finding Aids at the end of this volume.
    What if the material incorporated by reference cannot be found? If 
you have any problem locating or obtaining a copy of material listed in 
the Finding Aids of this volume as an approved incorporation by 
reference, please contact the agency that issued the regulation 
containing that incorporation. If, after contacting the agency, you find 
the material is not available, please notify the Director of the Federal 
Register, National Archives and Records Administration, Washington DC 
20408, or call (202) 523-4534.

CFR INDEXES AND TABULAR GUIDES

    A subject index to the Code of Federal Regulations is contained in a 
separate volume, revised annually as of January 1, entitled CFR Index 
and Finding Aids. This volume contains the Parallel Table of Statutory 
Authorities and Agency Rules (Table I). A list of CFR titles, chapters, 
and parts and an alphabetical list of agencies publishing in the CFR are 
also included in this volume.
    An index to the text of ``Title 3--The President'' is carried within 
that volume.
    The Federal Register Index is issued monthly in cumulative form. 
This index is based on a consolidation of the ``Contents'' entries in 
the daily Federal Register.
    A List of CFR Sections Affected (LSA) is published monthly, keyed to 
the revision dates of the 50 CFR titles.

[[Page vii]]


REPUBLICATION OF MATERIAL

    There are no restrictions on the republication of material appearing 
in the Code of Federal Regulations.

INQUIRIES

    For a legal interpretation or explanation of any regulation in this 
volume, contact the issuing agency. The issuing agency's name appears at 
the top of odd-numbered pages.
    For inquiries concerning CFR reference assistance, call 202-523-5227 
or write to the Director, Office of the Federal Register, National 
Archives and Records Administration, Washington, DC 20408.

SALES

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site also contains links to GPO Access.

                              Raymond A. Mosley,
                                    Director,
                          Office of the Federal Register.

July 1, 1999.



[[Page ix]]



                               THIS TITLE

    Title 40--Protection of Environment is composed of twenty-four 
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-End), 
parts 53-59, part 60, parts 61-62, part 63 (63.1-63.1199), part 63 
(63.1200-End), parts 64-71, parts 72-80, parts 81-85, part 86, parts 87-
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 700-789, and 
part 790 to End. The contents of these volumes represent all current 
regulations codified under this title of the CFR as of July 1, 1999.

    Chapter I--Environmental Protection Agency appears in all twenty-
four volumes. A Pesticide Tolerance Commodity/Chemical Index appears in 
parts 150-189. A Toxic Substances Chemical--CAS Number Index appears in 
parts 700-789 and part 790 to End. Redesignation Tables appear in the 
volumes containing parts 50-51, parts 150-189, and parts 700-789. 
Regulations issued by the Council on Environmental Quality appear in the 
volume containing part 790 to End. The OMB control numbers for title 40 
appear in Sec. 9.1 of this chapter.

    For this volume, Melanie L. Marcec was Chief Editor. The Code of 
Federal Regulations publication program is under the direction of 
Frances D. McDonald, assisted by Alomha S. Morris.

[[Page x]]





[[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)




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

                SUBCHAPTER D--WATER PROGRAMS (CONTINUED)
Part                                                                Page
136             Guidelines establishing test procedures for 
                    the analysis of pollutants..............           5
140             Marine sanitation device standard...........         328
141             National primary drinking water regulations.         331
142             National primary drinking water regulations 
                    implementation..........................         509
143             National secondary drinking water 
                    regulations.............................         558
144             Underground injection control program.......         560
145             State UIC program requirements..............         616
146             Underground injection control program: 
                    Criteria and standards..................         629
147             State underground injection control programs         659
148             Hazardous waste injection restrictions......         759
149             Sole source aquifers........................         768

[[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 alternate test procedures.
136.5  Approval of alternate test procedures.

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--Inductively Coupled Plasma--Atomic Emission 
          Spectrometric Method for Trace Element Analysis of Water and 
          Wastes 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.

    The procedures prescribed herein shall, except as noted in 
Sec. 136.5, be used to perform the measurements indicated whenever the 
waste constituent specified is required to be measured for:
    (a) An application submitted to the Administrator, or to a State 
having an approved NPDES program for a permit under section 402 of the 
Clean Water Act of 1977, as amended (CWA), and/or to reports required to 
be submitted under NPDES permits or other requests for quantitative or 
qualitative effluent data under parts 122 to 125 of title 40, and,
    (b) Reports required to be submitted by discharges under the NPDES 
established by parts 124 and 125 of this chapter, and,
    (c) Certifications issued by States pursuant to section 401 of the 
CWA, as amended.

[38 FR 28758, Oct. 16, 1973, as amended at 49 FR 43250, Oct. 26, 1984]



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 of the State Agency authorized to 
carry out an approved National Pollutant Discharge Elimination System 
Program under section 402 of the Act.
    (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 greater than zero 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]



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, and IF. The full text of the referenced test 
procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, 
and IF. The references and the sources which are available are given in 
paragraph (b) of this section. These test procedures are incorporated as 
they exist on the day of approval and a notice of any change in these 
test procedures will be published in the Federal Register. The discharge 
parameter values for which reports are required must be determined by 
one of

[[Page 6]]

the standard analytical test procedures incorporated by reference and 
described in Tables IA, IB, IC, ID, IE, and IF, or by any alternate test 
procedure which has been approved by the Administrator under the 
provisions of paragraph (d) of this section and Secs. 136.4 and 136.5. 
Under certain circumstances (paragraph (b) or (c) of this section or 40 
CFR 401.13) other test procedures may be used that may be more 
advantageous when such other test procedures have been previously 
approved by the Regional Administrator of the Region in which the 
discharge will occur, and providing the Director of the State in which 
such discharge will occur does not object to the use of such alternate 
test procedure.

[[Page 7]]



                                                     Table IA.--List of Approved Biological Methods
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                 Method \1\                    EPA            Standard methods, 18th Ed.      ASTM              USGS
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
    1. Coliform (fecal), number     Most Probable Number        p. 132 \3\              9221C E \4\                  ...........  ......................
     per 100 mL.                     (MPN), 5 tube.             p. 124 \3\              9222D \4\                                 B-0050-85 \5\
                                    3 dilution, or Membrane
                                     filter (MF) \2\, single
                                     step.
    2. Coliform (fecal) in          MPN, 5 tube, 3 dilution,    p. 132 \3\              9221C E \4\                  ...........  ......................
     presence of chlorine, number    or.                        p. 124 \3\              9222D \4\
     per 100 mL.                    MF, single step \6\.......
    3. Coliform (total), number     MPN, 5 tube, 3 dilution,    p. 114 \3\              9221B \4\                    ...........  ......................
     per 100 mL.                     or.                        p. 108 \3\              9222B \4\                                 B-0025-85 \5\
                                    MF \2\ single step or two
                                     step.
    4. Coliform (total), in         MPN, 5 tube, 3 dilution,    p. 114 \3\              9221B \4\                    ...........  ......................
     presence of chlorine, number    or.                        p. 111 \3\              9222(B+B.5c) \4\
     per 100 mL.                    MF \2\ with enrichment....
    5. Fecal streptococci, number   MPN, 5 tube, 3 dilution...  p. 139 \3\              9230B \4\                    ...........  ......................
     per 100 mL.                    MF \2\, or................  p. 136 \3\              9230C \4\                                 B-0055-85 \5\
                                    Plate count...............  p. 143 \3\
Aquatic Toxicity:
    6. Toxicity, acute, fresh       Daphnia, Ceriodaphnia,      Sec. 9 \7\              ...........................  ...........  ......................
     water organisms, LC50,          Fathead Minnow, Rainbow
     percent effluent.               Trout, Brook Trout, or
                                     Bannerfish Shiner
                                     mortality.
    7. Toxicity, acute, estuarine   Mysid, Sheepshead Minnow,   Sec. 9 \7\              ...........................  ...........  ......................
     and marine organisms, LC50,     or Menidia spp. mortality.
     percent effluent.
    8. Toxicity, chronic, fresh     Fathead minnow larval       1000.0 \8\              ...........................  ...........  ......................
     water organisms, NOEC or        survival and growth.       1001.0 \8\
     IC25, percent effluent.        Fathead minnow embryo-
                                     larval survival and        1002.0 \8\
                                     teratogenicity.            1003.0 \8\
                                    Ceriodaphnia survival and
                                     reproduction.
                                    Selenastrum growth........
    9. Toxicity, chronic,           Sheepshead minnow larval    1004.0 \9\              ...........................  ...........  ......................
     estuarine and marine            survival and growth.       1005.0 \9\
     organisms, NOEC or IC25,       Sheepshead minnow embryo-
     percent effluent.               larval survival and        1006.0 \9\
                                     teratogenicity.            1007.0 \9\
                                    Menidia beryllina larval    1008.0 \9\
                                     and growth.                1009.0 \9\
                                    Mysidopsis bahia survival,
                                     growth, and fecundity.
                                    Arbacia punctulata
                                     fertilization.
                                    Champia parvula
                                     reproduction.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Notes to Table IA:
\1\ The method must be specified when results are reported.
\2\ A 0.45 um 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\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
  Environmental Protection Agency, Cincinnati, Ohio. EPA/600/8-78/017.
\4\ APHA. 1992. Standard Methods for the Examination of Water and Wastewater. American Public Health Association. 18th Edition. Amer. Publ. Hlth.
  Assoc., Washington, DC.
\5\ USGS. 1989. 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, U.S. Geological Survey, U.S. Department of Interior, Reston, Virginia.
\6\ 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.
\7\ USEPA. 1993. Methods for Measuring the Acute Toxicity of Effluents to Freshwater and Marine Organisms. Fourth Edition. Environmental Monitoring
  Systems Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. August 1993, EPA/600/4-90/027F.

[[Page 8]]

 
\8\ USEPA. 1994. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Third Edition.
  Environmental Monitoring Systems Laboratory, U.S. Environmental Protection Agency USEPA. 1994, Cincinnati, Ohio (July 1994, EPA/600/4-91/002).
\9\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. Second Edition.
  Environmental Monitoring Systems Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio (July 1994, EPA/600/4-91/003). These methods do
  not apply to marine waters of the Pacific Ocean.


                                                  Table IB.--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                            Reference (method number or page)
  Parameter, units and method  -------------------------------------------------------------------------------------------------------------------------
                                  EPA 1,35      STD methods  18th ed.                 ASTM                       USGS \2\                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:
    Electrometric endpoint or         305.1  2310 B(4a)................  D1067-92
     phenolphthalein endpoint.
2. Alkalinity, as CaCO3, mg/L:
    Electrometric or                  310.1  2320 B....................  D1067-92.....................  I-1030-85................  973.43.\3\
     Colorimetric titration to        310.2                                                             I-2030-85................
     pH 4.5, manual or
     automated.
3. Aluminum--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        202.1  3111 D....................  .............................  I-3051-85
    AA furnace................        202.2  3113 B
    Inductively Coupled Plasma/   \5\ 200.7  3120 B
     Atomic Emission
     Spectrometry (ICP/AES)
     \36\.
    Direct Current Plasma       ...........  ..........................  D4190-82(88).................  .........................  Note 34.
     (DCP) \36\.
    Colorimetric (Eriochrome    ...........  3500-Al D
     cyanine R).
4. Ammonia (as N), mg/L:
    Manual, distillation (at          350.2  4500-NH3B.................  .............................  .........................  973.49.\3\
     pH 9.5),\6\ followed by.
    Nesslerization............        350.2  4500-NH3C.................  D1426-93(A)..................  I-3520-85................  973.49.\3\
    Titration.................        350.2  4500-NH3E
    Electrode.................        350.3  4500-NH3F or G............  D1426-93(B)
    Automated phenate, or.....        350.1  4500-NH3H.................  .............................  I-4523-85
    Automated electrode.......  ...........  ..........................  .............................  .........................  Note 7.
5. Antimony-Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        204.1  3111 B
    AA furnace................        204.2  3113 B
    ICP/AES \36\..............    \5\ 200.7  3120 B
6. Arsenic-Total,\4\ mg/L:
    Digestion \4\ followed by.        206.5
        AA gaseous hydride....        206.3  3114 B 4.d................  D2972-93(B)..................  I-3062-85
        AA furnace............        206.2  3113 B....................  D2972-93(C)
        ICP/AES,\36\ or.......    \5\ 200.7  3120 B
        Colorimetric (SDDC)...        206.4  3500-As C.................  D2972-93(A)..................  I-3060-85
7. Barium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        208.1  3111 D....................  .............................  I-3084-85
    AA furnace................        208.2  3113 B....................  D4382-91
    ICP/AES \36\..............    \5\ 200.7  3120 B
    DCP \36\..................  ...........  ..........................  .............................  .........................  Note 34.
8. Beryllium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        210.1  3111 D....................  D3645-93(88)(A)..............  I-3095-85
    AA furnace................        210.2  3113 B....................  D3645-93(88)(B)
    ICP/AES...................    \5\ 200.7  3120 B
    DCP, or...................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.

[[Page 9]]

 
    Colorimetric (aluminon)...  ...........  3500-Be D
9. Biochemical oxygen demand
 (BOD5), mg/L:
    Dissolved Oxygen Depletion        405.1  5210 B....................  .............................  I-1578-78 \8\............  973.44,\3\ p. 17.\9\
10. Boron \37\--Total, mg/L:
    Colorimetric (curcumin)...        212.3  4500-B B..................  .............................  I-3112-85
    ICP/AES, or...............    \5\ 200.7  3120 B
    DCP.......................  ...........  ..........................  D4190-82(88).................  .........................  Note 34
11. Bromide, mg/L:
    Titrimetric...............        320.1  ..........................  D1246-82(88)(C)..............  I-1125-85................  p. S44.\10\
12. Cadmium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        213.1  3111 B or C...............  D3557-90(A or B).............  I-3135-85 or I-3136-85...  974.27,\3\ p. 37.\9\
    AA furnace................        213.2  3113 B....................  D3557-90(D)
    ICP/AES \36\..............    \5\ 200.7  3120 B....................  .............................  I-1472-85
    DCP \36\..................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Voltametry,\11\ or........  ...........  ..........................  D3557-90(C)
    Colorimetric (Dithizone)..  ...........  3500-Cd D
13. Calcium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        215.1  3111 B....................  D511-93(B)...................  I-3152-85
    ICP/AES...................    \5\ 200.7  3120 B
    DCP, or...................  ...........  ..........................  .............................  .........................  Note 34.
    Titrimetric (EDTA)........        215.2  3500-Ca D.................  D511-93(A)
14. Carbonaceous biochemical
 oxygen demand (CBOD5), mg/L
 \12\:
    Dissolved Oxygen Depletion  ...........  5210 B
     with nitrification
     inhibitor.
15. Chemical oxygen demand            410.1  5220 C....................  D1252-88(A)..................  I-3560-85................  973.46,\3\ p. 17.\9\
 (COD), mg/L; Titrimetric, or.        410.2                                                             I-3562-85................
                                      410.3
    Spectrophotometric, manual        410.4  5220 D....................  D1252-88(B)..................  I-3561-85................  Notes 13 or 14.
     or automated.
16. Chloride, mg/L:
    Titrimetric (silver         ...........  4500-Cl- B................  D512-89(B)...................  I-1183-85
     nitrate) or.
    (Mercuric nitrate)........        325.3  4500-Cl- C................  D512-89(A)...................  I-1184-85................  973.51.\3\
    Colorimetric, manual or...  ...........  ..........................  .............................  I-1187-85
    Automated (Ferricyanide)..     325.1 or  4500-Cl-E.................  .............................  I-2187-85
                                      325.2
17. Chlorine--Total residual,
 mg/L; Titrimetric:
    Amperometric direct.......        330.1  4500-Cl D.................  D1253-86(92)
    Iodometric direct.........        330.3  4500-Cl B
    Back titration ether end-         330.2  4500-Cl C
     point \15\ or.
    DPD-FAS...................        330.4  4500-Cl F
    Spectrophotometric, DPD...        330.5  4500-Cl G
    Or Electrode..............  ...........  ..........................  .............................  .........................  Note 16.
18. Chromium VI dissolved, mg/
 L; 0.45 micron filtration
 followed by:
    AA chelation-extraction or        218.4  3111 C....................  .............................  I-1232-85
    Colorimetric                ...........  3500-Cr D.................  D1687-92(A)..................  I-1230-85
     (Diphenylcarbazide).
19. Chromium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        218.1  3111 B....................  D1687-92(B)..................  I-3236-85................  974.27.\3\
    AA chelation-extraction...        218.3  3111 C
    AA furnace................        218.2  3113 B....................  D1687-92(C)

[[Page 10]]

 
    ICP/AES \36\..............    \5\ 200.7  3120 B
    DCP,\36\ or...............  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric                ...........  3500-Cr D
     (Diphenylcarbazide)
20. Cobalt--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        219.1  3111 B or C...............  D3558-90(A or B).............  I-3239-85................  p. 37.\9\
    AA furnace................        219.2  3113 B....................  D3558-90(C)
    ICP/AES...................    \5\ 200.7  3120 B
    DCP.......................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
21. Color platinum cobalt
 units or dominant wavelength,
 hue, luminance purity:
    Colorimetric (ADMI), or...        110.1  2120 E....................  .............................  .........................  Note 18.
    (Platinum cobalt), or.....        110.2  2120 B....................  .............................  I-1250-85................  .....................
    Spectrophotometric........        110.3  2120 C
22. Copper--Total,4 mg/L;
 Digestion 4 followed by:
    AA direct aspiration 36...        220.1  3111 B or C...............  D1688-90(A or B).............  I-3270-85 or I3271-85....  974.27 3 p. 37.9
    AA furnace................        220.2  3113 B....................  D1688-90(C)
    ICP/AES 36................      5 200.7  3120 B
    DCP 36 or.................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric (Neocuproine)  ...........  3500-Cu D
     or.
    (Bicinchoninate)..........  ...........  Or E......................  .............................  .........................  Note 19.
23. Cyanide--Total, mg/L:
    Manual distillation with    ...........  4500-CN C.................  D2036-91(A)
     MgCl2 followed by.
    Titrimetric, or...........  ...........  4500-CN D.................  .............................  .........................  p. 22.9
    Spectrophotometric, manual     31 335.2  4500-CN E.................  D2036-91(A)..................  I-3300-85
     or.
    Automated 20..............     31 335.3
24. Cyanide amenable to
 chlorination,mg/L:
    Manual distillation with          335.1  4500-CN G.................  D2036-91(B)
     MgCl2 followed by
     titrimetric or
     Spectrophotometric.
25. Fluoride--Total, mg/L:
    Manual distillation 6       ...........  4500-F B
     followed by.
    Electrode, manual or......        340.2  4500-F C..................  D1179-93(B)
    Automated.................  ...........  ..........................  .............................  I-4327-85
    Colorimetric (SPADNS).....        340.1  4500-F D..................  D1179-93(A)
    Or Automated complexone...        340.3  4500-F E
26. Gold--Total,4 mg/L;
 Digestion 4 followed by:
    AA direct aspiration......        231.1  3111 B
    AA furnace, or............        231.2
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
27. Hardness--Total, as CaCO3,
 mg/L
    Automated colorimetric,...        130.1
    Titrimetric (EDTA), or Ca         130.2  2340 B or C...............  D1126-86(92).................  I-1338-85................  973.52B.3
     plus Mg as their
     carbonates, by
     inductively coupled
     plasma or AA direct
     aspiration. (See
     Parameters 13 and 33).
28. Hydrogen ion (pH), pH
 units

[[Page 11]]

 
    Electrometric measurement,        150.1  4500-H= B.................  D1293-84(90)(A or B).........  I-1586-85................  973.41.3
     or.
    Automated electrode.......  ...........  ..........................  .............................  .........................  Note 21.
29. Iridium--Total,4 mg/L;
 Digestion 4 followed by:
    AA direct aspiration or...        235.1  3111 B
    AA furnace................        235.2
30. Iron--Total,4 mg/L;
 Digestion 4 followed by:
    AA direct aspiration 36...        236.1  3111 B or C...............  D1068-90(A or B).............  I-3381-85................  974.27.3
    AA furnace................        236.2  3113 B....................  D1068-90(C)
    ICP/AES 36................      5 200.7  3120 B
    DCP 36 or.................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric                ...........  3500-Fe D.................  D1068-90(D)..................  .........................  Note 22.
     (Phenanthroline).
31. Kjeldahl Nitrogen--Total,
 (as N), mg/L:
    Digestion and distillation        351.3  4500-NH3B or C............  D3590-89(A)..................  .........................  .....................
     followed by:.
    Titration.................        351.3  4500-NH3E.................  D3590-89(A)..................  .........................  973.483.
    Nesslerization............        351.3  4500-NH3C.................  D3590-89(A)..................  .........................  .....................
    Electrode.................        351.3  4500-NH3F or G............  .............................  .........................  .....................
    Automated phenate                 351.1  ..........................  .............................  I-4551-788...............  .....................
     colorimetric.
    Semi-automated block              351.2  ..........................  D3590-89(B)..................  .........................  .....................
     digester colorimetric.
    Manual or block digester          351.4  ..........................  D3590-89(A)..................  .........................  .....................
     potentiometric.
    Block Digester, followed
     by:.
    Auto distillation and       ...........  ..........................  .............................  .........................  Note 39.
     Titration, or.
    Nesslerization............  ...........  ..........................  .............................  .........................  Note 40.
    Flow injection gas          ...........  ..........................  .............................  .........................  Note 41.
     diffusion.
 
32. Lead--Total,4 mg/L;
 Digestion \4\ followed by:
    AA direct aspiration 36...        239.1  3111 B or C...............  D3559-90(A or B).............  I-3399-85................  974.27.3
    AA furnace................        239.2  3113 B....................  D3559-90(D)
    ICP/AES 36................      5 200.7  3120 B
    DCP 36....................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Voltametry 11 or..........  ...........  ..........................  D3559-90(C)
    Colorimetric (Dithizone)..  ...........  3500-Pb D
33. Magnesium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        242.1  3111 B....................  D511-93(B)...................  I-3447-85................  974.27.\3\
    ICP/AES...................    \5\ 200.7  3120 B
    DCP, or...................  ...........  ..........................  .............................  .........................  Note 34.
    Gravimetric...............  ...........  3500-Mg D
34. Manganese--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        243.1  3111 B....................  D858-90(A or B)..............  I-3454-85................  974.27.\3\
    AA furnace................        243.2  3113 B....................  D858-90(C)
    ICP/AES \36\..............    \5\ 200.7  3120 B
    DCP \36\ or...............  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric (Persulfate),  ...........  3500-Mn D.................  .............................  .........................  920.203.\3\
     or.
    (Periodate)...............  ...........  ..........................  .............................  .........................  Note 23.
35. Mercury--Total,\4\ mg/L:
    Cold vapor, manual, or....        245.1  3112 B....................  D3223-91.....................  I-3462-85................  \3\ 977.22
    Automated.................        245.2  ..........................  .............................  .........................  .....................
    Oxidation, purge and trap,    \43\ 1631  ..........................  .............................  .........................  .....................
     and cold vapor atomic
     fluorescence spectrometry
     (ng/L).
36. Molybdenum--Total,\4\ mg/
 L; Digestion \4\ followed by:
    AA direct aspiration......        246.1  3111 D....................  .............................  I-3490-85

[[Page 12]]

 
    AA furnace................        246.2  3113 B
    ICP/AES...................    \5\ 200.7  3120 B
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
37. Nickel--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration \36\.        249.1  3111 B or C...............  D1886-90(A or B).............  I-3499-85
    AA furnace................        249.2  3113 B....................  D1886-90(C)
    ICP/AES \36\..............    \5\ 200.7  3120 B
    DCP \36\, or..............  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric (heptoxime)..  ...........  3500-Ni D
38. Nitrate (as N), mg/L:
    Colorimetric (Brucine             352.1  ..........................  .............................  .........................  973.50,\3\ 419 D,\17\
     sulfate), or Nitrate-                                                                                                          p. 28.\9\
     nitrite N minus Nitrite N
     (See parameters 39 and
     40).
39. Nitrate-nitrite (as N), mg/
 L:
    Cadmium reduction, Manual         353.3  4500-NO3- E...............  D3867-90(B)
     or.
    Automated, or.............        353.2  4500-NO3- F...............  D3867-90(A)..................  I-4545-85
    Automated hydrazine.......        353.1  4500-NO3- H
40. Nitrite (as N), mg/L;
 Spectrophotometric:
    Manual or.................        354.1  4500-NO2- B...............  .............................  .........................  Note 25.
    Automated (Diazotization).  ...........  ..........................  .............................  I-4540-85
41. Oil and grease--Total             413.1  5520 B\38\................
 recoverable, mg/L:
 Gravimetric (extraction)
    Oil and grease and non-      1664, Rev.
     polar material, mg/L:                A
     Hexane extractable
     material (HEM): n-Hexane
     extraction and
     gravimetry\42\.
    Silica gel treated HEM       1664, Rev.
     (SGT-HEM): Silica gel                A
     treatment and
     gravimetry\42\.
42. Organic carbon--Total
 (TOC), mg/L:
    Combustion or oxidation...        415.1  5310 B, C, or D...........  D2579-93 (A or B)............  .........................  973.47,3 p. 14.24
43. Organic nitrogen (as N),
 mg/L:
    Total Kjeldahl N
     (Parameter 31) minus
     ammonia N (Parameter 4)
44. Orthophosphate (as P), mg/
 L; Ascorbic acid method:
    Automated, or.............        365.1  4500-P F..................  .............................  I-4601-85................  973.56.3
    Manual single reagent.....        365.2  4500-P E..................  D515-88(A)                     .........................  973.55 3.
    Manual two reagent........        365.3
45. Osmium--Total 4, mg/L;
 Digestion 4 followed by:
    AA direct aspiration, or..        252.1  3111 D
    AA furnace................        252.2
46. Oxygen, dissolved, mg/L:
    Winkler (Azide                    360.2  4500-O C..................  D888-92(A)...................  I-1575-78 8..............  973.45B.3
     modification), or.
    Electrode.................        360.1  4500-O G..................  D888-92(B)...................  I-1576-78 8
47. Palladium--Total,4 mg/L;
 Digestion 4 followed by:
    AA direct aspiration, or..        253.1  3111 B....................  .............................  .........................  p. S27.10
    AA furnace................        253.2  ..........................  .............................  .........................  p. S28.10

[[Page 13]]

 
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
48. Phenols, mg/L:
    Manual distillation \26\..        420.1  ..........................  .............................  .........................  Note 27.
    Followed by:
        Colorimetric (4AAP)           420.1  ..........................  .............................  .........................  Note 27.
         manual, or
        Automated \19\........        420.2
49. Phosphorus (elemental), mg/
 L:
    Gas-liquid chromatography.  ...........  ..........................  .............................  .........................  Note 28.
50. Phosphorus--Total, mg/L:
    Persulfate digestion              365.2  4500-P B,5................  .............................  .........................  973.55.\3\
     followed by.
    Manual or.................     365.2 or  4500-P E..................  D515-88(A)
                                      365.3
    Automated ascorbic acid           365.1  4500-P F..................  .............................  I-4600-85................  973.56.\3\
     reduction.
    Semi-automated block              365.4  ..........................  D515-88(B)
     digestor.
51. Platinum--Total,\4\ mg/L;
 Digestion \4\ followed by:
  AA direct aspiration........        255.1  3111 B
    AA furnace................        255.2
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
52. Potassium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        258.1  3111 B....................  .............................  I-3630-85................  973.53.\3\
    ICP/AES...................    \5\ 200.7  3120 B
    Flame photometric, or.....  ...........  3500-K D
    Colorimetric..............  ...........  ..........................  .............................  .........................  317 B.\17\
53. Residue--Total, mg/L:
    Gravimetric, 103-105 deg..        160.3  2540 B....................  .............................  I-3750-85
54. Residue--filterable, mg/L:
    Gravimetric, 180 deg......        160.1  2540 C....................  .............................  I-1750-85
55. Residue--nonfilterable
 (TSS), mg/L:
    Gravimetric, 103-105 deg.         160.2  2540 D....................  .............................  I-3765-85
     post washing of residue.
56. Residue--settleable, mg/L:
    Volumetric, (Imhoff cone),        160.5  2540 F
     or gravimetric.
57. Residue--Volatile, mg/L:
    Gravimetric, 550 deg......        160.4  ..........................  .............................  I-3753-85
58. Rhodium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration, or..        265.1  3111 B
    AA furnace................        265.2
59. Ruthenium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration, or..        267.1  3111 B
    AA furnace................        267.2
60. Selenium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA furnace................        270.2  3113 B....................  D3859-93(B)
    ICP/AES,\36\ or...........    \5\ 200.7  3120 B
    AA gaseous hydride........  ...........  3114 B....................  D3859-93(A)..................  I-3667-85
61. Silica \37\--Dissolved, mg/
 L; 0.45 micron filtration
 followed by:
    Colorimetric, Manual or...        370.1  4500-Si D.................  D859-88......................  I-1700-85
    Automated                   ...........  ..........................  .............................  I-2700-85
     (Molybdosilicate), or.
    ICP.......................    \5\ 200.7  3120 B
62. Silver--Total,\4\ mg/L;
 Digestion 4, 29 followed by:
    AA direct aspiration......        272.1  3111 B or C...............  .............................  I-3720-85................  974.27,\3\ p. 37.\9\

[[Page 14]]

 
    AA furnace................        272.2  3113 B
    ICP/AES...................    \5\ 200.7  3120 B
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
63. Sodium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        273.1  3111 B....................  .............................  I-3735-85................  973.54.\3\
    ICP/AES...................    \5\ 200.7  3120 B
    DCP, or...................  ...........  ..........................  .............................  .........................  Note 34.
    Flame photometric.........  ...........  3500 Na D
64. Specific conductance,
 micromhos/cm at 25  deg.C:
    Wheatstone bridge.........        120.1  2510 B....................  D1125-91(A)..................  I-1780-85................  973.40.\3\
65. Sulfate (as SO4), mg/L:
    Automated colorimetric            375.1
     (barium chloranilate).
    Gravimetric...............        375.3  4500-SO4-2 C or D.........  .............................  .........................  925.54.\3\
    Turbidimetric, or.........        375.4  ..........................  D516-90......................  .........................  426C.\30\
66. Sulfide (as S), mg/L:
    Titrimetric (iodine), or..        376.1  4500-S-2E.................  .............................  I-3840-85
    Colorimetric (methylene           376.2  4500-S-2D
     blue).
67. Sulfite (as SO3), mg/L:
    Titrimetric (iodine-              377.1  4500-SO3-2 B
     iodate).
68. Surfactants, mg/L:
    Colorimetric (methylene           425.1  5540 C....................  D2330-88
     blue).
69. Temperature,  deg.C:
    Thermometric..............        170.1  2550 B....................  .............................  .........................  Note 32.
70. Thallium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        279.1  3111 B
    AA furnace................        279.2
    ICP/AES, or...............    \5\ 200.7  3120 B
71. Tin--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        282.1  3111 B....................  .............................  I-3850-78 \8\
    AA furnace, or............        282.2  3113 B
    ICP/AES...................    \5\ 200.7
72. Titanium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        283.1  3111 D
    AA furnace................        283.2
    DCP.......................  ...........  ..........................  .............................  .........................  Note 34.
73. Turbidity, NTU:
    Nephelometric.............        180.1  2130 B....................  D1889-88(A)..................  I-3860-85
74. Vanadium--Total,\4\ mg/L;
 Digestion \4\ followed by:
    AA direct aspiration......        286.1  3111 D
    AA furnace................        286.2  ..........................  D3373-93
    ICP/AES...................    \5\ 200.7  3120 B
    DCP, or...................  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric (Gallic acid)  ...........  3500-V D
75. Zinc--Total,\4\ mg/L;
 Digestion \4\ followed by:

[[Page 15]]

 
    AA direct aspiration \36\.        289.1  3111 B or C...............  D1691-90 (A or B)............  I-3900-85................  974.27,\3\ p. 37.\9\
    AA furnace................        289.2
    ICP/AES \36\..............    \5\ 200.7  3120 B
    DCP,\36\ or...............  ...........  ..........................  D4190-82(88).................  .........................  Note 34.
    Colorimetric (Dithizone)    ...........  3500-Zn E
     or.
    (Zincon)..................  ...........  3500-Zn F.................  .............................  .........................  Note 33.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes'', Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-
  CI), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.
\2\ Fishman, M.J., et al, ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques
  of Water--Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' methods manual, 15th ed. (1990).
\4\ For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended
  material and to destroy possible organic-metal complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes,
  1979 and 1983''. One (section 4.1.3), is a vigorous digestion using nitric acid. A less vigorous digestion using nitric and hydrochloric acids
  (section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types. Particularly,
  if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive
  state. In those situations, the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing
  large amounts of organic materials may also benefit by this vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert
  antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as well as determinations for certain elements such as
  antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all cases the
  method write-up should be consulted for specific instructions and/or cautions.
Note to Table IB Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the
  above, the EPA procedure must be used.
Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the
  referenced procedure for total metals must be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample
  solution for total metals) may be omitted for AA (direct aspiration or graphite furnace) and ICP analyses, provided the sample solution to be analyzed
  meets the following criteria:
  a. has a low COD (20)
  b. is visibly transparent with a turbidity measurement of 1 NTU or less
  c. is colorless with no perceptible odor, and
  d. is of one liquid phase and free of particulate or suspended matter following acidification.
\5\ The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,''
  is given at Appendix C of this Part 136.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary
  distillation step is not necessary: however, manual distillation will be required to resolve any controversies.
\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, (Bran & Luebbe (Technicon) Auto Analyzer II, Bran
  & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.
\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5,
  Chapter A1 (1979).
\9\ American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 1430 Broadway, New York, NY 10018.
\10\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of
  Standard Methods for the Examination of Water and Wastewater (1981).
\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 which measures ``total 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 the nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.
\14\ Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\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, 840 Memorial Drive, Cambridge, MA
  02138. 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\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
\18\ National Council of the Paper Industry for Air and Stream Improvement, (Inc.) Technical Bulletin 253, December 1971.
\19\ Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\20\ After the manual distillation is completed, the autoanalyzer manifolds in EPA Methods 335.3 (cyanide) or 420.2 (phenols) are simplified by
  connecting the re-sample line directly to the sampler. When using the mainfold setup shown in Method 335.3, the buffer 6.2 should be replaced with the
  buffer 7.6 found in Method 335.2.
\21\ Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran &
  Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.

[[Page 16]]

 
\23\ Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company,
  Loveland, CO 80537.
\24\ Wershaw, R.L., et al, ``Methods for Analysis of Organic Substances in Water,'' Techniques of Water-Resources Investigation of the U.S. Geological
  Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14.
\25\ Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted
  at a pH of 10.00.2. The approved methods are given on pp 576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the
  manual colorimetric procedure, or Method 510C for the manual spectophotometric procedure.
\28\ R. F. Addison and R.G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,'' Journal of Chromatography, vol. 47,
  No. 3, pp. 421-426, 1970.
\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 Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
  approved method is satisfactory.
\30\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition.
\31\ EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of
  total cyanide.
\32\ Stevens, H.H., Ficke, J.F., and Smoot, G.F., ``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.
\33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\ ``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--
  Revised 1991, Fison Instruments, Inc., 32 Commerce Center, Cherry Hill Drive, Danvers, MA 01923.
\35\ Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC
  method for arsenic are provided in Appendix D of this part titled, ``Precision and Recovery Statements for Methods for Measuring Metals''.
\36\ ``Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals'', CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200,
  April 16, 1992. Available from the 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 the trichlorofluoromethane extraction solvent is approved.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, Perstop Analytical
  Corporation.
\40\ Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, Perstop Analytical
  Corporation.
\41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, Perstop Analytical Corporation.
\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractablke Material (SGT-HEM; Non-
  polar Material) by Extraction and Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port
  Royal, Springfield, Virginia 22161.
\43\ The application of clean techniques described in EPA's draft 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.


                                     Table IC.--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                 EPA method number 2 7
        Parameter \1\         --------------------------------------------------------------------------------------------------------------------------
                                       GC                 GC/MS           HPLC         Standard method 18th Ed.              ASTM              Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
 1. Acenaphthene.............                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 2. Acenaphthylene...........                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 3. Acrolein.................                 603       \4\ 604, 1624  .........  .................................  ....................
 4. Acrylonitrile............                 603       \4\ 624, 1624        610  .................................  ....................
 5. Anthracene...............                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 6. Benzene..................                 602           624, 1624  .........  6210 B, 6220 B                     ....................
 7. Benzidine................  ..................       \5\ 625, 1625        605  .................................  ....................  Note 3, p.1.
 8. Benzo(a)anthracene.......                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 9. Benzo(a)pyrene...........                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 10. Benzo(b)fluoranthene....                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 11. Benzo(g, h, i)perylene..                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 12. Benzo(k)fluoranthene....                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 13. Benzyl chloride.........  ..................  ..................  .........  .................................  ....................  Note 3,
                                                                                                                                            p.130: Note
                                                                                                                                            6, p. S102.

[[Page 17]]

 
 14. Benzyl butyl phthalate..                 606           625, 1625  .........  6410 B                             ....................  .............
 15. Bis(2-chloroethoxy)                      611           625, 1625  .........  6410 B                             ....................
 methane.
 16. Bis(2-chloroethyl) ether                 611           625, 1625  .........  6410 B                             ....................
 17. Bis (2-ethylhexyl)                       606           625, 1625  .........  6410 B, 6230 B                     ....................
 phthalate.
 18. Bromodichloromethane....                 601           624, 1624  .........  6210 B, 6230 B                     ....................
 19. Bromoform...............                 601           624, 1624  .........  6210 B, 6230 B                     ....................
 20. Bromomethane............                 601           624, 1624  .........  6210 B, 6230 B                     ....................
 21. 4-Bromophenylphenyl                      611           625, 1625  .........  6410 B                             ....................
 ether.
 22. Carbon tetrachloride....                 601           624, 1624  .........  6230 B, 6410 B                     ....................  Note 3,
                                                                                                                                            p.130.
 23. 4-Chloro-3-methylphenol.                 604           625, 1625  .........  6410 B, 6420 B                     ....................
 24. Chlorobenzene...........            601, 602           624, 1624  .........  6210 B, 6220 B                     ....................  Note 3,
                                                                                  6230 B                                                    p.130.
 25. Chloroethane............                 601           624, 1624  .........  6210 B, 6230 B                     ....................
 26. 2-Chloroethylvinyl ether                 601           624, 1624  .........  6210 B, 6230 B                     ....................  .............
 27. Chloraform..............                 601           624, 1624  .........  6210 B, 6230 B                     ....................  Note, p.130.
 28. Chloromethane...........                 601           624, 1624  .........  6210 B. 6230 B                     ....................
 29. 2-Chloronaphthalene.....                 612           625, 1625  .........  6410 B                             ....................
 30. 2-Chlorophenol..........                 604           625, 1625  .........  6410 B, 6420 B                     ....................
 31. 4-Chlorophenylphenyl                     611           625, 1625  .........  6410 B                             ....................
 ether.
 32. Chrysene................                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 33. Dibenzo(a,h)anthracene..                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 34. Dibromochloromethane....                 601           624, 1624  .........  6210 B, 6230 B                     ....................
 35. 1, 2-Dichlorobenzene....         601,602,612        624,625,1625  .........  6410 B, 6230 B, 6220 B             ....................
 36. 1, 3-Dichlorobenzene....         601,602,612        624,625,1625  .........  6410 B, 6230 B, 6220 B             ....................
 37. 1,4-Dichlorobenzene.....       601, 602, 612      624, 625, 1625  .........  6410 B, 6220 B, 6230 B
 38. 3, 3-Dichlorobenzidine..  ..................           625, 1625        605  6410 B                             ....................
 39. Dichlorodifluoromethane.                 601  ..................  .........  6230 B                             ....................
 40. 1, 1-Dichloroethane.....                 601           624, 1624  .........  6230 B, 6210 B                     ....................
 41. 1, 2-Dichloroethane.....                 601           624, 1624  .........  6230 B, 6210 B                     ....................
 42. 1, 1-Dichloroethene.....                 601           624, 1624  .........  6230 B, 6210 B                     ....................
 43. trans-1, 2-                              601           624, 1624  .........  6230 B, 6210 B                     ....................
 Dichloroethene.
 44. 2, 4-Dichlorophenol.....                 604           625, 1625  .........  6420 B, 6410 B                     ....................
 45. 1, 2-Dichloropropane....                 601           624, 1624  .........  6230 B, 6210 B                     ....................
 46. cis-1, 3-Dichloropropene                 601           624, 1624  .........  6230 B, 6210 B                     ....................
 47. trans-1, 3-                              601           624, 1624  .........  6230 B, 6210 B                     ....................
 Dichloropropene.
 48. Diethyl phthalate.......                 606           625, 1625  .........  6410 B                             ....................
 49. 2, 4-Dimethylphenol.....                 604           625, 1625  .........  6420 B, 6410 B                     ....................
 50. Dimethyl phthalate......                 606           625, 1625  .........  6410 B                             ....................
 51. Di-n-butyl phthalate....                 606           625, 1625  .........  6410 B                             ....................
 52. Di-n-octyl phthalate....                 606           625, 1625  .........  6410 B                             ....................
 53. 2,4-Dinitrophenol.......                 604           625, 1625  .........  6420 B, 6410 B                     ....................
 54. 2,4-Dinitrotoluene......                 609           625, 1625  .........  6410 B
 55. 2, 6-Dinitrotoluene.....                 609           625, 1625  .........  6410 B                             ....................
 56. Epichlorohydrin.........  ..................  ..................  .........  .................................  ....................  Note 3, p.130
                                                                                                                                            Note 6,
                                                                                                                                            p.S102.
 57. Ethylbenzene............                 602           624, 1624  .........  6220 B, 6210 B                     ....................
 58. Fluoranthene............                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 59. Fluorene................                 610           625, 1625        610  6410 B, 6440 B                     D4657-92
 60. 1,2,3,4,6,7,8-            ..................                1613  .........
 Heptachlorodibenzofuran.

[[Page 18]]

 
 61. 1,2,3,4,7,8,9-            ..................                1613  .........
 Heptachlorodibenzofuran.
 62. 1,2,3,4,6,7,8-            ..................                1613  .........
 Heptachlorodibenzo-p-dioxin.
 63. Hexachlorobenzene.......                 612           625, 1625  .........  6410 B
 64. Hexachlorobutadiene.....                 612           625, 1625  .........  6410 B
 65.                                          612       625, 1625 \5\  .........  6410 B
 Hexachlorocyclopentadiene.
 66. 1,2,3,4,7,8-              ..................                1613  .........
 Hexachlorodibenzofuran.
 67. 1,2,3,6,7,8-              ..................                1613  .........
 Hexachlorodibenzofuran.
 68. 1,2,3,7,8,9-              ..................                1613  .........
 Hexachlorodibenzofuran.
 69. 2,3,4,6,7,8-              ..................                1613  .........
 Hexachlorodibenzofuran.
 70. 1,2,3,4,7,8-              ..................                1613  .........
 Hexachlorodibenzo-p-dioxin.
 71. 1,2,3,6,7,8-              ..................                1613  .........
 Hexachlorodibenzo-p-dioxin.
 72. 1,2,3,7,8,9-              ..................                1613  .........
 Hexachlorodibenzo-p-dioxin.
 73. Hexachloroethane........                 616           625, 1625  .........  6410 B
 74. Ideno(1,2,3-cd)pyrene...                 610           625, 1625        610  6410 B, 6440 B                     D4657-87
 75. Isophorone..............                 609           625, 1625  .........  6410 B
 76. Methylene chloride......                 601           624, 1624  .........  6230 B                                                   Note 3, p.
                                                                                                                                            130.
 77. 2-Methyl-4,6-                            604           625, 1625  .........  6420 B, 6410 B
 dinitrophenol.
 78. Naphthalene.............                 610           625, 1625        610  6410 B, 6440 B
 79. Nitrobenzene............                 609           625, 1625  .........  6410 B                             D4657-87
 80. 2-Nitrophenol...........                 604           625, 1625  .........  6410 B, 6420 B
 81. 4-Nitrophenol...........                 604           625, 1625  .........  6410 B, 6420 B
 82. N-Nitrosodimethylamine..                 607           625, 1625  .........  6410 B
 83. N-Nitrosodi-n-                           607       625, 1625 \5\  .........  6410 B
 propylamine.
 84. N-Nitrosodiphenylamine..                 607       625, 1625 \5\  .........  6410 B
 85. Octachlorodibenzofuran..  ..................                1613  .........
 86. Octachlorodibenzo-p-      ..................                1613  .........
 dioxin.
 87. 2,2-Oxybis(1-                            611           625, 1625  .........  6410 B
 chloropropane).
 88. PCB-1016................                 608                 625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            43.
 89. PCB-1221................                 608                 625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            43.
 90. PCB-1232................                 608                 625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            43.
 91. PCB 1242................                 608                 625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            43.
 92. PCB-1248................                 608                 625  .........
 93. PCB-1254................                 608                 625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            43.
 94. PCB-1260................                 608                 625  .........  6410 B, 6630 B                                           Note 3, p.
                                                                                                                                            43.
 95. 1,2,3,7,8-                ..................                1613  .........
 Pentachlorodibenzofuran.
 96. 2,3,4,7,8-                ..................                1613  .........
 Pentachlorodibenzofuran.
 97. 1,2,3,7,8-                ..................                1613  .........
 Pentachlorodibenzo-p-dioxin.
 98. Pentachlorophenol                        604           625, 1625  .........  6410 B, 6630 B                                           Note 3, p.
                                                                                                                                            140.
 99. Phenanthrene............                 610           625, 1625        610  6410 B, 6440 B                     D4657-87
 100. Phenol.................                 604           625, 1625  .........  6420 B, 6410 B
 101. Pyrene.................                 610           625, 1625        610  6410 B, 6440 B                     D4657-87
 102. 2,3,7,8-                 ..................                1613  .........
 Tetrachlorodibenzofuran.
 103. 2,3,7,8-                 ..................       613, 1613 \5\  .........
 Tetrachlorodibenzo-p-dioxin.
 104. 1,1,2,2-                                601           624, 1624  .........  6230 B, 6210 B                                           Note 3, p.
 Tetrachloroethane.                                                                                                                         130.

[[Page 19]]

 
 105. Tetrachloroethene......                 601           624, 1624  .........  6230 B, 6410 B                                           Note 3, p.
                                                                                                                                            130.
 106. Toluene................                 602           624, 1624  .........  6210 B, 6220 B
 107. 1,2,4-Trichlorobenzene.                 612           625, 1625  .........  6410 B                                                   Note 3, p.
                                                                                                                                            130.
 108. 1,1,1-Trichloroethane..                 601           624, 1624  .........  6210 B, 6230 B
 109. 1,1,2-Trichloroethane..                 601           624, 1624  .........  6210 B, 6230 B                                           Note 3, p.
                                                                                                                                            130.
 110. Trichloroethene........                 601           624, 1624  .........  6210 B, 6230 B
 111. Trichlorofluoromethane.                 601                 624  .........  6210 B, 6230 B
 112. 2,4,6-Trichlorophenol..                 604           625, 1625  .........  6410 B, 6240 B
 113. Vinyl chloride.........                 601           624, 1624  .........  6210 B, 6230 B
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1C notes:
\1\ All parameters are expressed in micrograms per liter (g/L) except for Method 1613 in which the parameters are expressed in picograms per
  liter (pg/L).
\2\ The full text of Methods 601-613, 624, 625, 1624, and 1625, are given at appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this
  part 136. The full text of Method 1613 is incorporated by reference into this part 136 and is available from the National Technical Information
  Services as stock number PB95-104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test
  procedures is given at appendix B, ``Definition and Procedures for the Determination of the Method Detection Limit,'' of this part 136.
\3\ ``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
  Agency, September, 1978.
\4\ Method 624 may be extended to screen samples for Acrolein and Acrylonitrile. However, when they are known to be present, the preferred method for
  these two compounds is Method 603 or Method 1624.
\5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they
  are known to be present, Methods 605, 607, and 612, or Method 1625, are preferred methods for these compounds.
5a 625, Screening only.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of
  Standard Methods for the Examination of Water and Wastewater (1981).
\7\ Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624,
  625, 1624, and 1625 (See Appendix A of this Part 136) 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 and 625 and 100% for methods 1624 and 1625) 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
  warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory
  compliance.
Note: These warning limits are promulgated as an ``interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'', 3M Corporation Revised 10/28/94.


                                              Table ID.--List of Approved Test Procedures for Pesticides 1
--------------------------------------------------------------------------------------------------------------------------------------------------------
            Parameter                        Method           EPA \2\ \7\  Standard methods 18th Ed.            ASTM                      Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin........................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
2. Ametryn.......................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
3. Aminocarb.....................  TLC                        ...........  .........................  ........................  Note 3, p. 94; Note 6,
                                                                                                                                 p. S16.
4. Atraton.......................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
5. Atrazine......................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
6. Azinphos methyl...............  GC                         ...........  .........................  ........................  Note 3, p. 25; Note 6,
                                                                                                                                 p. S51.
7. Barban........................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
8. -BHC.................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
9. -BHC.................  GC                                 608  6630 C...................  D3086-90................  Note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
10. -BHC................  GC                                 608  6630 C...................  D3086-90................  Note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
11. -BHC (Lindane)......  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
 

[[Page 20]]

 
12. Captan.......................  GC                         ...........  6630 B                     D3086-90                  Note 3, p. 7.
13. Carbaryl.....................  TLC                        ...........  .........................  ........................  Note 3, p. 94: Note 6,
                                                                                                                                 p. S60.
14. Carbophenothion..............  GC                         ...........  .........................  ........................  Note 4, p. 30; Note 6,
                                                                                                                                 p. S73.
15. Chlordane....................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
 
16. Chloropropham................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
17. 2,4-D........................  GC                         ...........  6640 B...................  ........................  Note 3, p. 115; Note 4,
                                                                                                                                 p. 35.
18. 4,4'-DDD.....................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
19. 4,4'-DDE.....................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
20. 4,4'-DDT.....................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
 
21. Demeton-O....................  GC                         ...........  .........................  ........................  Note 3, p. 25; Note 6,
                                                                                                                                 p. S51.
22. Demeton-S....................  GC                         ...........  .........................  ........................  Note 3, p. 25: Note 6,
                                                                                                                                 p. S51.
23. Diazinon.....................  GC                         ...........  .........................  ........................  Note 3, p. 25; Note 4,
                                                                                                                                 p. 30; Note 6, p. S51.
24. Dicamba......................  GC                         ...........  .........................  ........................  Note 3, p. 115.
25. Dichlofenthion...............  GC                         ...........  .........................  ........................  Note 4, p. 30; Note 6,
                                                                                                                                 p. S73.
26. Dichloran....................  GC                         ...........  6630 B & C...............  ........................  Note 3, p. 7.
27. Dicofol......................  GC                         ...........  .........................  D3086-90................  ........................
28. Dieldrin.....................  GC                                 608  6630 B & C...............  ........................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
 
29. Dioxathion...................  GC                         ...........  .........................  ........................  Note 4, p. 30; Note 6,
                                                                                                                                 p. S73.
30. Disulfoton...................  GC                         ...........  .........................  ........................  Note 3, p. 25; Note 6,
                                                                                                                                 p. S51.
31. Diuron.......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
32. Endosulfan I.................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
33. Endosulfan II................  GC                                 608  6630 B & C...............   D3086-90...............  Note 3, p. 7; note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
34. Endosulfan Sulfate...........  GC                                 608  6630 C...................  ........................  Note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
35. Endrin.......................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                          \5\ 625  6410 B...................  ........................  ........................
36. Endrin aldehyde..............  GC                                 608  .........................  ........................  Note 8.
                                   GC/MS                              625  .........................  ........................  ........................
 
37. Ethion.......................  GC                         ...........  .........................  ........................  Note 4, p. 30; Note 6,
                                                                                                                                 p. S73.
38. Fenuron......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
39. Fenuron-TCA..................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
40. Heptachlor...................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
41. Heptachlor epoxide...........  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 6, p. S73;
                                                                                                                                 note 8.

[[Page 21]]

 
                                   GC/MS                              625  6410 B...................  ........................  ........................
 
42. Isodrin......................  GC                         ...........  .........................  ........................  Note 4, p. 30; Note 6,
                                                                                                                                 p. S73.
43. Linuron......................  GC                         ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
44. Malathion....................  GC                         ...........  6630 C...................  ........................  Note 3, p. 25; Note 4,
                                                                                                                                 p. 30; Note 6, p. S51.
45. Methiocarb...................  TLC                        ...........  .........................  ........................  Note 3, p. 94; Note 6,
                                                                                                                                 p. S60.
46. Methoxychlor.................  GC                         ...........  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
 
47. Mexacarbate..................  TLC                        ...........  .........................  ........................  Note 3, p. 94; Note 6,
                                                                                                                                 p. S60.
48. Mirex........................  GC                         ...........  6630 B & C...............  ........................  Note 3, p. 7.
49. Monuron......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
50. Monuron......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
51. Nuburon......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
52. Parathion methyl.............  GC                         ...........  6630 C...................  ........................  Note 3, p. 25; Note 4,
                                                                                                                                 p. 30.
53. Parathion ethyl..............  GC                         ...........  6630 C...................  ........................  Note 3, p. 25.
54. PCNB.........................  GC                         ...........  6630 B & C...............  ........................  Note 3, p. 7.
55. Perthane.....................  GC                         ...........  .........................  D3086-90................  ........................
56. Prometron....................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
57. Prometryn....................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
58. Propazine....................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
59. Propham......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
60. Propoxur.....................  TLC                        ...........  .........................  ........................  Note 3, p. 94; Note 6,
                                                                                                                                 p. S60.
61. Secbumeton...................  TLC                        ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
62. Siduron......................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
63. Simazine.....................  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
64. Strobane.....................  GC                         ...........  6630 B & C...............  ........................  Note 3, p. 7.
65. Swep.........................  TLC                        ...........  .........................  ........................  Note 3, p. 104; Note 6,
                                                                                                                                 p. S64.
66. 2,4,5-T......................  GC                         ...........  6640 B...................  ........................  Note 3, p. 115; Note 4,
                                                                                                                                 p. 35.
67. 2,4,5-TP (Silvex)............  GC                         ...........  6640 B...................  ........................  Note 3, p. 115
68. Terbuthylazine...............  GC                         ...........  .........................  ........................  Note 3, p. 83; Note 6,
                                                                                                                                 p. S68.
69. Toxaphene....................  GC                                 608  6630 B & C...............  D3086-90................  Note 3, p. 7; note 4, p.
                                                                                                                                 30; note 8.
                                   GC/MS                              625  6410 B...................  ........................  ........................
70. Trifluralin..................  GC                         ...........  6630 B...................  ........................  Note 3, p. 7.
--------------------------------------------------------------------------------------------------------------------------------------------------------
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 1C, where
  entries are listed by chemical name.
\2\ The full text of Methods 608 and 625 are given at Appendix A. ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The
  standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B. ``Definition
  and Procedure for the Determination of the Method Detection Limit'', of this Part 136.
\3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
  Agency, September, 1978. This EPA publication includes thin-layer chromatography (TLC) methods.
\4\ ``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 (1987).
\5\ The method may be extended to include -BHC, -BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
  Method 608 is the preferred method.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of
  Standard Methods for the Examination of Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625
  (See Appendix A of this Part 136) in accordance with procedures given in section 8.2 of each of these methods. Additionally, each laboratory, on an-
  going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 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 and cannot be reported to demonstrate regulatory compliance. These
  quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
Note: These warning limits are promulgated as an ``Interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'', 3M Corporation, Revised 10/28/94.


[[Page 22]]


                                                 Table IE.--List of Approved Radiologic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                          Reference (method number or page)
                                                           ---------------------------------------------------------------------------------------------
       Parameter and units                 Method                                     Standard methods
                                                                    EPA\1\                18th Ed.                ASTM                  USGS \2\
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter...  Proportional or           900...................  7110 B                D1943-90              pp. 75 and 78.\3\
                                   scintillation counter.
2. Alpha-Counting error, pCi per  Proportional or           Appendix B............  7110 B                D1943-90              P. 79.
 liter.                            scintillation counter.
3. Beta-Total, pCi per liter....  Proportional counter....  900.0.................  7110 B                D1890-90              pp. 75 and 78.\3\
4. Beta-Counting error, pCi.....  Proportional counter....  Appendix B............  7110 B                D1890-90              p. 79.
5. (a) Radium Total pCi per       Proportional counter....  903.0.................  7500Ra B              D2460-90
 liter.
  (b)Ra, pCi per liter..........  Scintillation counter...  903.1.................  7500Ra C              D3454-91              p. 81.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IE notes:
\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 23]]


                        Table IF.--List of Approved Methods for Pharmaceutical Pollutants
----------------------------------------------------------------------------------------------------------------
   Pharmaceuticals pollutants              CAS registry No.                    Analytical method number
----------------------------------------------------------------------------------------------------------------
acetonitrile...................  75-05-8............................  1666/1671/D3371/D3695.
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.
n-butyl-acetate................  123-86-4...........................  1666/D3695.
tert-butyl alcohol.............  75-65-0............................  1666.
chlorobenzene..................  108-90-7...........................  502.2/524.2.
chloroform.....................  67-66-3............................  502.2/524.2/551.
o-dichlorobenzene..............  95-50-1............................  1625C/502.2/524.2.
1,2-dichloroethane.............  107-06-2...........................  D3695/502.2/524.2.
diethylamine...................  109-89-7...........................  1666/1671.
dimethyl sulfoxide.............  67-68-5............................  1666/1671.
ethanol........................  64-17-5............................  1666/1671/D3695.
ethyl acetate..................  141-78-6...........................  1666/D3695.
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.
Methyl Cellosolve ....  109-86-4...........................  1666/1671
methylene chloride.............  75-09-2............................  502.2/524.2
methyl formate.................  107-31-3...........................  1666.
4-methyl-2-pentanone (MIBK)....  108-10-1...........................  1624C/1666/D3695/D4763/524.2.
phenol.........................  108-95-2...........................  D4763.
n-propanol.....................  71-23-8............................  1666/1671/D3695.
2-propanone (acetone)..........  67-64-1............................  D3695/D4763/524.2.
tetrahydrofuran................  109-99-9...........................  1666/524.2.
toluene........................  108-88-3...........................  D3695/D4763/502.2/524.2.
triethlyamine..................  121-44-8...........................  1666/1671.
xylenes........................  (Note 1)...........................  1624C/1666.
----------------------------------------------------------------------------------------------------------------
Table 1F 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.

    (b) The full texts of the methods from the following references 
which are cited in Tables IA, IB, IC, ID, IE,and IF are incorporated by 
reference into this regulation and may be obtained from the sources 
identified. All costs cited are subject to change and must be verified 
from the indicated sources. The full texts of all the test procedures 
cited are available for inspection at the National Exposure Research 
Laboratory, Office of Research and Development, U.S. Environmental 
Protection Agency, 26 West Martin Luther King Dr., Cincinnati, OH 45268 
and the Office of the Federal Register, 800 North Capitol Street, NW., 
Suite 700, Washington, DC.

            References, Sources, Costs, and Table Citations:

    (1) The full texts of Methods 601-613, 624, 625, 1613, 1624, and 
1625 are printed in appendix A of this part 136. The full text for 
determining the method detection limit when using the test procedures is 
given in appendix B of this part 136. The full text of Method 200.7 is 
printed in appendix C of this part 136. Cited in: Table IB, Note 5; 
Table IC, Note 2; and Table ID, Note 2.
    (2) USEPA. 1978. Microbiological Methods for Monitoring the 
Environment, Water, and Wastes. Environmental Monitoring and Support 
Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. EPA/
600/8-78/017. Available from: National Technical Information Service, 
5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB-290329/
AS. Cost: $36.95. Table IA, Note 3.
    (3) ``Methods for Chemical Analysis of Water and Wastes,'' U.S. 
Environmental Protection Agency, EPA-600/4-79-020, March 1979, or 
``Methods for Chemical Analysis of Water and Wastes,'' U.S. 
Environmental Protection Agency, EPA-600/4-79-020, Revised March 1983. 
Available from: ORD Publications, CERI, U.S. Environmental

[[Page 24]]

Protection Agency, Cincinnati, Ohio 45268, Table IB, Note 1.
    (4) ``Methods for Benzidine, Chlorinated Organic Compounds, 
Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. 
Environmental Protection Agency, 1978. Available from: ORD Publications, 
CERI, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268, 
Table IC, Note 3; Table D, Note 3.
    (5) ``Prescribed Procedures for Measurement of Radioactivity in 
Drinking Water,'' U.S. Environmental Protection Agency, EPA-600/4-80-
032, 1980. Available from: ORD Publications, CERI, U.S. Environmental 
Protection Agency, Cincinnati, Ohio 45268, Table IE, Note 1.
    (6) American Public Health Association. 1992. Standard Methods for 
the Examination of Water and Wastewater. 18th Edition. Amer. Publ. Hlth. 
Assoc., 1015 15th Street NW, Washington, DC 20005. Cost: $160.00. Table 
IA, Note 4.
    (7) Ibid, 15th Edition, 1980. Table IB, Note 30; Table ID.
    (8) Ibid, 14th Edition, 1975. Table IB, Notes 17 and 27.
    (9) ``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. 
Available from: American Public Health Association, 1015 Fifteenth 
Street NW., Washington, DC 20036. Cost available from publisher. Table 
IB, Note 10; Table IC, Note 6; Table ID, Note 6.
    (10) Annual Book of ASTM Standards, Water and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02, 1994 in 40 CFR 136.3, 
Tables IB, IC, ID and IE.
    (11) USGS. 1989. 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, U.S. Geological Survey, U.S. Department of the 
Interior, Reston, Virginia. Available from: USGS Books and Open-File 
Reports Section, Federal Center, Box 25425, Denver, Colorado 80225. 
Cost: $18.00. Table IA, Note 5.
    (12) ``Methods for Determination of Inorganic Substances in Water 
and Fluvial Sediments,'' by M.J. Fishman and Linda C. Friedman, 
Techniques of Water-Resources Investigations of the U.S. Geological 
Survey, Book 5 Chapter A1 (1989). Available from: U.S. Geological 
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: 
$108.75 (subject to change). Table IB, Note 2.
    (13) ``Methods for Determination of Inorganic Substances in Water 
and Fluvial Sediments,'' N.W. Skougstad and others, editors. Techniques 
of Water-Resources Investigations of the U.S. Geological Survey, Book 5, 
Chapter A1 (1979). Available from: U.S. Geological Survey, Denver 
Federal Center, Box 25425, Denver, CO 80225. Cost: $10.00 (subject to 
change), Table IB, Note 8.
    (14) ``Methods for the Determination of Organic Substances in Water 
and Fluvial Sediments,'' Wershaw, R.L., et al, Techniques of Water-
Resources Investigations of the U.S. Geological Survey, Book 5, Chapter 
A3 (1987). Available from: U.S. Geological Survey, Denver Federal 
Center, Box 25425, Denver, CO 80225. Cost: $0.90 (subject to change). 
Table IB, Note 24; Table ID, Note 4.
    (15) ``Water Temperature--Influential Factors, Field Measurement and 
Data Presentation,'' by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot, 
Techniques of Water-Resources Investigations of the U.S. Geological 
Survey, Book 1, Chapter D1, 1975. Available from: U.S. Geological 
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $1.60 
(subject to change). Table IB, Note 32.
    (16) ``Selected Methods of the U.S. Geological Survey of Analysis of 
Wastewaters,'' by M.J. Fishman and Eugene Brown; U.S. Geological Survey 
Open File Report 76-77 (1976). Available from: U.S. Geological Survey, 
Branch of Distribution, 1200 South Eads Street, Arlington, VA 22202. 
Cost: $13.50 (subject to change). Table IE, Note 2.
    (17) ``Official Methods of Analysis of the Association of Official 
Analytical Chemicals'', Methods manual, 15th Edition (1990). Price: 
$240.00. Available from: The Association of Official Analytical 
Chemists, 2200 Wilson Boulevard, Suite 400, Arlington, VA 22201. Table 
IB, Note 3.
    (18) ``American National Standard on Photographic Processing 
Effluents,'' April 2, 1975. Available from: American

[[Page 25]]

National Standards Institute, 1430 Broadway, New York, New York 10018. 
Table IB, Note 9.
    (19) ``An Investigation of Improved Procedures for Measurement of 
Mill Effluent and Receiving Water Color,'' NCASI Technical Bulletin No. 
253, December 1971. Available from: National Council of the Paper 
Industry for Air and Stream Improvements, Inc., 260 Madison Avenue, New 
York, NY 10016. Cost available from publisher. Table IB, Note 18.
    (20) Ammonia, Automated Electrode Method, Industrial Method Number 
379-75WE, dated February 19, 1976. Technicon Auto Analyzer II. Method 
and price available from Technicon Industrial Systems, Tarrytown, New 
York 10591. Table IB, Note 7.
    (21) Chemical Oxygen Demand, Method 8000, Hach Handbook of Water 
Analysis, 1979. Method price available from Hach Chemical Company, P.O. 
Box 389, Loveland, Colorado 80537. Table IB, Note 14.
    (22) OIC Chemical Oxygen Demand Method, 1978. Method and price 
available from Oceanography International Corporation, 512 West Loop, 
P.O. Box 2980, College Station, Texas 77840. Table IB, Note 13.
    (23) ORION Research Instruction Manual, Residual Chlorine Electrode 
Model 97-70, 1977. Method and price available from ORION Research 
Incorporation, 840 Memorial Drive, Cambridge, Massachusetts 02138. Table 
IB, Note 16.
    (24) Bicinchoninate Method for Copper. Method 8506, Hach Handbook of 
Water Analysis, 1979, Method and price available from Hach Chemical 
Company, P.O. Box 300, Loveland, Colorado 80537. Table IB, Note 19.
    (25) Hydrogen Ion (pH) Automated Electrode Method, Industrial Method 
Number 378-75WA. October 1976. Bran & Luebbe (Technicon) Auto Analyzer 
II. Method and price available from Bran & Luebbe Analyzing 
Technologies, Inc. Elmsford, N.Y. 10523. Table IB, Note 21.
    (26) 1,10-Phenanthroline Method using FerroVer Iron Reagent for 
Water, Hach Method 8008, 1980. Method and price available from Hach 
Chemical Company, P.O. Box 389 Loveland, Colorado 80537. Table IB, Note 
22.
    (27) Periodate Oxidation Method for Manganese, Method 8034, Hach 
Handbook for Water Analysis, 1979. Method and price available from Hach 
Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 
23.
    (28) Nitrogen, Nitrite--Low Range, Diazotization Method for Water 
and Wastewater, Hach Method 8507, 1979. Method and price available from 
Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, 
Note 25.
    (29) Zincon Method for Zinc, Method 8009. Hach Handbook for Water 
Analysis, 1979. Method and price available from Hach Chemical Company, 
P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 33.
    (30) ``Direct Determination of Elemental Phosphorus by Gas-Liquid 
Chromatography,'' by R.F. Addison and R.G. Ackman, Journal of 
Chromatography, Volume 47, No. 3, pp. 421-426, 1970. Available in most 
public libraries. Back volumes of the Journal of Chromatography are 
available from Elsevier/North-Holland, Inc., Journal Information Centre, 
52 Vanderbilt Avenue, New York, NY 10164. Cost available from publisher. 
Table IB, Note 28.
    (31) ``Direct Current Plasma (DCP) Optical Emission Spectrometric 
Method for Trace Elemental Analysis of Water and Wastes'', Method AES 
0029, 1986-Revised 1991, Fison Instruments, Inc., 32 Commerce Center, 
Cherry Hill Drive, Danvers, MA 01923. Table B, Note 34.
    (32) ``Closed Vessel Microwave Digestion of Wastewater Samples for 
Determination of Metals, CEM Corporation, P.O. Box 200, Matthews, North 
Carolina 28106-0200, April 16, 1992. Available from the CEM Corporation. 
Table IB, Note 36.
    (33) ``Organochlorine Pesticides and PCBs in Wastewater Using Empore 
TM Disk'' Test Method 3M 0222, Revised 10/28/94. 3M 
Corporation, 3M Center Building 220-9E-10, St. Paul, MN 55144-1000. 
Method available from 3M Corporation. Table IC, Note 8 and Table ID, 
Note 8.
    (34) USEPA. 1993. Methods for Measuring the Acute Toxicity of 
Effluents to Freshwater and Marine Organisms.

[[Page 26]]

Fourth Edition, December 1993. Environmental Monitoring Systems 
Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio (EPA/
600/4-90/027F). Available from: National Technical Information Service, 
5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB-91-
167650. Cost: $31.00. Table IA, Note 17. See changes in the manual, 
listed in Part V of this rule.
    (35) ``Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, 
Steam Distillation, Titrimetric Detection)'', revised 12/22/94. 
Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd., 
Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 39.
    (36) ``Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, 
Steam Distillation, Colorimetric Detection)'', revised 12/22/94. 
Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd., 
Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 40.
    (37) ``Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, 
Automated FIA Gas Diffusion)'', revised 12/22/94. Available from 
Perstorp Analytical Corporation, 9445 SW Ridder Rd., Suite 310, P.O. Box 
648, Wilsonville, OK 97070. Table IB, Note 41.
    (38) USEPA. 1994. Short-term Methods for Estimating the Chronic 
Toxicity of Effluents and Receiving Waters to Freshwater Organisms. 
Third Edition. July 1994. Environmental Monitoring Systems Laboratory, 
U.S. Environmental Protection Agency, Cincinnati, Ohio. (EPA/600/4-91/
002). Available from: National Technical Information Service, 5285 Port 
Royal Road, Springfield, Virginia 22161, Publ. No. PB-92-139492. Cost: 
$31.00. Table IA, Note 8.
    (39) USEPA. 1994. Short-term Methods for Estimating the Chronic 
Toxicity of Effluents and Receiving Waters to Marine and Estuarine 
Organisms. Second Edition, July 1994. Environmental Monitoring Systems 
Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. EPA/
600/4-91/003. Available from: National Technical Information Service, 
5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB-92-
139484. Cost: $45.00. Table IA, Note 9.
    (40) EPA Methods 1666, 1667, and 1671 listed in the table above are 
published in the compendium titled Analytical Methods for the 
Determination of Pollutants in Pharmaceutical Manufacturing Industry 
Wastewaters (EPA 821-B-98-016). EPA Methods 502.2 and 524.2 have been 
incorporated by reference into 40 CFR 141.24 and are in Methods for the 
Determination of Organic Compounds in Drinking Water, EPA-600/4-88-039, 
December 1988, Revised, July 1991, and Methods for the Determination of 
Organic Compounds in Drinking Water-Supplement II, EPA-600/R-92-129, 
August 1992, respectively. These EPA test method compendia are available 
from the National Technical Information Service, NTIS PB91-231480 and 
PB92-207703, U.S. Department of Commerce, 5285 Port Royal Road, 
Springfield, Virginia 22161. The toll-free number is 800-553-6847. ASTM 
test methods D3371, D3695, and D4763 are available from the American 
Society for Testing and Materials, 100 Barr Harbor Drive, West 
Conshohocken, PA 19428-2959.

    Editorial Note: At 64 FR 30434, June 8, 1999, the following 
paragraph (40) was added, effective July 8, 1999; however paragraph (40) 
was previously added to the 1999 volume.

    (40) USEPA. 1999. Method 1631, Revision B, ``Mercury in Water by 
Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence 
Spectrometry.'' May 1999. Office of Water, U.S. Environmental Protection 
Agency (EPA 821-R-99-005). Available from: National Technical 
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161. 
Publication No. PB99-131989. Cost: $25.50. Table IB, Note 43.
    (41) USEPA, January 1999 Errata for the Effluent and Receiving Water 
Testing Manuals: Acute Toxicity of Effluents and Receiving Waters to 
Freshwater and Marine Organisms; Short-Term Methods for Estimating the 
Chronic Toxicity of Effluents and Receiving Waters to Freshwater 
Organisms; and Short-Term Methods for Estimating the Chronic Toxicity of 
Effluents and Receiving Waters to Marine and Estuarine Organisms. U.S. 
Environmental Protection Agency, Office of Research and Development, 
Duluth, MN. EPA-600/R-98/182.
    (c) Under certain circumstances the Regional Administrator or the 
Director

[[Page 27]]

in the Region or State where the discharge will occur may determine for 
a particular discharge that additional parameters or pollutants must be 
reported. Under such circumstances, additional test procedures for 
analysis of pollutants may be specified by the Regional Administrator, 
or the Director upon the recommendation of the Director of the 
Environmental Monitoring Systems Laboratory--Cincinnati.
    (d) Under certain circumstances, the Administrator may approve, upon 
recommendation by the Director, Environmental Monitoring Systems 
Laboratory--Cincinnati, additional alternate test procedures for 
nationwide use.
    (e) Sample preservation procedures, container materials, and maximum 
allowable holding times for parameters cited in Tables IA, IB, IC, ID, 
and IE are prescribed in Table II. Any person may apply for a variance 
from the prescribed preservation techniques, container materials, and 
maximum holding times applicable to samples taken from a specific 
discharge. Applications for variances may be made by letters to the 
Regional Administrator in the Region in which the discharge will occur. 
Sufficient data should be provided to assure such variance does not 
adversely affect the integrity of the sample. Such data will be 
forwarded, by the Regional Administrator, to the Director of the 
Environmental Monitoring Systems Laboratory--Cincinnati, Ohio for 
technical review and recommendations for action on the variance 
application. Upon receipt of the recommendations from the Director of 
the Environmental Monitoring Systems Laboratory, the Regional 
Administrator may grant a variance applicable to the specific charge to 
the applicant. A decision to approve or deny a variance will be made 
within 90 days of receipt of the application by the Regional 
Administrator.

                    Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
       Parameter No./name           Container \1\          Preservation \2\,\3\         Maximum holding time \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacteria Tests:
  1-4 Coliform, fecal and total.  P,G..............  Cool, 4C, 0.008% Na2S2O3 5......  6 hours.
  5 Fecal streptococci..........  P,G..............  Cool, 4C, 0.008% Na2S2O3 5......  6 hours.
Table IA--Aquatic Toxicity
 Tests:
  6-10 Toxicity, acute and        P,G..............  Cool, 4  deg.C 16...............  36 hours.
   chronic.
 
Table IB--Inorganic Tests:
  1. Acidity....................  P, G.............  Cool, 4C........................  14 days.
  2. Alkalinity.................  P, G.............  ......do........................      Do.
  4. Ammonia....................  P, G.............  Cool, 4C, H2SO4 to pH<2.........  28 days.
  9. Biochemical oxygen demand..  P, G.............  Cool, 4C........................  48 hours.
  10. Boron.....................  P, PFTE, or        HNO3 TO pH2.....................  6 months.
                                   Quartz.
  11. Bromide...................  P, G.............  None required...................  28 days.
  14. Biochemical oxygen demand,  P, G.............  Cool, 4C........................  48 hours.
   carbonaceous.
  15. Chemical oxygen demand....  P, G.............  Cool, 4C, H2SO4 to pH<2.........  28 days.
  16. Chloride..................  P, G.............  None required...................      Do.
  17. Chlorine, total residual..  P, G.............  ......do........................  Analyze immediately.
  21. Color.....................  P, G.............  Cool, 4C........................  48 hours.
  23-24. Cyanide, total and       P, G.............  Cool, 4C, NaOH to pH>12, 0.6g     14 days.6
   amenable to chlorination.                          ascorbic acid 5.
  25. Fluoride..................  P................  None required...................  28 days.
  27. Hardness..................  P, G.............  HNO3 to pH<2, H2SO4 to pH<2.....  6 months.
  28. Hydrogen ion (pH).........  P, G.............  None required...................  Analyze immediately.
  31, 43. Kjeldahl and organic    P, G.............  Cool, 4C, H2SO4 to pH<2.........  28 days.
   nitrogen.
Metals:7
  18. Chromium VI...............  P, G.............  Cool, 4C........................  24 hours.
  35. Mercury...................  P, G.............  HNO3 to pH<2....................  28 days.
  3, 5-8, 12, 13, 19, 20, 22,     P, G.............  ......do........................  6 months.
   26, 29, 30, 32-34, 36, 37,
   45, 47, 51, 52, 58-60, 62,
   63, 70-72, 74, 75. Metals,
   except boron, chromium VI and
   mercury.
  38. Nitrate...................  P, G.............  Cool, 4C........................  48 hours.
  39. Nitrate-nitrite...........  P, G.............  Cool, 4C, H2SO4 to pH<2.........  28 days.
  40. Nitrite...................  P, G.............  Cool, 4C........................  48 hours.
  41. Oil and grease............  G................  Cool to 4C, HCl or H2SO4 to pH<2  28 days.
  42. Organic Carbon............  P, G.............  Cool to 4  deg.C HC1 or H2SO4 or  28 days.
                                                      H3PO4, to pH2.

[[Page 28]]

 
  44. Orthophosphate............  P, G.............  Filter immediately, Cool, 4C....  48 hours.
  46. Oxygen, Dissolved Probe...  G Bottle and top.  None required...................  Analyze immediately.
  47. Winkler...................  ......do.........  Fix on site and store in dark...  8 hours.
  48. Phenols...................  G only...........  Cool, 4C, H2SO4 to pH<2.........  28 days.
  49. Phosphorus (elemental)....  G................  Cool, 4C........................  48 hours.
  50. Phosphorus, total.........  P, G.............  Cool, 4C, H2SO4 to pH<2.........  28 days.
  53. Residue, total............  P, G.............  Cool, 4C........................  7 days.
  54. Residue, Filterable.......  P, G.............  ......do........................  7 days.
  55. Residue, Nonfilterable      P, G.............  ......do........................  7 days.
   (TSS).
  56. Residue, Settleable.......  P, G.............  ......do........................  48 hours.
  57. Residue, volatile.........  P, G.............  ......do........................  7 days.
  61. Silica....................  P, PFTE, or        Cool, 4  deg.C..................  28 days.
                                   Quartz.
  64. Specific conductance......  P, G.............  ......do........................      Do.
  65. Sulfate...................  P, G.............  ......do........................      Do.
  66. Sulfide...................  P, G.............  Cool, 4C add zinc acetate plus    7 days.
                                                      sodium hydroxide to pH>9.
  67. Sulfite...................  P, G.............  None required...................  Analyze immediately.
  68. Surfactants...............  P ,G.............  Cool, 4C........................  48 hours.
  69. Temperature...............  P, G.............  None required...................  Analyze.
  73. Turbidity.................  P, G.............  Cool, 4C........................  48 hours.
Table IC--Organic Tests \8\
  13, 18-20, 22, 24-28, 34-37,    G, Teflon-lined    Cool, 4  deg.C, 0.008% Na2S2O3    14 days.
   39-43, 45-47, 56, 76, 104,      septum.            \5\..
   105, 108-111, 113. Purgeable
   Halocarbons.
  6, 57, 106. Purgeable aromatic  ......do.........  Cool, 4  deg.C, 0.008%                Do.
   hydrocarbons.                                      Na2S2O3,\5\ HCl to pH2\9\.
  3, 4. Acrolein and              ......do.........  Cool, 4  deg.C, 0.008%                Do.
   acrylonitrile.                                     Na2S2O3,\5\ adjust pH to 4-510.
  23, 30, 44, 49, 53, 77, 80,     G, Teflon-lined    Cool, 4  deg.C, 0.008% Na2S2O3    7 days until extraction;
   81, 98, 100, 112. Phenols 11.   cap..              \5\.                              40 days after
                                                                                        extraction.
  7, 38. Benzidines 11..........  ......do.........  ......do........................  7 days until
                                                                                        extraction.13
  14, 17, 48, 50-52. Phthalate    ......do.........  Cool, 4  deg.C..................  7 days until extraction;
   esters 11.                                                                           40 days after
                                                                                        extraction.
  82-84. Nitrosamines 11 14.....  ......do.........  Cool, 4  deg.C, 0.008%                Do.
                                                      Na2S2O3,\5\ store in dark.
  88-94. PCBs 11................  .....do..........  Cool, 4  deg.C..................      Do.
  54, 55, 75, 79. Nitroaromatics  ......do.........  Cool, 4  deg.C, 0.008%                Do.
   and isophorone 11.                                 Na2S2O3,\5\ store in dark.
  1, 2, 5, 8-12, 32, 33, 58, 59,  ......do.........  ......do........................      Do.
   74, 78, 99, 101. Polynuclear
   aromatic hydrocarbons 11.
  15, 16, 21, 31, 87. Haloethers  ......do.........  Cool, 4  deg.C, 0.008% Na2S2O3        Do.
   11.                                                \5\.
  29, 35-37, 63-65, 73, 107.      ......do.........  Cool, 4  deg.C..................      Do.
   Chlorinated hydrocarbons 11.
  60-62, 66-72, 85, 86, 95-97,
   102, 103. CDDs/CDFs 11.
  aqueous: field and lab          G................  Cool, 0-4  deg.C, pH9, 0.008%     1 year.
   preservation..                                     Na2S2O3 \5\.
  Solids, mixed phase, and        ......do.........  Cool, 4  deg.C..................  7 days.
   tissue: field preservation..
  Solids, mixed phase, and        ......do.........  Freeze, -10  deg.C..............  1 year.
   tissue: lab preservation.
Table ID--Pesticides Tests:
  1-70. Pesticides \11\.........  ......do.........  Cool, 4C, pH 5-9 15.............      Do.
Table IE--Radiological Tests:
  1-5. Alpha, beta and radium...  P, G.............  HNO3 to pH<2....................  6 months.
----------------------------------------------------------------------------------------------------------------
Table II Notes
\1\ Polyethylene (P) or glass (G). For microbiology, plastic sample containers must be made of sterilizable
  materials (polypropylene or other autoclavable plastic).
2 Sample preservation should be performed immediately upon sample collection. For composite chemical samples
  each aliquot should be preserved at the time of collection. When use of an automated sampler makes it
  impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4C until
  compositing and sample splitting is completed.
3 When any sample is to be shipped by common carrier or sent through the United States Mails, 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
  requirements 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).

[[Page 29]]

 
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
  samples may be held before analysis and still be considered valid. Samples may be held for longer periods only
  if the permittee, or monitoring laboratory, has 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
  Administrator under Sec.  136.3(e). 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 knowledge
  exists to show that this is necessary to maintain sample stability. See Sec.  136.3(e) for details. The term
  ``analyze immediately'' usually means within 15 minutes or less of sample collection.
5 Should only be used in the presence of residual chlorine.
6 Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead
  acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can
  be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is
  filtered and then NaOH is added to pH 12.
7 Samples should be filtered immediately on-site before adding preservative for dissolved metals.
8 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
9 Sample receiving no pH adjustment 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. When the analytes of
  concern fall within two or more chemical categories, the sample may be preserved by cooling to 4C, 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 (re the
  requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of
  benzidine).
12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.00.2 to
  prevent rearrangement to benzidine.
13 Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)
  atmosphere.
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\ Sufficient ice should be placed 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, it
  is necessary to immediately measure the temperature of the samples and confirm that the 4C temperature maximum
  has not been exceeded. In the isolated cases where it can be documented that this holding temperature can not
  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.

[38 FR 28758, Oct. 16, 1973, as amended at 41 FR 52781, Dec. 1, 1976; 49 
FR 43251, 43258, 43259, Oct. 26, 1984; 50 FR 691, 692, 695, Jan. 4, 
1985; 51 FR 23693, June 30, 1986; 52 FR 33543, Sept. 3, 1987; 55 FR 
24534, June 15, 1990; 55 FR 33440, Aug. 15, 1990; 56 FR 50759, Oct. 8, 
1991; 57 FR 41833, Sept. 11, 1992; 58 FR 4505, Jan. 31, 1994; 60 FR 
17160, Apr. 4, 1995; 60 FR 39588, 39590, Aug. 2, 1995; 60 FR 44672, Aug. 
28, 1995; 60 FR 53542, 53543, Oct. 16, 1995; 62 FR 48403, 48404, Sept. 
15, 1997; 63 FR 50423, Sept. 21, 1998; 64 FR 4978, Feb. 2, 1999; 64 FR 
10392, Mar. 4, 1999; 64 FR 26327, May 14, 1999; 64 FR 30433, 30434, June 
8, 1999]

    Effective Date Note: At 64 FR 30433, June 8, 1999, Sec. 136.3, 
paragraph (a), Table IB was amended by revising entry 35, effective July 
8, 1999. For the convenience of the user, the superseded text is set 
forth as follows:

Sec. 136.3  Identification of test procedures.

    (a) * * *

[[Page 30]]



                                                  Table IB.--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                            Reference (method number or page)
  Parameter, units and method  -------------------------------------------------------------------------------------------------------------------------
                                  EPA 1,35      STD methods  18th ed.                 ASTM                       USGS \2\                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                         *                *                *                *                *                *                *
35. Mercury--Total,\4\ mg/L:
    Cold vapor, manual or.....        245.1  3112 B....................  D3223-91.....................  I-3462-85................  977.22.\3\
    Automated.................        245.2
                         *                *                *                *                *                *                *
--------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 31]]



Sec. 136.4  Application for alternate test procedures.

    (a) Any person may apply to the Regional Administrator in the Region 
where the discharge occurs for approval of an alternative test 
procedure.
    (b) When the discharge for which an alternative test procedure is 
proposed occurs within a State having a permit program approved pursuant 
to section 402 of the Act, the applicant shall submit his application to 
the Regional Administrator through the Director of the State agency 
having responsibility for issuance of NPDES permits within such State.
    (c) Unless and until printed application forms are made available, 
an application for an alternate test procedure may be made by letter in 
triplicate. Any application for an alternate test procedure under this 
paragraph (c) shall:
    (1) Provide the name and address of the responsible person or firm 
making the discharge (if not the applicant) and the applicable ID number 
of the existing or pending permit, issuing agency, and type of permit 
for which the alternate test procedure is requested, and the discharge 
serial number.
    (2) Identify the pollutant or parameter for which approval of an 
alternate testing procedure is being requested.
    (3) Provide justification for using testing procedures other than 
those specified in Table I.
    (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.
    (d) An application for approval of an alternate test procedure for 
nationwide use may be made by letter in triplicate to the Director, 
Analytical Methods Staff, Office of Science and Technology (4303), 
Office of Water, U.S. Environmental Protection Agency, 401 M Street, 
SW., Washington, DC 20460. Any application for an alternate test 
procedure under this paragraph (d) 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 testing procedure is being requested.
    (3) Provide a detailed description of the proposed alternate 
procedure, together with references to published or other studies 
confirming the general applicability of the alternate test procedure to 
the pollutant(s) or parameter(s) in waste water discharges from 
representative and specified industrial or other categories.
    (4) Provide comparability data for the performance of the proposed 
alternate test procedure compared to the performance of the approved 
test procedures.

[38 FR 28760, Oct. 16, 1973, as amended at 41 FR 52785, Dec. 1, 1976; 62 
FR 30763, June 5, 1997]



Sec. 136.5  Approval of alternate test procedures.

    (a) The Regional Administrator of the region in which the discharge 
will occur has final responsibility for approval of any alternate test 
procedure proposed by the responsible person or firm making the 
discharge.
    (b) Within thirty days of receipt of an application, the Director 
will forward such application proposed by the responsible person or firm 
making the discharge, together with his recommendations, to the Regional 
Administrator. Where the Director recommends rejection of the 
application for scientific and technical reasons which he provides, the 
Regional Administrator shall deny the application, and shall forward a 
copy of the rejected application and his decision to the Director of the 
State Permit Program and to the Director of the Analytical Methods 
Staff, Washington, DC.
    (c) Before approving any application for an alternate test procedure 
proposed by the responsible person or firm making the discharge, the 
Regional Administrator shall forward a copy of the application to the 
Director of the Analytical Methods Staff, Washington, DC.
    (d) Within ninety days of receipt by the Regional Administrator of 
an application for an alternate test procedure, proposed by the 
responsible person or firm making the discharge, the Regional 
Administrator shall notify the applicant and the appropriate

[[Page 32]]

State agency of approval or rejection, or shall specify the additional 
information which is required to determine whether to approve the 
proposed test procedure. Prior to the expiration of such ninety day 
period, a recommendation providing the scientific and other technical 
basis for acceptance or rejection will be forwarded to the Regional 
Administrator by the Director of the Analytical Methods Staff, 
Washington, DC. A copy of all approval and rejection notifications will 
be forwarded to the Director, Analytical Methods Staff, Washington, DC, 
for the purposes of national coordination.
    (e) Approval for nationwide use. (1) Within sixty days of the 
receipt by the Director of the Analytical Methods Staff, Washington, DC, 
of an application for an alternate test procedure for nationwide use, 
the Director of the Analytical Methods Staff shall notify the applicant 
in writing whether the application is complete. If the application is 
incomplete, the applicant shall be informed of the information necessary 
to make the application complete.
    (2) Within ninety days of the receipt of a complete package, the 
Analytical Methods Staff shall perform any analysis necessary to 
determine whether the alternate method satisfies the applicable 
requirements of this part, and the Director of the Analytical Methods 
Staff shall recommend to the Administrator that he/she approve or reject 
the application and shall also notify the applicant of such 
recommendation.
    (3) As expeditiously as practicable, an alternate method determined 
by the Administrator to satisfy the applicable requirements of this part 
shall be proposed by EPA for incorporation in subsection 136.3 of 40 CFR 
part 136. EPA shall make available for review all the factual bases for 
its proposal, including any performance data submitted by the applicant 
and any available EPA analysis of those data.
    (4) Following a period of public comment, EPA shall, as 
expeditiously as practicable, publish in the Federal Register a final 
decision to approve or reject the alternate method.

[38 FR 28760, Oct. 16, 1973, as amended at 41 FR 52785, Dec. 1, 1976; 55 
FR 33440, Aug. 15, 1990; 62 FR 30763, June 5, 1997]

    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 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.

[[Page 33]]

    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 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

[[Page 34]]

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-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+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 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.
    6.5.2.2  Gases--To prepare standards for any of the six halocarbons 
that boil below 30  deg. C (bromomethane, chloroethane, chloromethane, 
dichlorodifluoromethane, trichlorofluoromethane, vinyl chloride), fill

[[Page 35]]

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 g/
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 
L of one or more secondary dilution standards to 100, 500, or 
1000 L of reagent water. A 25-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 g/mL of each internal standard compound. 
The addition of 10 L of this standard to 5.0 mL of sample or 
calibration standard would be equivalent to 30 g/L.
    7.4.3  Analyze each calibration standard according to Section 10, 
adding 10 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.
[GRAPHIC] [TIFF OMITTED] TC15NO91.094


[[Page 36]]


                                                              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 
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 g/L of each 
parameter by adding 200 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 g/L, and the 
standard deviation of the recovery (s) in 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 37]]

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 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 
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 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 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

[[Page 38]]

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 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/L. Add 10 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 L of the surrogate spiking solution (Section 8.7) and 
10.0 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 11.00.1 
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 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

[[Page 39]]

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 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 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).
    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

[[Page 40]]

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 (g/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 C for 3
  min then programmed at 8 C/min to 220 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 C for 3 min then
  programmed at 6 C/min to 170 C and held for 4 min.
nd=not determined.


                          Table 2--Calibration and QC Acceptance Criteria--Method 601 a
----------------------------------------------------------------------------------------------------------------
                                                                         Limit for s
                       Parameter                          Range for Q   (g/    Range for X    Range P,
                                                        (g/L)       L)       (g/L)    Ps (%)
----------------------------------------------------------------------------------------------------------------
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
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

[[Page 41]]

 
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 g/L.
Q=Concentration measured in QC check sample, in g/L (Section 7.5.3).
s=Standard deviation of four recovery measurements, in g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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' (g/L)              m>g/L)               (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 g/L.
sn'=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S\1\=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.
a Estimates based upon the performance in a single laboratory.\10\


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[[Page 43]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.001


[[Page 44]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.002


[[Page 45]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.003


[[Page 46]]

                     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 47]]

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-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 48]]

    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-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 g/
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 
L of one or more secondary dilution standards to 100, 500, or 
1000 mL of reagent water. A 25-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, ,,,-
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 g/mL of each internal standard compound. 
The addition of 10 l of this

[[Page 49]]

standard to 5.0 mL of sample or calibration standard would be equivalent 
to 30 g/L.
    7.4.3  Analyze each calibration standard according to Section 10, 
adding 10 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 mimimum 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 
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 g/L of each 
parameter by adding 200 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 g/L, and the 
standard deviation of the recovery (s) in 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

[[Page 50]]

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 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 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 
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 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) plus-minus 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 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 51]]

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. , , ,-
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 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/L. Add 10 
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 L of the surrogate spiking solution (Section 8.7) and 
10.0 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 12.00.1 
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 52]]

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 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 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 53]]

    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  (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 C for 2 min then programmed at 6 C/min to 90 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 C for 2 min then programmed at 2 C/min to 100 C
  for a final hold.


                          Table 2--Calibration and QC Acceptance Criteria--Method 602 a
----------------------------------------------------------------------------------------------------------------
                                                                                          Range for X
                                                              Range for Q   Limit for s  (g/  Range for
                         Parameter                           (g/  (g/       L)        P, Ps(%)
                                                                  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 g/L (Section 7.5.3).
s=Standard deviation of four recovery measurements, in g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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 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
                                                                  (g/L)  (g/L)  (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 g/L.
S=Expected single analyst standard deviation of measurements at an average concentration found of X, in X g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the Concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 54]]

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[[Page 58]]

                 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 59]]

                       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-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 60]]

    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-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 g/
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 
L of one or more secondary dilution standards to 100, 500, or 
1000 mL of reagent water. A 25-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 g/mL of each internal standard compound. 
The addition of 10 L of this standard to 5.0 mL of sample or 
calibration standard would be equivalent to 30 g/L.
    7.4.3  Analyze each calibration standard according to Section 10, 
adding 10 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 61]]



 
                                                                   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 25 
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 g/L of each 
parameter by adding 200 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 g/L, and the 
standard deviation of the recovery (s) in 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

[[Page 62]]

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 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 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 
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 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

[[Page 63]]

range pH paper. Samples for acrolein analysis receiving no pH adjustment 
must be analyzed within 3 days of sampling.
    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 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 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

[[Page 64]]

zero.1 The MDL concentrations listed in Table 1 were obtained 
using reagent water.9 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   (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 C for 1.5 min
  (during desorption), then heated as rapidly as possible to 150 C and
  held for 20 min; column bakeout at 190 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
----------------------------------------------------------------------------------------------------------------
                                                                              Average      Standard
                                                    Sample    Spike conc.    recovery      deviation    Average
                    Parameter                       matrix   (g/  (g/  (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
----------------------------------------------------------------------------------------------------------------
 ARW=Reagent water.
 APOTW=Prechlorination secondary effluent from a municipal sewage treatment plant.
 AIW=Industrial wastewater containing an unidentified acrolein reactant.


[[Page 65]]


                          Table 3--Calibration and QC Acceptance Criteria--Method 603 a
----------------------------------------------------------------------------------------------------------------
                                                              Range for Q   Limit for S   Range for X
                         Parameter                           (g/  (g/  (g/  Range for
                                                                  L)            L)            L)       P, Ps (%)
----------------------------------------------------------------------------------------------------------------
Acrolein...................................................    45.9-54.1         4.6       42.9-60.1      88-118
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 g/L.9
Q=Concentration measured in QC check sample, in g/L (Section 7.5.3).
s=Standard deviation of four recovery measurements, in g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in g/L (Section 8.2.4).
P, Ps=Percent recovery measured (Section 8.3.2, Section 8.4.2).


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                           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 70]]

    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 71]]

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 (-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 g/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 72]]

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 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 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 (g/
L).

    Cs=Concentration of the parameter to be measured 
(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

[[Page 73]]

range of concentrations found in real samples or should define the 
working range of the detector.
    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 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 
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 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 g/L, and the 
standard deviation of the recovery (s) in 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.

[[Page 74]]

    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 100 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 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 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

[[Page 75]]

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 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

[[Page 76]]

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 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 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush 
technique.11 Smaller (1.0 L) volumes may be injected 
if automatic devices are employed. Record the volume injected to the 
nearest 0.05 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

[[Page 77]]

achieved by this column is shown in Figure 2.
    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 L of the column fractions into the gas 
chromatograph using the solvent-flush technique. Smaller (1.0 
L) volumes can be injected if automatic devices are employed. 
Record the volume injected to the nearest 0.05 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 (L).
    Vt=Volume of total extract (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 
(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 (L).
    Vt=Total volume of column eluate or combined fractions 
from which Vi was taken (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 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 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

[[Page 78]]

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 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
                                                              detection
                   Parameter                     Retention      limit
                                                time (min)  (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 C at injection,
  programmed immediately at 8 C/min to 150 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)    (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 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 79]]


                                   Table 3--QC Acceptance Criteria--Method 604
----------------------------------------------------------------------------------------------------------------
                                                                                        Range for X
                                                            Test conc.    Limit for s  (g/   Range for
                        Parameter                          (g/  (g/       L)          P, Ps
                                                                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 g/L (Section 8.2.4).
X--Average recovery for four recovery measurements, in 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'
                                                           (g/L)     (g/L)     (g/L)
----------------------------------------------------------------------------------------------------------------
4-Chloro-3-methylphenol................................         0.87C-1.97         0.11X-0.21         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         0.17X-0.02         0.18X+0.62
2,4-Dimethylphenol.....................................         0.62C-1.64         0.30X-0.89         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         0.27X-1.15         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         0.22X-0.58         0.23X+0.57
Phenol.................................................         0.43C+0.11         0.20X-0.88         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 g/L.
sr'=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 80]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.012


[[Page 81]]

[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

[[Page 82]]

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

[[Page 83]]

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 an stirring, or by purging with 
helium.
    6.11  Stock standard solutions (1.00 g/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.

[[Page 84]]

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

[[Page 85]]

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 benzidine and/or 3,3'-dichlorobenzidine at a concentration of 
50 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 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 g/L, and the 
standard deviation of the recovery (s) in 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 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 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 
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 86]]

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 
separation. The optimum technique depends upon the sample, but may 
include stirring, filtration of the emulsion through glass

[[Page 87]]

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 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 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.
    12.7  If the measurement of the peak response for benzidine is 
prevented by the presence of interferences, reduce the electrode

[[Page 88]]

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 (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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 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 89]]



     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                                               Method
                                      Retention    Column     detection
              Parameter                  time     capacity      limit
                                        (min)      factor   (g/
                                                    (k)          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
----------------------------------------------------------------------------------------------------------------
                                                                                          Range for X
                                                              Test conc.    Limit for s  (g/  Range for
                         Parameter                           (g/  (g/       L)         P, Ps
                                                                  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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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
                                                                     recovery,    Single analyst      Overall
                            Parameter                              X(g/   precision, sr   precision, S
                                                                        L)        (g/L)  (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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 90]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.014


[[Page 91]]

                       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 92]]

    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 93]]

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 g/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 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 
concentraton 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 94]]

    7.3.2  Using injections of 2 to 5 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 (g/
L).
    Cs=Concentration of the parameter to be measured 
(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 g/mL; bis(2-ethylhexyl) 
phthalate, 50 g/mL; di-n-octyl phthalate, 50 g/mL; any 
other phthlate, 25 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 g/L, and the 
standard deviation of the recovery (s) in g/L, for each 
parameter using the four results.

[[Page 95]]

    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 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%.

[[Page 96]]

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\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

[[Page 97]]

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.
    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 L of the sample extract or standard 
into the gas-chromatograph using the solvent-flush technique.\11\ 
Smaller (1.0 L) volumes may be injected if automatic devices 
are employed. Record the volume injected to the nearest 0.05 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.

[[Page 98]]

    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] TC15NO91.103

                                                              Equation 2

where:
    A=Amount of material injected (ng).
    Vi=Volume of extract injected (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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 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.

[[Page 99]]

    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.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                   Retention time (min)        Method
                               ----------------------------   detection
           Parameter                                            limit
                                  Column 1      Column 2    (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 180C, 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 C, except where otherwise indicated.
a 220 C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 606
----------------------------------------------------------------------------------------------------------------
                                                                                          Range for X
                                                              Test conc.    Limit for s  (g/  Range for
                         Parameter                           (g/  (g/       L)         P, Ps
                                                                  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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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'
                                                                  (g/L)  (g/L)  (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 g/L.
sr'=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S'=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 100]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.015


[[Page 101]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.016


[[Page 102]]

                        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 reported6-9 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 103]]

                                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 104]]

    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 g/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 concentraton 
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 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 105]]

    7.3.2  Using injections of 2 to 5 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 (g/
L).
    Cs=Concentration of the parameter to be measured 
(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 
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 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 g/L, and the 
standard deviation of the recovery (s) in 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 106]]

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 20 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 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 
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 crtieria 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

[[Page 107]]

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 \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).

[[Page 108]]

    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 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

[[Page 109]]

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.
    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 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush technique.\21\ 
Smaller (1.0 L) volumes may be injected if automatic devices 
are employed. Record the volume injected to the nearest 0.05 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 (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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

[[Page 110]]

over the range 0.8 to 55 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.

                               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     Method
                                                 (min)        detection
                 Parameter                 ----------------     limit
                                            Column  Column  (g/
                                               1       2         L)
------------------------------------------------------------------------
N-Nitrosodimethylamine....................     4.1    0.88          0.15
N-Nitrosodi-n-propylamine.................    12.1     4.2           .46

[[Page 111]]

 
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 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 C,
  except where otherwise indicated.
a  Measured as diphenylamine.
b 220 C column temperature.
c 210 C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 607
----------------------------------------------------------------------------------------------------------------
                                                                                        Range for X
                                                            Test conc.    Limit for s  (g/   Range for
                        Parameter                          (g/  (g/       L)          P, Ps
                                                                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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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
                                                                  (g/L)  (g/L)  (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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 112]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.017


[[Page 113]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.018


[[Page 114]]

             Method 608--Organochlorine Pesticides and PCBs

                        1. Scope and Application

    1.1  This method covers the determination of certain organochlorine 
pesticides and PCBs. The following parameters can be determined by this 
method:

------------------------------------------------------------------------
                  Parameter                    STORET No.      CAS No.
------------------------------------------------------------------------
Aldrin......................................         39330      309-00-2
-BHC...............................         39337      319-84-6
-BHC...............................         39338      319-85-7
-BHC...............................         34259      319-86-8
-BHC...............................         39340       58-89-9
Chlordane...................................         39350       57-74-9
4,4-DDD.....................................         39310       72-54-8
4,4-DDE.....................................         39320       72-55-9
4,4-DDT.....................................         39300       50-29-3
Dieldrin....................................         39380       60-57-1
Endosulfan I................................         34361      959-98-8
Endosulfan II...............................         34356    33212-65-9
Endosulfan sulfate..........................         34351     1031-07-8
Eldrin......................................         39390       72-20-8
Endrin aldehyde.............................         34366     7421-93-4
Heptachlor..................................         39410       76-44-8
Heptachlor epoxide..........................         39420     1024-57-3
Toxaphene...................................         39400     8001-35-2
PCB-1016....................................         34671    12674-11-2
PCB-1221....................................         39488     1104-28-2
PCB-1232....................................         39492    11141-16-5
PCB-1242....................................         39496    53469-21-9
PCB-1248....................................         39500    12672-29-6
PCB-1254....................................         39504    11097-69-1
PCB-1260....................................         39508    11096-82-5
------------------------------------------------------------------------

    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 606, 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 parameters are then measured with an electron 
capture detector.\2\
    2.2  The method provides a Florisil column cleanup procedure and an 
elemental sulfur removal 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.

[[Page 115]]

    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  Interferences by phthalate esters can pose a major problem in 
pesticide analysis when using the electron capture detector. These 
compounds generally appear in the chromatogram as large late eluting 
peaks, especially in the 15 and 50% fractions from Florisil. Common 
flexible plastics contain varying amounts of phthalates. These 
phthalates are easily 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 the use of plastics in the laboratory. 
Exhaustive cleanup of reagents and glassware may be required to 
eliminate background phthalate contamination.4, 5 The 
interferences from phthalate esters can be avoided by using a 
microcoulometric or electrolytic conductivity detector.
    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.
    4.2  The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: 4,4'-DDT, 4,4'-DDD, the BHCs, and the PCBs. 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 composting. 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  22 mm ID, with Teflon 
stopcock and coarse frit filter disc (Kontes K-42054 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 gas 
chromatograph suitable for on-column injection and all required 
accessories including syringes, analytical columns, gases, detector, and 
strip-

[[Page 116]]

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 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  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  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 to 
H2SO4 (ACS, sp. gr. 1.84) to 50 mL of reagent 
water.
    6.5  Acetone, hexane, isooctane, methylene chloride--Pesticide 
quality or equivalent.
    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  Sodium sulfate--(ACS) Granular, anhydrous. Purify by heating at 
400  deg.C for 4 h in a shallow tray.
    6.8  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.
    6.9  Mercury--Triple distilled.
    6.10  Copper powder--Activated.
    6.11  Stock standard solutions (1.00 g/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 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.
    6.11.2  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 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 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

[[Page 117]]

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 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] TC15NO91.107

                                                              Equation 1
where:
    As=Response for the parameter to be measured.
    Ais=Response for the internal standard.
    Cis=Concentration of the internal standard (g/
L).
    Cs=Concentraton of the parameter to be measured 
(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  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 \9\ 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 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.

[[Page 118]]

    8.2.1  A quality control (QC) check sample concentrate is required 
containing each single-component parameter of interest at the following 
concentrations in acetone: 4,4'-DDD, 10 g/mL; 4,4'-DDT, 10 
g/mL; endosulfan II, 10 g/mL; endosulfan sulfate, 10 
g/mL; endrin, 10 g/mL; any other single-component 
pesticide, 2 g/mL. If this method is only to be used to analyze 
for PCBs, chlordane, or toxaphene, the QC check sample concentrate 
should contain the most representative multicomponent parameter at a 
concentration of 50 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 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 g/mL; and the 
standard deviation of the recovery (s) in g/mL, 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 compmunds 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.\10\ 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'

[[Page 119]]

for X; (3) calculate the range for recovery at the spike concentration 
as (100 X'/T)2.44(100 S'/T)%.\10\
    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 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 standards 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-2 sp to P+2 sp. 
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 \11\ 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. If the samples will not be 
extracted within 72 h of collection, the sample should be adjusted to a 
pH range of 5.0 to 9.0 with sodium hydroxide solution or sulfuric acid. 
Record the volume of acid or base used. If aldrin is to be determined, 
add sodium thiosulfate when residual chlorine is present. EPA Methods 
330.4 and 330.5 may be used for measurement of residual chlorine.\12\ 
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 optium 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.

[[Page 120]]

    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.
    10.7  Increase the temperature of the hot water bath to about 80 
deg.C. Momeltarily 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. 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 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. The Florisil column allows for a 
select fractionation of the compounds and will eliminate polar 
interferences. Elemental sulfur, which interferes with the electron 
capture gas chromatography of certain pesticides, can be removed by the 
technique described in Section 11.3.
    11.2  Florisil column cleanup:
    11.2.1  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.
    11.2.2  Add 60 mL of hexane to wet and rinse the sodium sulfate and 
Florisil. 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 eluate.
    11.2.3  Adjust the sample extract volume to 10 mL with hexane and 
transfer it from the K-D concentrator tube onto the column. Rinse the 
tube twice with 1 to 2 mL of hexane, adding each rinse to the column.
    11.2.4  Place a 500-mL K-D flask and clean concentrator tube under 
the chromatographic column. Drain the column into the flask until the 
sodium sulfate layer is nearly exposed. Elute the column with 200 mL of 
6% ethyl ether in hexane (V/V) (Fraction 1) at a rate of about 5 mL/min. 
Remove the K-D flask and set it aside for later concentration. Elute the 
column again, using 200 mL of 15% ethyl ether in hexane (V/V) (Fraction 
2), into a second K-D flask. Perform the third elution using 200 mL of 
50% ethyl ether in hexane (V/V) (Fraction 3). The elution patterns for 
the pesticides and PCBs are shown in Table 2.
    11.2.5  Concentrate the fractions as in Section 10.6, 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 each fraction to 10 mL with hexane and analyze by gas 
chromatography (Section 12).
    11.3  Elemental sulfur will usually elute entirely in Fraction 1 of 
the Florisil column cleanup. To remove sulfur interference from this 
fraction or the original extract, pipet 1.00 mL of the concentrated 
extract into a clean concentrator tube or Teflon-sealed vial. Add one to 
three drops of mercury and

[[Page 121]]

seal.\13\ Agitate the contents of the vial for 15 to 30 s. Prolonged 
shaking (2 h) may be required. If so, this may be accomplished with a 
reciprocal shaker. Alternatively, activated copper powder may be used 
for sulfur removal.\14\ Analyze by gas chromatography.

                         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 to 10. 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 chromatograph.
    12.4  Inject 2 to 5 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush technique.\15\ 
Smaller (1.0 uL) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 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] TC15NO91.108

                                                              Equation 2

where:
    A=Amount of material injected (ng).
    Vi=Volume of extract injected (L).
    Vt=Volume of total extract (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] TC15NO91.109

                                                              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 
(g).
    Vo=Volume of water extracted (L).

    13.2  When it is apparent that two or more PCB (Aroclor) mixtures 
are present, the Webb and McCall procedure \16\ may be used to identify 
and quantify the Aroclors.
    13.3  For multicomponent mixtures (chlordane, toxaphene, and PCBs) 
match retention times of peaks in the standards with peaks in the 
sample. Quantitate every identifiable peak unless interference with 
individual peaks persist after cleanup. Add peak height or peak area of 
each identified peak in the chromatogram. Calculate as total response in 
the sample versus total response in the standard.
    13.4  Report results in 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.\17\ 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 with the following 
exceptions: Chlordane recovery at 4 x MDL was low (60%);

[[Page 122]]

Toxaphene recovery was demonstrated linear over the range of 10 x MDL to 
1000 x MDL.\17\
    14.3  This method was tested by 20 laboratories using reagent water, 
drinking water, surface water, and three industrial wastewaters spiked 
at six concentrations.\18\ Concentrations used in the study ranged from 
0.5 to 30 g/L for single-component pesticides and from 8.5 to 
400 g/L for multicomponent parameters. 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 Pesticides and PCBs in Industrial and 
Municipal Wastewaters,'' EPA 600/4-82-023, National Technical 
Information Service, PB82-214222, 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. 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., 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. 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).
    10. 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.)
    11. ASTM Annual Book of Standards, Part 31, D3370-76. ``Standard 
Practices for Sampling Water,'' American Society for Testing and 
Materials, Philadelphia.
    12. ``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.
    13. Goerlitz, D.F., and Law, L.M. Bulletin for Environmental 
Contamination and Toxicology, 6, 9 (1971).
    14. ``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.
    15. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    16. Webb, R.G., and McCall, A.C. ``Quantitative PCB Standards for 
Election Capture Gas Chromatography,'' Journal of Chromatographic 
Science, 11, 366 (1973).
    17. ``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.
    18. ``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.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                          Retention time       Method
                                               (min)          detection
               Parameter               --------------------     limit
                                                            (g/
                                         Col. 1    Col. 2        L)
------------------------------------------------------------------------
-BHC.........................      1.35      1.82       0.003
-BHC.........................      1.70      2.13       0.004
-BHC.........................      1.90      1.97       0.006
Heptachlor............................      2.00      3.35       0.003
-BHC.........................      2.15      2.20       0.009
Aldrin................................      2.40      4.10       0.004
Heptachlor epoxide....................      3.50      5.00       0.083
Endosulfan I..........................      4.50      6.20       0.014
4,4-DDE...............................      5.13      7.15       0.004
Dieldrin..............................      5.45      7.23       0.002
Endrin................................      6.55      8.10       0.006
4,4-DDD...............................      7.83      9.08       0.011
Endosulfan II.........................      8.00      8.28       0.004
4,4-DDT...............................      9.40     11.75       0.012
Endrin aldehyde.......................     11.82      9.30       0.023
Endosulfan sulfate....................     14.22     10.70       0.066
Chlordane.............................     mr        mr          0.014
Toxaphene.............................     mr        mr          0.24
PCB-1016..............................     mr        mr         nd
PCB-1221..............................     mr        mr         nd
PCB-1232..............................     mt        mr         nd
PCB-1242..............................     mr        mr          0.065
PCB-1248..............................     mr        mr         nd

[[Page 123]]

 
PCB-1254..............................     mr        mr         nd
PCB-1260..............................     mr        mr         nd
------------------------------------------------------------------------
 AColumn 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 200 C, except for PCB-1016 through PCB-
  1248, should be measured at 160 C.
 AColumn 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 C for the pesticides; at 140 C for PCB-1221 and
  1232; and at 170 C for PCB-1016 and 1242 to 1268.
 Amr=Multiple peak response. See Figures 2 thru 10.
 And=Not determined.


 Table 2--Distribution of Chlorinated Pesticides and PCBs into Florisil
                           Column Fractions 2
------------------------------------------------------------------------
                                          Percent recovery by fraction a
               Parameter                --------------------------------
                                             1          2          3
------------------------------------------------------------------------
Aldrin.................................        100  .........  .........
-BHC..........................        100  .........  .........
-BHC..........................         97  .........  .........
-BHC..........................         98  .........  .........
-BHC..........................        100  .........  .........
Chlordane..............................        100  .........  .........
4,4-DDD................................         99  .........  .........
4,4-DDE................................         98  .........  .........
4,4-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...............................         95  .........  .........
------------------------------------------------------------------------
a  Eluant composition:
    Fraction 1-6% ethyl ether in hexane.
    Fraction 2-15% ethyl ether in hexane.
    Fraction 3-50% ethyl ether in hexane.


                                   Table 3--QC Acceptance Criteria--Method 608
----------------------------------------------------------------------------------------------------------------
                                                                                           Range for X
                                                               Test conc.    Limit for s  (g/    Range
                          Parameter                           (g/  (g/       L)        for P,
                                                                   L)            L)                       Ps(%)
----------------------------------------------------------------------------------------------------------------
Aldrin......................................................        2.0           0.42    1.08-2.24       42-122
-BHC...............................................        2.0           0.48    0.98-2.44       37-134
-BHC...............................................        2.0           0.64    0.78-2.60       17-147
-BHC...............................................        2.0           0.72    1.01-2.37       19-140
-BHC...............................................        2.0           0.46    0.86-2.32       32-127
Chlordane...................................................       50            10.0     27.6-54.3       45-119
4,4 -DDD....................................................       10             2.8     4.8-12.6        31-141
4,4 -DDE....................................................        2.0           0.55    1.08-2.60       30-145
4,4-DDT.....................................................       10             3.6     4.6-13.7        25-160
Dieldrin....................................................        2.0           0.76    1.15-2.49       36-146
Endosulfan I................................................        2.0           0.49    1.14-2.82       45-153
Endosulfan II...............................................       10             6.1     2.2-17.1         D-202
Endosulfan Sulfate..........................................       10             2.7     3.8-13.2        26-144
Endrin......................................................       10             3.7     5.1-12.6        30-147
Heptachlor..................................................        2.0           0.40    0.86-2.00       34-111
Heptachlor epoxide..........................................        2.0           0.41    1.13-2.63       37-142
Toxaphene...................................................       50.0          12.7     27.8-55.6       41-126
PCB-1016....................................................       50            10.0     30.5-51.5       50-114
PCB-1221....................................................       50            24.4     22.1-75.2       15-178
PCB-1232....................................................       50            17.9     14.0-98.5       10-215
PCB-1242....................................................       50            12.2     24.8-69.6       39-150
PCB-1248....................................................       50            15.9     29.0-70.2       38-158
PCB-1254....................................................       50            13.8     22.2-57.9       29-131
PCB-1260....................................................       50            10.4     18.7-54.9        8-127
----------------------------------------------------------------------------------------------------------------
s=Standard deviation of four recovery measurements, in g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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.


                Table 4--Method Accuracy and Precision as Functions of Concentration--Method 608
----------------------------------------------------------------------------------------------------------------
                                                         Accuracy, as       Single analyst
                      Parameter                           recovery, X        precision, sr    Overall precision,
                                                        (g/L)      (g/L)     S (g/L)
----------------------------------------------------------------------------------------------------------------
Aldrin..............................................          0.81C+0.04          0.16X-0.04          0.20X-0.01
-BHC.......................................          0.84C+0.03          0.13X+0.04          0.23X-0.00
-BHC.......................................          0.81C+0.07          0.22X-0.02          0.33X-0.05
-BHC.......................................          0.81C+0.07          0.18X+0.09          0.25X+0.03
-BHC.......................................          0.82C-0.05          0.12X+0.06          0.22X+0.04
Chlordane...........................................          0.82C-0.04          0.13X+0.13          0.18X+0.18
4,4-DDD.............................................          0.84C+0.30          0.20X-0.18          0.27X-0.14
4,4-DDE.............................................          0.85C+0.14          0.13X+0.06          0.28X-0.09
4,4-DDT.............................................          0.93C-0.13          0.17X+0.39          0.31X-0.21
Dieldrin............................................          0.90C+0.02          0.12X+0.19          0.16X+0.16
Endosulfan I........................................          0.97C+0.04          0.10X+0.07          0.18X+0.08
Endosulfan II.......................................          0.93C+0.34         0.41X--0.65          0.47X-0.20

[[Page 124]]

 
Endosulfan Sulfate..................................          0.89C-0.37          0.13X+0.33          0.24X+0.35
Endrin..............................................          0.89C-0.04          0.20X+0.25          0.24X+0.25
Heptachlor..........................................          0.69C+0.04          0.06X+0.13          0.16X+0.08
Heptachlor epoxide..................................          0.89C+0.10          0.18X-0.11          0.25X-0.08
Toxaphene...........................................          0.80C+1.74          0.09X+3.20          0.20X+0.22
PCB-1016............................................          0.81C+0.50          0.13X+0.15          0.15X+0.45
PCB-1221............................................          0.96C+0.65          0.29X-0.76          0.35X-0.62
PCB-1232............................................         0.91C+10.79          0.21X-1.93          0.31X+3.50
PCB-1242............................................          0.93C+0.70          0.11X+1.40          0.21X+1.52
PCB-1248............................................          0.97C+1.06          0.17X+0.41          0.25X-0.37
PCB-1254............................................          0.76C+2.07          0.15X+1.66          0.17X+3.62
PCB-1260............................................          0.66C+3.76          0.22X-2.37          0.39X-4.86
----------------------------------------------------------------------------------------------------------------
X=Expected recovery for one or more measurements of a sample containing a concentration of C, in g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


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                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

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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 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.

[[Page 136]]

                       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--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 g/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.

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

[[Page 138]]

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 in acetone at a concentration of 
20 g/mL for each dinitrotoluene and 100 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 g/L, and the 
standard deviation of the recovery (s) in 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

[[Page 139]]

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 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

[[Page 140]]

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  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.

[[Page 141]]

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 standard must be added to the same extract and mixed 
thoroughly immediately before injection into the gas chromatograph.
    12.4  Inject 2 to 5 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush technique.\9\ Smaller 
(1.0 L) volumes may be injected if automatic devices are 
employed. Record the volume injected to the nearest 0.05 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 (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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 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.

[[Page 142]]

    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. ``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
                                                         ----------------------------       (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          -
----------------------------------------------------------------------------------------------------------------
 AAColumn 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 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 C.
 AAColumn 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 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 C.


                                   Table 2--QC Acceptance Criteria--Method 609
----------------------------------------------------------------------------------------------------------------
                                                                                        Range for X
                                                            Test Conc.    Limit for s  (g/   Range for
                        Parameter                          (g/  (g/       L)        P, Ps (%)
                                                                L)            L)
----------------------------------------------------------------------------------------------------------------
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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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
                                                           (g/L)     (g/L)     (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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 143]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.029


[[Page 144]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.030


[[Page 145]]

              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

[[Page 146]]

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.

[[Page 147]]

    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 g/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 L for HPLC and 2 to 5 
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 148]]

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 L for HPLC and 2 to 5 
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 (g/
L).
    Cs=Concentration of the parameter to be measured 
(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 g/mL of any

[[Page 149]]

of the six early-eluting PAHs (naphthalene, acenaphthylene, 
acenaphthene, fluorene, phenanthrene, and anthracene); 5 g/mL 
of benzo(k)fluoranthene; and 10 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 g/L, and the 
standard deviation of the recovery (s) in 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 150]]

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 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. 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 151]]

    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

[[Page 152]]

these conditions. The UV detector is recommended for the determination 
of naphthalene, acenaphthylene, acenapthene, and 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 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 
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 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush technique.\10\ 
Smaller (1.0 L) volumes may be injected if automatic devices 
are employed. Record the volume injected to the nearest 0.05 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 153]]

[GRAPHIC] [TIFF OMITTED] TC15NO91.114

                                                              Equation 2

where:
    A=Amount of material injected (ng).
    Vi=Volume of extract injected (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    14.2  Report results in 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 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 154]]



  Table 1--High Performance Liquid Chromatography Conditions and Method
                            Detection Limits
------------------------------------------------------------------------
                                                               Method
                                       Retention   Column     detection
              Parameter                   time    capacity      limit
                                         (min)     factor   (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
------------------------------------------------------------------------
 AAAHPLC 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 C for 4
  min., then programmed at 8 C/min. to a final hold at 280 C.


                                   Table 3--QC Acceptance Criteria--Method 610
----------------------------------------------------------------------------------------------------------------
                                                                                        Range for X
                                                            Test conc.    Limit for s  (g/   Range for
                        Parameter                          (g/  (g/       L)        P, Ps (%)
                                                                L)            L)
----------------------------------------------------------------------------------------------------------------
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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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.


                Table 4--Method Accuracy and Precision as Functions of Concentration--Method 610
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                               recovery, X    precision, sr   precision, S
                                                                  (g/L)  (g/L)  (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

[[Page 155]]

 
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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.

[GRAPHIC] [TIFF OMITTED] TC02JY92.031


[[Page 156]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.032


[[Page 157]]

[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
Bis(2-chloroisopropyl) ether..................        34283     108-60-1
4-Bromophenyl phenyl ether....................        34636     101-55-3
4-Chlorophenyl phenyl either..................        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.
    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

[[Page 158]]

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 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

[[Page 159]]

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 g/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 
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

[[Page 160]]

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

[[Page 161]]

    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 
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 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 g/L, and the 
standard deviation of the recovery (s) in 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 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 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.\8\ If spiking was performed at a concentration lower than 100 
g/L, the analyst must use either the QC acceptance criteria in 
Table 2, or optional QC

[[Page 162]]

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 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 practices9 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+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 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

[[Page 163]]

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).

                         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.

[[Page 164]]

    12.4  Inject 2 to 5 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush 
technique.11 Smaller (1.0 L) volumes may be injected 
if automatic devices are employed. Record the volume injected to the 
nearest 0.05 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 (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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 /
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.
    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

[[Page 165]]

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      Method
                                                 (min)        detection
                Parameters                ------------------    limit
                                            Column   Column  (/
                                              1        2          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
------------------------------------------------------------------------
 AColumn 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 C for 2 min.
  after injection then programmed at 8 C/min. to 230 C and held for 4
  min. Under these conditions the retention time for Aldrin is 22.6 min.
 AColumn 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 C for 4 min. after injection then
  programmed at 16 C/min. to 310 C. Under these conditions the retention
  time for Aldrin is 18.4 min.


                                   Table 2--QC Acceptance Criteria--Method 611
----------------------------------------------------------------------------------------------------------------
                                                                                        Range for X
                                                            Test conc.    Limit for s  (g/   Range for
                        Parameter                          (g/  (g/       L)          P, Ps
                                                                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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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
                                                                  (g/L)  (g/L)  (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
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 g/L.
sr = Expected single analyst standard deviation of measurements at an average concentration found of X, in
  g/L.
S = Expected interlaboratory standard deviation of measurements at an average concentration found of X, in
  g/L.
C =True value for the concentration, in g/L.
X = Average recovery found for measurements of samples containing a concentration of C, in g/L.


[[Page 166]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.034


[[Page 167]]

[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 168]]

 
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)1for 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.3Clean 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 169]]

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 g/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 +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 170]]

    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 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 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 (g/
L).
    Cs=Concentration of the parameter to be measured 
(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 171]]

    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 g/mL; any other 
chlorinated hydrocarbon, 100 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 g/L, and the 
standard deviation of the recovery (s) in 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 172]]

    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 
5:1.7If 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 173]]

    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 174]]

                         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 L of the sample extract or standard 
into the gas chromatograph using the solvent-flush 
techlique.9 Smaller (1.0 L) volumes may be injected 
if automatic devices are employed. Record the volume injected to the 
nearest 0.05 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 (L).
    Vt=Volume of total extract (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 
(g).
    Vo=Volume of water extracted (L).

    13.2  Report results in 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 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 175]]

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   (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 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 C, except where otherwise indicated.
nd=Not determined.
a 150 C column temperature.
b 165 C column temperature.
c 100 C column temperature.


                                   Table 2--QC Acceptance Criteria--Method 612
----------------------------------------------------------------------------------------------------------------
                                                                                          Range for X
                                                              Test conc.    Limit for s  (g/  Range for
                         Parameter                           (g/  (g/       L)         P, Ps
                                                                  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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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 176]]


                Table 3--Method Accuracy and Precision as Functions of Concentration--Method 612
----------------------------------------------------------------------------------------------------------------
                                                                      Single analyst
               Parameter                Acccuracy, as recovery,   precision, sr (g/L)              m>g/L)              (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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.
 
a Estimates based upon the performance in a single laboratory.\12\


[[Page 177]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.036


[[Page 178]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.037


[[Page 179]]

             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 180]]

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 g per wipe. Less than 1 g of 
2,3,7,8-TCDD per sample indicates acceptable cleanliness; anything 
higher warrants further cleaning. More than 10 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 g)

[[Page 181]]

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 
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.

[[Page 182]]

    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 g/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 37C14 2,3,7,8-TCDD (mol wt 328) or 
13C112 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 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 (g/
L).
    Cs=Concentration of 2,3,7,8-TCDD (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 183]]

    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 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 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 g/L, and the 
standard deviation of the recovery (s) in 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 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 184]]

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 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 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 185]]

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 186]]

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 
37Cl4 2,3,7,8-TCDD or m/z 332 for 
13C12 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 
37Cl4 2,3,7,8-TCDD or m/z 331.9367 for 
13C12 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 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 187]]

and the m/z 332 peak for 13C12 2,3,7,8-TCDD or the 
m/z 328 peak for 37Cl4 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 37Cl4 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 37Cl4 
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 
(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 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 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 188]]

    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)    (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 200C for 1 min, then programmed at 8C/min to 250 C and
  held. Use of helium carrier gas will approximately double the
  retention time.


                                   Table 2--QC Acceptance Criteria--Method 613
----------------------------------------------------------------------------------------------------------------
                                                              Test conc.    Limit for s                   Range
                         Parameter                           (g/  (g/    Range for X    for P,
                                                                  L)            L)       (g/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 g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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,   Overall precision,
                      Parameter                           recovery, X        precision, sr    S  (/g/L)
                                                        (g/L)       (/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 g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.

                         Method 624--Purgeables

                        1. Scope and Application

    1.1  This method covers the determination of a number of purgeable 
organics. The following parameters may be determined by this method:

------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
Benzene..........................................     34030      71-43-2
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     110-75-8
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
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
Ethyl benzene....................................     34371     100-41-4
Methylene chloride...............................     34423      75-09-2
1,1,2,2-Tetrachloroethane........................     34516      79-34-5
Tetrachloroethene................................     34475     127-18-4
Toluene..........................................     34010     108-88-3
1,1,1-Trichloroethene............................     34506      71-55-6
1,1,2-Trichloroethene............................     34511      79-00-5
Trichloroethane..................................     39180      79-01-6
Trichlorofluoromethane...........................     34488      75-69-4
Vinyl chloride...................................     39175      75-01-4
------------------------------------------------------------------------


[[Page 189]]

    1.2  The method may be extended to screen samples for acrolein 
(STORET No. 34210, CAS No. 107-02-8) and acrylonitrile (STORET No. 
34215, CAS No. 107-13-1), however, the preferred method for these two 
compounds in Method 603.
    1.3  This is a purge and trap gas chromatographic/mass spectrometer 
(GC/MS) method applicable to the determination of the compounds listed 
above in municipal and industrial discharges as provided under 40 CFR 
136.1.
    1.4  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.
    1.5  Any modification to 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. Depending upon the nature of the modification and the extent 
of intended use, the applicant may be required to demonstrate that the 
modifications will produce equivalent results when applied to relevant 
wastewaters.
    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 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 
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 inert gas to desorb the purgeables onto a gas 
chromatographic column. The gas chromatograph is temperature programmed 
to separate the purgeables which are then detected with a mass 
spectrometer.2,3

                            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 demonstated 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 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 pureeable 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 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 methmd. 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 
identified4-6 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, 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

[[Page 190]]

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 silicane (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 though 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 6.3.2), 15 cm of 2,6-dyphenylene oxide polymer 
(Section 6.3.1), and 8 cm of silica gel (Section 6.3.3). The minimum 
specifications for the trap are illustrated in Figure 2.
    5.2.3  The desorber should 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  GC/MS system:
    5.3.1  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, and gases.
    5.3.2  Column--6 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 
14. Guidelines for the use of alternate column packings are provided in 
Section 11.1.
    5.3.3  Mass spectrometer--Capable of scanning from 20 to 260 amu 
every 7 s or less, utilizing 70 V (nominal) electron energy in the 
electron impact ionization mode, and producing a mass spectrum which 
meets all the criteria in Table 2 when 50 ng of 4-bromofluorobenzene 
(BFB) is injected through the GC inlet.
    5.3.4  GC/MS interface--Any GC to MS interface that gives acceptable 
calibration points at 50 ng or less per injection for each of the 
parameters of interest and achieves all acceptable performance criteria 
(Section 10) may be used. GC to MS interfaces constructed of all glass 
or glass-lined materials are recommended. Glass can be deactivated by 
silanizing with dichlorodimethylsilane.
    5.3.5  Data system--A computer system must be interfaced to the mass 
spectrometer that allows the continuous acquisition and storage on 
machine-readable media of all mass spectra obtained throughout the 
duration of the chromatographic program. The computer must have software 
that allows searching any GC/MS data file for specific m/z (masses) and 
plotting such 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 in any EICP 
between specified time or scan number limits.
    5.4  Syringes--5-mL, glass hypodermic with Luerlok tip (two each), 
if applicable to the purging device.
    5.5  Micro syringes--25-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  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.

[[Page 191]]

    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 
compounds, 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 nearest 0.1 mg.
    6.5.2  Add the assayed reference material:
    6.5.2.1  Liquids--Using a 100-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.
    6.5.2.2  Gases--To prepare standards for any of the four halocarbons 
that boil below 30  deg.C (bromomethane, chloroethane, chloromethane, 
and 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 in the 
methanol).
    6.5.3  Reweigh, dilute to volume, stopper, then mix by inverting the 
flask several times. Calculate the concentration in g/
L from the net gain in weight. 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  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 four 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 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 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  Surrogate standard spiking solution--Select a minimum of three 
surrogate compounds from Table 3. Prepare stock standard solutions for 
each surrogate standard in methanol as described in Section 6.5. Prepare 
a surrogate standard spiking solution from these stock standards at a 
concentration of 15 g/mL in water. Store the solutions at 4 
deg.C in Teflon-sealed glass containers with a minimum of headspace. The 
solutions should be checked frequently for stability. The addition of 10 
L of this solution of 5 mL of sample or standard is equivalent 
to a concentration of 30 g/L of each surrogate standard.
    6.8  BFB Standard--Prepare a 25 g/mL solution of BFB in 
methanol.
    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. 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.
    7.3  Internal standard calibration procedure--To use this approach, 
the analyst must select three 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. Some recommended 
internal standards are listed in Table 3.
    7.3.1  Prepare calibration standards at a minimum of three 
concentration levels for each parameter by carefully adding 20.0 
L of one or more secondary dilution standards to 50, 250, or 
500 mL of reagent water. A 25-L syringe with a 0.006 in. ID 
needle should be used for this operation. One of the calibration 
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 GC/MS system. 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  Prepare a spiking solution containing each of the internal 
standards using the procedures described in Sections 6.5 and

[[Page 192]]

6.6. It is recommended that the secondary dilution standard be prepared 
at a concentration of 15 g/mL of each internal standard 
compound. The addition of 10 L of this standard to 5.0 mL of 
sample or calibration standard would be equivalent to 30 g/L.
    7.3.3  Analyze each calibration standard according to Section 11, 
adding 10 L of internal standard spiking solution directly to 
the syringe (Section 11.4). Tabulate the area response of the 
characteristic m/z against concentration for each compound and internal 
standard, and calculate response factors (RF) for each compound using 
Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.124

                                                              Equation 1

where:
    As=Area of the characteristic m/z for the parameter to be 
measured.
    Ais=Area of the characteristic m/z for the inernal 
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 (<35% 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 or RF must be verified on each 
working day by the measurement of a QC check sample.
    7.4.1  Prepare the QC check sample as described in Section 8.2.2.
    7.4.2  Analyze the QC check sample according to the method beginning 
in Section 10.
    7.4.3  For each parameter, compare the response (Q) with the 
corresponding calibration acceptance criteria found in Table 5. 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 7.4.4.
    Note: The large number of parameters in Table 5 present a 
substantial probability that one or more will not meet the calibration 
acceptance criteria when all parameters are analyzed.
    7.4.4  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 or RF must be prepared for that parameter according to Section 
7.3.

                           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 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  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 5% 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 5% 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 spike all samples with surrogate 
standards to monitor continuing laboratory performance. This procedure 
is described in Section 8.5.
    8.1.7  The laboratory must maintain performance records to document 
the quality of data that is generated. This procedure is described in 
Section 8.6.
    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 
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

[[Page 193]]

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 g/L of each 
parameter by adding 200 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 the method beginning in Section 10.
    8.2.4  Calculate the average recovery (X) in g/L, and the 
standard deviation of the recovery (s) in 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, found in 
Table 5. 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 5 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 5% of 
the samples from each sample site being monitored to assess accuracy. 
For laboratories analyzing 1 to 20 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 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 
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 5. These acceptance 
criteria wer 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 g/L, 
the analyst must use either the QC acceptance criteria in Table 5, or 
optional QC acceptance criteria calculated for the specific spike 
concentration. To calculate optional acceptance criteria for the 
recoveryof a parameter: (1) Calculate accuracy (X') using the equation 
in Table 6, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 6, 
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 anlaysis 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 5 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 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

[[Page 194]]

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 
5. 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 a quality control check, the laboratory must spike all 
samples with the surrogate standard spiking solutions as described in 
Section 11.4, and calculate the percent recovery of each surrogate 
compound.
    8.6  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 a regular basis (e.g. after each five to 
ten new accuracy measurements).
    8.7  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  All samples must be iced or refrigerated from the time of 
collection until analysis. If the sample contains residual 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  Experimental evidence indicates that some aromatic compounds, 
notably benzene, toluene, and ethyl benzene are susceptible to rapid 
biological degradation under certain environmental conditions.\3\ 
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 1+1 HCl while stirring 
vigorously, Check pH with narrow range (1.4 to 2.8) pH paper. Fill a 
sample container as described in Section 9.2.
    9.4  All samples must be analyzed within 14 days of collection.\3\

                    10. Daily GC/MS Performance Tests

    10.1  At the beginning of each day that analyses are to be 
performed, the GC/MS system must be checked to see if acceptable 
performance criteria are achieved for BFB.\9\ The performance test must 
be passed before any samples, blanks, or standards are analyzed, unless 
the instrument has met the DFTPP test described in Method 625 earlier in 
the day.\10\
    10.2  These performance tests require the following instrumental 
parameters:

    Electron Energy: 70 V (nominal)
    Mass Range: 20 to 260 amu
    Scan Time: To give at least 5 scans per peak but not to exceed 7 s 
per scan.

    10.3  At the beginning of each day, inject 2 L of BFB 
solution directly on the column. Alternatively, add 2 L of BFB 
solution to 5.0 mL of reagent water or standard solution and analyze the 
solution according to section 11. Obtain a background-corrected mass 
spectrum of BFB and confirm that all the key m/z criteria in Table 2 are 
achieved. If all the criteria are not achieved, the analyst must retune 
the mass spectrometer and repeat the test until all criteria are 
achieved.

                11. Sample Purging and 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 5. Other packed 
columns or chromatographic conditions may be used if the requirements of 
Section 8.2 are met.

[[Page 195]]

    11.2  After achieving the key m/z abundance criteria in Section 10, 
calibrate the system daiy as described in Section 7.
    11.3  Adjust the purge gas (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.
    11.4  Allow the sample to come to ambient temperature prior to 
introducing it into 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 L of the surrogate spiking solution (Section 6.7) and 
10.0 L of the internal standard spiking solution (Section 
7.3.2) through the valve bore, then close the valve. The surrogate and 
internal standards may be mixed and added as a single spiking solution.
    11.5  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.
    11.6  Close both valves and purge the sample for 11.00.1 
min at ambient temperature.
    11.7  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 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 cloumn must be used as a secondary trap by cooling it 
to 30  deg.C (subambient temperature, if problems persist) instead of 
the initial program temperature of 45  deg.C.
    11.8  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.
    11.9  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.
    11.10  If the response for any m/z 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.

                     12. Qualitative Identification

    12.1  Obtain EICPs for the primary m/z (Table 4) and at least two 
secondary masses for each parameter of interest. The following criteria 
must be met to make a qualitative identification:
    12.1.1  The characteristic masses of each parameter of interest must 
maximize in the same or within one scan of each other.
    12.1.2  The retention time must fall within 30 s of the 
retention time of the authentic compound.
    12.1.3  The relative peak heights of the three characteristic masses 
in the EICPs must fall within 20% of the relative 
intensities of these masses in a reference mass spectrum. The reference 
mass spectrum can be obtained from a standard analyzed in the GC/MS 
system or from a reference library.
    12.2  Structural isomers that have very similar mass spectra and 
less than 30 s difference in retention time, can be explicitly 
identified only if the resolution between authentic isomers in a 
standard mix is acceptable. Acceptable resolution is achieved if the 
baseline to valley height between the isomers is less than 25% of the 
sum of the two peak heights. Otherwise, structural isomers are 
identified as isomeric pairs.

                            13. Calculations

    13.1  When a parameter has been identified, the quantitation of that 
parameter should be based on the integrated abundance from the EICP of 
the primary characteristic m/z given in Table 4. If the sample produces 
an interference for the primary m/z, use a secondary characteristic m/z 
to quantitate.
    Calculate the concentration in the sample using the response factor 
(RF) determined in Section 7.3.3 and Equation 2.
[GRAPHIC] [TIFF OMITTED] TC15NO91.125

                                                              Equation 2

where:
    AS=Area of the characteristic m/z for the parameter or 
surrogate standard to be measured.
    Ais=Area of the characteristic m/z for the internal 
standard.
    Cis=Concentration of the internal standard.

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

[[Page 196]]

                         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.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.
    14.2  This method was tested by 15 laboratories using reagent water, 
drinking water, surface water, and industrial wastewaters spiked at six 
concentrations over the range 5-600 g/L.12Single 
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 5.

                               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. 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. ``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 8.2.3 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. Budde, W.L., and Eichelberger, J.W. ``Performance Tests for the 
Evaluation of Computerized Eas 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.
    10. Eichelberger, J.W., Harris, L.E., and Budde, W.L. ``Reference 
Compound to Calibrate Ion Abundance Measurement in Gas Chromatography--
Mass Spectrometry Systems,'' Analytical Chemistry, 47, 995-1000 (1975).
    11. ``Method Detection Limit for Methods 624 and 625,'' Olynyk, P., 
Budde, W.L., and Eichelberger, J.W. Unpublished report, May 14, 1980.
    12. ``EPA Method Study 29 EPA Method 624--Purgeables,'' EPA 600/4-
84-054, National Technical Information Service, PB84-209915, 
Springfield, Virginia 22161, June 1984.
    13.``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.

     Table 1--Chromatographic Conditions and Method Detection Limits
------------------------------------------------------------------------
                                                               Method
                                                              detection
                   Parameter                     Retention      limit
                                                time (min)  (g/
                                                                 L)
------------------------------------------------------------------------
Chloromethane.................................         2.3           nd
Bromomethane..................................         3.1           nd
Vinyl chloride................................         3.8           nd
Chloroethane..................................         4.6           nd
Methylene chloride............................         6.4          2.8
Trichlorofluoromethane........................         8.3           nd
1,1-Dichloroethene............................         9.0          2.8
1,1-Dichloroethane............................        10.1          4.7
trans-1,2-Dichloroethene......................        10.8          1.6
Chloroform....................................        11.4          1.6
1,2-Dichloroethane............................        12.1          2.8
1,1,1-Trichloroethane.........................        13.4          3.8
Carbon tetrachloride..........................        13.7          2.8
Bromodichloromethane..........................        14.3          2.2
1,2-Dichloroproane............................        15.7          6.0
cis-1,3-Dichloropropene.......................        15.9          5.0
Trichloroethene...............................        16.5          1.9
Benzene.......................................        17.0          4.4
Dibromochloromethane..........................        17.1          3.1
1,1,2-Trichloroethane.........................        17.2          5.0
trans-1,3-Dichloropropene.....................        17.2           nd
2-Chloroethylvinlyl ether.....................        18.6           nd
Bromoform.....................................        19.8          4.7
1,1,2,2-Tetrachloroethane.....................        22.1          6.9
Tetrachloroethene.............................        22.2          4.1
Toluene.......................................        23.5          6.0
Chlorobenzene.................................        24.6          6.0
Ethyl benzene.................................        26.4          7.2
1,3-Dichlorobenzene...........................        33.9           nd
1,2-Dichlorobenzene...........................        35.0           nd

[[Page 197]]

 
1,4-Dichlorobenzene...........................        35.4           nd
------------------------------------------------------------------------
Column conditions: Carbopak B (60/80 mesh) coated with 1% SP-1000 packed
  in a 6 ft by 0.1 in. ID glass column with helium carrier gas at 30 mL/
  min. flow rate. Column temperature held at 45C for 3 min., then
  programmed at 8C/min. to 220C and held for 15 min.
nd=not determined.


                 Table 2--BFB Key m/z Abundance Criteria
------------------------------------------------------------------------
                   Mass                        m/z Abundance criteria
------------------------------------------------------------------------
50........................................  15 to 40% of mass 95.
75........................................  30 to 60% of mass 95.
95........................................  Base Peak, 100% Relative
                                             Abundance.
96........................................  5 to 9% of mass 95.
173.......................................  <2% of mass 174.
174.......................................  >50% of mass 95.
175.......................................  5 to 9% of mass 174.
176.......................................  >95% but <101% of mass 174.
177.......................................  5 to 9% of mass 176.
------------------------------------------------------------------------


           Table 3--Suggested Surrogate and Internal Standards
------------------------------------------------------------------------
                                         Retention
                Compound                    time    Primary   Secondary
                                           (min)a     m/z       masses
------------------------------------------------------------------------
Benzene d-6............................     17.0        84   ...........
4-Bromofluorobenzene...................     28.3        95      174, 176
1,2-Dichloroethane d-4.................     12.1       102   ...........
1,4-Difluorobenzene....................     19.6       114        63, 88
Ethylbenzene d-5.......................     26.4       111   ...........
Ethylbenzene d-10......................     26.4        98   ...........
Fluorobenzene..........................     18.4        96            70
Pentafluorobenzene.....................     23.5       168   ...........
Bromochloromethane.....................      9.3       128   49, 130, 51
2-Bromo-1-chloropropane................     19.2        77       79, 156
1, 4-Dichlorobutane....................     25.8        55        90, 92
------------------------------------------------------------------------
a For chromatographic conditions, see Table 1.


          Table 4--Characteristic Masses for Purgeable Organics
------------------------------------------------------------------------
              Parameter                Primary          Secondary
------------------------------------------------------------------------
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.................     127   83, 85, and 129.
1,2-Dichloropropane..................     112   63, 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.
Ethyl benzene........................     106   91.
1,3-Dichlorobenzene..................     146   148 and 113.
1,2-Dichlorobenzene..................     146   148 and 113.
1,4-Dichlorobenzene..................     146   148 and 113.
------------------------------------------------------------------------


                          Table 5--Calibration and QC Acceptance Criteria--Method 624a
----------------------------------------------------------------------------------------------------------------
                                                       Range for Q   Limit for s    Range for X
                     Parameter                        (/g/  (/   (/g/   Range for P,
                                                           L)            g/L)           L)            Ps (%)
----------------------------------------------------------------------------------------------------------------
Benzene............................................       12.8-27.2         6.9        15.2-26.0          37-151
Bromodichloromethane...............................       13.1-26.9         6.4        10.1-28.0          35-155
Bromoform..........................................       14.2-25.8         5.4        11.4-31.1          45-169
Bromomethane.......................................        2.8-37.2        17.9           D-41.2           D-242
Carbon tetrachloride...............................       14.6-25.4         5.2        17.2-23.5          70-140
Chlorobenzene......................................       13.2-26.8         6.3        16.4-27.4          37-160
Chloroethane.......................................        7.6-32.4        11.4         8.4-40.4          14-230
2-Chloroethylvinyl ether...........................          D-44.8        25.9           D-50.4           D-305
Chloroform.........................................       13.5-26.5         6.1        13.7-24.2          51-138
Chloromethane......................................          D-40.8        19.8           D-45.9           D-273
Dibromochloromethane...............................       13.5-26.5         6.1        13.8-26.6          53-149
1,2-Dichlorobenzene................................       12.6-27.4         7.1        11.8-34.7          18-190
1,3-Dichlorobenzene................................       14.6-25.4         5.5        17.0-28.8          59-156
1,4-Dichlorobenzene................................       12.6-27.4         7.1        11.8-34.7          18-190
1,1-Dichloroethane.................................       14.5-25.5         5.1        14.2-28.5          59-155
1,2-Dichloroethane.................................       13.6-26.4         6.0        14.3-27.4          49-155
1,1-Dichlorothene..................................       10.1-29.9         9.1         3.7-42.3           D-234
trans-1,2-Dichloroethene...........................       13.9-26.1         5.7        13.6-28.5          54-156

[[Page 198]]

 
1,2-Dichloropropane................................        6.8-33.2        13.8         3.8-36.2           D-210
cis-1,3-Dichloropropene............................        4.8-35.2        15.8         1.0-39.0           D-227
trans-1,3-Dichloropropene..........................       10.0-30.0        10.4         7.6-32.4          17-183
Ethyl benzene......................................       11.8-28.2         7.5        17.4-26.7          37-162
Methylene chloride.................................       12.1-27.9         7.4           D-41.0           D-221
1,1,2,2-Tetrachloroethane..........................       12.1-27.9         7.4        13.5-27.2          46-157
Tetrachloroethene..................................       14.7-25.3         5.0        17.0-26.6          64-148
Toluene............................................       14.9-25.1         4.8        16.6-26.7          47-150
1,1,1-Trichloroethane..............................       15.0-25.0         4.6        13.7-30.1          52-162
1,1,2-Trichloroethane..............................       14.2-25.8         5.5        14.3-27.1          52-150
Trichloroethene....................................       13.3-26.7         6.6        18.6-27.6          71-157
Trichlorofluoromethane.............................        9.6-30.4        10.0         8.9-31.5          17-181
Vinyl chloride.....................................        0.8-39.2        20.0           D-43.5           D-251
----------------------------------------------------------------------------------------------------------------
Q= Concentration measured in QC check sample, in g/L (Section 7.5.3).
s= Standard deviation of four recovery measurements, in g/L (Section 8.2.4).
X= Average recovery of four recovery measurements, in 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.
aCriteria were calculated assuming a QC check sample concentration of 20 g/L.
 
Note: These criteria are based directly upon the method performance data in Table 6. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limits to concentrations below those used to
  develop Table 6.


                Table 6--Method Accuracy and Precision as Functions of Concentration--Method 624
----------------------------------------------------------------------------------------------------------------
                                                                      Single analyst
               Parameter                 Accuracy, as recovery,   precision, sr (g/L)              m>g/L)              (g/L)
----------------------------------------------------------------------------------------------------------------
Benzene...............................  0.93C+2.00               0.26X-1.74               0.25X-1.33
Bromodichloromethane..................  1.03C-1.58               0.15X+0.59               0.20X+1.13
Bromoform.............................  1.18C-2.35               0.12X+0.36               0.17X+1.38
Bromomethane a........................  1.00C                    0.43X                    0.58X
Carbon tetrachloride..................  1.10C-1.68               0.12X+0.25               0.11X+0.37
Chlorobenzene.........................  0.98C+2.28               0.16X-0.09               0.26X-1.92
Chloroethane..........................  1.18C+0.81               0.14X+2.78               0.29X+1.75
2-Chloroethylvinyl ether a............  1.00C                    0.62X                    0.84X
Chloroform............................  0.93C+0.33               0.16X+0.22               0.18X+0.16
Chloromethane.........................  1.03C+0.81               0.37X+2.14               0.58X+0.43
Dibromochloromethane..................  1.01C-0.03               0.17X-0.18               0.17X+0.49
1,2-Dichlorobenzene b.................  0.94C+4.47               0.22X-1.45               0.30X-1.20
1,3-Dichlorobenzene...................  1.06C+1.68               0.14X-0.48               0.18X-0.82
1,4-Dichlorobenzene b.................  0.94C+4.47               0.22X-1.45               0.30X-1.20
1,1-Dichloroethane....................  1.05C+0.36               0.13X-0.05               0.16X+0.47
1,2-Dichloroethane....................  1.02C+0.45               0.17X-0.32               0.21X-0.38
1,1-Dichloroethene....................  1.12C+0.61               0.17X+1.06               0.43X-0.22
trans-1,2,-Dichloroethene.............  1.05C+0.03               0.14X+0.09               0.19X+0.17
1,2-Dichloropropane a.................  1.00C                    0.33X                    0.45X
cis-1,3-Dichloropropene a.............  1.00C                    0.38X                    0.52X
trans-1,3-Dichloropropene a...........  1.00C                    0.25X                    0.34X
Ethyl benzene.........................  0.98C+2.48               0.14X+1.00               0.26X-1.72
Methylene chloride....................  0.87C+1.88               0.15X+1.07               0.32X+4.00
1,1,2,2-Tetrachloroethane.............  0.93C+1.76               0.16X+0.69               0.20X+0.41
Tetrachloroethene.....................  1.06C+0.60               0.13X-0.18               0.16X-0.45
Toluene...............................  0.98C+2.03               0.15X-0.71               0.22X-1.71
1,1,1-Trichloroethane.................  1.06C+0.73               0.12X-0.15               0.21X-0.39
1,1,2-Trichloroethane.................  0.95C+1.71               0.14X+0.02               0.18X+0.00
Trichloroethene.......................  1.04C+2.27               0.13X+0.36               0.12X+0.59
Trichloroflouromethane................  0.99C+0.39               0.33X-1.48               0.34X-0.39
Vinyl chloride........................  1.00C                    0.48X                    0.65X
----------------------------------------------------------------------------------------------------------------
X=Expected recovery for one or more measurements of a sample containing a concentration of C, in g/L.
Sr=Expected single analyst standard deviation of measurements at an average concentration found ofX, in g/L.
S=Expected interlaboratory standard deviation of measurements at an average concentration found ofX, in g/L.
C=True value for the concentration, in g/L.
X=Average recovery found for measurements of samples containing a concentration of C, in g/L.
a Estimates based upon the performance in a single laboratory.13
b Due to chromatographic resolution problems, performance statements for these isomers are based upon the sums
  of their concentrations.


[[Page 199]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.038


[[Page 200]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.039


[[Page 201]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.040


[[Page 202]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.041

                   Method 625--Base/Neutrals and Acids

                        1. Scope and Application

    1.1  This method covers the determination of a number of organic 
compounds that are partitioned into an organic solvent and are amenable 
to gas chromatography. The parameters listed in Tables 1 and 2 may be 
qualitatively and quantitatively determined using this method.
    1.2  The method may be extended to include the parameters listed in 
Table 3. Benzidine can be subject to oxidative losses during solvent 
concentration. Under the alkaline conditions of the extraction step, 
-BHC, -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-
nitrosodimethylamine is difficult to separate from the solvent under the 
chromatographic conditions described. N-nitrosodiphenylamine decomposes 
in the gas chromatographic inlet and cannot be separated from 
diphenylamine. The preferred method for each of these parameters is 
listed in Table 3.
    1.3  This is a gas chromatographic/mass spectrometry (GC/MS) method 
2,14 applicable to the determination of the compounds listed 
in Tables 1, 2, and 3 in municipal and industrial discharges as provided 
under 40 CFR 136.1.

[[Page 203]]

    1.4  The method detection limit (MDL, defined in Section 
16.1)1 for each parameter is listed in Tables 4 and 5. The 
MDL for a specific wastewater may differ from those listed, depending 
upon the nature of interferences in the sample matrix.
    1.5  Any modification to 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. Depending upon the nature of the modification and the extent 
of intended use, the applicant may be required to demonstrate that the 
modifications will produce equivalent results when applied to relevant 
wastewaters.
    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 serially 
extracted with methylene chloride at a pH greater than 11 and again at a 
pH less than 2 using a separatory funnel or a continuous extractor.\2\ 
The methylene chloride extract is dried, concentrated to a volume of 1 
mL, and analyzed by GC/MS. Qualitative identification of the parameters 
in the extract is performed using the retention time and the relative 
abundance of three characteristic masses (m/z). Quantitative analysis is 
performed using internal standard techniques with a single 
characteristic m/z.

                            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 the total ion current 
profiles. 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. Thmrough 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.
    3.3  The base-neutral extraction may cause significantly reduced 
recovery of phenol, 2-methylphenol, and 2,4-dimethylphenol. The analyst 
must recognize that results obtained under these conditions are minimum 
concentrations.
    3.4  The packed gas chromatographic columns recommended for the 
basic fraction may not exhibit sufficient resolution for certain 
isomeric pairs including the following: anthracene and phenanthrene; 
chrysene and benzo(a)anthracene; and benzo(b)fluoranthene and 
benzo(k)fluoranthene. The gas chromatographic retention time and mass 
spectra for these pairs of compounds are not sufficiently different to 
make an unambiguous identification. Alternative techniques should be 
used to identify and quantify these specific compounds, such as Method 
610.
    3.5  In samples that contain an inordinate number of interferences, 
the use of chemical ionization (CI) mass spectrometry may make 
identification easier. Tables 6 and 7 give characteristic CI ions for 
most of the compounds covered by this method. The use of CI mass 
spectrometry to support electron ionization (EI) mass spectrometry is 
encouraged but not required.

                                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.

[[Page 204]]

    4.2  The following parameters covered by this method have been 
tentatively classified as known or suspected, human or mammalian 
carcinogens: benzo(a)anthracene, benzidine, 3,3'-dichlorobenzidine, 
benzo(a)pyrene, -BHC, -BHC, -BHC, -
BHC, dibenzo(a,h)anthracene, N-nitrosodimethylamine, 4,4'-DDT, and 
polychlorinated biphenyls (PCBs). 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 composit sampling.
    5.1.1  Grab sample bottle--1-L or 1-gt, 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 throughly 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, 19 mm ID, with coarse 
frit
    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-57001-
0500 or equivalent). Attach to concentrator tube with springs.
    5.2.5  Snyder column, Kuderna-Danish--Three all macro (Kontes K-
503000-0121 or equivalent).
    5.2.6  Snyder column, Kuderna-Danish--Two-ball macro (Kontes K-
569001-0219 or equivalent).
    5.2.7  Vials--10 to 15-mL, amber glass, with Teflon-lined screw cap.
    5.2.8  Continuous liquid--liquid extractor--Equipped with Teflon or 
glass connecting joints and stopcocks requiring no lubrication. 
(Hershberg-Wolf Extractor, Ace Glass Company, Vineland, N.J., P/N 6841-
10 or equivalent.)
    5.3  Boiling chips--Approximately 10/40 mesh. Heat to 400  deg.C for 
30 min of 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  GC/MS system:
    5.6.1  Gas Chromatograph--An analytical system complete with a 
temperature programmable gas chromatograph and all required accessores 
including syringes, analytical columns, and gases. The injection port 
must be designed for on-column injection when using packed columns and 
for splitless injection when using capillary columns.
    5.6.2  Column for base/neutrals--1.8 m long x 2 mm ID glass, packed 
with 3% SP-2250 on Supelcoport (100/120 mesh) or equivalent. This column 
was used to develop the method performance statements in Section 16. 
Guidelines for the use of alternate column packings are provided in 
Section 13.1.
    5.6.3  Column for acids--1.8 m long x 2 mm ID glass, packed with 1% 
SP-1240DA on Supelcoport (100/120 mesh) or equivalent. This column was 
used to develop the method performance statements in Section 16. 
Guidelines for the use of alternate column packings are given in Section 
13.1.
    5.6.4  Mass spectrometer--Capable of scanning from 35 to 450 amu 
every 7 s or less, utilizing a 70 V (nominal) electron energy in the 
electron impact ionization mode, and producing a mass spectrum which 
meets all the criteria in Table 9 when 50 ng of decafluorotriphenyl 
phosphine (DFTPP; bis(perfluorophenyl) phenyl phosphine) is injected 
through the GC inlet.
    5.6.5  GC/MS interface--Any GC to MS interface that gives acceptable 
calibration points at 50 ng per injection for each of the parameters of 
interest and achieves all acceptable performance criteria (Section 12) 
may be used. GC to MS interfaces constructed of all glass or glass-lined 
materials are recommended. Glass can be deactivated by silanizing with 
dichlorodimethylsilane.
    5.6.6  Data system--A computer system must be interfaced to the mass 
spectrometer that allows the contiluous acquisition and storage on 
machine-readable media of all mass spectra obtained throughout the 
duration of the chromatographic program. The computer must have software 
that allows searching any GC/MS data file for specific m/z and plotting 
such 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

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allows integrating the abundance in any EICP between specified time or 
scan number limits.

                               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 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, methlylene chloride--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  Stock standard solutions (1.00 g/L)--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 pesticide quality 
acetone or other suitable solvent 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 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  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 quality control check samples indicate a 
problem.
    6.8  Surrogate standard spiking solution--Select a minimum of three 
surrogate compounds from Table 8. Prepare a surrogate standard spiking 
solution containing each selected surrogate compound at a concentration 
of 100 g/mL in acetone. Addition of 1.00 mL of this solution to 
1000 mL of sample is equivalent to a concentration of 100 g/L 
of each surrogate standard. Store the spiking solution at 4  deg.C in 
Teflon-sealed glass container. The solution should be checked frequently 
for stability. The solution must be replaced after six months, or sooner 
if comparison with quality control check standards indicates a problem.
    6.9  DFTPP standard--Prepare a 25 g/mL solution of DFTPP in 
acetone.
    6.10  Quality control check sample concentrate--See Section 8.2.1.

                             7. Calibration

    7.1  Establish gas chromatographic operating parameters equivalent 
to those indicated in Table 4 or 5.
    7.2  Internal standard calibration procedure--To use this approach, 
the analyst must select three 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 standards 
is not affected by method or matrix interferences. Some recommended 
internal standards are listed in Table 8. Use the base peak m/z as the 
primary m/z for quantification of the standards. If interferences are 
noted, use one of the next two most intense m/z quantities for 
quantification.
    7.2.1  Prepare calibration standards at a minimum of three 
concentration levels for each parameter of interest by adding 
appropriate volumes of one or more stock standards to a volumetric 
flask. To each calibration standard or standard mixture, add a known 
constant amount of one or more internal standards, and and dilute to 
volume with acetone. One of the calibration 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 GC/MS system.
    7.2.2  Using injections of 2 to 5 L, analyze each 
calibration standard according to Section 13 and tabulate the area of 
the primary characteristic m/z (Tables 4 and 5) against concentration 
for each compound and internal standard. Calculate response factors (RF) 
for each compound using Equation 1.
[GRAPHIC] [TIFF OMITTED] TC15NO91.126

                                                              Equation 1
where:
    As=Area of the characteristic m/z for the parameter to be 
measured.
    Ais=Area of the characteristic m/z for the internal 
standard.
    Cis=Concentration of the internal standard (g/
L).
    Cs=Concentration of the parameter to be measured 
(g/L).

If the RF value over the working range is a constant (<35% 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.
    7.3  The working calibration curve or RF must be verified on each 
working day by the

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measurement of one or more calibration standards. If the response for 
any parameter varies from the predicted response by more than 
20%, the test must be repeated uning a fresh calibration 
standard. Alternatively, a new calibration curve must be prepared for 
that compound.

                           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 occuring in 
chromatography, the analyst is permitted certain options (detailed in 
Sections 10.6 and 13.1) 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 5% 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 5% 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 
g/mL in acetone. Multiple solutions may be required. PCBs and 
multicomponent pesticides may be omitted from this test. 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 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 or 11.
    8.2.4  Calculate the average recovery (X) in g/L, and the 
standard deviation of the recovery (s) in 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 6. 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 6 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 5% of 
the samples from each sample site being monitored to assess

[[Page 207]]

accuracy. For laboratories analyzing 1 to 20 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  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 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 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 6. 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 
100 g/L, the analyst must use either the QC acceptance criteria 
in Table 6, 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 7, substituting the spike concentration (T) for C; (2) 
calculate overall precision (S') using the equation in Table 7, 
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 single-component parameters in Table 6 
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 
6. 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 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  As a quality control check, the laboratory must spike all 
samples with the surrogate standard spiking solution as described in 
Section 10.2, and calculate the percent recovery of each surrogate 
compound.
    8.7  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 208]]

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 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 sampling 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.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.

                    10. Separatory Funnel Extraction

    10.1  Samples are usually extracted using separatory funnel 
techniques. If emulsions will prevent achieving acceptable solvent 
recovery with separatory funnel extractions, continuous extraction 
(Section 11) may be used. The separatory funnel extraction scheme 
described below assumes a sample volume of 1 L. When sample volumes of 2 
L are to be extracted, use 250, 100, and 100-mL volumes of methylene 
chloride for the serial extraction of the base/neutrals and 200, 100, 
and 100-mL volumes of methylene chloride for the acids.
    10.2  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. Pipet 1.00 mL of the surrogate standard spiking 
solution into the separatory funnel and mix well. Check the pH of the 
sample with wide-range pH paper and adjust to pH>11 with sodium 
hydroxide solution.
    10.3  Add 60 mL of methylene chloride to the sample bottle, seal, 
and shake for 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. 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 11.3.
    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. Label the combined extract as the base/neutral fraction.
    10.5  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 250-mL Erlenmeyer flask and label the combined extracts as 
the acid fraction.
    10.6  For each fraction, 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  For each fraction, 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 and attach a three-ball 
Snyder column to the evaporative flask for each fraction. Prewet each 
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 from the water 
bath and allow it to drain and cool for at least 10 min. 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.

[[Page 209]]

    10.9  Add another one or two clean boiling chips to the concentrator 
tube for each fraction and attach a two-ball micro-Snyder column. Prewet 
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 to 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 to 10 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 about 0.5 mL, remove the K-D apparatus from the 
water bath and allow it to drain and cool for at least 10 min. Remove 
the Snyder column and rinse the flask and its lower joint into the 
concentrator tube with approximately 0.2 mL of acetone or methylene 
chloride. Adjust the final volume to 1.0 mL with the solvent. 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 Teflon-sealed screw-cap vials 
and labeled base/neutral or acid fraction as appropriate.
    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. Continuous Extraction

    11.1  When experience with a sample from a given source indicates 
that a serious emulsion problem will result or an emulsion is 
encountered using a separatory funnel in Section 10.3, a continuous 
extractor should be used.
    11.2  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 with sodium hydroxide solution. 
Transfer the sample to the continuous extractor and using a pipet, add 
1.00 mL of surrogate standard spiking solution and mix well. Add 60 mL 
of methylene chloride to the sample bottle, seal, and shake for 30 s to 
rinse the inner surface. Transfer the solvent to the extractor.
    11.3  Repeat the sample bottle rinse with an additional 50 to 100-mL 
portion of methylene chloride and add the rinse to the extractor.
    11.4  Add 200 to 500 mL of methylene chloride to the distilling 
flask, add sufficient reagent water to ensure proper operation, and 
extract for 24 h. Allow to cool, then detach the distilling flask. Dry, 
concentrate, and seal the extract as in Sections 10.6 through 10.9.
    11.5  Charge a clean distilling flask with 500 mL of 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 24 h. Dry, concentrate, and seal the extract 
as in Sections 10.6 through 10.9.

                    12. Daily GC/MS Performance Tests

    12.1  At the beginning of each day that analyses are to be 
performed, the GC/MS system must be checked to see if acceptable 
performance criteria are achieved for DFTPP.10 Each day that 
benzidine is to be determined, the tailing factor criterion described in 
Section 12.4 must be achieved. Each day that the acids are to be 
determined, the tailing factor criterion in Section 12.5 must be 
achieved.
    12.2  These performance tests require the following instrumental 
parameters:

    Electron Energy: 70 V (nominal)
    Mass Range: 35 to 450 amu
    Scan Time: To give at least 5 scans per peak but not to exceed 7 s 
per scan.

    12.3  DFTPP performance test--At the beginning of each day, inject 2 
L (50 ng) of DFTPP standard solution. Obtain a background-
corrected mass spectra of DFTPP and confirm that all the key m/z 
criteria in Table 9 are achieved. If all the criteria are not achieved, 
the analyst must retune the mass spectrometer and repeat the test until 
all criteria are achieved. The performance criteria must be achieved 
before any samples, blanks, or standards are analyzed. The taililg 
factor tests in Sections 12.4 and 12.5 may be performed simultaneously 
with the DFTPP test.
    12.4  Column performance test for base/neutrals--At the beginning of 
each day that the base/neutral fraction is to be analyzed for benzidine, 
the benzidine tailing factor must be calculated. Inject 100 ng of 
benzidine either separately or as a part of a standard mixture that may 
contain DFTPP and calculate the tailing factor. The benzidine tailing 
factor must be less than 3.0. Calculation of the tailing factor is 
illustrated in Figure 13.11 Replace the column packing if the 
tailing factor criterion cannot be achieved.
    12.5  Column performance test for acids--At the beginning of each 
day that the acids are to be determined, inject 50 ng of 
pentachlorophenol either separately or as a part of a standard mix that 
may contain DFTPP. The tailing factor for pentachlorophenol must be less 
than 5. Calculation of the tailing factor is illustrated in Figure 
13.11 Replace the column packing if the tailing factor 
criterion cannot be achieved.

                13. Gas Chromatography/Mass Spectrometry

    13.1  Table 4 summarizes the recommended gas chromatographic 
operating conditions for the base/neutral fraction. Table 5 summarizes 
the recommended gas chromatographic

[[Page 210]]

operating conditions for the acid fraction. Included in these tables are 
retention times and MDL that can be achieved under these conditions. 
Examples of the separations achieved by these columns are shown in 
Figures 1 through 12. Other packed or capillary (open-tubular) columns 
or chromatographic conditions may be used if the requirements of Section 
8.2 are met.
    13.2  After conducting the GC/MS performance tests in Section 12, 
calibrate the system daily as described in Section 7.
    13.3  The internal standard must be added to sample extract and 
mixed thoroughly immediately before it is injected into the instrument. 
This procedure minimizes losses due to adsorption, chemical reaction or 
evaporation.
    13.4  Inject 2 to 5 L of the sample extract or standard 
into the GC/MS system using the solvent-flush technique.12 
Smaller (1.0 L) volumes may be injected if automatic devices 
are employed. Record the volume injected to the nearest 0.05 L.
    13.5  If the response for any m/z exceeds the working range of the 
GC/MS system, dilute the extract and reanalyze.
    13.6  Perform all qualitative and quantitative measurements as 
described in Sections 14 and 15. When the extracts are not being used 
for analyses, store them refrigerated at 4 deg.C, protected from light 
in screw-cap vials equipped with unpierced Teflon-lined septa.

                     14. Qualitative Identification

    14.1  Obtain EICPs for the primary m/z and the two other masses 
listed in Tables 4 and 5. See Section 7.3 for masses to be used with 
internal and surrogate standards. The following criteria must be met to 
make a qualitative identification:
    14.1.1  The characteristic masses of each parameter of interest must 
maximize in the same or within one scan of each other.
    14.1.2  The retention time must fall within 30 s of the 
retention time of the authentic compound.
    14.1.3  The relative peak heights of the three characteristic masses 
in the EICPs must fall within 20% of the relative 
intensities of these masses in a reference mass spectrum. The reference 
mass spectrum can be obtained from a standard analyzed in the GC/MS 
system or from a reference library.
    14.2  Structural isomers that have very similar mass spectra and 
less than 30 s difference in retention time, can be explicitly 
identified only if the resolution between authentic isomers in a 
standard mix is acceptable. Acceptable resolution is achieved if the 
baseline to valley height between the isomers is less than 25% of the 
sum of the two peak heights. Otherwise, structural isomers are 
identified as isomeric pairs.

                            15. Calculations

    15.1  When a parameter has been identified, the quantitation of that 
parameter will be based on the integrated abundance from the EICP of the 
primary characteristic m/z in Tables 4 and 5. Use the base peak m/z for 
internal and surrogate standards. If the sample produces an interference 
for the primary m/z, use a secondary characteristic m/z to quantitate.
    Calculate the concentration in the sample using the response factor 
(RF) determined in Section 7.2.2 and Equation 3.
[GRAPHIC] [TIFF OMITTED] TC15NO91.127

                                                              Equation 3

where:
    As=Area of the characteristic m/z for the parameter or 
surrogate standard to be measured.
    Ais=Area of the characteristic m/z for the internal 
standard.
    Is=Amount of internal standard added to each extract 
(g).
    Vo=Volume of water extracted (L).

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

                         16. Method Performance

    16.1  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 4 and 5 were obtained using reagent 
water.13 The MDL actually achieved in a given analysis will 
vary depending on instrument sensitivity and matrix effects.
    16.2  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 to 1300 g/L.14 
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 7.

    17. Screening Procedure for 2,3,7,8-Tetrachlorodibenzo-p-dioxin 
                             (2,3,7,8-TCDD)

    17.1  If the sample must be screened for the presence of 2,3,7,8-
TCDD, it is recommended that the reference material not be handled in 
the laboratory unless extensive safety precautions are employed. It is 
sufficient to analyze the base/neutral extract by selected ion 
monitoring (SIM) GC/MS techniques, as follows:
    17.1.1  Concentrate the base/neutral extract to a final volume of 
0.2 ml.

[[Page 211]]

    17.1.2  Adjust the temperature of the base/neutral column (Section 
5.6.2) to 220  deg.C.
    17.1.3  Operate the mass spectrometer to acquire data in the SIM 
mode using the ions at m/z 257, 320 and 322 and a dwell time no greater 
than 333 milliseconds per mass.
    17.1.4  Inject 5 to 7 L of the base/neutral extract. 
Collect SIM data for a total of 10 min.
    17.1.5  The possible presence of 2,3,7,8-TCDD is indicated if all 
three masses exhibit simultaneous peaks at any point in the selected ion 
current profiles.
    17.1.6  For each occurrence where the possible presence of 2,3,7,8-
TCDD is indicated, calculate and retain the relative abundances of each 
of the three masses.
    17.2  False positives to this test may be caused by the presence of 
single or coeluting combinations of compounds whose mass spectra contain 
all of these masses.
    17.3  Conclusive results of the presence and concentration level of 
2,3,7,8-TCDD can be obtained only from a properly equipped laboratory 
through the use of EPA Method 613 or other approved alternate test 
procedures.

                               References

    1. 40 CFR part 136, appendix B.
    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. Available from Effluent 
Guidelines Division, Washington, DC 20460.
    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. Eichelberger, J.W., Harris, L.E., and Budde, W.L. ``Reference 
Compound to Calibrate Ion Abundance Measurement in Gas Chromatography-
Mass Spectometry,'' Analytical Chemistry, 47, 995 (1975).
    11. McNair, N.M. and Bonelli, E.J. ``Basic Chromatography,'' 
Consolidated Printing, Berkeley, California, p. 52, 1969.
    12. Burke, J.A. ``Gas Chromatography for Pesticide Residue Analysis; 
Some Practical Aspects,'' Journal of the Association of Official 
Analytical Chemists, 48, 1037 (1965).
    13. Olynyk, P., Budde, W.L., and Eichelberger, J.W. ``Method 
Detection Limit for Methods 624 and 625,'' Unpublished report, May 14, 
1980.
    14. ``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.

                   Table 1--Base/Neutral Extractables
------------------------------------------------------------------------
                                                    STORET
                    Parameter                         No.      CAS No.
------------------------------------------------------------------------
Acenaphthene.....................................     34205      83-32-9
Acenaphthylene...................................     34200     208-96-8
Anthracene.......................................     34220     120-12-7
Aldrin...........................................     39330     309-00-2
Benzo(a)anthracene...............................     34526      56-55-3
Benzo(b)fluoranthene.............................     34230     205-99-2
Benzo(k)fluoranthene.............................     34242     207-08-9
Benzo(a)pyrene...................................     34247      50-32-8
Benzo(ghi)perylene...............................     34521     191-24-2
Benzyl butyl phthalate...........................     34292      85-68-7
-BHC....................................     39338     319-85-7
-BHC....................................     34259     319-86-8
Bis(2-chloroethyl) ether.........................     34273     111-44-4
Bis(2-chloroethoxy)methane.......................     34278     111-91-1
Bis(2-ethylhexyl) phthalate......................     39100     117-81-7
Bis(2-chloroisopropyl) ethera....................     34283     108-60-1
4-Bromophenyl phenyl ethera......................     34636     101-55-3
Chlordane........................................     39350      57-74-9
2-Chloronaphthalele..............................     34581      91-58-7
4-Chlorophenyl phenyl ether......................     34641    7005-72-3
Chrysene.........................................     34320     218-01-9
4,4-DDD..........................................     39310      72-54-8
4,4-DDE..........................................     39320      72-55-9
4,4-DDT..........................................     39300      50-29-3
Dibenzo(a,h)anthracene...........................     34556      53-70-3
Di-n-butylphthalate..............................     39110      84-74-2
1,3-Dichlorobenzene..............................     34566     541-73-1
1,2-Dichlorobenzene..............................     34536      95-50-1
1,4-Dichlorobenzene..............................     34571     106-46-7
3,3-Dichlorobenzidine............................     34631      91-94-1
Dieldrin.........................................     39380      60-57-1
Diethyl phthalate................................     34336      84-66-2
Dimethyl phthalate...............................     34341     131-11-3
2,4-Dinitrotoluene...............................     34611     121-14-2
2,6-Dinitrotoluene...............................     34626     606-20-2
Di-n-octylphthalate..............................     34596     117-84-0
Endosulfan sulfate...............................     34351    1031-07-8

[[Page 212]]

 
Endrin aldehyde..................................     34366    7421-93-4
Fluoranthene.....................................     34376     206-44-0
Fluorene.........................................     34381      86-73-7
Heptachlor.......................................     39410      76-44-8
Heptchlor epoxide................................     39420    1024-57-3
Hexachlorobenzene................................     39700     118-74-1
Hexachlorobutadiene..............................     34391      87-68-3
Hexachloroethane.................................     34396      67-72-1
Indeno(1,2,3-cd)pyrene...........................     34403     193-39-5
Isophorone.......................................     34408      78-59-1
Naphthalene......................................     34696      91-20-3
Nitrobenzene.....................................     34447      98-95-3
N-Nitrosodi-n-propylamine........................     34428     621-64-7
PCB-1016.........................................     34671   12674-11-2
PCB-1221.........................................     39488   11104-28-2
PCB-1232.........................................     39492   11141-16-5
PCB-1242.........................................     39496   53469-21-9
PCB-1248.........................................     39500   12672-29-6
PCB-1254.........................................     39504   11097-69-1
PCB-1260.........................................     39508   11096-82-5
Phenanthrene.....................................     34461      85-01-8
Pyrene...........................................     34469     129-00-0
Toxaphene........................................     39400    8001-35-2
1,2,4-Trichlorobenzene...........................     34551     120-82-1
------------------------------------------------------------------------
a The proper chemical name is 2,2-oxybis(1-chloropropane).


                       Table 2--Acid Extractables
------------------------------------------------------------------------
                                                    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
------------------------------------------------------------------------


              Table 3--Additional Extractable Parameters a
------------------------------------------------------------------------
                                            STORET
                Parameter                     No.      CAS No.    Method
------------------------------------------------------------------------
Benzidine................................     39120      92-87-5     605
-BHC............................     39337     319-84-6     608
-BHC............................     39340      58-89-8     608
Endosulfan I.............................     34361     959-98-8     608
Endosulfan II............................     34356   33213-65-9     608
Endrin...................................     39390      72-20-8     608
Hexachlorocylopentadiene.................     34386      77-47-4     612
N-Nitrosodimethylamine...................     34438      62-75-9     607
N-Nitrosodiphenylamine...................     34433      86-30-6     607
------------------------------------------------------------------------
a See Section 1.2.


                  Table 4--Chromatographic Conditions, Method Detection Limits, and Characteristic Masses for Base/Neutral Extractables
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                 Method                         Characteristic masses
                                                                   Retention    detection  -------------------------------------------------------------
                            Parameter                                 time        limit             Electron impact              Chemical ionization
                                                                     (min)    (g/ -------------------------------------------------------------
                                                                                   L)        Primary  Secondary  Secondary   Methane   Methane   Methane
--------------------------------------------------------------------------------------------------------------------------------------------------------
1,3-Dichlorobenzene..............................................        7.4         1.9         146        148        113       146       148       150
1,4-Dichlorobenzene..............................................        7.8         4.4         146        148        113       146       148       150
Hexachloroethane.................................................        8.4         1.6         117        201        199       199       201       203
Bis(2-chloroethyl) ethera........................................        8.4         5.7          93         63         95        63       107       109
1,2-Dichlorobenzene..............................................        8.4         1.9         146        148        113       146       148       150
Bis(2-chloroisopropyl) ethera....................................        9.3         5.7          45         77         79        77       135       137
N-Nitrosodi-n-propylamine........................................  .........  ............       130         42        101  ........  ........  ........
Nitrobenzene.....................................................       11.1         1.9          77        123         65       124       152       164
Hexachlorobutadiene..............................................       11.4         0.9         225        223        227       223       225       227
1,2,4-Trichlorobenzene...........................................       11.6         1.9         180        182        145       181       183       209
Isophorone.......................................................       11.9         2.2          82         95        138       139       167       178
Naphthalene......................................................       12.1         1.6         128        129        127       129       157       169
Bis(2-chloroethoxy) methane......................................       12.2         5.3          93         95        123        65       107       137
Hexachlorocyclopentadiene a......................................       13.9  ............       237        235        272       235       237       239
2-Chloronaphthalene..............................................       15.9         1.9         162        164        127       163       191       203
Acenaphthylene...................................................       17.4         3.5         152        151        153       152       153       181
Acenaphthene.....................................................       17.8         1.9         154        153        152       154       155       183
Dimethyl phthalate...............................................       18.3         1.6         163        194        164       151       163       164
2,6-Dinitrotoluene...............................................       18.7         1.9         165         89        121       183       211       223
Fluorene.........................................................       19.5         1.9         166        165        167       166       167       195
4-Chlorophenyl phenyl ether......................................       19.5         4.2         204        206        141  ........  ........  ........
2,4-Dinitrotoluene...............................................       19.8         5.7         165         63        182       183       211       223
Diethyl phthalate................................................       20.1         1.9         149        177        150       177       223       251
N-Nitrosodiphenylamine b.........................................       20.5         1.9         169        168        167       169       170       198
Hexachlorobenzene................................................       21.0         1.9         284        142        249       284       286       288
-BHC b..................................................       21.1  ............       183        181        109  ........  ........  ........
4-Bromophenyl phenyl ether.......................................       21.2         1.9         248        250        141       249       251       277
-BHC b..................................................       22.4  ............       183        181        109  ........  ........  ........
Phenanthrene.....................................................       22.8         5.4         178        179        176       178       179       207
Anthracene.......................................................       22.8         1.9         178        179        176       178       179       207
-BHC....................................................       23.4         4.2         181        183        109  ........  ........  ........

[[Page 213]]

 
Heptachlor.......................................................       23.4         1.9         100        272        274  ........  ........  ........
-BHC....................................................       23.7         3.1         183        109        181  ........  ........  ........
Aldrin...........................................................       24.0         1.9          66        263        220  ........  ........  ........
Dibutyl phthalate................................................       24.7         2.5         149        150        104       149       205       279
Heptachlor epoxide...............................................       25.6         2.2         353        355        351  ........  ........  ........
Endosulfan I b...................................................       26.4  ............       237        339        341  ........  ........  ........
Fluoranthene.....................................................       26.5         2.2         202        101        100       203       231       243
Dieldrin.........................................................       27.2         2.5          79        263        279  ........  ........  ........
4,4-DDE..........................................................       27.2         5.6         246        248        176  ........  ........  ........
Pyrene...........................................................       27.3         1.9         202        101        100       203       231       243
Endrin b.........................................................       27.9  ............        81        263         82  ........  ........  ........
Endosulfan II b..................................................       28.6  ............       237        339        341  ........  ........  ........
4,4-DDD..........................................................       28.6         2.8         235        237        165  ........  ........  ........
Benzidine b......................................................       28.8          44         184         92        185       185       213       225
4,4-DDT..........................................................       29.3         4.7         235        237        165  ........  ........  ........
Endosulfan sulfate...............................................       29.8         5.6         272        387        422  ........  ........  ........
Endrin aldehyde..................................................  .........  ............        67        345        250  ........  ........  ........
Butyl benzyl phthalate...........................................       29.9         2.5         149         91        206       149       299       327
Bis(2-ethylhexyl) phthalate......................................       30.6         2.5         149        167        279       149  ........  ........
Chrysene.........................................................       31.5         2.5         228        226        229       228       229       257
Benzo(a)anthracene...............................................       31.5         7.8         228        229        226       228       229       257
3,3-Dichlorobenzidine............................................       32.2        16.5         252        254        126  ........  ........  ........
Di-n-octyl phthalate.............................................       32.5         2.5         149  .........  .........  ........  ........  ........
Benzo(b)fluoranthene.............................................       34.9         4.8         252        253        125       252       253       281
Benzo(k)fluoranthene.............................................       34.9         2.5         252        253        125       252       253       281
Benzo(a)pyrene...................................................       36.4         2.5         252        253        125       252       253       281
Indeno(1,2,3-cd) pyrene..........................................       42.7         3.7         276        138        277       276       277       305
Dibenzo(a,h)anthracene...........................................       43.2         2.5         278        139        279       278       279       307
Benzo(ghi)perylene...............................................       45.1         4.1         276        138        277       276       277       305
N-Nitrosodimethylamine b.........................................  .........  ............        42         74         44  ........  ........  ........
Chlordane c......................................................      19-30  ............       373        375        377  ........  ........  ........
Toxaphene c......................................................      25-34  ............       159        231        233  ........  ........  ........
PCB 1016 c.......................................................      18-30  ............       224        260        294  ........  ........  ........
PCB 1221 c.......................................................      15-30          30         190        224        260  ........  ........  ........
PCB 1232 c.......................................................      15-32  ............       190        224        260  ........  ........  ........
PCB 1242 c.......................................................      15-32  ............       224        260        294  ........  ........  ........
PCB 1248 c.......................................................      12-34  ............       294        330        262  ........  ........  ........
PCB 1254 c.......................................................      22-34          36         294        330        362  ........  ........  ........
PCB 1260 c.......................................................      23-32  ............       330        362        394  ........  ........  ........
--------------------------------------------------------------------------------------------------------------------------------------------------------
a The proper chemical name is 2,2-bisoxy(1-chloropropane).
b See Section 1.2.
c These compounds are mixtures of various isomers (See Figures 2 through 12). Column conditions: Supelcoport (100/120 mesh) coated with 3% SP-2250
  packed in a 1.8 m long x 2 mm ID glass column with helium carrier gas at 30 mL/min. flow rate. Column temperature held isothermal at 50 C for 4 min.,
  then programmed at 8 C/min. to 270 C and held for 30 min.


                      Table 5--Chromatographic Conditions, Method Detection Limits, and Characteristic Masses for Acid Extractables
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                 Method                         Characteristic masses
                                                                   Retention    detection  -------------------------------------------------------------
                            Parameter                                 time        limit             Electron Impact              Chemical ionization
                                                                     (min)    (g/ -------------------------------------------------------------
                                                                                   L)        Primary  Secondary  Secondary   Methane   Methane   Methane
--------------------------------------------------------------------------------------------------------------------------------------------------------
2-Chlorophenol...................................................        5.9         3.3         128         64        130       129       131       157
2-Nitrophenol....................................................        6.5         3.6         139         65        109       140       168       122
Phenol...........................................................        8.0         1.5          94         65         66        95       123       135
2,4-Dimethylphenol...............................................        9.4         2.7         122        107        121       123       151       163
2,4-Dichlorophenol...............................................        9.8         2.7         162        164         98       163       165       167
2,4,6-Trichlorophenol............................................       11.8         2.7         196        198        200       197       199       201
4-Chloro-3-methylphenol..........................................       13.2         3.0         142        107        144       143       171       183
2,4-Dinitrophenol................................................       15.9          42         184         63        154       185       213       225
2-Methyl-4,6-dinitrophenol.......................................       16.2          24         198        182         77       199       227       239
Pentachlorophenol................................................       17.5         3.6         266        264        268       267       265       269

[[Page 214]]

 
4-Nitrophenol....................................................       20.3         2.4          65        139        109       140       168       122
--------------------------------------------------------------------------------------------------------------------------------------------------------
Column conditions: Supelcoport (100/120 mesh) coated with 1% SP-1240DA packed in a 1.8 m long x 2mm ID glass column with helium carrier gas at 30 mL/
  min. flow rate. Column temperature held isothermal at 70 C for 2 min. then programmed at 8 C/min. to 200 C.


                                   Table 6--QC Acceptance Criteria--Method 625
----------------------------------------------------------------------------------------------------------------
                                                              Test
                                                           conclusion   Limits for s    Range for     Range for
                        Parameter                         (g/  (g/  X(g/     P, Ps
                                                               L)            L)             L)        (Percent)
----------------------------------------------------------------------------------------------------------------
Acenaphthene............................................           100          27.6    60.1-132.3        47-145
Acenaphthylene..........................................           100          40.2    53.5-126.0        33-145
Aldrin..................................................           100          39.0     7.2-152.2         D-166
Anthracene..............................................           100          32.0    43.4-118.0        27-133
Benzo(a)anthracene......................................           100          27.6    41.8-133.0        33-143
Benzo(b)fluoranthene....................................           100          38.8    42.0-140.4        24-159
Benzo(k)fluoranthene....................................           100          32.3    25.2-145.7        11-162
Benzo(a)pyrene..........................................           100          39.0    31.7-148.0        17-163
Benzo(ghi)perylene......................................           100          58.9       D-195.0         D-219
Benzyl butyl phthalate..................................           100          23.4       D-139.9         D-152
-BHC...........................................           100          31.5    41.5-130.6        24-149
-BHC...........................................           100          21.6       D-100.0         D-110
Bis(2-chloroethyl) ether................................           100          55.0    42.9-126.0        12-158
Bis(2-chloroethoxy)methane..............................           100          34.5    49.2-164.7        33-184
Bis(2-chloroisopropyl) ethera...........................           100          46.3    62.8-138.6        36-166
Bis(2-ethylhexyl) phthalate.............................           100          41.1    28.9-136.8         8-158
4-Bromophenyl phenyl ether..............................           100          23.0    64.9-114.4        53-127
2-Chloronaphthalene.....................................           100          13.0    64.5-113.5        60-118
4-Chlorophenyl phenyl ether.............................           100          33.4    38.4-144.7        25-158
Chrysene................................................           100          48.3    44.1-139.9        17-168
4,4'-DDD................................................           100          31.0       D-134.5         D-145
4,4'-DDE................................................           100          32.0    19.2-119.7         4-136
4,4'-DDT................................................           100          61.6       D-170.6         D-203
Dibenzo(a,h)anthracene..................................           100          70.0       D-199.7         D-227
Di-n-butyl phthalate....................................           100          16.7     8.4-111.0         1-118
1,2-Dichlorobenzene.....................................           100          30.9    48.6-112.0        32-129
1,3-Dichlorobenzene.....................................           100          41.7    16.7-153.9         D-172
1,4,-Dichlorobenzene....................................           100          32.1    37.3-105.7        20-124
3,3'-Dhlorobenzidine....................................           100          71.4     8.2-212.5         D-262
Dieldrin................................................           100          30.7    44.3-119.3        29-136
Diethyl phthalate.......................................           100          26.5       D-100.0         D-114
Dimethyl phthalate......................................           100          23.2       D-100.0         D-112
2,4-Dinitrotoluene......................................           100          21.8    47.5-126.9        39-139
2,6-Dinitrotoluene......................................           100          29.6    68.1-136.7        50-158
Di-n-octyl phthalate....................................           100          31.4    18.6-131.8         4-146
Endosulfan sulfate......................................           100          16.7       D-103.5         D-107
Endrin aldehyde.........................................           100          32.5       D-188.8         D-209
Fluoranthene............................................           100          32.8    42.9-121.3        26-137
Fluorene................................................           100          20.7    71.6-108.4        59-121
Heptachlor..............................................           100          37.2       D-172.2         D-192
Heptachlor epoxide......................................           100          54.7    70.9-109.4        26-155
Hexachlorobenzene.......................................           100          24.9     7.8-141.5         D-152
Hexachlorobutadiene.....................................           100          26.3    37.8-102.2        24-116
Hexachloroethane........................................           100          24.5    55.2-100.0        40-113
Indeno(1,2,3-cd)pyrene..................................           100          44.6       D-150.9         D-171
Isophorone..............................................           100          63.3    46.6-180.2        21-196
Naphthalene.............................................           100          30.1    35.6-119.6        21-133
Nitrobenzene............................................           100          39.3    54.3-157.6        35-180
N-Nitrosodi-n-propylamine...............................           100          55.4    13.6-197.9         D-230
PCB-1260................................................           100          54.2    19.3-121.0         D-164
Phenanthrene............................................           100          20.6    65.2-108.7        54-120
Pyrene..................................................           100          25.2    69.6-100.0        52-115
1,2,4-Trichlorobenzene..................................           100          28.1    57.3-129.2        44-142
4-Chloro-3-methylphenol.................................           100          37.2    40.8-127.9        22-147
2-Chlorophenol..........................................           100          28.7    36.2-120.4        23-134

[[Page 215]]

 
2,4-Dichlorophenol......................................           100          26.4    52.5-121.7        39-135
2,4-Dimethylphenol......................................           100          26.1    41.8-109.0        32-119
2,4-Dinitrophenol.......................................           100          49.8       D-172.9         D-191
2-Methyl-4,6-dinitrophenol..............................           100          93.2    53.0-100.0         D-181
2-Nitrophenol...........................................           100          35.2    45.0-166.7        29-182
4-Nitrophenol...........................................           100          47.2    13.0-106.5         D-132
Pentachlorophenol.......................................           100          48.9    38.1-151.8        14-176
Phenol..................................................           100          22.6    16.6-100.0         5-112
2,4,6-Trichlorophenol...................................           100          31.7    52.4-129.2        37-144
----------------------------------------------------------------------------------------------------------------
s=Standard deviation for four recovery measurements, in g/L (Section 8.2.4).
X=Average recovery for four recovery measurements, in 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 7. Where necessary, the limits
  for recovery have been broadened to assure applicability of the limts to concentrations below those used to
  develop Table 7.
a The proper chemical name is 2,2oxybis(1-chloropropane).


                Table 7--Method Accuracy and Precision as Functions of Concentration--Method 625
----------------------------------------------------------------------------------------------------------------
                                                                   Accuracy, as   Single analyst      Overall
                            Parameter                               recovery, X   precision, sr'   precision, S
                                                                  (g/L)  (g/L)  (g/L)
----------------------------------------------------------------------------------------------------------------
Acenaphthene....................................................      0.96C=0.19      0.15X-0.12      0.21X-0.67
Acenaphthylene..................................................      0.89C=0.74      0.24X-1.06      0.26X-0.54
Aldrin..........................................................      0.78C=1.66      0.27X-1.28      0.43X=1.13
Anthracene......................................................      0.80C=0.68      0.21X-0.32      0.27X-0.64
Benzo(a)anthracene..............................................      0.88C-0.60      0.15X=0.93      0.26X-0.28
Benzo(b)fluoranthene............................................      0.93C-1.80      0.22X=0.43      0.29X=0.96
Benzo(k)fluoranthene............................................      0.87C-1.56      0.19X=1.03      0.35X=0.40
Benzo(a)pyrene..................................................      0.90C-0.13      0.22X=0.48      0.32X=1.35
Benzo(ghi)perylene..............................................      0.98C-0.86      0.29X=2.40      0.51X-0.44
Benzyl butyl phthalate..........................................      0.66C-1.68      0.18X=0.94      0.53X=0.92
-BHC...................................................      0.87C-0.94      0.20X-0.58      0.30X-1.94
-BHC...................................................      0.29C-1.09      0.34X=0.86      0.93X-0.17
Bis(2-chloroethyl) ether........................................      0.86C-1.54      0.35X-0.99      0.35X=0.10
Bis(2-chloroethoxy)methane......................................      1.12C-5.04      0.16X=1.34      0.26X=2.01
Bis(2-chloroisopropyl) ethera...................................      1.03C-2.31      0.24X=0.28      0.25X=1.04
Bis(2-ethylhexyl) phthalate.....................................      0.84C-1.18      0.26X=0.73      0.36X=0.67
4-Bromophenyl phenyl ether......................................      0.91C-1.34      0.13X=0.66      0.16X=0.66
2-Chloronaphthalene.............................................      0.89C=0.01      0.07X=0.52      0.13X=0.34
4-Chlorophenyl phenyl ether.....................................      0.91C=0.53      0.20X-0.94      0.30X-0.46
Chrysene........................................................      0.93C-1.00      0.28X=0.13      0.33X-0.09
4,4-DDD.........................................................      0.56C-0.40      0.29X-0.32      0.66X-0.96
4,4-DDE.........................................................      0.70C-0.54      0.26X-1.17      0.39X-1.04
4,4-DDT.........................................................      0.79C-3.28      0.42X=0.19      0.65X-0.58
Dibenzo(a,h)anthracene..........................................      0.88C=4.72      0.30X=8.51      0.59X=0.25
Di-n-butyl phthalate............................................      0.59C=0.71      0.13X=1.16      0.39X=0.60
1,2-Dichlorobenzene.............................................      0.80C=0.28      0.20X=0.47      0.24X=0.39
1,3-Dichlorobenzene.............................................      0.86C-0.70      0.25X=0.68      0.41X=0.11
1,4-Dichlorobenzene.............................................      0.73C-1.47      0.24X=0.23      0.29X=0.36
3,3-Dichlorobenzidine...........................................     1.23C-12.65      0.28X=7.33      0.47X=3.45
Dieldrin........................................................      0.82C-0.16      0.20X-0.16      0.26X-0.07
Diethyl phthalate...............................................      0.43C=1.00      0.28X=1.44      0.52X=0.22
Dimethyl phthalate..............................................      0.20C=1.03      0.54X=0.19      1.05X-0.92
2,4-Dinitrotoluene..............................................      0.92C-4.81      0.12X=1.06      0.21X=1.50
2,6-Dinitrotoluene..............................................      1.06C-3.60      0.14X=1.26      0.19X=0.35
Di-n-octyl phthalate............................................      0.76C-0.79      0.21X=1.19      0.37X=1.19
Endosulfan sulfate..............................................      0.39C=0.41      0.12X=2.47      0.63X-1.03
Endrin aldehyde.................................................      0.76C-3.86      0.18X=3.91      0.73X-0.62
Fluoranthene....................................................      0.81C=1.10      0.22X-0.73      0.28X-0.60
Fluorene........................................................      0.90C-0.00      0.12X=0.26      0.13X=0.61
Heptachlor......................................................      0.87C-2.97      0.24X-0.56      0.50X-0.23
Heptachlor epoxide..............................................      0.92C-1.87      0.33X-0.46      0.28X=0.64
Hexachlorobenzene...............................................      0.74C=0.66      0.18X-0.10      0.43X-0.52
Hexachlorobutadiene.............................................      0.71C-1.01      0.19X=0.92      0.26X=0.49
Hexachloroethane................................................      0.73C-0.83      0.17X=0.67      0.17X=0.80
Indeno(1,2,3-cd)pyrene..........................................      0.78C-3.10      0.29X=1.46      0.50X=0.44
Isophorone......................................................      1.12C=1.41      0.27X=0.77      0.33X=0.26
Naphthalene.....................................................      0.76C=1.58      0.21X-0.41      0.30X-0.68

[[Page 216]]

 
Nitrobenzene....................................................      1.09C-3.05      0.19X=0.92      0.27X=0.21
N-Nitrosodi-n-propylamine.......................................      1.12C-6.22      0.27X=0.68      0.44X=0.47
PCB-1260........................................................     0.81C-10.86      0.35X=3.61      0.43X=1.82
Phenanthrene....................................................      0.87C-0.06      0.12X=0.57      0.15X=0.25
Pyrene..........................................................      0.84C-0.16      0.16X=0.06      0.15X=0.31
1,2,4-Trichlorobenzene..........................................      0.94C-0.79      0.15X=0.85      0.21X=0.39
4-Chloro-3-methylphenol.........................................      0.84C=0.35      0.23X=0.75      0.29X=1.31
2-Chlorophenol..................................................      0.78C=0.29      0.18X=1.46      0.28X=0.97
2,4-Dichlorophenol..............................................      0.87C=0.13      0.15X=1.25      0.21X=1.28
2,4-Dimethylphenol..............................................      0.71C=4.41      0.16X=1.21      0.22X=1.31
2,4-Dinitrophenol...............................................     0.81C-18.04      0.38X=2.36     0.42X=26.29
2-Methyl-4,6-Dinitrophenol......................................     1.04C-28.04     0.05X=42.29     0.26X=23.10
2-Nitrophenol...................................................      1.07C-1.15      0.16X=1.94      0.27X=2.60
4-Nitrophenol...................................................      0.61C-1.22      0.38X=2.57      0.44X=3.24
Pentachlorophenol...............................................      0.93C=1.99      0.24X=3.03      0.30X=4.33
Phenol..........................................................      0.43C=1.26      0.26X=0.73      0.35X=0.58
2,4,6-Trichlorophenol...........................................      0.91C-0.18      0.16X=2.22      0.22X=1.81
----------------------------------------------------------------------------------------------------------------
X=Expected recovery for one or more measurements of a sample containing a concentration of C, in g/L.
sr=Expected single analyst standard deviation of measurements at an average concentration found of X, in g/L.
S= Expected interlaboratory standard deviation of measurements at an average concentration found of X, in g/L.
C= True value for the concentration, in g/L.
X= Average recovery found for measurements of samples containing a concentration of C, in g/L.
a The proper chemical name is 2,2oxybis(1-chloropropane).


           Table 8--Suggested Internal and Surrogate Standards
------------------------------------------------------------------------
           Base/neutral fraction                    Acid fraction
------------------------------------------------------------------------
Aniline-d5................................  2-Fluorophenol.
Anthracene-d10............................  Pentafluorophenol.
Benzo(a)anthracene-d12....................  Phenol-d5
4,4-Dibromobiphenyl.......................  2-Perfluoromethyl phenol.
4,4-Dibromooctafluorobiphenyl.............  ............................
Decafluorobiphenyl........................  ............................
2,2 \1\-Difluorobiphenyl..................  ............................
4-Fluoroaniline...........................  ............................
1-Fluoronaphthalene.......................  ............................
2-Fluoronaphthalene.......................  ............................
Naphthalene-d8............................  ............................
Nitrobenzene-d5...........................  ............................
2,3,4,5,6-Pentafluorobiphenyl.............  ............................
Phenanthrene-d10..........................  ............................
Pyridine-d5...............................  ............................
------------------------------------------------------------------------


            Table 9--DFTPP Key Masses and Abundance Criteria
------------------------------------------------------------------------
  Mass                        m/z Abundance criteria
------------------------------------------------------------------------
     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.
    198  Base peak, 100 percent relative abundance.
    199  5-9 percent of mass 198.
    275  10-30 percent of mass 198.
    365  Greater than 1 percent of mass 198.
    441  Present but less than mass 443.
    442  Greater than 40 percent of mass 198.
    443  17-23 percent of mass 442.
------------------------------------------------------------------------


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[[Page 229]]

                         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.
    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, 37Cl4-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

[[Page 230]]

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.

                            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

[[Page 231]]

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 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.

[[Page 232]]

    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 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 g per wipe; 
analysis using this method can achieve an even lower detection limit. 
Less than 0.1 g per wipe indicates acceptable cleanliness; 
anything higher warrants further cleaning. More than 10 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

[[Page 233]]

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).
    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 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.

[[Page 234]]

    6.7.2.2  Injector--Rheodyne 7120 (or equivalent) with 50 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.
    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--605 m long  x  0.320.02 mm ID; 
0.25 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--
305 m long  x  0.320.02 mm ID; 0.25 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

[[Page 235]]

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.
    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.

[[Page 236]]

    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 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 37Cl4-2,3,7,8-
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 13C12-1,2,3,4-TCDD and 
13C2-1,2,3,7,8,9-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 
13C12-1,2,3,4-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 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

[[Page 237]]

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 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:

[[Page 238]]

    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.
    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

[[Page 239]]

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 chlorination given in Table 2 (assuming a response factor of 1 
relative to the 13C12-1,2,3,4-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

[[Page 240]]

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 
L or 2 L, consistent with the capability of the HRGC/
HRMS instrument. Inject a 1 L or 2 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.
    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 13C12-
1,2,3,4-TCDD (Section 7.12) shall exceed 25.0 minutes on the DB-5 
column, and the retention time of 13C12-1,2,3,4-
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

[[Page 241]]

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 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 37Cl4-2,3,7,8-
TCDD. See Table 8.

    10.6.2  To calibrate the analytical system by internal standard, 
inject 1.0 L or 2.0 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

[[Page 242]]

(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.
    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 10.00.02 mL of well-mixed sample 
through the filter.
    11.2.1.3  Dry the filter a minimum of 12 hours at 1105 
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 1105  deg.C, and 
cool in a dessicator.
    11.2.2.3  Calculate percent solids as follows:
    [GRAPHIC] [TIFF OMITTED] TR15SE97.005
    

[[Page 243]]


    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 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

[[Page 244]]

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 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.

[[Page 245]]

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 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

[[Page 246]]

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 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.

[[Page 247]]

    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.
    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.

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    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.
    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

[[Page 249]]

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 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 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 
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 L. Add 10 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

[[Page 250]]

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 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 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.

[[Page 251]]

    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/L in methylene chloride.
    13.6.1.2  Inject 30 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 methylene chloride, 
including a minimum of five 50 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 L of extract. If the extract cannot be 
concentrated to less than 30 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 L of 
methylene chloride and reduce to 30 L with the evaporation 
apparatus (Section 12.7).
    13.6.2.2  Inject the 30 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 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 
L as described in Section

[[Page 252]]

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 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 L or 2.0 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

[[Page 253]]

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 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 
13C12-1,2,3,4-TCDD and 
13C12-1,2,3,7,8,9-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

[[Page 254]]

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 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 13C12-1,2,3,7,8,9-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 
13C-labeled analogs and the 37C-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 37Cl-labeled 
standard.

    17.2.2 Using the concentration in the extract determined above, 
compute the percent recovery of the 13C-labeled compounds and

[[Page 255]]

the 37C-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 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/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).

[[Page 256]]

    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 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 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).
    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).

[[Page 257]]

                            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-
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

[[Page 258]]

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

  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  13C12-2,3,7,8-TCDD..............      76523-40-5
                                                                37Cl4-2,3,7,8-TCDD..............      85508-50-5
Total TCDD....................................      41903-57-5
2,3,7,8-TCDF..................................      51207-31-9  13C12-2,3,7,8-TCDF..............      89059-46-1
Total-TCDF....................................      55722-27-5
1,2,3,7,8-PeCDD...............................      40321-76-4  13C12-1,2,3,7,8-PeCDD...........     109719-79-1
Total-PeCDD...................................      36088-22-9
1,2,3,7,8-PeCDF...............................      57117-41-6  13C12-1,2,3,7,8-PeCDF...........     109719-77-9
2,3,4,7,8-PeCDF...............................      57117-31-4  13C12-2,3,4,7,8-PeCDF...........     116843-02-8
Total-PeCDF...................................      30402-15-4
1,2,3,4,7,8-HxCDD.............................      39227-28-6  13C12-1,2,3,4,7,8-HxCDD.........     109719-80-4
1,2,3,6,7,8-HxCDD.............................      57653-85-7  13C12-1,2,3,6,7,8-HxCDD.........     109719-81-5
1,2,3,7,8,9-HxCDD.............................      19408-74-3  13C12-1,2,3,7,8,9-HxCDD.........     109719-82-6
Total-HxCDD...................................      34465-46-8
1,2,3,4,7,8-HxCDF.............................      70648-26-9  13C12-1,2,3,4,7,8-HxCDF.........     114423-98-2
1,2,3,6,7,8-HxCDF.............................      57117-44-9  13C12-1,2,3,6,7,8-HxCDF.........     116843-03-9
1,2,3,7,8,9-HxCDF.............................      72918-21-9  13C12-1,2,3,7,8,9-HxCDF.........     116843-04-0
2,3,4,6,7,8-HxCDF.............................      60851-34-5  13C12-2,3,4,6,7,8-HxCDF.........     116843-05-1
Total-HxCDF...................................      55684-94-1
1,2,3,4,6,7,8-HpCDD...........................      35822-46-9  13C12-1,2,3,4,6,7,8-HpCDD.......     109719-83-7
Total-HpCDD...................................      37871-00-4
1,2,3,4,6,7,8-HpCDF...........................      67562-39-4  13C12-1,2,3,4,6,7,8-HpCDF.......     109719-84-8
1,2,3,4,7,8,9-HpCDF...........................      55673-89-7  13C12-1,2,3,4,7,8,9-HpCDF.......     109719-94-0
Total-HpCDF...................................      38998-75-3
OCDD..........................................       3268-87-9  13C12-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\
                                                                              ----------------------------------
               CDD/CDF                   Retention time and       Relative                           Extract (pg/
                                      quantitation  reference  retention time  Water (pg/ Solid (ng/ L;
                                                                                L; ppq)    kg; ppt)      ppb)
----------------------------------------------------------------------------------------------------------------
                     Compounds using 13 C12-1,2,3,4-TCDD as the Injection Internal Standard
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½
2,3,7,8-TCDF........................  13 C12-2,3,7,8-TCDF....     0.999-1.003         10          1         0.5

[[Page 259]]

 
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  .........  .........  ...........
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½
                   Compounds using 13 C12-1,2,3,7,8,9-HxCDD as the Injection Internal Standard
ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½ï¿½
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.
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 13C12-1,2,3,6,7,8-HxCDD, and 1,2,3,7,8,9-HxCDD is
  quantified using the averaged responses for 13C12-1,2,3,4,7,8-HxCDD and 13C12-1,2,3,6,7,8-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 \3\  solution \4\
                                                          solution \1\  solution \2\     (ng/mL)       (ng/mL)
                                                             (ng/mL)       (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
13C12-2,3,7,8-TCDD......................................         100               2  ............  ............

[[Page 260]]

 
13C12-2,3,7,8-TCDF......................................         100               2  ............  ............
13C12-1,2,3,7,8-PeCDD...................................         100               2  ............  ............
13C12-1,2,3,7,8-PeCDF...................................         100               2  ............  ............
13C12-2,3,4,7,8-PeCDF...................................         100               2  ............  ............
13C12-1,2,3,4,7,8-HxCDD.................................         100               2  ............  ............
13C12-1,2,3,6,7,8-HxCDD.................................         100               2  ............  ............
13C12-1,2,3,4,7,8-HxCDF.................................         100               2  ............  ............
13C12-1,2,3,6,7,8-HxCDF.................................         100               2  ............  ............
13C12-1,2,3,7,8,9-HxCDF.................................         100               2  ............  ............
13C12-2,3,4,6,7,8-HxCDF.................................         100               2  ............  ............
13C12-1,2,3,4,6,7,8-HpCDD...............................         100               2  ............  ............
13C12-1,2,3,4,6,7,8-HpCDF...............................         100               2  ............  ............
13C12-1,2,3,4,7,8,9-HpCDF...............................         100               2  ............  ............
13C12-OCDD..............................................         200               4  ............  ............
Cleanup Standard \5\
    37Cl4-2,3,7,8-TCDD..................................           0.8  ............  ............  ............
Internal Standards \6\
    13C12-1,2,3,4-TCDD..................................         200    ............  ............  ............
    13C12-1,2,3,7,8,9-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.
\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)
----------------------------------------------------------------------------------------------------------------
                                                               CS2  (ng/    CS3  (ng/    CS4  (ng/    CS5  (ng/
                                                   CDD/CDF        mL)          mL)          mL)          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:

[[Page 261]]

 
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
 


              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
13C12-2,3,7,8-TCDD.........................          100          37     28-134        20-175        82-121
13C12-2,3,7,8-TCDF.........................          100          35     31-113        22-152        71-140
13C12-1,2,3,7,8-PeCDD......................          100          39     27-184        21-227        62-160
13C12-1,2,3,7,8-PeCDF......................          100          34     27-156        21-192        76-130
13C12-2,3,4,7,8-PeCDF......................          100          38     16-279        13-328        77-130
13C12-1,2,3,4,7,8-HxCDD....................          100          41     29-147        21-193        85-117
13C12-1,2,3,6,7,8-HxCDD....................          100          38     34-122        25-163        85-118
13C12-1,2,3,4,7,8-HxCDF....................          100          43     27-152        19-202        76-131
13C12-1,2,3,6,7,8-HxCDF....................          100          35     30-122        21-159        70-143
13C12-1,2,3,7,8,9-HxCDF....................          100          40     24-157        17-205        74-135
13C12-2,3,4,6,7,8,-HxCDF...................          100          37     29-136        22-176        73-137
13C12-1,2,3,4,6,7,8-HpCDD..................          100          35     34-129        26-166        72-138
13C12-1,2,3,4,6,7,8-HpCDF..................          100          41     32-110        21-158        78-129

[[Page 262]]

 
13C12-1,2,3,4,7,8,9-HpCDF..................          100          40     28-141        20-186        77-129
13C12-OCDD.................................          200          95     41-276        26-397        96-415
37Cl4-2,3,7,8-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 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
13C12-2,3,7,8-TCDD..........................          100           35   32-115        25-141        85-117
13C12-2,3,7,8-TCDF..........................          100           34    35-99        26-126        76-131
37Cl4-2,3,7,8-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 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
                                   Test conc.           recovery
            Compound                (ng/mL)   --------------------------
                                                 (ng/mL) 1       (%)
------------------------------------------------------------------------
13C12-2,3,7,8-TCDD..............          100   25-164            25-164
13C12-2,3,7,8-TCDF..............          100   24-169            24-169
13C12-1,2,3,7,8-PeCDD...........          100   25-181            25-181
13C12-1,2,3,7,8-PeCDF...........          100   24-185            24-185
13C12-2,3,4,7,8-PeCDF...........          100   21-178            21-178
13C12-1,2,3,4,7,8-HxCDD.........          100   32-141            32-141
13C12-1,2,3,6,7,8-HxCDD.........          100   28-130            28-130
13C12-1,2,3,4,7,8-HxCDF.........          100   26-152            26-152
13C12-1,2,3,6,7,8-HxCDF.........          100   26-123            26-123
13C12-1,2,3,7,8,9-HxCDF.........          100   29-147            29-147
13C12-2,3,4,6,7,8-HxCDF.........          100   28-136            28-136
13C12-1,2,3,4,6,7,8-HpCDD.......          100   23-140            23-140
13C12-1,2,3,4,6,7,8-HpCDF.......          100   28-143            28-143
13C12-1,2,3,4,7,8,9-HpCDF.......          100   26-138            26-138
13C12-OCDD......................          200   34-313            17-157
37Cl4-2,3,7,8-TCDD..............           10  3.5-19.7           35-197
------------------------------------------------------------------------
1 Specification given as concentration in the final extract, assuming a
  20-L volume.


     Table 7a.--Labeled Compound Recovery in Samples When Only Tetra
                          Compounds are Tested
------------------------------------------------------------------------
                                                    Labeled compound
                                   Test conc.           recovery
            Compound                (ng/mL)   --------------------------
                                                (ng/mL) \1\      (%)
------------------------------------------------------------------------
13C12-2,3,7,8-TCDD..............          100   31-137            31-137
13C12-2,3,7,8-TCDF..............          100   29-140            29-140
37Cl4-2,3,7,8-TCDD..............           10  4.2-16.4           42-164
------------------------------------------------------------------------
\1\ Specification given as concentration in the final extract, assuming
  a 20 L volume.


[[Page 263]]


         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                          C12H435Cl4O..............  TCDF
                              305.8987  M=2                        C12H435Cl337ClO..........  TCDF
                              315.9419  M                          13C12H435Cl4O............  TCDF \3\
                              317.9389  M=2                        13C12H435Cl337ClO........  TCDF \3\
                              319.8965  M                          C12H435Cl4O2.............  TCDD
                              321.8936  M=2                        C12H435Cl337ClO2.........  TCDD
                              327.8847  M                          C12H437Cl4O2.............  TCDD \4\
                              330.9792  QC                         C7F13....................  PFK
                              331.9368  M                          13C12H435Cl4O2...........  TCDD \3\
                              333.9339  M=2                        13C12H435Cl337ClO2.......  TCDD \3\
                              375.8364  M=2                        C12H435Cl537ClO..........  HxCDPE
2........................     339.8597  M=2                        C12H335Cl437ClO..........  PeCDF
                              341.8567  M=4                        C12H335Cl337Cl2O.........  PeCDF
                              351.9000  M=2                        13C12H335Cl437ClO........  PeCDF
                              353.8970  M=4                        13C12H335Cl337Cl2O.......  PeCDF \3\
                              354.9792  Lock                       C9F13....................  PFK
                              355.8546  M=2                        C12H335Cl437ClO2.........  PeCDD
                              357.8516  M=4                        C12H335Cl337Cl2O2........  PeCDD
                              367.8949  M=2                        13C12H335Cl437ClO2.......  PeCDD \3\
                              369.8919  M=4                        13C12H335Cl337Cl2O2......  PeCDD \3\
                              409.7974  M=2                        C12H335Cl637ClO..........  HpCDPE
3........................     373.8208  M=2                        C12H235Cl537ClO..........  HxCDF
                              375.8178  M=4                        C12H235Cl437Cl2O.........  HxCDF
                              383.8639  M                          13C12H235Cl6O............  HxCDF \3\
                              385.8610  M=2                        13C12H235Cl537ClO........  HxCDF \3\
                              389.8157  M=2                        C12H235Cl537ClO2.........  HxCDD
                              391.8127  M=4                        C12H235Cl437Cl2O2........  HxCDD
                              392.9760  Lock                       C9F15....................  PFK
                              401.8559  M=2                        13C12H235Cl537ClO2.......  HxCDD \3\
                              403.8529  M=4                        13C12H235Cl437Cl2O2......  HxCDD \3\
                              430.9729  QC                         C9F17....................  PFK
                              445.7555  M=4                        C12H235Cl637Cl2O.........  OCDPE
4........................     407.7818  M=2                        C12H35Cl637ClO...........  HpCDF
                              409.7789  M=4                        C12H35Cl537Cl2O..........  HpCDF
                              417.8253  M                          13C12H35Cl7O.............  HpCDF \3\
                              419.8220  M=2                        13C12H35Cl637ClO.........  HpCDF \3\
                              423.7766  M=2                        C12H35Cl637ClO2..........  HpCDD
                              425.7737  M=4                        C12H35Cl537Cl2O2.........  HpCDD
                              430.9729  Lock                       C9F17....................  PFK
                              435.8169  M=2                        13C12H35Cl637ClO2........  HpCDD \3\
                              437.8140  M=4                        13C12H35Cl537Cl2O2.......  HpCDD \3\
                              479.7165  M=4                        C12H35Cl737Cl2O..........  NCDPE
5........................     441.7428  M=2                        C1235Cl737ClO............  OCDF
                              442.9728  Lock                       C10F17...................  PFK
                              443.7399  M=4                        C1235Cl637Cl2O...........  OCDF
                              457.7377  M=2                        C1235Cl737ClO2...........  OCDD
                              459.7348  M=4                        C1235Cl637Cl2O2..........  OCDD
                              469.7779  M=2                        13C1235Cl737ClO2.........  OCDD\3\
                              471.7750  M=4                        13C1235Cl637Cl2O2........  OCDD\3\
                              513.6775  M=4                        C1235Cl837Cl2O...........  DCDPE
----------------------------------------------------------------------------------------------------------------
\1\ Nuclidic masses used:
  H = 1.007825.
  O = 15.994915.
  C = 12.00000.
  35Cl = 34.968853.
  13C = 13.003355.
  37Cl = 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.

[[Page 264]]

 
  NCDPE = Nonachlorodiphenyl ether.
  PFK = Perfluorokerosene.
\3\ Labeled compound.
\4\ There is only one m/z for 37Cl4-2,3,7,8,-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 37Cl4-2,3,7,8-TCDD (cleanup standard).
\3\ Used for 13C12-HxCDF only.
\4\ Used for 13C12-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         ..............  ....................  .................
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
L--microliter
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 272]]

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 273]]

    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.

[[Page 274]]

                               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 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 (g/
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 L spike 
into each 5 mL sample, blank, or aqueous standard analyzed will result 
in a concentration of 20 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 g/L 
may be used. Include the internal standards (Section 7.5) in this 
solution so that a concentration of 20 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 
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 L syringe, 
add 20 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 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 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 g/L 
of the labeled and pollutant gases and water soluble compounds, 10 
g/L BFB, and 20 g/L of all other pollutants, labeled 
compounds, and internal standards. It may be the nominal 20 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 g/mL or 500 g/mL of 
the gases and water soluble compounds, and 100 g/mL of the 
remaining pollutants

[[Page 276]]

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 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 (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 Rx>Ry. 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 277]]


    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 278]]

    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 g/L and the standard 
deviation of the recovery (s) in 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 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 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 
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 279]]

            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 280]]

    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

[[Page 281]]

calibration curve given in Figure 5 indicates a concentration of 31.8 
g/L.
    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 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 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

[[Page 282]]

 
Bromodichloromethane.........     32101      75-27-4     048 V     012 V
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    (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

[[Page 283]]

 
286  Toluene-d8...........................  183     1603           10
386  Toluene..............................  286     1619           10
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 C, 8 C per min to 240 C,
  hold at 240 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 g/L
                                                        --------------------------------------------------------
                                                             Initial precision and       Labeled      On-going
                                                            accuracy section 8.2.3       compound     accuracy
                        Compound                        ------------------------------   recovery     sec. 11.5
                                                                                         sec. 8.3  -------------
                                                          s (g/    and 14.2    R (g/L)           L)       -------------    m>g/L)
                                                                                       P (percent)
----------------------------------------------------------------------------------------------------------------
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

[[Page 284]]

 
Trans-1,2-dichloroethene...............................           7.4       10.5-31.5       15-195          8-34
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.
 
Note 1: Specifications not available for these compounds at time of release of this method.
Note 2: Specifications not developed for these compounds; use method 603.


[[Page 285]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.055


[[Page 286]]

[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 287]]

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 
-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 288]]

    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--305 m x 0.250.02 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 calibration (Section 7) and calibration verification (12.5) 
require high

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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 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 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 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 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 g/mL 
of the pollutants and a constant nominal 100 g/mL of the 
labeled compounds. Spike each solution with 10 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 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 sensitivity 
problems (Section 15.4). The 20 ug/mL calibration standard (Section 
6.13) can be used to demonstrate this performance.

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    7.3.1  Polar compound detection--demonstrate that unlabeled 
pentachlorophenol and benzidine are detectable at the 50 g/mL 
level (per all criteria in Section 13). The 50 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 Rx> Ry. 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 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 
(g/mL)
    Cs is the concentration of the compound in the daily 
standard (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 g/mL. The amount of 
internal standard added to each extract is the same (100 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 
point calibration range, an averaged response factor may be used for 
that compound; otherwise, the complete calibration

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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 
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 g/mL and the standard deviation of the 
recovery (s) in g/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 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)

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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 
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.

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    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 
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 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

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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 295]]

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 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(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 
(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 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 
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 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 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 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 296]]

    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 297]]

 
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.\1\                         Compound                           Mean                              (g/
                                                                  (sec)    EGD Ref     Relative          L)
----------------------------------------------------------------------------------------------------------------
   164  2,2-difluorobiphenyl (int std)........................      1163       164     1.000-1.000          10
   061  N-nitrosodimethylamine................................       385       164        ns                50
   603  alpha picoline-d7.....................................       417       164     0.326-0.393          50
   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-chloroethyl) ether-d8...........................       696       164     0.584-0.607          10
   318  bis(2-chloroethyl) ether..............................       704       218     1.007-1.016          10
   617  n-decane-d22..........................................       698       164     0.585-0.615          10
   717  n-decane..............................................       720       617     1.022-1.038          10
   226  1,3-dichlorobenzene-d4................................       722       164     0.605-0.636          10
   326  1,3-dichlorobenzene...................................       724       226     0.998-1.008          10
   227  1,4-dichlorobenzene-d4................................       737       164     0.601-0.666          10
   327  1,4-dichlorobenzene...................................       740       227     0.997-1.009          10
   225  1,2-dichlorobenzene-d4................................       758       164     0.632-0.667          10
   325  1,2-dichlorobenzene...................................       760       225     0.995-1.008          10
   242  bis(2-chloroisopropyl) ether-d12......................       788       164     0.664-0.691          10
   342  bis(2-chloroisopropyl) ether..........................       799       242     1.010-1.016          10
   212  hexachloroethane-13C..................................       819       164     0.690-0.717          10
   312  hexachloroethane......................................       823       212     0.999-1.001          10
   063  N-nitrosodi-n-propylamine.............................       830       164        ns                20
   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 phenol-d3................................       921       164     0.781-0.803          10
   334  2,4-dimethylphenol....................................       924       234     0.999-1.003          10
   043  bis(2-chloroethoxy) methane...........................       939       164        ns                10
   208  1,2,4-trichlorobenzene-d3.............................       955       164     0.813-0.830          10
   308  1,2,4-trichlorobenzene................................       958       208     1.000-1.005          10
   255  naphthalene-d8........................................       963       164     0.819-0.836          10
   355  naphthalene...........................................       967       255     1.001-1.006          10
   609  alpha-terpineol-d3....................................       973       164     0.829-0.844          10

[[Page 298]]

 
   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-trichlorobenzene................................      1003       164        ns                10
   252  hexachlorobutadiene-13C4..............................      1005       164     0.856-0.871          10
   352  hexachlorobutadiene...................................      1006       252     0.999-1.002          10
   253  hexachlorocyclopentadiene-13C4........................      1147       164     0.976-0.986          10
   353  hexachlorocyclopentadiene.............................      1142       253     0.999-1.001          10
   220  2-chloronaphthalene-d7................................      1185       164     1.014-1.024          10
   320  2-chloronaphthalene...................................      1200       220     0.997-1.007          10
   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-d10....................................      1211       164     1.036-1.047          10
   708  Diphenyl ether........................................      1216       608     0.997-1.009          10
   277  Acenaphthylene-d8.....................................      1265       164     1.080-1.095          10
   377  Acenaphthylene........................................      1247       277     1.000-1.004          10
   271  Dimethyl phthalate-d4.................................      1269       164     1.083-1.102          10
   371  Dimethyl phthalate....................................      1273       271     0.998-1.005          10
   236  2,6-dinitrotoluene-d3.................................      1283       164     1.090-1.112          10
   336  2,6-dinitrotoluene....................................      1300       236     1.001-1.005          10
   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-naphthylamine-d7.................................      1368       164     1.163-1.189          50
   702  Beta-naphthylamine....................................      1371       602     0.996-1.007          50
   280  Fluorene-d10..........................................      1395       164     1.185-1.214          10
   380  Fluorene..............................................      1401       281     0.999-1.008          10
   240  4-chlorophenyl phenyl ether-d5........................      1406       164     1.194-1.223          10
   340  4-chlorophenyl phenyl ether...........................      1409       240     0.990-1.015          10
   270  Diethyl phthalate-d4..................................      1409       164     1.197-1.229          10
   370  Diethyl phthalate.....................................      1414       270     0.996-1.006          10
   619  n-hexadecane-d34......................................      1447       164     1.010-1.478          10
   719  n-hexadecane..........................................      1469       619     1.013-1.020          10
   235  2,4-dinitrotoluene-d3.................................      1359       164     1.152-1.181          10
   335  2,4-dinitrotoluene....................................      1344       235     1.000-1.002          10
   237  1,2-diphenylhydrazine-d8..............................      1433       164     1.216-1.248          20
   337  1,2-diphenylhydrazine (\3\)...........................      1439       237     0.999-1.009          20
   607  Diphenylamine-d10.....................................      1437       164     1.213-1.249          20
   707  Diphenylamine.........................................      1439       607     1.000-1.007          20
   262  N-nitrosodiphenylamine-d6.............................      1447       164     1.225-1.252          20
   362  N-nitrosodiphenylamine (\4\)..........................      1464       262     1.000-1.002          20
   041  4-bromophenyl phenyl ether............................      1498       164     1.271-1.307          10
   209  Hexachlorobenzene-13C6................................      1521       164     1.288-1.327          10
   309  Hexachlorobenzene.....................................      1522       209     0.999-1.001          10
   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-d8...................................      1559       164     1.314-1.361          10
   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 phthalate-d4...............................      1719       164     1.446-1.510          10
   368  Di-n-butyl phthalate..................................      1723       268     1.000-1.003          10
   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-d50.....................................      1997       164     1.671-1.764          10
   723  n-tetracosane.........................................      2025       612     1.012-1.015          10
   067  Butylbenzyl phthalate.................................      2060       164        ns                10
   276  Chrysene-d12..........................................      2081       164     1.743-1.837          10
   376  Chrysene..............................................      2083       276     1.000-1.004          10

[[Page 299]]

 
   272  Benzo(a)anthracene-d12................................      2082       164     1.735-1.846          10
   372  Benzo(a)anthracene....................................      2090       272     0.999-1.007          10
   228  3,3-dichlorobenzidine-d6..............................      2088       164     1.744-1.848          50
   328  3,3-dichlorobenzidine.................................      2086       228     1.000-1.001          50
   266  Bis(2-ethylhexyl) phthalate-d4........................      2123       164     1.771-1.880          10
   366  Bis(2-ethylhexyl) phthalate...........................      2124       266     1.000-1.002          10
   524  n-hexacosane..........................................      2147       164        ns                10
   269  di-n-octyl phthalate-d4...............................      2239       164     1.867-1.982          10
   369  di-n-octyl phthalate..................................      2240       269     1.000-1.002          10
   525  n-octacosane..........................................      2272       164        ns                10
   274  Benzo(b)fluoranthene-d12..............................      2281       164     1.902-2.025          10
   354  Benzo(b)fluoranthene..................................      2293       274     1.000-1.005          10
   275  Benzo(k)fluoranthene-d12..............................      2287       164     1.906-2.033          10
   375  Benzo(k)fluoranthene..................................      2293       275     1.000-1.005          10
   273  Benzo(a)pyrene-d12....................................      2351       164     1.954-2.088          10
   373  Benzo(a)pyrene........................................      2350       273     1.000-1.004          10
   626  N-triacontane-d62.....................................      2384       164     1.972-2.127          10
   726  N-triacontane.........................................      2429       626     1.011-1.028          10
   083  Indeno(1,2,3-cd)pyrene................................      2650       164        ns                20
   082  Dibenzo(a,h)anthracene................................      2660       164        ns                20
   279  Benzo(ghi)perylene-d12................................      2741       164     2.187-2.524          20
   379  Benzo(ghi)perylene....................................      2750       279     1.001-1.006          20
----------------------------------------------------------------------------------------------------------------
\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 C; 30 - 280 C at 8 C per min; isothermal at 280 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. 1                         Compound                           Mean                              (g/
                                                                  (sec)    EGD Ref     Relative          L)
----------------------------------------------------------------------------------------------------------------
   164  2,2'-difluorobiphenyl (int std).......................      1163       164     1.000-1.000          10
   224  2-chlorophenol-d4.....................................       701       164     0.587-0.618          10
   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-dichlorophenol-d3.................................       944       164     0.802-0.822          10
   331  2,4-dichlorophenol....................................       947       231     0.997-1.006          10
   222  4-chloro-3-methylphenol-d2............................      1086       164     0.930-0.943          10
   322  4-chloro-3-methylphenol...............................      1091       222     0.998-1.003          10
   221  2,4,6-trichlorophenol-d2..............................      1162       164     0.994-1.005          10
   321  2,4,6-trichlorophenol.................................      1165       221     0.998-1.004          10
   531  2,4,5-trichlorophenol.................................      1170       164        ns                10
   530  2,3,6-trichlorophenol.................................      1195       164        ns                10
   259  2,4-dinitrophenol-d3..................................      1323       164     1.127-1.149          50
   359  2,4-dinitrophenol.....................................      1325       259     1.000-1.005          50
   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-dinitrophenol-d2.........................      1433       164     1.216-1.249          20
   360  2-methyl-4,6-dinitrophenol............................      1435       260     1.000-1.002          20
   264  Pentachlorophenol-13C6................................      1559       164     1.320-1.363          50
   364  Pentachlorophenol.....................................      1561       264     0.998-1.002          50
----------------------------------------------------------------------------------------------------------------
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: 302m x 0.250.02mm i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase fused silica
  capillary.
Temperature program: 5 min at 30 C; 8  deg.C/min. to 250C or until pentachlorophenol elutes.
Gas velocity: 305 cm/sec.


[[Page 300]]


              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 77--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
                                              ------------------------------------------------------------------
                                               Initial precision and      Labeled      Calibration    On-going
  EGD                  Compound                   accuracy section       compound     verification    accuracy
 No.1                                           8.2.3 (g/L)   recovery sec.    sec. 12.5    sec. 11.6 R
                                              ----------------------- 8.3 and 14.2 P  (g/  (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 301]]

 
   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 302]]

 
   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 303]]

 
   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 304]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.057


[[Page 305]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.058


[[Page 306]]

[GRAPHIC] [TIFF OMITTED] TC02JY92.059

[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]

[[Page 307]]

 Appendix B to Part 136--Definition and Procedure for the Determination 
              of the Method Detection Limit--Revision 1.11

                               Definition

    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 analyte concentration is greater than zero and is 
determined from analysis of a sample in a given matrix containing the 
analyte.

                          Scope and Application

    This procedure is designed for applicability to a wide variety of 
sample types ranging from reagent (blank) water containing analyte to 
wastewater containing analyte. The MDL for an analytical procedure may 
vary as a function of sample type. The procedure requires a complete, 
specific, and well defined analytical method. It is essential that all 
sample processing steps of the analytical method be included in the 
determination of the method detection limit.
    The MDL obtained by this procedure is used to judge the significance 
of a single measurement of a future sample.
    The MDL procedure was designed for applicability to a broad variety 
of physical and chemical methods. To accomplish this, the procedure was 
made device- or instrument-independent.

                                Procedure

    1. Make an estimate of the detection limit using one of the 
following:
    (a) The concentration value that corresponds to an instrument 
signal/noise in the range of 2.5 to 5.
    (b) The concentration equivalent of three times the standard 
deviation of replicate instrumental measurements of the analyte in 
reagent water.
    (c) That region of the standard curve where there is a significant 
change in sensitivity, i.e., a break in the slope of the standard curve.
    (d) Instrumental limitations.
    It is recognized that the experience of the analyst is important to 
this process. However, the analyst must include the above considerations 
in the initial estimate of the detection limit.
    2. Prepare reagent (blank) water that is as free of analyte as 
possible. Reagent or interference free water is defined as a water 
sample in which analyte and interferent concentrations are not detected 
at the method detection limit of each analyte of interest. Interferences 
are defined as systematic errors in the measured analytical signal of an 
established procedure caused by the presence of interfering species 
(interferent). The interferent concentration is presupposed to be 
normally distributed in representative samples of a given matrix.
    3. (a) If the MDL is to be determined in reagent (blank) water, 
prepare a laboratory standard (analyte in reagent water) at a 
concentration which is at least equal to or in the same concentration 
range as the estimated method detection limit. (Recommend between 1 and 
5 times the estimated method detection limit.) Proceed to Step 4.
    (b) If the MDL is to be determined in another sample matrix, analyze 
the sample. If the measured level of the analyte is in the recommended 
range of one to five times the estimated detection limit, proceed to 
Step 4.
    If the measured level of analyte is less than the estimated 
detection limit, add a known amount of analyte to bring the level of 
analyte between one and five times the estimated detection limit.
    If the measured level of analyte is greater than five times the 
estimated detection limit, there are two options.
    (1) Obtain another sample with a lower level of analyte in the same 
matrix if possible.
    (2) The sample may be used as is for determining the method 
detection limit if the analyte level does not exceed 10 times the MDL of 
the analyte in reagent water. The variance of the analytical method 
changes as the analyte concentration increases from the MDL, hence the 
MDL determined under these circumstances may not truly reflect method 
variance at lower analyte concentrations.
    4. (a) Take a minimum of seven aliquots of the sample to be used to 
calculate the method detection limit and process each through the entire 
analytical method. Make all computations according to the defined method 
with final results in the method reporting units. If a blank measurement 
is required to calculate the measured level of analyte, obtain a 
separate blank measurement for each sample aliquot analyzed. The average 
blank measurement is subtracted from the respective sample measurements.
    (b) It may be economically and technically desirable to evaluate the 
estimated method detection limit before proceeding with 4a. This will: 
(1) Prevent repeating this entire procedure when the costs of analyses 
are high and (2) insure that the procedure is being conducted at the 
correct concentration. It is quite possible that an inflated MDL will be 
calculated from data obtained at many times the real MDL even though the 
level of analyte is less than five times the calculated method detection 
limit. To insure that the estimate of the method detection limit is a 
good estimate, it is necessary to determine that a lower concentration 
of analyte will not result in a significantly lower method detection 
limit. Take two aliquots of the sample to be used to calculate the 
method detection limit and process each

[[Page 308]]

through the entire method, including blank measurements as described 
above in 4a. Evaluate these data:
    (1) If these measurements indicate the sample is in desirable range 
for determination of the MDL, take five additional aliquots and proceed. 
Use all seven measurements for calculation of the MDL.
    (2) If these measurements indicate the sample is not in correct 
range, reestimate the MDL, obtain new sample as in 3 and repeat either 
4a or 4b.
    5. Calculate the variance (S2) and standard deviation (S) 
of the replicate measurements, as follows:
[GRAPHIC] [TIFF OMITTED] TC15NO91.208

where:

X; i=1 to n, are the analytical results in the final method 
          reporting units obtained from the n sample aliquots and 
           refers to the sum of the X values from i=l to n.
    6. (a) Compute the MDL as follows:

        MDL = t(n-1,1-=0.99)  (S)

where:
    MDL = the method detection limit
    t(n-1,1-=.99) = the students' t value 
appropriate for a 99% confidence level and a standard deviation estimate 
with n-1 degrees of freedom. See Table.
    S = standard deviation of the replicate analyses.

    (b) The 95% confidence interval estimates for the MDL derived in 6a 
are computed according to the following equations derived from 
percentiles of the chi square over degrees of freedom distribution 
(2/df).
    LCL = 0.64 MDL
    UCL = 2.20 MDL
    where: LCL and UCL are the lower and upper 95% confidence limits 
respectively based on seven aliquots.

    7. Optional iterative procedure to verify the reasonableness of the 
estimate of the MDL and subsequent MDL determinations.
    (a) If this is the initial attempt to compute MDL based on the 
estimate of MDL formulated in Step 1, take the MDL as calculated in Step 
6, spike the matrix at this calculated MDL and proceed through the 
procedure starting with Step 4.
    (b) If this is the second or later iteration of the MDL calculation, 
use S2 from the current MDL calculation and S2 
from the previous MDL calculation to compute the F-ratio. The F-ratio is 
calculated by substituting the larger S2 into the numerator 
S2A and the other into the denominator 
S2B. The computed F-ratio is then compared with 
the F-ratio found in the table which is 3.05 as follows: if 
S2A/S2B<3.05, then compute 
the pooled standard deviation by the following equation:
[GRAPHIC] [TIFF OMITTED] TC15NO91.209

    if S2A/S2B>3.05, respike 
at the most recent calculated MDL and process the samples through the 
procedure starting with Step 4. If the most recent calculated MDL does 
not permit qualitative identification when samples are spiked at that 
level, report the MDL as a concentration between the current and 
previous MDL which permits qualitative identification.

    (c) Use the Spooled as calculated in 7b to compute The 
final MDL according to the following equation:

                     MDL=2.681 (Spooled)

where 2.681 is equal to 
t(12,1-=.99).
    (d) The 95% confidence limits for MDL derived in 7c are computed 
according to the following equations derived from precentiles

[[Page 309]]

of the chi squared over degrees of freedom distribution.
    LCL=0.72 MDL
    UCL=1.65 MDL
where LCL and UCL are the lower and upper 95% confidence limits 
respectively based on 14 aliquots.

     Tables of Students' t Values at the 99 Percent Confidence Level
------------------------------------------------------------------------
                                                   Degrees
                                                      of
              Number of replicates                 freedom    tcn-1,.99)
                                                    (n-1)
------------------------------------------------------------------------
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
61..............................................         60        2.390
00..............................................         00        2.326
------------------------------------------------------------------------

                                Reporting

    The analytical method used must be specifically identified by number 
or title ald the MDL for each analyte expressed in the appropriate 
method reporting units. If the analytical method permits options which 
affect the method detection limit, these conditions must be specified 
with the MDL value. The sample matrix used to determine the MDL must 
also be identified with MDL value. Report the mean analyte level with 
the MDL and indicate if the MDL procedure was iterated. If a laboratory 
standard or a sample that contained a known amount analyte was used for 
this determination, also report the mean recovery.
    If the level of analyte in the sample was below the determined MDL 
or exceeds 10 times the MDL of the analyte in reagent water, do not 
report a value for the MDL.

[49 FR 43430, Oct. 26, 1984; 50 FR 694, 696, Jan. 4, 1985, as amended at 
51 FR 23703, June 30, 1986]

  Appendix C to Part 136--Inductively Coupled Plasma--Atomic Emission 
  Spectrometric Method for Trace Element Analysis of Water and Wastes 
                              Method 200.7

                        1. Scope and Application

    1.1  This method may be used for the determination of dissolved, 
suspended, or total elements in drinking water, surface water, and 
domestic and industrial wastewaters.
    1.2  Dissolved elements are determined in filtered and acidified 
samples. Appropriate steps must be taken in all analyses to ensure that 
potential interferences are taken into account. This is especially true 
when dissolved solids exceed 1500 mg/L. (See Section 5.)
    1.3  Total elements are determined after appropriate digestion 
procedures are performed. Since digestion techniques increase the 
dissolved solids content of the samples, appropriate steps must be taken 
to correct for potential interference effects. (See Section 5.)
    1.4  Table 1 lists elements for which this method applies along with 
recommended wavelengths and typical estimated instrumental detection 
limits using conventional pneumatic nebulization. Actual working 
detection limits are sample dependent and as the sample matrix varies, 
these concentrations may also vary. In time, other elements may be added 
as more information becomes available and as required.
    1.5  Because of the differences between various makes and models of 
satisfactory instruments, no detailed instrumental operating 
instructions can be provided. Instead, the analyst is referred to the 
instruction provided by the manufacturer of the particular instrument.

                          2. Summary of Method

    2.1  The method describes a technique for the simultaneous or 
sequential multielement determination of trace elements in solution. The 
basis of the method is the measurement of atomic emission by an optical 
spectroscopic technique. Samples are nebulized and the aerosol that is 
produced is transported to the plasma torch where excitation occurs. 
Characteristic atomic-line emission spectra are produced by a radio-
frequency inductively coupled plasma (ICP). The spectra are dispersed by 
a grating spectrometer and the intensities of the lines are monitored by 
photomultiplier tubes. The photocurrents from the photomultiplier tubes 
are processed and controlled by a computer system. A background 
correction technique is required to compensate for variable background 
contribution to the determination of trace elements. Background must be 
measured adjacent to analyte lines on samples during analysis. The 
position selected for the background intensity measurement, on either or 
both sides of the analytical line, will be determined by the complexity 
of the spectrum adjacent to the analyte line. The position used must be 
free of spectral interference and reflect the same change in background 
intensity as occurs at the analyte wavelength measured. Background 
correction is not required in cases of line broadening where a 
background correction measurement would actually degrade the analytical 
result. The possibility of additional interferences named in 5.1 (and 
tests for their presence as described in 5.2) should also be recognized 
and appropriate corrections made.

[[Page 310]]

                             3. Definitions

    3.1  Dissolved--Those elements which will pass through a 0.45 
m membrane filter.
    3.2  Suspended--Those elements which are retained by a 0.45 
m membrane filter.
    3.3  Total--The concentration determined on an unfiltered sample 
following vigorous digestion (Section 9.3), or the sum of the dissolved 
plus suspended concentrations. (Section 9.1 plus 9.2).
    3.4  Total recoverable--The concentration determined on an 
unfiltered sample following treatment with hot, dilute mineral acid 
(Section 9.4).
    3.5  Instrumental detection limit--The concentration equivalent to a 
signal, due to the analyte, which is equal to three times the standard 
deviation of a series of ten replicate measurements of a reagent blank 
signal at the same wavelength.
    3.6  Sensitivity--The slope of the analytical curve, i.e. functional 
relationship between emission intensity and concentration.
    3.7  Instrument check standard--A multielement standard of known 
concentrations prepared by the analyst to monitor and verify instrument 
performance on a daily basis. (See 7.6.1)
    3.8  Interference check sample--A solution containing both 
interfering and analyte elemelts of known concentration that can be used 
to verify background and interelement correction factors. (See 7.6.2.)
    3.9  Quality control sample--A solution obtained from an outside 
source having known, concentration values to be used to verify the 
calibration standards. (See 7.6.3)
    3.10  Calibration standards--A series of known standard solutions 
used by the analyst for calibration of the instrument (i.e., preparation 
of the analytical curve). (See 7.4)
    3.11  Linear dynamic range--The concentration range over which the 
analytical curve remains linear.
    3.12  Reagent blank--A volume of deionized, distilled water 
containing the same acid matrix as the calibration standards carried 
through the entire analytical scheme. (See 7.5.2)
    3.13  Calibration blank--A volume of deionized, distilled water 
acidified with HNO3 and HCl. (See 7.5.1)
    3.14  Methmd of standard addition-- The standard addition technique 
involves the use of the unknown and the unknown plus a known amount of 
standard. (See 10.6.1.)

                                4. Safety

    4.1  The toxicity of 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 repsonsible 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 
(14.7,14.8and14.9) for the information of the analyst.

                            5. Interferences

    5.1  Several types of interference effects may contribute to 
inaccuracies in the determination of trace elements. They can be 
summarized as follows:
    5.1.1  Spectral interferences can be categorized as (1) overlap of a 
spectral line from another element; (2) unresolved overlap of molecular 
band spectra; (3) background contribution from continuous or 
recombination phenomena; and (4) background contribution from stray 
light from the line emission of high concentration elements. The first 
of these effects can be compensated by utilizing a computer correction 
of the raw data, requiring the monitoring and measurement of the 
interfering element. The second effect may require selection of an 
alternate wavelength. The third and fourth effects can usually be 
compensated by a background correction adjacent to the analyte line. In 
addition, users of simultaneous multi-element instrumentation must 
assume the responsibility of verifying the absence of spectral 
interference from an element that could occur in a sample but for which 
there is no channel in the instrument array. Listed in Table 2 are some 
interference effects for the recommended wavelengths given in Table 1. 
The data in Table 2 are intended for use only as a rudimentary guide for 
the indication of potential spectral interferences. For this purpose, 
linear relations between concentration and intensity for the analytes 
and the interferents can be assumed. The Interference information, which 
was collected at the Ames Laboratory,1 is expressed as 
analyte concentration equivalents (i.e. false analyte concentrations) 
arising from 100 mg/L of the interferent element. The suggested use of 
this information is as follows: Assume that arsenic (at 193.696 nm) is 
to be determined in a sample containing approximately 10 mg/L of 
aluminum. According to Table 2, 100 mg/L of aluminum would yield a false 
signal for arsenic equivalent to approximately 1.3 mg/L. Therefore, 10 
mg/L of aluminum would result in a false signal for arsenic equivalent 
to approximately 0.13 mg/L. The reader is cautioned that other 
analytical systems may exhibit somewhat different levels of interference 
than those shown in Table

[[Page 311]]

2, and that the interference effects must be evaluated for each 
individual system.
---------------------------------------------------------------------------

    \1\ Ames Laboratory, USDOE, Iowa State University, Ames Iowa 50011.
---------------------------------------------------------------------------

    Only those interferents listed were investigated and the blank 
spaces in Table 2 indicate that measurable interferences were not 
observed for the interferent concentrations listed in Table 3. 
Generally, interferences were discernible if they produced peaks or 
background shifts corresponding to 2-5% of the peaks generated by the 
analyte concentrations also listed in Table 3.
    At present, information on the listed silver and potassium 
wavelengths are not available but it has been reported that second order 
energy from the magnesium 383.231 nm wavelength interferes with the 
listed potassium line at 766.491 nm.
    5.1.2  Physical interferences are generally considered to be effects 
associated with the sample nebulization and transport processes. Such 
properties as change in viscosity and surface tension can cause 
significant inaccuracies especially in samples which may contain high 
dissolved solids and/or acid concentrations. The use of a peristaltic 
pump may lessen these interferences. If these types of interferences are 
operative, they must be reduced by dilution of the sample and/or 
utilization of standard addition techniques. Another problem which can 
occur from high dissolved solids is salt buildup at the tip of the 
nebulizer. This affects aersol flow rate causing instrumental drift. 
Wetting the argon prior to nebulization, the use of a tip washer, or 
sample dilution have been used to control this problem. Also, it has 
been reported that better control of the argon flow rate improves 
instrument performance. This is accomplished with the use of mass flow 
controllers.
    5.1.3  Chemical Interferences are characterized by molecular 
compound formation, ionization effects and solute vaporization effects. 
Normally these effects are not pronounced with the ICP technique, 
however, if observed they can be minimized by careful selection of 
operating conditions (that is, incident power, observation position, and 
so forth), by buffering of the sample, by matrix matching, and by 
standard addition procedures. These types of interferences can be highly 
dependent on matrix type and the specific analyte element.
    5.2  It is recommended that whenever a new or unusual sample matrix 
is encountered, a series of tests be performed prior to reporting 
concentration data for analyte elements. These tests, as outlined in 
5.2.1 through 5.2.4, will ensure the analyst that neither positive nor 
negative interference effects are operative on any of the analyte 
elements thereby distorting the accuracy of the reported values.
    5.2.1  Serial dilution. If the analyte concentration is sufficiently 
high (minimally a factor of 10 above the instrumental detection limit 
after dilution), an analysis of a dilution should agree within 5 percent 
of the original determination (or within some acceptable control limit 
(14.3) that has been established for that matrix.). If not, a chemical 
or physical interference effect should be suspected.
    5.2.2  Spike addition. The recovery of a spike addition added at a 
minimum level of 10X the instrumental detection limit (maximum 100X) to 
the original determination should be recovered to within 90 to 110 
percent or within the established control limit for that matrix. If not, 
a matrix effect should be suspected. The use of a standard addition 
analysis procedure can usually compensate for this effect.
    Caution: The standard addition technique does not detect coincident 
spectral overlap. If suspected, use of computerized compensation, an 
alternate wavelength, or comparison with an alternate method is 
recommended (See 5.2.3).
    5.2.3  Comparison with alternate method of analysis. When 
investigating a new sample matrix, comparison tests may be performed 
with other analytical techniques such as atomic absorption spectrometry, 
or other approved methodology.
    5.2.4  Wavelength scanning of analyte line region. If the 
appropriate equipment is available, wavelength scanning can be performed 
to detect potential spectral interferences.

                              6. Apparatus

    6.1  Inductively Coupled Plasma-Atomic Emission Spectrometer.
    6.1.1  Computer controlled atomic emission spectrometer with 
background correction.
    6.1.2  Radiofrequency generator.
    6.1.3  Argon gas supply, welding grade or better.
    6.2  Operating conditions--Because of the differences between 
various makes and models of satisfactory instruments, no detailed 
operating instructions can be provided. Instead, the analyst should 
follow the instructions provided by the manufacturer of the particular 
instrument. Sensitivity, instrumental detection limit, precision, linear 
dynamic range, and interference effects must be investigated and 
established for each individual analyte line on that particular 
instrument. It is the responsibility of the analyst to verify that the 
instrument configuration and operating conditions used satisfy the 
analytical requirements and to maintain quality control data confirming 
instrument performance and analytical results.

                        7. Reagents and Standards

    7.1  Acids used in the preparation of standards and for sample 
processing must be ultra-high purity grade or equivalent. Redistilled 
acids are acceptable.
    7.1.1  Acetic acid, conc. (sp gr 1.06).

[[Page 312]]

    7.1.2  Hydrochloric acid, conc. (sp gr 1.19).
    7.1.3  Hydrochloric acid, (1+1): Add 500 mL conc. HCl (sp gr 1.19) 
to 400 mL deionized, distilled water and dilute to 1 liter.
    7.1.4  Nitric acid, conc. (sp gr 1.41).
    7.1.5  Nitric acid, (1+1): Add 500 mL conc. HNO3 (sp gr 
1.41) to 400 mL deionized, distilled water and dilute to 1 liter.
    7.2  Deionized, distilled water: Prepare by passing distilled water 
through a mixed bed of cation and anion exchange resins. Use deionized, 
distilled water for the preparation of all reagents, calibration 
standards and as dilution water. The purity of this water must be 
equivalent to ASTM Type II reagent water of Specification D 1193 (14.6).
    7.3  Standard stock solutions may be purchased or prepared from 
ultra high purity grade chemicals or metals. All salts must be dried for 
1 h at 105  deg.C unless otherwise specified.
    (CAUTION: Many metal salts are extremely toxic and may be fatal if 
swallowed. Wash hands thoroughly after handling.)
    Typical stock solution preparation procedures follow:
    7.3.1  Aluminum solution, stock, 1 mL=100g Al: Dissolve 
0.100 g of aluminum metal in an acid mixture of 4 mL of (1+1) HCl and 1 
mL of conc. HNO3 in a beaker. Warm gently to effect solution. 
When solution is complete, transfer quantitatively to a liter flask add 
an additional 10 mL of (1+1) HCl and dilute to 1,000 mL with deionized, 
distilled water.
    7.3.2  Antimony solution stock, 1 mL=100 g Sb: Dissolve 
0.2669 g K(SbO)C4H4O6 in deionized 
distilled water, add 10 mL (1+1) HCl and dilute to 1,000 mL with 
deionized, distilled water.
    7.3.3  Arsenic solution, stock, 1 mL=100 g As: Dissolve 
0.1320 g of As2O3 in 100 mL of deionized, 
distilled water containing 0.4 g NaOH. Acidify the solution with 2 mL 
conc. HNO3 and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.4  Barium solution, stock, 1 mL=100 g Ba: Dissolve 
0.1516 g BaCl2 (dried at 250  deg.C for 2 hrs) in 10 mL 
deionized, distilled water with 1 mL (1+1) HCl. Add 10.0 mL (1+1) HCl 
and dilute to 1,000 with mL deionized, distilled water.
    7.3.5  Beryllium solution, stock, 1 mL=100 g Be: Do not 
dry. Dissolve 1.966 g BeSO44H2O, in 
deionized, distilled water, add 10.0 mL conc. HNO3 and dilute 
to 1,000 mL with deionized, distilled water.
    7.3.6  Boron solution, stock, 1 mL=100g B: Do not dry. 
Dissolve 0.5716 g anhydrous H3BO3 in deionized, 
distilled water and dilute to 1,000 mL. Use a reagent meeting ACS 
specifications, keep the bottle tightly stoppered and store in a 
desiccator to prevent the entrance of atmospheric moisture.
    7.3.7  Cadmium solution, stock, 1 mL=100 g Cd: Dissolve 
0.1142 g CdO in a minimum amount of (1+1) HNO3. Heat to 
increase rate of dissolution. Add 10.0 mL conc. HNO3 and 
dilute to 1,000 mL with deionized, distilled water.
    7.3.8  Calcium solution, stock, 1 mL=100 g Ca: Suspend 
0.2498 g CaCO3 dried at 180  deg.C for 1 h before weighing in 
deionized, distilled water and dissolve cautiously with a minimum amount 
of (1+1) HNO3. Add 10.0 mL conc. HNO3 and dilute 
to 1,000 mL with deionized, distilled water.
    7.3.9  Chromium solution, stock, 1 mL=100 g Cr: Dissolve 
0.1923 g of CrO3 in deionized, distilled water. When solution 
is complete, acidify with 10 mL conc. HNO3 and dilute to 
1,000 mL with deionized, distilled water.
    7.3.10  Cobalt solution, stock, 1 mL=100 g Co: Dissolve 
0.1000 g of cobalt metal in a minimum amount of (1+1) HNO3. 
Add 10.0 mL (1+1) HCl and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.11  Copper solution, stock, 1 mL=100 g Cu: Dissolve 
0.1252 g CuO in a minimum amount of (1+1) HNO3. Add 10.0 mL 
conc. HNO3 and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.12  Iron solution, stock, 1 mL=100 g Fe: Dissolve 
0.1430 g Fe2O3 in a warm mixture of 20 mL (1+1) 
HCl and 2 mL of conc. HNO3. Cool, add an additional 5 mL of 
conc. HNO3 and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.13  Lead solution, stock, 1 mL=100 g Pb: Dissolve 
0.1599 g Pb(NO3)2 in a minimum amount of (1+1) 
HNO3. Add 10.0 mL conc. HNO3 and dilute to 1,000 
mL with deionized, distilled water.
    7.3.14  Magnesium solution, stock, 1 mL=100 g Mg: Dissolve 
0.1658 g MgO in a minimum amount of (1+1) HNO3. Add 10.0 mL 
conc. HNO3 and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.15  Manganese solution, stock, 1 mL=100 g Mn: Dissolve 
0.1000 g of manganese metal in the acid mixture 10 mL conc. HCl and 1 mL 
conc. HNO3, and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.16  Molybdenum solution, stock, 1 mL=100 g Mo: Dissolve 
0.2043 g (NH4)2 MoO4 in deionized, 
distilled water and dilute to 1,000 mL.
    7.3.17  Nickel solution, stock, 1 mL=100 g Ni: Dissolve 
0.1000 g of nickel metal in 10 mL hot conc. HNO3, cool and 
dilute to 1,000 mL with deionized, distilled water.
    7.3.18  Potassium solution, stock, 1 mL=100 g K: Dissolve 
0.1907 g KCl, dried at 110  deg.C, in deionized, distilled water and 
dilute to 1,000 mL.
    7.3.19  Selenium solution, stock, 1 mL=100 g Se: Do not 
dry. Dissolve 0.1727 g H2SeO3 (actual assay 94.6%) 
in deionized, distilled water and dilute to 1,000 mL.
    7.3.20  Silica solution, stock, 1 mL=100 g SiO2: 
Do not dry. Dissolve 0.4730 g 
Na2SiO39H2O in deionized, 
distilled water. Add 10.0 mL conc. HNO3 and dilute to 1,000 
mL with deionized, distilled water.

[[Page 313]]

    7.3.21  Silver solution, stock, 1 mL=100 g Ag: Dissolve 
0.1575 g AgNO3 in 100 mL of deionized, distilled water and 10 
mL conc. HNO3. Dilute to 1,000 mL with deionized, distilled 
water.
    7.3.22  Sodium solution, stock, 1 mL=100 g Na: Dissolve 
0.2542 g NaCl in deionized, distilled water. Add 10.0 mL conc. 
HNO3 and dilute to 1,000 mL with deionized, distilled water.
    7.3.23  Thallium solution, stock, 1 mL=100 g Tl: Dissolve 
0.1303 g TlNO3 in deionized, distilled water. Add 10.0 mL 
conc. HNO3 and dilute to 1,000 mL with deionized, distilled 
water.
    7.3.24  Vanadium solution, stock, 1 mL=100 g V: Dissolve 
0.2297 NH4 VO3 in a minimum amount of conc. 
HNO3. Heat to increase rate of dissolution. Add 10.0 mL conc. 
HNO3 and dilute to 1,000 mL with deionized, distilled water.
    7.3.25  Zinc solution, stock, 1 mL=100 g Zn: Dissolve 
0.1245 g ZnO in a minimum amount of dilute HNO3. Add 10.0 mL 
conc. HNO3 and dilute to 1,000 mL deionized, distilled water.
    7.4  Mixed calibration standard solutions--Prepare mixed calibration 
standard solutions by combining appropriate volumes of the stock 
solutions in volumetric flasks. (See 7.4.1 thru 7.4.5) Add 2 mL of (1+1) 
HNO3 and 10 mL of (1+1) HC1 and dilute to 100 mL with 
deionized, distilled water. (See Notes 1 and 6.) Prior to preparing the 
mixed standards, each stock solution should be analyzed separately to 
determine possible spectral interference or the presence of impurities. 
Care should be taken when preparing the mixed standards that the 
elemelts are compatible and stable. Transfer the mixed standard 
solutions to a FEP fluorocarbon or unused polyethylene bottle for 
storage. Fresh mixed standards should be prepared as needed with the 
realization that concentration can change on aging. Calibration 
standards must be initially verified using a quality control sample and 
monitored weekly for stability (See 7.6.3). Although not specifically 
required, some typical calibration standard combinations follow when 
using those specific wavelengths listed in Table 1.
    7.4.1  Mixed standard solution I--Manganese, beryllium, cadmium, 
lead, and zinc.
    7.4.2  Mixed standard solution II--Barium, copper, iron, vanadium, 
and cobalt.
    7.4.3  Mixed standard solution III--Molybdenum, silica, arsenic, and 
selenium.
    7.4.4  Mixed standard solution IV--Calcium, sodium, potassium, 
aluminum, chromium and nickel.
    7.4.5  Mixed standard solution V-- Antimony, boron, magnesium, 
silver, and thallium.
    Note: 1. If the addition of silver to the recommended acid 
combination results in an initial precipitation, add 15 mL of deionized 
distilled water and warm the flask until the solution clears. Cool and 
dilute to 100 mL with deionized, distilled water. For this acid 
combination the silver concentration should be limited to 2 mg/L. Silver 
under these conditions is stable in a tap water matrix for 30 days. 
Higher concentrations of silver require additional HCl.
    7.5  Two types of blanks are required for the analysis. The 
calibration blank (3.13) is used in establishing the analytical curve 
while the reagent blank (3.12) is used to correct for possible 
contamination resulting from varying amounts of the acids used in the 
sample processing.
    7.5.1  The calibration blank is prepared by diluting 2 mL of (1+1) 
HNO3 and 10 mL of (1+1) HCl to 100 mL with deionized, 
distilled water. (See Note 6.) Prepare a sufficient quantity to be used 
to flush the system between standards and samples.
    7.5.2  The reagent blank must contain all the reagents and in the 
same volumes as used in the processing of the samples. The reagent blank 
must be carried through the complete procedure and contain the same acid 
concentration in the final solution as the sample solution used for 
analysis.
    7.6  In addition to the calibration standards, an instrument check 
standard (3.7), an interference check sample (3.8) and a quality control 
sample (3.9) are also required for the analyses.
    7.6.1  The instrument check standard is prepared by the analyst by 
combining compatible elements at a concentration equivalent to the 
midpoint of their respective calibration curves. (See 12.1.1.)
    7.6.2  The interference check sample is prepared by the analyst in 
the following manner. Select a representative sample which contains 
minimal concentrations of the analytes of interest but known 
concentration of interfering elements that will provide an adequate test 
of the correction factors. Spike the sample with the elements of 
interest at the approximate concentration of either 100 g/L or 
5 times the estimated detection limits given in Table 1. (For effluent 
samples of expected high concentrations, spike at an appropriate level.) 
If the type of samples analyzed are varied, a synthetically prepared 
sample may be used if the above criteria and intent are met.
    7.6.3  The quality control sample should be prepared in the same 
acid matrix as the calibration standards at a concentration near 1 mg/L 
and in accordance with the instructions provided by the supplier. The 
Quality Assurance Branch of EMSL-Cincinnati will either supply a quality 
control sample or information where one of equal quality can be 
procured. (See 12.1.3.)

                   8. Sample Handling and Preservation

    8.1  For the determination of trace elements, contamination and loss 
are of prime concern. Dust in the laboratory environment, impurities in 
reagents and impurities

[[Page 314]]

on laboratory apparatus which the sample contacts are all sources of 
potential contamination. Sample containers can introduce either positive 
or negative errors in the measurement of trace elements by (a) 
contributing contaminants through leaching or surface desorption and (b) 
by depleting concentrations through adsorption. Thus the collection and 
treatment of the sample prior to analysis requires particular attention. 
Laboratory glassware including the sample bottle (whether polyethylene, 
polyproplyene or FEP-fluorocarbon) should be thoroughly washed with 
detergent and tap water; rinsed with (1+1) nitric acid, tap water, (1+1) 
hydrochloric acid, tap and finally deionized, distilled water in that 
order (See Notes 2 and 3).
    Note: 2. Chromic acid may be useful to remove organic deposits from 
glassware; however, the analyst should be cautioned that the glassware 
must be thoroughly rinsed with water to remove the last traces of 
chromium. This is especially important if chromium is to be included in 
the analytical scheme. A commercial product, NOCHROMIX, available from 
Godax Laboratories, 6 Varick St., New York, NY 10013, may be used in 
place of chromic acid. Chromic acid should not be used with plastic 
bottles.
    Note: 3. If it can be documented through an active analytical 
quality control program using spiked samples and reagent blanks, that 
certain steps in the cleaning procedure are not required for routine 
samples, those steps may be eliminated from the procedure.
    8.2  Before collection of the sample a decision must be made as to 
the type of data desired, that is dissolved, suspended or total, so that 
the appropriate preservation and pretreatment steps may be accomplished. 
Filtration, acid preservation, etc., are to be performed at the time the 
sample is collected or as soon as possible thereafter.
    8.2.1  For the determination of dissolved elements the sample must 
be filtered through a 0.45-m membrane filter as soon as 
practical after collection. (Glass or plastic filtering apparatus are 
recommended to avoid possible contamination.) Use the first 50-100 mL to 
rinse the filter flask. Discard this portion and collect the required 
volume of filtrate. Acidify the filtrate with (1+1) HNO3 to a 
pH of 2 or less. Normally, 3 mL of (1+1) acid per liter should be 
sufficient to preserve the sample.
    8.2.2  For the determination of suspended elements a measured volume 
of unpreserved sample must be filtered through a 0.45-m 
membrane filter as soon as practical after collection. The filter plus 
suspended material should be transferred to a suitable container for 
storage and/or shipment. No preservative is required.
    8.2.3  For the determination of total or total recoverable elements, 
the sample is acidified with (1+1) HNO3 to pH 2 or less as 
soon as possible, preferably at the time of collection. The sample is 
not filtered before processing.

                          9. Sample Preparation

    9.1  For the determinations of dissolved elements, the filtered, 
preserved sample may often be analyzed as received. The acid matrix and 
concentration of the samples and calibration standards must be the same. 
(See Note 6.) If a precipitate formed upon acidification of the sample 
or during transit or storage, it must be redissolved before the analysis 
by adding additional acid and/or by heat as described in 9.3.
    9.2  For the determination of suspended elements, transfer the 
membrane filter containing the insoluble material to a 150-mL Griffin 
beaker and add 4 mL conc. HNO3. Cover the beaker with a watch 
glass and heat gently. The warm acid will soon dissolve the membrane. 
Increase the temperature of the hot plate and digest the material. When 
the acid has nearly evaporated, cool the beaker and watch glass and add 
another 3 mL of conc. HNO3. Cover and continue heating until 
the digestion is complete, generally indicated by a light colored 
digestate. Evaporate to near dryness (2 mL), cool, and 10 mL HCl (1+1) 
and 15 mL deionized, distilled water per 100 mL dilution and warm the 
beaker gently for 15 min. to dissolve any precipitated or residue 
material. Allow to cool, wash down the watch glass and beaker walls with 
deionized distilled water and filter the sample to remove insoluble 
material that could clog the nebulizer. (See Note 4.) Adjust the volume 
based on the expected concentrations of elements present. This volume 
will vary depending on the elements to be determined (See Note 6). The 
sample is now ready for analysis. Concentrations so determined shall be 
reported as ``suspended.''
    Note: 4. In place of filtering, the sample after diluting and mixing 
may be centrifuged or allowed to settle by gravity overnight to remove 
insoluble material.
    9.3  For the determination of total elements, choose a measured 
volume of the well mixed acid preserved sample appropriate for the 
expected level of elements and transfer to a Griffin beaker. (See Note 
5.) Add 3 mL of conc. HNO3. Place the beaker on a hot plate 
and evaporate to near dryness cautiously, making certain that the sample 
does not boil and that no area of the bottom of the beaker is allowed to 
go dry. Cool the beaker and add another 5 mL portion of conc. 
HNO3. Cover the beaker with a watch glass and return to the 
hot plate. Increase the temperature of the hot plate so that a gently 
reflux action occurs. Continue heating, adding additional acid as 
necessary, until the digestion is complete (generally indicated when the 
digestate is light in color or does not change in appearance with 
continued refluxing.) Again, evaporate to near

[[Page 315]]

dryness and cool the beaker. Add 10 mL of 1+1 HCl and 15 mL of 
deionized, distilled water per 100 mL of final solution and warm the 
beaker gently for 15 min. to dissolve any precipitate or residue 
resulting from evaporation. Allow to cool, wash down the beaker walls 
and watch glass with deionized distilled water and filter the sample to 
remove insoluble material that could clog the nebulizer. (See Note 4.) 
Adjust the sample to a predetermined volume based on the expected 
concentrations of elements present. The sample is now ready for analysis 
(See Note 6). Concentrations so determined shall be reported as 
``total.''
    Note: 5. If low determinations of boron are critical, quartz 
glassware should be used.
    Note: 6. If the sample analysis solution has a different acid 
concentration from that given in 9.4, but does not introduce a physical 
interference or affect the analytical result, the same calibration 
standards may be used.
    9.4  For the determination of total recoverable elements, choose a 
measured volume of a well mixed, acid preserved sample appropriate for 
the expected level of elements and transfer to a Griffin beaker. (See 
Note 5.) Add 2 mL of (1+1) HNO3 and 10 mL of (1+1) HCl to the 
sample and heat on a steam bath or hot plate until the volume has been 
reduced to near 25 mL making certain the sample does not boil. After 
this treatment, cool the sample and filter to remove insoluble material 
that could clog the nebulizer. (See Note 4.) Adjust the volume to 100 mL 
and mix. The sample is now ready for analysis. Concentrations so 
determined shall be reported as ``total.''

                              10. Procedure

    10.1  Set up instrument with proper operating parameters established 
in Section 6.2. The instrument must be allowed to become thermally 
stable before beginning. This usually requires at least 30 min. of 
operation prior to calibration.
    10.2  Initiate appropriate operating configuration of computer.
    10.3  Profile and calibrate instrument according to instrument 
manufacturer's recommended procedures, using the typical mixed 
calibration standard solutions described in Section 7.4. Flush the 
system with the calibration blank (7.5.1) between each standard. (See 
Note 7.) (The use of the average intensity of multiple exposures for 
both standardization and sample analysis has been found to reduce random 
error.)
    Note: 7. For boron concentrations greater than 500 g/L 
extended flush times of 1 to 2 minutes may be required.
    10.4  Before beginning the sample run, reanalyze the highest mixed 
calibration standard as if it were a sample. Concentration values 
obtained should not deviate from the actual values by more than 
5 percent (or the established control limits whichever is 
lower). If they do, follow the recommendations of the instrument 
manufacturer to correct for this condition.
    10.5  Begin the sample run flushing the system with the calibration 
blank solution (7.5.1) between each sample. (See Note 7.) Analyze the 
instrument check standard (7.6.1) and the calibration blank (7.5.1) each 
10 samples.
    10.6  If it has been found that methods of standard addition are 
required, the following procedure is recommended.
    10.6.1  The standard addition technique (14.2) involves preparing 
new standards in the sample matrix by adding known amounts of standard 
to one or more aliquots of the processed sample solution. This technique 
compensates for a sample constitutent that enhances or depresses the 
analyte signal thus producing a different slope from that of the 
calibration standards. It will not correct for additive interference 
which causes a baseline shift. The simplest version of this technique is 
the single-addition method. The procedure is as follows. Two identical 
aliquots of the sample solution, each of volume Vx, are 
taken. To the first (labeled A) is added a small volume Vs of 
a standard analyte solution of concentration cs. To the 
second (labeled B) is added the same volume Vs of the 
solvent. The analytical signals of A and B are measured and corrected 
for nonanalyte signals. The unknown sample concentration cx 
is calculated:
[GRAPHIC] [TIFF OMITTED] TC15NO91.128

where SA and SB are the analytical signals 
(corrected for the blank) of solutions A and B, respectively. 
Vs and cs should be chosen so that SA 
is roughly twice SB on the average. It is best if 
Vs is made much less than Vx, and thus 
cs is much greater than cx, to avoid excess 
dilution of the sample matrix. If a separation or concentration step is 
used, the additions are best made first and carried through the entire 
procedure. For the results from this technique to be valid, the 
following limitations must be taken into consideration:
    1. The analytical curve must be linear.
    2. The chemical form of the analyte added must respond the same as 
the analyte in the sample.
    3. The interference effect must be constant over the working range 
of concern.
    4. The signal must be corrected for any additive interference.

                             11. Calculation

    11.1  Reagent blanks (7.5.2) should be subtracted from all samples. 
This is particularly important for digested samples requiring

[[Page 316]]

large quantities of acids to complete the digestion.
    11.2  If dilutions were performed, the appropriate factor must be 
applied to sample values.
    11.3  Data should be rounded to the thousandth place and all results 
should be reported in mg/L up to three significant figures.

                   12. Quality Control (Instrumental)

    12.1  Check the instrument standardization by analyzing appropriate 
quality control check standards as follow:
    12.1.1  Analyze and appropriate instrument check standard (7.6.1) 
containing the elements of interest at a frequency of 10%. This check 
standard is used to determine instrument drift. If agreement is not 
within 5% of the expected values or within the established 
control limits, whichever is lower, the analysis is out of control. The 
analysis should be terminated, the problem corrected, and the instrument 
recalibrated.
    Analyze the calibration blank (7.5.1) at a frequency of 10%. The 
result should be within the established control limits of 2 standard 
deviations of the meal value. If not, repeat the analysis two more times 
and average the three results. If the average is not wihin the control 
limit, terminate the analysis, correct the problem and recalibrate the 
instrument.
    12.1.2  To verify interelement and background correction factors 
analyze the interference check sample (7.6.2) at the beginning, end, and 
at periodic intervals throughout the sample run. Results should fall 
within the established control limits of 1.5 times the standard 
deviation of the mean value. If not, terminate the analysis, correct the 
problem and recalibrate the instrument.
    12.1.3   A quality control sample (7.6.3) obtained from an outside 
source must first be used for the initial verification of the 
calibration standards. A fresh dilution of this sample shall be analyzed 
every week thereafter to monitor their stability. If the results are not 
within 5% of the true value listed for the control sample, 
prepare a new calibration standard and recalibrate the instrument. If 
this does not correct the problem, prepare a new stock standard and a 
new calibration standard and repeat the calibration.

                       13. Precision and Accuracy

    13.1  An interlaboratory study of 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 the twenty-five elements 
listed in Table 4 were added to reagent water, surface water, drinking 
water and three effluents. These samples were digested by both the total 
digestion procedure (9.3) and the total recoverable procedure (9.4). 
Results for both digestions for the twenty-five elements in reagent 
water are given in Table 4; results for the other matrices can be found 
in Reference 14.10.

                             14. References

    14.1  Winge, R.K., V.J. Peterson, and V.A. Fassel, ``Inductively 
Coupled Plasma-Atomic Emission Spectroscopy: Prominent Lines, EPA-600/4-
79-017.
    14.2  Winefordner, J.D., ``Trace Analysis: Spectroscopic Methods for 
Elements,'' Chemical Analysis, Vol, 46, pp. 41-42.
    14.3  Handbook for Analytical Quality Control in Water and 
Wastewater Laboratories, EPA-600/4-79-019.
    14.4  Garbarino, J.R. and Taylor, H.E., ``An Inductively-Coupled 
Plasma Atomic Emission Spectrometric Method for Routine Water Quality 
Testing,'' Applied Spectroscopy 33, No. 3 (1979).
    14.5  ``Methods for Chemical Analysis of Water and Wastes,'' EPA-
600/4-79-020.
    14.6  Annual Book of ASTM Standards, Part 31.
    14.7  ``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.
    14.8  ``OSHA Safety and Health Standards, General Industry,'' (29 
CFR Part 1910), Occupational Safety and Health Administration, OSHA 
2206, (Revised, January 1976).
    14.9  ``Safety in Academic Chemistry Laboratories, American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
    14.10  Maxfield R. and Minak B., ``EPA Method Study 27, Method 200.7 
Trace Metals by ICP,'' National Technical Information Service, Order No. 
PB 85-248-656, November 1983.

 Table 1--Recommended Wavelengths 1 and Estimated Instrumental Detection
                                 Limits
------------------------------------------------------------------------
                                                              Estimated
                                                              detection
                    Element                     Wavelength,     limit,
                                                     nm      g/
                                                                  L2
------------------------------------------------------------------------
Aluminum......................................     308.215          45
Arsenic.......................................     193.696          53
Antimony......................................     206.833          32
Barium........................................     455.403           2
Beryllium.....................................     313.042           0.3
Boron.........................................     249.773           5
Cadmium.......................................     226.502           4
Calcium.......................................     317.933          10
Chromium......................................     267.716           7
Cobalt........................................     228.616           7
Copper........................................     324.754           6
Iron..........................................     259.940           7
Lead..........................................     220.353          42
Magnesium.....................................     279.079          30
Manganese.....................................     257.610           2

[[Page 317]]

 
Molybdenum....................................     202.030           8
Nickel........................................     231.604          15
Potassium.....................................     766.491           3
Selenium......................................     196.026          75
Silica (SiO2).................................     288.158          58
Silver........................................     328.068           7
Sodium........................................     588.995          29
Thallium......................................     190.864          40
Vanadium......................................     292.402           8
Zinc..........................................     213.856           2
------------------------------------------------------------------------
\1\The wavelengths listed are recommended because of their sensitivity
  and overall acceptance. Other wavelengths may be substituted if they
  can provide the needed sensitivity and are treated with the same
  corrective techniques for spectral interference. (See 5.1.1).
\2\The estimated instrumental detection limits as shown are taken from
  ``Inductively Coupled Plasma-Atomic Emission Spectroscopy-Prominent
  Lines,'' EPA-600/4-79-017. They are given as a guide for an
  instrumental limit. The actual method detection limits are sample
  dependent and may vary as the sample matrix varies.
\3\Highly dependent on operating conditions and plasma position.


[[Page 318]]


                                                Table 1--Analyte Concentration Equivalents (mg/L) Arising From Interferents at the 100 mg/L Level
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                 Interferent--
                             Analyte                              Wavelength, ------------------------------------------------------------------------------------------------------------------
                                                                       nm          A1          Ca         Cr          Cu         Fe          Mg          Mn         Ni         Ti          V
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Aluminum........................................................     308.214   ..........  .........  ..........  .........  ..........  ..........       0.21  .........  .........        1.4
Antimony........................................................     206.833      0.47     .........        2.9   .........       0.08   ..........  .........  .........       0.25        0.45
Arsenic.........................................................     193.696      1.3      .........        0.44  .........  ..........  ..........  .........  .........  .........        1.1
Barium..........................................................     455.403   ..........  .........  ..........  .........  ..........  ..........  .........  .........  .........  ..........
Beryllium.......................................................     313.042   ..........  .........  ..........  .........  ..........  ..........  .........  .........       0.04        0.05
Boron...........................................................     249.773      0.04     .........  ..........  .........       0.32   ..........  .........  .........  .........  ..........
Cadmium.........................................................     226.502   ..........  .........  ..........  .........       0.03   ..........  .........       0.02  .........  ..........
Calcium.........................................................     317.933   ..........  .........        0.08  .........       0.01        0.01        0.04  .........       0.03        0.03
Chromium........................................................     267.716   ..........  .........  ..........  .........       0.003  ..........       0.04  .........  .........        0.04
Cobalt..........................................................     228.616   ..........  .........        0.03  .........       0.005  ..........  .........       0.03       0.15  ..........
Copper..........................................................     324.754   ..........  .........  ..........  .........       0.003  ..........  .........  .........       0.05        0.02
Iron............................................................     259.940   ..........  .........  ..........  .........  ..........  ..........       0.12  .........  .........  ..........
Lead............................................................     220.353      0.17     .........  ..........  .........  ..........  ..........  .........  .........  .........  ..........
Magnesium.......................................................     279.079   ..........       0.02        0.11  .........       0.13   ..........       0.25  .........       0.07        0.12
Manganese.......................................................     257.610      0.005    .........        0.01  .........       0.002       0.002  .........  .........  .........  ..........
Molybdenum......................................................     202.030      0.05     .........  ..........  .........       0.03   ..........  .........  .........  .........  ..........
Nickel..........................................................     231.604   ..........  .........  ..........  .........  ..........  ..........  .........  .........  .........  ..........
Selenium........................................................     196.026      0.23     .........  ..........  .........       0.09   ..........  .........  .........  .........  ..........
Silicon.........................................................     288.158   ..........  .........        0.07  .........  ..........  ..........  .........  .........  .........        0.01
Sodium..........................................................     588.995   ..........  .........  ..........  .........  ..........  ..........  .........  .........       0.08  ..........
Thallium........................................................     190.864      0.30     .........  ..........  .........  ..........  ..........  .........  .........  .........  ..........
Vanadium........................................................     292.402   ..........  .........        0.05  .........       0.005  ..........  .........  .........       0.02  ..........
Zinc............................................................     213.856   ..........  .........  ..........       0.14  ..........  ..........  .........       0.29  .........  ..........
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------


[[Page 319]]


     Table 3--Interferent and Analyte Elemental Concentrations Used for Interference Measuremelts in Table 2
----------------------------------------------------------------------------------------------------------------
                          Analytes         (mg/L)                  Interferents       (mg/L)
----------------------------------------------------------------------------------------------------------------
                    Al..................        10             Al..................     1,000  .................
                    AS..................        10             Ca..................     1,000  .................
                    B...................        10             Cr..................       200  .................
                    Ba..................         1             Cu..................       200  .................
                    Be..................         1             Fe..................     1,000  .................
                    Ca..................         1             Mg..................     1,000  .................
                    Cd..................        10             Mn..................       200  .................
                    Co..................         1             Ni..................       200
                    Cr..................         1             Ti..................       200
                    Cu..................         1             V...................       200  .................
                    Fe..................         1
                    Mg..................         1
                    Mn..................         1
                    Mo..................        10
                    Na..................        10
                    Ni..................        10
                    Pb..................        10
                    Sb..................        10
                    Se..................        10
                    Si..................         1
                    Tl..................        10
                    V...................         1
                    Zn..................        10
----------------------------------------------------------------------------------------------------------------


                                    Table 4--ICP Precision and Recovery Data
----------------------------------------------------------------------------------------------------------------
                                                  Concentration    Total digestion (9.3)   Recoverable digestion
                    Analyte                       g/L         g/L         (9.4) g/L
----------------------------------------------------------------------------------------------------------------
Aluminum......................................           69-4792     X=0.9273(C)+3.6         X=0.9380(C)+22.1
                                                                     S=0.0559(X)+18.6        S=0.0873(X)+31.7
                                                                    SR=0.0507(X)+3.5        SR=0.0481(X)+18.8
Antimony......................................           77-1406     X=0.7940(C)-17.0        X=0.8908(C)+0.9
                                                                     S=0.1556(X)-0.6         S=0.0982(X)+8.3
                                                                    SR=0.1081(X)+3.9        SR=0.0682(X)+2.5
Arsenic.......................................           69-1887     X=1.0437(C)-12.2        X=1.0175(C)+3.9
                                                                     S=0.1239(X)+2.4         S=0.1288(X)+6.1
                                                                    SR=0.0874(X)+6.4        SR=0.0643(X)+10.3
Barium........................................             9-377     X=0.7683(C)+0.47        X=0.8380(C)+1.68
                                                                     S=0.1819(X)+2.78        S=0.2540(X)+0.30
                                                                    SR=0.1285(X)+2.55       SR=0.0826(X)+3.54
Beryllium.....................................            3-1906     X=0.9629(C)+0.05        X=1.0177(C)-0.55
                                                                     S=0.0136(X)+0.95        S=0.0359(X)+0.90
                                                                    SR=0.0203(X)-0.07       SR=0.0445(X)-0.10
Boron.........................................           19-5189     X=0.8807(C)+9.0         X=0.9676(C)+18.7
                                                                     S=0.1150(X)+14.1        S=0.1320(X)+16.0
                                                                    SR=0.0742(X)+23.2       SR=0.0743(X)+21.1
Cadmium.......................................            9-1943     X=0.9874(C)-0.18        X=1.0137(C)-0.65
                                                                      S=0.557(X)+2.02        S=0.0585(X)+1.15
                                                                    SR=0.0300(X)+0.94        SR=0.332(X)+0.90
Calcium.......................................          17-47170     X=0.9182(C)-2.6         X=0.9658(C)+0.8
                                                                     S=0.1228(X)+10.1        S=0.0917(X)+6.9
                                                                    SR=0.0189(X)+3.7        SR=0.0327(X)+10.1
Chromium......................................           13-1406     X=0.9544(C)+3.1         X=1.0049(C)-1.2
                                                                     S=0.0499(X)+4.4         S=0.0698(X)+2.8
                                                                    SR=0.0009(X)+7.9        SR=0.0571(X)+1.0
Cobalt........................................           17-2340     X=0.9209(C)-4.5         X=0.9278(C)-1.5
                                                                     S=0.0436(X)+3.8         S=0.0498(X)+2.6
                                                                    SR=0.0428(X)+0.5        SR=0.0407(X)+0.4
Copper........................................            8-1887     X=0.9297(C)-0.30        X=0.9647(C)-3.64
                                                                     S=0.0442(X)+2.85        S=0.0497(X)+2.28
                                                                    SR=0.0128(X)+2.53       SR=0.0406(X)+0.96
Iron..........................................           13-9359     X=0.8829(C)+7.0         X=0.9830(C)+5.7
                                                                     S=0.0683(X)+11.5        S=0.1024(X)+13.0
                                                                    SR=0.0046(X)+10.0       SR=0.0790(X)+11.5
Lead..........................................           42-4717     X=0.9699(C)-2.2         X=1.0056(C)+4.1
                                                                     S=0.0558(X)+7.0         S=0.0779(X)+4.6
                                                                    SR=0.0353(X)+3.6        SR=0.0448(X)+3.5
Magnesium.....................................          34-13868     X=0.9881(C)-1.1         X=0.9879(C)+2.2
                                                                     S=0.0607(C)+11.6        S=0.0564(X)+13.2

[[Page 320]]

 
                                                                    SR=0.0298(X)+0.6        SR=0.0268(X)+8.1
Manganese.....................................            4-1887     X=0.9417(C)+0.13        X=0.9725(C)+0.07
                                                                     S=0.0324(X)+0.88        S=0.0557(X)+0.76
                                                                    SR=0.0153(X)+0.91       SR=0.0400(X)+0.82
Molybdenum....................................           17-1830     X=0.9682(C)+0.1         X=0.9707(C)-2.3
                                                                     S=0.0618(X)+1.6         S=0.0811(X)+3.8
                                                                    SR=0.0371(X)+2.2        SR=0.0529(X)+2.1
Nickel........................................          17-47170     X=0.9508(C)+0.4         X=0.9869(C)+1.5
                                                                     S=0.0604(X)+4.4         S=0.0526(X)+5.5
                                                                    SR=0.0425(X)+3.6        SR=0.0393(X)+2.2
Potassium.....................................         347-14151     X=0.8669(C)-36.4        X=0.9355(C)-183.1
                                                                     S=0.0934(X)+77.8        S=0.0481(X)+177.2
                                                                    SR=0.0099(X)+144.2      SR=0.0329(X)+60.9
Selenium......................................           69-1415     X=0.9363(C)-2.5         X=0.9737(C)-1.0
                                                                     S=0.0855(X)+17.8        S=0.1523(X)+7.8
                                                                    SR=0.0284(X)+9.3        SR=0.0443(X)+6.6
Silicon.......................................          189-9434     X=0.5742(C)-35.6        X=0.9737(C)-60.8
                                                                     S=0.4160(X)+37.8        S=0.3288(X)+46.0
                                                                    SR=0.1987(X)+8.4        SR=0.2133(X)+22.6
Silver........................................             8-189     X=0.4466(C)+5.07        X=0.3987(C)+8.25
                                                                     S=0.5055(X)-3.05        S=0.5478(X)-3.93
                                                                    SR=0.2086(X)-1.74       SR=0.1836(X)-0.27
Sodium........................................          35-47170     X=0.9581(C)+39.6        X=1.0526(C)+26.7
                                                                     S=0.2097(X)+33.0        S=0.1473(X)+27.4
                                                                    SR=0.0280(X)+105.8      SR=0.0884(X)+50.5
Thallium......................................           79-1434     X=0.9020(C)-7.3         X=0.9238(C)+5.5
                                                                     S=0.1004(X)+18.3        S=0.2156(X)+5.7
                                                                    SR=0.0364(X)+11.5       SR=0.0106(X)+48.0
Vanadium......................................           13-4698     X=0.9615(C)-2.0         X=0.9551(C)+0.4
                                                                     S=0.0618(X)+1.7         S=0.0927(X)+1.6
                                                                    SR=0.0220(X)+0.7        SR=0.0472(X)+0.5
Zinc..........................................            7-7076     X=0.9356(C)-0.30        X=0.9500(C)+1.82
                                                                     S=0.0914(X)+3.75        S=0.0597(X)+6.50
                                                                    SR=0.0130(X)+10.7       SR=0.0153(X)+7.78
----------------------------------------------------------------------------------------------------------------
 AAAAAX=Mean Recovery, g/L
 AAAAAC=True Value for the Concentration, g/L
 AAAAAS=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

[49 FR 43431, Oct. 26, 1984; 50 FR 695, 696, Jan. 4, 1985, as amended at 
51 FR 23703, June 30, 1986; 55 FR 33440, Aug. 15, 1990]

 Appendix D to Part 136--Precision and Recovery Statements for Methods 
                          for Measuring Metals

    Twenty-eight 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 following precision and 
recovery statements are presented in this appendix and incorporated into 
part 136:

                              Method 202.1

    For Aluminum, Method 202.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trace Methods in water by 
Atomic Absorption Spectroscopy (Direction Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June, 1986.
    For a concentration range of 500-1200 g/L

X=0.979(C)+6.16
S=0.066(X)+125
SR=0.086(X)+40.5

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L

[[Page 321]]

S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 206.4

    For Arsenic, Method 206.4 (Spectrophotometric-SDDC) add the 
following to the Precision and Accuracy Section:

                         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 and a natural water or effluent of the analyst's choice. 
Results for the reagent water are given below. Results for other water 
types and study details are found in ``USEPA Method Study 7, Analyses 
for Trace Methods in Water by Atomic Absorption Spectroscopy (Direct 
Aspiration) and Colorimetry'', National Technical Information Service, 
5285 Port Royal Road, Springfield, VA 22161, Order No. PB86-208709/AS, 
Winter, J.A. and Britton, P.W., June, 1986.
    For a concentration range of 20-292 g/L

X=0.850(C)-0.25
S=0.198(X)+5.93
SR=0.122(X)+3.10

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 213.1

    For Cadmium, Method 213.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trace Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June, 1986.
    For a concentration range of 14-78 g/L

X=0.919(C)+2.97
S=0.108(X)+5.08
SR=0.120(X)+0.89

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 218.1

    For Chromium, Method 218.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trace Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June 1986.
    For a concentration range of 74-407 g/L

X=0.976(C)+3.94
S=0.131(X)+4.26
SR=0.052(X)+3.01

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 220.1

    For Copper, Method 220.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a

[[Page 322]]

natural water or effluent of the analyst's choice. The digestion 
procedure was not specified. Results for the reagent water are given 
below. Results for other water types and study details are found in 
``USEPA Method Study 7, Analyses for Trace Methods in Water by Atomic 
Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', National 
Technical Information Service, 5285 Port Royal Road, Springfield, VA 
22161, Order No. PB86-208709/AS, Winter, J.A. and Britton, P.W., June, 
1986.
    For concentration range 60-332 g/L
X=0.963(C)+3.49
S=0.047(X)+12.3
SR=0.042(X)+4.60

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 236.1

    For Iron, Method 236.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trade Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June, 1986.
    For concentration range 350-840 g/L

X=0.999(C)-2.21
S=0.022(X)+41.0
SR=0.019(X)+21.2

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-Laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 239.1

    For Lead, Method 239.1 (Atomic Absorption, Direct Aspiration) 
replace Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7 Analyses for Trace Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry''; 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June, 1986.
    For concentration range of 84-367 g/L

X=0.961(C)+13.8
S=0.028(C)+33.9
SR=0.011(X)+16.1

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L
S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 243.1

    For Manganese, Method 243.1 (Atomic Absorption, Direct Aspiration) 
replace Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trace Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J.A. and 
Britton, P.W., June, 1986.
    For concentration range 84-469 g/L

X=0.987(C)-1.27
S=0.042(X)+8.95
SR=0.023(X)+4.90

Where:

C=True Value for the Concentration, g/L
X=Mean Recovery, g/L

[[Page 323]]

S=Multi-laboratory Standard Deviation, g/L
SR=Single-analyst Standard Deviation, g/L

                              Method 289.1

    For Zinc, Method 289.1 (Atomic Absorption, Direct Aspiration) 
replace the Precision and Accuracy Section 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 and a natural water or effluent of the analyst's choice. 
The digestion procedure was not specified. Results for the reagent water 
are given below. Results for other water types and study details are 
found in ``USEPA Method Study 7, Analyses for Trace Methods in Water by 
Atomic Absorption Spectroscopy (Direct Aspiration) and Colorimetry'', 
National Technical Information Service, 5285 Port Royal Road, 
Springfield, VA 22161, Order No. PB86-208709/AS, Winter, J. A. and 
Britton, P. W., June, 1986.

For concentration range 56-310 g/L
    X=0.999(C)+0.033
    S=0.078(X)+10.8
    SR=0.049(X)+1.10

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 202.2

    For Aluminum, Method 202.2 (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 0.46-125 g/L
    X=1.1579(C)-0.121
    S=0.4286(X)-0.124
    SR=0.2908(X)-0.082

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 204.2

    For Antimony, Method 204.2 (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 as modified by this method. 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 10.50-240 g/L
    X=0.7219(C)-0.986
    S=0.3732(X)+0.854
    SR=0.1874(X)-0.461

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 206.2

    For Arsenic, Method 206.2 (Atomic Absorption, Furnace Technique) add 
the following to the existing Precision and Accuracy statement:

                         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-

[[Page 324]]

Cincinnati (EMSL-CI). Synthetic concentrates containing various levels 
of this element were added to reagent water, surface water, drinking 
water and three effluents. 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 9.78-237 g/L
    X=0.9652(C)+2.112
    S=0.1411(X)+1.873
    SR=0.0464(X)+2.109

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 208.2

    For Barium, Method 208.2 (Atomic Absorption, Furnace Technique) add 
the following to the existing Precision and Accuracy information:

                         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 56.50-437 g/L
    X=0.8268(C)+59.459
    S=0.2466(X)+6.436
    SR=0.1393(X)-0.428

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 210.2

    For Beryllium, Method 210.2 (Atomic Absorption, Furnace Technique) 
replace the existing Precision and Accuracy 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 0.45-11.4 g/L
    X=1.0682(C)-0.158
    S=0.2167(X)+0.090
    SR=0.1096(X)+0.061

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 213.2

    For Cadmium, Method 213.2 (Atomic Absorption, Furnace Technique) add 
the following to the existing Precision and Accuracy information:

                         Precision and Accuracy

    An interlaboratory study on metal analyses by this method was 
conducted by the Quality Assurance Branch (QAB) of the Environmental 
Monitoring System 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 0.43-12.5 g/L

[[Page 325]]

    X=0.9826(C)+0.171
    S=0.2300(X)+0.045
    SR=0.1031(X)+0.116

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Devision, g/L

                              Method 218.2

    For Chromium, Method 218.2 (Atomic Absorption, Furnace Technique) 
add the following to the existing Precision and Accuracy Section:

                         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 9.87-246 g/L
    X=0.9120(C)+0.234
    S=0.1684(X)+0.852
    SR=0.1469(X)+0.315

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Devision, g/L

                              Method 219.2

    For Cobalt, Method 219.2 (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 21.10-461 g/L
    X=0.8875(C)+0.859
    S=0.2481(X)-2.541
    SR=0.0969(X)+0.134

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,  g/L

                              Method 220.2

    For Copper, Method 220.2 (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 0.30-245 g/L
    X=0.9253(C)+0.010
    S=0.2735(X)-0.058
    SR=0.2197(X)-0.050

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,  g/L

                              Method 236.2

    For Iron, Method 236.2 (Atomic Absorption, Furnace Technique) 
replace the Precision and Accuracy Section statement with the following:

[[Page 326]]

                         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 0.37-455 g/L
    X=1.4494(C)-0.229
    S=0.3611(X)-0.079
    SR=0.3715(X)-0.161

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,  g/L

                              Method 239.2

    For Lead, Method 239.2 (Atomic Absorption, Furnace Technique) add 
the following to the existing Precisions and Accuracy Section:

                         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 10.40-254 g/L
    X=0.9430(C)-0.504
    S=0.2224(X)+0.507
    SR=0.1931(X)-0.378

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,  g/L

                              Method 243.2

    For Manganese, Method 243.2 (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 0.42-666 g/L
    X=1.0480(C)+1.404
    S=0.2001(X)+1.042
    SR=0.1333(X)+0.680

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 249.2

    For Nickel, Method 249.2 (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,

[[Page 327]]

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 26.20-482 g/L
    X=0.8812(C)+2.426
    S=0.2475(X)+1.896
    SR=0.1935(X)+1.315

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 270.2

    For Selenium, Method 270.2 (Atomic Absorption, Furnace Technique) 
add the following to the existing Precision and Accuracy Section:

                         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. 
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 10.00-246 g/L
    X=0.9564(C)+0.476
    S=0.1584(X)+0.878
    SR=0.0772(X)+0.547

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 272.2

    For Silver, Method 272.2 (Atomic Absorption, Furnace Technique) add 
the following to the existing Precision and Accuracy Section:

                         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 0.45-56.5 g/L
    X=0.9470(C)+0.181
    S=0.1805(X)+0.153
    SR=0.1417(X)+0.039

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

                              Method 279.2

    For Thalliu, 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 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, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation, g/L

[[Page 328]]

                              Method 286.2

    For Vanadium, Method 286.2 (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 1.36-982 g/L.
    X=0.8486(C)+0.252
    S=0.3323(X)-0.428
    SR=0.1195(X)-0.121

Where:

    C=True Value for the Concentration, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,   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 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, g/L
    X=Mean Recovery, g/L
    S=Multi-laboratory Standard Deviation, g/L
    SR=Single-analyst Standard Deviation,   g/L


[55 FR 33442, Aug. 15, 1990]



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, 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

[[Page 329]]

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) 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

[[Page 330]]

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):
    (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) [Reserved]
    (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

[[Page 331]]

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 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]



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  Maximum contaminant levels for total trihalomethanes.
141.13  Maximum contaminant levels for turbidity.
141.15  Maximum contaminant levels for radium-226, radium-228, and gross 
          alpha particle radioactivity in community water systems.
141.16  Maximum contaminant levels for beta particle and photon 
          radioactivity from man-made radionuclides in community water 
          systems.

            Subpart C--Monitoring and Analytical Requirements

141.21  Coliform sampling.
141.22  Turbidity sampling and analytical requirements.

[[Page 332]]

141.23  Inorganic chemical sampling and analytical requirements.
141.24  Organic chemicals other than total trihalomethanes, sampling and 
          analytical requirements.
141.25  Analytical methods for radioactivity.
141.26  Monitoring frequency for radioactivity in community water 
          systems.
141.27  Alternate analytical techniques.
141.28  Certified laboratories.
141.29  Monitoring of consecutive public water systems.
141.30  Total trihalomethanes sampling, analytical and other 
          requirements.

       Subpart D--Reporting, Public Notification and Recordkeeping

141.31  Reporting requirements.
141.32  Public notification.
141.33  Record maintenance.
141.34  [Reserved]
141.35  Reporting and public notification for certain unregulated 
          contaminants.

  Subpart E--Special Regulations, Including Monitoring Regulations and 
                         Prohibition on Lead Use

141.40  Special monitoring for inorganic and organic 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.
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.

Subpart G--National Revised 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.

                 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.

                  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.

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 Subpart M--Information Collection Requirements (ICR) for Public Water 
                                 Systems

141.140  Definitions specific to subpart M.
141.141  General requirements, applicability, and schedule for 
          information collection.
141.142  Disinfection byproduct and related monitoring.
141.143  Microbial monitoring.
141.144  Disinfection byproduct precursor removal studies.

                 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--Converting MCL Compliance Values for Consumer 
          Confidence Reports
Appendix B to Subpart O--Regulated Contaminants
Appendix C to Subpart O--Health Effects Language

             Subpart P--Enhanced Filtration and Disinfection

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.

    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.
    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 Secs. 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.
    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.
    Coagulation means a process using coagulant chemicals and mixing by 
which colloidal and suspended materials are destabilized and 
agglomerated into flocs.
    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

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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 purposes of 
compliance with subpart P 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.
    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
[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

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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 daily Giardia lamblia 
inactivation through the treatment plant. The procedure for developing a 
disinfection profile is contained in Sec. 141.172.
    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).
    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.
    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.
    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.
    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.
    Ground water under the direct influence of surface water 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 (for subpart H systems serving at least 10,000 
people only) 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

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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.
    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.
    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 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.

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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.
    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.
    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 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 is a treatment device applied to a 
single tap used for the purpose of reducing contaminants in drinking 
water at that one tap.
    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.''
    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 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

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source, facilities, equipment, operation and maintenance for producing 
and distributing safe drinking water.
    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.
    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,

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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.
    Uncovered finished water storage facility is a tank, reservoir, or 
other facility used to store water that will undergo no further 
treatment except residual disinfection and is 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.

[40 FR 59570, Dec. 24, 1975, as amended at 41 FR 28403, July 9, 1976; 44 
FR 68641, Nov. 29, 1979; 51 FR 11410, Apr. 2, 1986; 52 FR 20674, June 2, 
1987; 52 FR 25712, July 8, 1987; 53 FR 37410, Sept. 26, 1988; 54 FR 
27526, 27562, June 29, 1989; 56 FR 3578, Jan. 30, 1991; 56 FR 26547, 
June 7, 1991; 57 FR 31838, July 17, 1992; 59 FR 34322, July 1, 1994; 61 
FR 24368, May 14, 1996; 63 FR 23366, Apr. 28, 1998; 63 FR 69463, 69515, 
Dec. 16, 1998]

    Effective Date Note: At 61 FR 24368, May 14, 1996, Sec. 141.2 was 
amended by adding ``or PWS'' to the definition for ``Public water 
system'', effective June 18, 1996 and will expire on Dec. 31, 2000.



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 MCL for total coliforms 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.

[54 FR 27562, June 29, 1989, as amended at 56 FR 1557, Jan. 15, 1991; 63 
FR 43846, Aug. 14, 1998]



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.

[[Page 340]]



Sec. 141.6  Effective dates.

    (a) Except as provided in paragraphs (a) through (i) 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 Secs. 141.11 (a), (d) and (e); 
141.14(a)(1); 141.14(b)(1)(i); 141.14(b)(2)(i); 141.14(d); 141.21 (a), 
(c) and (i); 141.22 (a) and (e); 141.23 (a)(3) and (a)(4); 141.23(f); 
141.24(a)(3); 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 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 Secs. 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 Secs. 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) Regulations for information collection requirements listed in 
subpart M are effective August 14, 1996, and shall remain effective 
until December 31, 2000.

[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]

    Effective Date Note: At 61 FR 24368, May 14, 1996, Sec. 141.6 is 
amended in paragraph (a) by revising the reference ``(a) through (h)'' 
to read ``(a) through (i)'' and by adding paragraph (i), effective June 
18, 1996 and will expire on Dec. 31, 2000.



                  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. Compliance with the MCL for arsenic is 
calculated pursuant to Sec. 141.23.
    (b) The maximum contaminant level for arsenic is 0.05 milligrams per 
liter.
    (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) There will be continuous posting of the fact that nitrate levels 
exceed 10 mg/l and the potential health effects of exposure; and

[[Page 341]]

    (3) Local and State public health authorities will be notified 
annually of nitrate levels that exceed 10 mg/l; and
    (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]



Sec. 141.12  Maximum contaminant levels for total trihalomethanes.

    The maximum contaminant level of 0.10 mg/L for total trihalomethanes 
(the sum of the concentrations of bromodichloromethane, 
dibromochloromethane, tribromomethane (bromoform), and trichloromethane 
(chloroform)) applies to subpart H community water systems which serve a 
population of 10,000 people or more until December 16, 2001. This level 
applies to community water systems that use only ground water not under 
the direct influence of surface water and serve a population of 10,000 
people or more until December 16, 2003. Compliance with the maximum 
contaminant level for total trihalomethanes is calculated pursuant to 
Sec. 141.30. After December 16, 2003, this section is no longer 
applicable.

[63 FR 69463, Dec. 16, 1998]



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:

    Editorial Note: At 54 FR 27527, June 29, 1988, Sec. 141.13 was 
amended by adding introductory text, effective December 31, 1990. This 
section already contains an introductory text.
    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 Sec. 1412(b)(7)(C)(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 
Sec. 1412(b)(7)(C)(iii), must install filtration, until June 29, 1993, 
or until filtration is installed, whichever is later.
    (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]



Sec. 141.15  Maximum contaminant levels for radium-226, radium-228, and gross alpha particle radioactivity in community water systems.

    The following are the maximum contaminant levels for radium-226, 
radium-228, and gross alpha particle radioactivity:
    (a) Combined radium-226 and radium-228--5 pCi/1.
    (b) Gross alpha particle activity (including radium-226 but 
excluding radon and uranium)--15 pCi/1.

[41 FR 28404, July 9, 1976]



Sec. 141.16  Maximum contaminant levels for beta particle and photon radioactivity from man-made radionuclides in community water systems.

    (a) The average annual concentration of beta particle and photon 
radioactivity from man-made radionuclides in drinking water shall not 
produce an annual dose equivalent to the total body or any internal 
organ greater than 4 millirem/year.
    (b) Except for the radionuclides listed in Table A, the 
concentration of man-made radionuclides causing 4 mrem total body or 
organ dose equivalents shall be calculated on the basis of a 2 liter per 
day drinking water intake

[[Page 342]]

using the 168 hour data listed in ``Maximum Permissible Body Burdens and 
Maximum Permissible Concentration of Radionuclides in Air or Water for 
Occupational Exposure,'' NBS Handbook 69 as amended August 1963, U.S. 
Department of Commerce. 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 millirem/year.

 Table A--Average Annual Concentrations Assumed to Produce a Total Body
                       or Organ Dose of 4 mrem/yr
------------------------------------------------------------------------
                                                                 pCi per
             Radionuclide                   Critical organ        liter
------------------------------------------------------------------------
Tritium..............................  Total body..............   20,000
Strontium-90.........................  Bone marrow.............        8
------------------------------------------------------------------------


[41 FR 28404, July 9, 1976]



            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:
    (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

[[Page 343]]

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 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

[[Page 344]]

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 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.

[[Page 345]]

    (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 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.

[[Page 346]]

    (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.
    (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. 
These methods are contained in the 18th edition of Standard Methods for 
the Examination of Water and Wastewater, 1992, American Public Health 
Association, 1015 Fifteenth Street NW., Washington, DC 20005. A 
description of the Colisure Test may be obtained from the Millipore 
Corporation, Technical Services Department, 80 Ashby Road, Bedford, MA 
01730. The toll-free phone number is (800) 645-5476.

------------------------------------------------------------------------
            Organism                 Methodology           Citation
------------------------------------------------------------------------
Total Coliforms 1..............  Total Coliform      9221A, B.
                                  Fermentation
                                  Technique 2,3,4.
                                 Total Coliform      9222A, B, C.
                                  Membrane Filter
                                  Technique.
                                 Presence-Absence    9221D.
                                  (P-A) Coliform
                                  Test 4,5.
                                 ONPG-MUG Test 6     9223.
                                 Colisure Test 7...
------------------------------------------------------------------------
\1\ 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.
\2\ Lactose broth, as commercially available, may be used in lieu of
  laurel 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 coliforms, using
  lactose broth, is less than 10 percent.
\3\ 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.
\4\ No requirement exists to run the completed phase on 10 percent of
  all total coliform-positive confirmed tubes.
\5\ Six-times formulation strength may be used if the medium is filter-
  sterilized rather than autoclaved.
\6\ The ONPG-MUG Test is also known as the Autoanalysis Colilert System.
\7\ The Colisure Test must be incubated for 28 hours before examining
  the results. If an examination of the results at 28 hours is not
  convenient, then results may be examined at any time between 28 hours
  and 48 hours.

    (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

[[Page 347]]

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 the 18th edition of Standard Methods for the Examination of Water and 
Wastewater, 1992, Method 9221E--p. 9-52, paragraph 1a. Public water 
systems need only determine the presence or absence of fecal coliforms; 
a determination of fecal coliform density is not required.
    (6) Public water systems must conduct analysis of Escherichia coli 
in accordance with one of the following analytical methods:
    (i) EC medium supplemented with 50 g/ml of 4-
methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration). EC 
medium is described in the 18th edition of Standard Methods for the 
Examination of Water and Wastewater, 1992, Method 9221E--p. 9-52, 
paragraph 1a. MUG may be added to EC medium before autoclaving. EC 
medium supplemented with 50 g/ml of MUG is commercially 
available. At least 10 ml of EC medium supplemented with MUG must be 
used. The inner inverted fermentation tube may be omitted. The procedure 
for transferring a total coliform-positive culture to EC medium 
supplemented with MUG shall be as specified in paragraph (f)(5) of this 
section for transferring a total coliform-positive culture to EC medium. 
Observe fluorescence with an ultraviolet light (366 nm) in the dark 
after incubating tube at 44.5  0.2  deg.C for 24 
 2 hours; or
    (ii) Nutrient agar supplemented with 100 g/ml 4-
methylumbelliferyl-beta-D-glucuronide (MUG) (final concentration). 
Nutrient Agar is described in the 18th edition of Standard Methods for 
the Examination of Water and Wastewater, 1992, p. 9-47 to 9-48. This 
test is used to determine if a total coliform-positive sample, as 
determined by the Membrane Filter Technique or any other method in which 
a membrane filter is used, contains E. coli. Transfer the membrane 
filter containing a total coliform colony(ies) to nutrient agar 
supplemented with 100 g/ml (final concentration) of MUG. After 
incubating the agar plate at 35  deg.C for 4 hours, 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.
    (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 + 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

[[Page 348]]

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 
may be obtained from the American Public Health Association et al.; 1015 
Fifteenth Street, NW.; Washington, DC 20005. Copies of the methods set 
forth in Microbiological Methods for Monitoring the Environment, Water 
and Wastes may be obtained from ORD Publications, U.S. EPA, 26 W. Martin 
Luther King Drive, Cincinnati, Ohio 45268. 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 Street, SW.; Washington, DC 20460, or at the Office 
of the Federal Register; 800 North Capitol Street, NW., suite 700, 
Washington, DC.
    (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 Sec. 141.32.
    (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 
Sec. 141.32.

[54 FR 27562, June 29, 1989, as amended at 54 FR 30001, July 17, 1989; 
55 FR 25064, June 19, 1990; 56 FR 642, Jan. 8, 1991; 57 FR 1852, Jan. 
15, 1992; 57 FR 24747, June 10, 1992; 59 FR 62466, Dec. 5, 1994; 60 FR 
34085, June 29, 1995]



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 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 
Secs. 141.31 and 141.32.

[[Page 349]]

    (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]



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 Secs. 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).
    (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.
Asbestos..................  7 MFL \1\..  Transmission      0.01 MFL
                                          Electron
                                          Microscopy.
Barium....................  2..........  Atomic            0.002
                                          Absorption;
                                          furnace
                                          technique.

[[Page 350]]

 
                                         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,     0.05
                                          Selective
                                          Electrode \3\.
                                         Distillation,     0.02
                                          Amenable,
                                          Spectrophotomet
                                          ric \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.
Nitrite...................  1 (as N)...  Spectrophotometr  0.01
                                          ic.
                                         Automated         0.05
                                          Cadmium
                                          Reduction.
                                         Manual Cadmium    0.01
                                          Reduction.
                                         Ion               0.004
                                          Chromatography.
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 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.
\5\ Lower MDLs are reported using stabilized temperature graphite
  furnace atomic absorption.

    (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 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 of collection.
    (5) The frequency of monitoring for asbestos shall be in accordance 
with paragraph (b) of this section: the frequency of monitoring for 
antimony, 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.

[[Page 351]]

    (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) 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, 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:

[[Page 352]]

    (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.
    (d) 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 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.

[[Page 353]]

    (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 asbestos, antimony, 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 the consumers 
served by the area served by the public water system in accordance with 
Sec. 141.32. 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 
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 Secs. 141.11 or 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, 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.
    (2) For systems which are monitoring annually, or less frequently, 
the system is out of compliance with the maximum contaminant levels for 
asbestos, antimony, barium, beryllium, cadmium, chromium, cyanide, 
fluoride, mercury, nickel, selenium or thallium if the level of a 
contaminant at any sampling point is greater than the MCL. If a 
confirmation sample is required by the State, the determination of 
compliance will be based on the average of the two samples.
    (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) If a public water system has a distribution system separable 
from other parts of the distribution system with no interconnections, 
the State may allow the system to give public notice to only the area 
served by that portion of the system which is out of compliance.
    (j) Each public water system shall monitor at the time designated by 
the State during each compliance period.
    (k) Inorganic analysis:

[[Page 354]]

    (1) Analysis for the following contaminants shall be conducted in 
accordance with the methods in the following table, 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 also 
contains approved analytical test methods which remain available for 
compliance monitoring until July 1, 1996. These methods will not be 
available for use after July 1, 1996. This document is available from 
the National Technical Information Service, NTIS PB95-104766, U.S. 
Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 
22161. The toll-free number is 800-553-6847.

[[Page 355]]



----------------------------------------------------------------------------------------------------------------
     Contaminant        Methodology        EPA            ASTM \3\               SM \4\               Other
----------------------------------------------------------------------------------------------------------------
Antimony............  ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Hydride-Atomic   ...........  D-3697-92
                       Absorption.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  ....................  3113B...............
                       Absorption;
                       Furnace.
Arsenic.............  Inductively        \2\ 200.7  ....................  3120B...............
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  D-2972-93C            3113B...............
                       Absorption;
                       Furnace.
                      Hydride Atomic   ...........  D-2972-93B            3114B...............
                       Absorption.
Asbestos............  Transmission       \9\ 100.1
                       Electron
                       Microscopy.
                      Transmission      \10\ 100.2
                       Electron
                       Microscopy.
Barium..............  Inductively        \2\ 200.7  ....................  3120B...............
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic           ...........  ....................  3111D...............
                       Absorption;
                       Direct.
                      Atomic           ...........  ....................  3113B...............
                       Absorption;
                       Furnace.
Beryllium...........  Inductively        \2\ 200.7  ....................  3120B...............
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  D-3645-93B            3113B...............
                       Absorption;
                       Furnace.
Cadmium.............  Inductively         \2\200.7
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  ....................  3113B...............
                       Absorption;
                       Furnace.
Chromium............  Inductively        \2\ 200.7  ....................  3120B...............
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  ....................  3113B...............
                       Absorption;
                       Furnace.
Cyanide.............  Manual           ...........  ....................  4500-CN-C...........
                       Distillation
                       followed by.
                        Spectrophotom  ...........  D2036-91B             4500CN-G............
                       etric,
                       Amenable.
                        Spectrophotom  ...........  D2036-91A             4500-CN-E...........  \5\ I-3300-85
                       etric Manual.
                          Semi-          \6\ 335.4
                       automated.
                      Selective        ...........  ....................  4500CN-F............
                       Electrode.
Fluoride............  Ion                \6\ 300.0  D4327-91              4110B...............
                       Chromatography.
                      Manual           ...........  ....................  4500F-B,D...........
                       Distill.;
                       Color. SPADNS.
                      Manual           ...........  D1179-93B             4500F-C.............
                       Electrode.
                      Automated        ...........  ....................  ....................  \11\ 380-75WE
                       Electrode.
                      Automated        ...........  ....................  4500F-E.............  \11\ 129-71W
                       Alizarin.
Mercury.............  Manual, Cold       \2\ 245.1  D3223-91              3112B...............
                       Vapor.
                      Automated, Cold    \1\ 245.2
                       Vapor.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
Nickel..............  Inductively        \2\ 200.7  ....................  3120B...............
                       Coupled Plasma.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  ....................  3111B...............
                       Absorption;
                       Direct.
                      Atomic           ...........  ....................  3113B...............
                       Absorption;
                       Furnace.
Nitrate.............  Ion                \6\ 300.0  D4327-91              4110B...............  \8\ B-1011
                       Chromatography.
                      Automated          \6\ 353.2  D3867-90A             4500-NO3-F..........
                       Cadmium
                       Reduction.
                      Ion Selective    ...........  ....................  4500-NO3-D..........  \7\ 601
                       Electrode.

[[Page 356]]

 
                      Manual Cadmium   ...........  D3867-90B             4500-NO3-E..........
                       Reduction.
Nitrite.............  Ion                \6\ 300.0  D4327-91              4110B...............  \8\ B-1011
                       Chromatography.
                      Automated          \6\ 353.2  D3867-90A             4500-NO3-F..........
                       Cadmium
                       Reduction.
                      Manual Cadmium   ...........  D3867-90B             4500-NO3-E..........
                       Reduction.
                      Spectrophotomet  ...........  ....................  4500-NO2-B..........
                       ric.
Selenium............  Hydride-Atomic   ...........  D3859-93A             3114B...............
                       Absorption.
                      ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
                      Atomic           ...........  D3859-93B             3113B...............
                       Absorption;
                       Furnace.
Thallium............  ICP-Mass           \2\ 200.8
                       Spectrometry.
                      Atomic             \2\ 200.9
                       Absorption;
                       Platform.
Lead................  Atomic           ...........  D3559-90D             3113B...............
                       absorption;
                       furnace.
                      ICP-Mass           \2\ 200.8
                       spectrometry.
                      Atomic             \2\ 200.9
                       absorption;
                       platform.
Copper..............  Atomic           ...........  D1688-90C             3113B...............
                       absorption;
                       furnace.
                      Atomic           ...........  D1688-90A             3111B...............
                       absorption;
                       direct
                       aspiration.
                      ICP............    \2\ 200.7  ....................  3120B...............
                      ICP-Mass           \2\ 200.8
                       spectrometry.
                      Atomic             \2\ 200.9
                       absorption;
                       platform.
pH..................  Electrometric..    \1\ 150.1  D1293-84              4500-H=-B...........
                      ...............    \1\ 150.2
Conductivity........  Conductance....  ...........  D1125-91A             2510B...............
Calcium.............  EDTA             ...........  D511-93A              3500-Ca-D...........
                       titrimetric.
                      Atomic           ...........  D511-93B              3111B...............
                       absorption;
                       direct
                       aspiration.
                      Inductively-       \2\ 200.7  ....................  3120B...............
                       coupled plasma.
Alkalinity..........  Titrimetric....  ...........  D1067-92B             2320B...............
                      Electrometric    ...........  ....................  ....................  \5\ I-1030-85
                       titration.
Orthophosphate \12\.  Colorimetric,      \6\ 365.1  ....................  4500-P-F............
                       automated,
                       ascorbic acid.
                      Colorimetric,    ...........  D515-88A              4500-P-E............
                       ascorbic acid,
                       single reagent.
                      Colorimetric,    ...........  ....................  ....................  \5\ I-1601-85
                       phosphomolybda
                       te;.
                        automated-     ...........  ....................  ....................  \5\ I-2601-90
                       segmented
                       flow;.
                        automated      ...........  ....................  ....................  \5\ I-2598-85
                       discrete.
                      Ion                \6\ 300.0  D4327-91              4110................
                       Chromatography.
Silica..............  Colorimetric,    ...........  ....................  ....................  \5\ I-1700-85
                       molybdate
                       blue;.
                        automated-     ...........  ....................  ....................  \5\ I-2700-85
                       segmented flow.
                      Colorimetric...  ...........  D859-88
                      Molybdosilicate  ...........  ....................  4500-Si-D...........
                      Heteropoly blue  ...........  ....................  4500-Si-E...........
                      Automated        ...........  ....................  4500-Si-F...........
                       method for
                       molybdate-
                       reactive
                       silica.
                      Inductively-       \2\ 200.7  ....................  3120B...............
                       coupled plasma.
Temperature.........  Thermometric...  ...........  ....................  2550................
Sodium..............  Inductively-       \2\ 200.7
                       coupled plasma.
                      Atomic           ...........  ....................  3111B...............
                       Absorption;
                       direct
                       aspiration.
----------------------------------------------------------------------------------------------------------------
Footnotes:
\1\ Methods 150.1, 150.2 and 245.2 are available from US EPA, EMSL, Cincinnati, OH 45268. The identical methods
  were formerly in ``Methods for Chemical Analysis of Water and Wastes'', EPA-600/4-79-020, March 1983, which is
  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, PB 94-184942.

[[Page 357]]

 
\3\ The procedures shall be done in accordance with the Annual Book of ASTM Standards, 1994, Vols. 11.01 and
  11.02, American Society for Testing and Materials. 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
  from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Copies may be
  inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the
  Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\4\ The procedures shall be done in accordance with the 18th edition of Standard Methods for the Examination of
  Water and Wastewater, 1992, American Public Health Association. 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 from the American Public Health Association, 1015 Fifteenth Street NW, Washington, DC 20005. Copies
  may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of
  the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\5\ Available from Books and Open-File Reports Section, U.S. Geological Survey, Federal Center, Box 25425,
  Denver, CO 80225-0425.
\6\ ``Methods for the Determination of Inorganic Substances in Environmental Samples'', EPA-600/R-93-100, August
  1993. Available at NTIS, PB94-121811.
\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. 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 from ATI Orion, 529 Main Street, Boston, MA 02129. Copies may be inspected at
  EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the Federal
  Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\8\ Method B-1011, ``Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion
  Chromatography'', Millipore Corporation, Waters Chromatography Division, 34 Maple Street, Milford, MA 01757.
\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-m In Length In Drinking Water'', EPA-
  600/R-94-134, June 1994. Available at NTIS, PB94-201902.
\11\ The procedures shall be done in accordance with the 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. 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 from the Technicon
  Industrial Systems, Tarrytown, NY 10591. Copies may be inspected at EPA's Drinking Water Docket, 401 M Street,
  SW., Washington, DC 20460; or at the Office of Federal Register, 800 Capitol Street, NW., Suite 700,
  Washington, DC.
\12\ Unfiltered, no digestion or hydrolysis.


[[Page 358]]

    (2) Sample collection for antimony, 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:

[[Page 359]]



----------------------------------------------------------------------------------------------------------------
               Contaminant                            Preservative \1\              Container \2\      Time \3\
----------------------------------------------------------------------------------------------------------------
Antimony.................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Asbestos.................................  Cool, 4 C............................  P or G...........  ...........
Barium...................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Beryllium................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Cadmium..................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Chromium.................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Cyanide..................................  Cool, 4  deg.C, NaOH to pH>12 \3\....  P or G...........  14 days
Fluoride.................................  None.................................  P or G...........  1 month.
Mercury..................................  Conc HNO3 to pH 2....................  P or G...........  28 days.
Nickel...................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Nitrate
  Chlorinated............................  Cool, 4 C............................  P or G...........  28 days.
  Non-chlorinated........................  Conc H2 SO4 to pH 2..................  P or G...........  14 days.
Nitrite..................................  Cool, 4 C............................  P or G...........  48 hours.
Selenium.................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
Thallium.................................  Conc HNO3 to pH 2....................  P or G...........  6 months.
----------------------------------------------------------------------------------------------------------------
\1\ P=plastic, hard or soft; G=glass, hard or soft.
\2\ In all cases, samples should be analyzed as soon after collection as possible.
\3\ See method(s) for the information for preservation.


[[Page 360]]

    (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, asbestos, barium, beryllium, cadmium, chromium, cyanide, 
fluoride, mercury, nickel, nitrate, nitrite and selenium and thallium, 
the laboratory must:
    (i) Analyze Performance Evaluation samples which include those 
substances provided by EPA Environmental Monitoring Systems Laboratory 
or equivalent samples provided by the State.
    (ii) Achieve quantitative results on the analyses that are within 
the following acceptance limits:

------------------------------------------------------------------------
             Contaminant                       Acceptance limit
------------------------------------------------------------------------
Antimony............................  30 at 0.006 mg/1
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.
    (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 
Sec. 141.32. 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 Sec. 141.32.
    (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, as amended at 56 FR 30274, July 1, 1991; 57 
FR 31838, July 17, 1992; 59 FR 34322, July 1, 1994; 59 FR 62466, Dec. 5, 
1994; 60 FR 33932, 34085, June 29, 1995]

[[Page 361]]



Sec. 141.24  Organic chemicals other than total trihalomethanes, sampling and analytical requirements.

    (a)-(d) [Reserved]
    (e) Analyses for the contaminants in this section shall be conducted 
using the following EPA methods or their equivalent as approved by EPA. 
Methods 502.2, 505, 507, 508, 508A, 515.1 and 531.1 are in Methods for 
the Determination of Organic Compounds in Drinking Water, EPA-600/4-88-
039, December 1988, Revised, July 1991. Methods 506, 547, 550, 550.1 and 
551 are in Methods for the Determination of Organic Compounds in 
Drinking Water--Supplement I, EPA-600-4-90-020, July 1990. Methods 
515.2, 524.2, 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. 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 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 the 18th 
edition of Standard Methods for the Examination of Water and Wastewater, 
1992, American Public Health Association. 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 from the American Public Health Association, 1015 Fifteenth 
Street NW., Washington, DC 20005. Copies may be inspected at EPA's 
Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at 
the Office of the Federal Register, 800 North Capitol Street, NW., Suite 
700, Washington, DC. Method 6610 shall be followed in accordance with 
the Supplement to the 18th edition of Standard Methods for the 
Examination of Water and Wastewater, 1994, American Public Health 
Association. 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 from the American Public Health 
Association, 1015 Fifteenth Street NW., Washington, DC 20005. Copies may 
be inspected at EPA's Drinking Water Docket, 401 M Street, SW., 
Washington, DC 20460; or at the Office of the Federal Register, 800 
North Capitol Street, NW., Suite 700, Washington, DC. Other analytical 
test procedures are contained in Technical Notes on Drinking Water 
Methods, EPA-600/R-94-173, October 1994, NTIS PB95-104766. This document 
also contains approved analytical methods which remain available for 
compliance monitoring until July 1, 1996. These methods will not be 
available for use after July 1, 1996. EPA Methods 504.1, 508.1 and 525.2 
are available from US EPA EMSL, Cincinnati, OH 45268. The phone number 
is 513-569-7586.

------------------------------------------------------------------------
                Contaminant                            Method
------------------------------------------------------------------------
Benzene...................................  502.2, 524.2.
Carbon tetrachloride......................  502.2, 524.2, 551.
Chlorobenzene.............................  502.2, 524.2.
1,2-Dichlorobenzene.......................  502.2, 524.2.
1,4-Dichlorobenzene.......................  502.2, 524.2.
1,2-Dichloroethane........................  502.2, 524.2.
cis-Dichloroethylene......................  502.2, 524.2.
trans-Dichloroethylene....................  502.2, 524.2.
Dichloromethane...........................  502.2, 524.2.
1,2-Dichloropropane.......................  502.2, 524.2.
Ethylbenzene..............................  502.2, 524.2.
Styrene...................................  502.2, 524.2.
Tetrachloroethylene.......................  502.2, 524.2, 551.
1,1,1-Trichloroethane.....................  502.2, 524.2, 551.
Trichloroethylene.........................  502.2, 524.2, 551.
Toluene...................................  502.2, 524.2.
1,2,4-Trichlorobenzene....................  502.2, 524.2.
1,1-Dichloroethylene......................  502.2, 524.2.
1,1,2-Trichloroethane.....................  502.2, 524.2.
Vinyl chloride............................  502.2, 524.2.
Xylenes (total)...........................  502.2, 524.2.
2,3,7,8-TCDD (dioxin).....................  1613.
2,4-D.....................................  515.2, 555, 515.1.
2,4,5-TP (Silvex).........................  515.2, 555, 515.1.
Alachlor..................................  505 \1\, 507, 525.2, 508.1.
Atrazine..................................  505 \1\, 507, 525.2, 508.1.
Benzo(a)pyrene............................  525.2, 550, 550.1.
Carbofuran................................  531.1, 6610.
Chlordane.................................  505, 508, 525.2, 508.1.
Dalapon...................................  552.1, 515.1.
Di(2-ethylhexyl) adipate..................  506, 525.2.
Di(2-ethylhexyl) phthalate................  506, 525.2.
Dibromochloropropane (DBCP)...............  504.1, 551.
Dinoseb...................................  515.2, 555, 515.1.
Diquat....................................  549.1.
Endothall.................................  548.1.
Endrin....................................  505, 508, 525.2, 508.1.
Ethylene dibromide (EDB)..................  504.1, 551.
Glyphosate................................  547, 6651.
Heptachlor................................  505, 508, 525.2, 508.1.
Heptachlor Epoxide........................  505, 508, 525.2, 508.1.
Hexachlorobenzene.........................  505, 508, 525.2, 508.1.
Hexachlorocyclopentadiene.................  505, 525.2, 508, 508.1.
Lindane...................................  505, 508, 525.2, 508.1.
Methoxychlor..............................  505, 508, 525.2, 508.1.
Oxamyl....................................  531.1, 6610.

[[Page 362]]

 
PCBs \2\ (as decachlorobiphenyl)..........  508A.
  (as Aroclors)...........................  505, 508.
Pentachlorophenol.........................  515.2, 525.2, 555, 515.1.
Picloram..................................  515.2, 555, 515.1.
Simazine..................................  505 \1\, 507, 525.2, 508.1.
Toxaphene.................................  505, 508, 525.2.
Total Trihalomethanes.....................  502.2, 524.2, 551.
------------------------------------------------------------------------
\1\ A nitrogen-phosphorous detector should be substituted for the
  electron capture detector in Method 505 (or another approved method
  should be used) to determine alachlor, atrazine and simazine, if lower
  detection limits are required.
\2\ PCBs are qualitatively identified as Aroclors and measured for
  compliance purposes as decachlorobiphenyl.

    (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 (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.

[[Page 363]]

    (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).
    (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.

[[Page 364]]

    (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 are available, the system may use these 
instead of resampling. The duplicate must be analyzed and the results 
reported to the State within 14 days of collection.
    (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.
    (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.
    (i) For systems which are conducting monitoring at a frequency 
greater than annual, compliance is determined by a running annual 
average of all samples taken at each sampling point. If the annual 
average of any sampling point is greater than the MCL, then the system 
is out of compliance. If the initial sample or a subsequent sample would 
cause the annual average to be exceeded, then the system is out of 
compliance immediately.
    (ii) If monitoring is conducted annually, or less frequently, the 
system is out of compliance if the level of a contaminant at any 
sampling point is greater than the MCL. If a confirmation sample is 
required by the State, the determination of compliance will be based on 
the average of two samples.
    (iii) If a public water system has a distribution system separable 
from other parts of the distribution system with no interconnections, 
the State may allow the system to give public notice to only that area 
served by that portion of the system which is out of compliance.
    (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):

[[Page 365]]

    (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 samples which include these 
substances provided by EPA Environmental Monitoring Systems Laboratory 
or equivalent samples provided by the State.
    (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 chemicals listed in Sec. 141.61(a) (2) through (21).
    (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 for vinyl chloride, the laboratory 
must:
    (A) Analyze Performance Evaluation samples provided by EPA 
Environmental Monitoring Systems Laboratory or equivalent samples 
provided by the State.
    (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.
    (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.
    (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: \7\
---------------------------------------------------------------------------

    \7\ Monitoring for the contaminants aldicarb, aldicarb sulfoxide, 
and aldicarb sulfone shall be conducted in accordance with Sec. 141.40.
---------------------------------------------------------------------------

    (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.

[[Page 366]]

    (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.
    (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 monitoring results in detection of one or more of certain 
related contaminants (aldicarb, aldicarb sulfone, aldicarb sulfoxide and 
heptachlor, heptachlor epoxide), then subsequent monitoring shall 
analyze for all related contaminants.

[[Page 367]]

    (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 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 are available, the system may use these 
duplicates instead of resampling. The duplicate must be analyzed and the 
results reported to the State within 14 days of collection.
    (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.
    (i) For systems which are conducting monitoring at a frequency 
greater than annual, compliance is determined by a running annual 
average of all samples taken at each sampling point. If the annual 
average of any sampling point is greater than the MCL, then the system 
is out of compliance. If the initial sample or a subsequent sample would 
cause the annual average to be exceeded, then the system is out of 
compliance immediately. Any samples below the detection limit shall be 
calculated as zero for purposes of determining the annual average.
    (ii) If monitoring is conducted annually, or less frequently, the 
system is out of compliance if the level of a contaminant at any 
sampling point is greater than the MCL. If a confirmation sample is 
required by the State, the determination of compliance will be based on 
the average of two samples.
    (iii) If a public water system has a distribution system separable 
from other parts of the distribution system with no interconnections, 
the State may allow the system to give public notice to only that 
portion of the system which is out of compliance.
    (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 505 or Method 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
                          Aroclor                           limit (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

[[Page 368]]

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
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 samples which include those 
substances provided by EPA Environmental Monitoring and Support 
Laboratory or equivalent samples provided by the State.
    (B) 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]

(Approved by the Office of Management and Budget under control number 
2040-0090)

[40 FR 59570, Dec. 24, 1975, as amended at 44 FR 68641, Nov. 29, 1979; 
45 FR 57345, Aug. 27, 1980; 47 FR 10998, Mar. 12, 1982; 52 FR 25712, 
July 8, 1987; 53 FR 5147, Feb. 19, 1988; 53 FR 25110, July 1, 1988; 56 
FR 3583, Jan. 30, 1991; 56 FR 30277, July 1, 1991; 57 FR 22178, May 27, 
1992; 57 FR 31841, July 17, 1992; 59 FR 34323, July 1, 1994; 59 FR 
62468, Dec. 5, 1994; 60 FR 34085, June 29, 1995]

[[Page 369]]



Sec. 141.25  Analytical methods for radioactivity.

    (a) Analysis for the following contaminants shall be conducted to 
determine compliance with Secs. 141.15 and 141.16 (radioactivity) in 
accordance with the methods in the following table, or their equivalent 
determined by EPA in accordance with Sec. 141.27.

[[Page 370]]



------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                           Reference (method or page number)
           Contaminant                Methodology     ------------------------------------------------------------------------------------------------------------------------------------------
                                                       EPA\1\      EPA\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         .............  .............
  Gross alpha \11\..............  Co-precipitation...  ......  .............  00-02          .............  7110 C............  ................  ................  .............
    Radium 226..................  Radon emanation,...   903.1  p 16           Ra-04          p 19           7500-Ra C.........  D 3454-91         R-1141-76         Ra-05          N.Y.\9\
                                  Radio chemical.....   903.0  p 13           Ra-03          .............  304, 305,.........  D 2460-90         R-1140-76         .............  .............
                                                                                                            7500-Ra B.........
    Radium 228..................  Radio chemical.....   904.0  p 24           Ra-05          p 19           304, 7500-Ra D....  ................  R-1142-76         .............  N.Y.\9\
                                                                                                                                                                                   N.J.\10\
    Uranium\12\.................  Radio chemical.....   908.0  .............  .............  .............  7500-U B..........  ................  ................  .............  .............
                                  Fluorometric.......   908.1  .............  .............  .............  7500-U C (17th       D2907-91         R-1180-76         U-04           .............
                                                                                                             Ed.).                                R-1181-76
                                  Alpha spectro metry  ......  .............  00-07          p33            7500-U C (18th or   D 3972-90         R-1182-76         U-02           .............
                                                                                                             19th Ed.).
                                  Laser Phospho        ......  .............  .............  .............  ..................  D 5174-91         ................  .............  .............
                                   rimetry.
Man-made:
    Radioactive cesium..........  Radio chemical.....   901.0  p 4            .............  .............  7500-Cs B.........  D 2459-72         R-1111-76         .............  .............
                                  Gamma ray             901.1  .............  .............  p 92           7120 (19th Ed.)...  D 3649-91         R-1110-76         4.5.2.3        .............
                                   spectrometry.
    Radioactive iodine..........  Radio chemical.....   902.0  p 6            .............  .............  7500-I B..........   D3649-91         ................  .............  .............
                                                               p 9                                          7500-I C..........
                                                                                                            7500-I D..........
                                  Gamma ray             901.1  .............  .............  p 92           7120 (19th Ed.)...  D 4785-88         ................  4.5.2.3
                                   spectrometry.
    Radioactive Strontium 89, 90  Radio chemical.....   905.0  p 29           Sr-04          p. 65          303, 7500-Sr B....  ................  R-1160-76         Sr-01          .............
                                                                                                                                                                    Sr-02
    Tritium.....................  Liquid                906.0  p 34           H-02           p. 87          306, 7500-3H B....  D 4107-91         R-1171-76         .............  .............
                                   scintillation.
  Gamma emitters................  Gamma ray..........   901.1  .............  .............  p92            7120 (19th Ed.)...  D 3649-91         R-1110-76         4.5.2.3        .............
                                  Spectrometry.......   902.0  .............  .............  .............  7500-Cs B.........  D 4785-88         ................  .............  .............
                                    .................   901.0  .............  .............  .............  7500-I B..........  ................  ................  .............  .............
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 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, 401 M Street, SW., Washington, DC 20460 (Telephone: 202-260-3027); or at the
  Office of Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\1\ ``Prescribed Procedures for Measurement of Radioactivity in Drinking Water'', EPA 600/4-80-032 , August 1980. Available at 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 at NTIS, ibid. PB 253258.
\3\ ``Radiochemistry Procedures Manual'', EPA 520/5-84-006, December 1987. Available at NTIS, ibid. PB 84-215581.
\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 Editions, 1971, 1989, 1992, 1995. Available at American Public Health Association, 1015 Fifteenth
  Street N.W., Washington, D.C. 20005. All methods are in the 17th, 18th and 19th editions except 7500-U C Fluorometric Uranium was discontinued after the 17th Edition, 7120 Gamma Emitters is
  only in the 19th Edition, and 302, 303, 304, 305 and 306 are only in the 13th Edition.
\6\ Annual Book of ASTM Standards, Vol. 11.02, 1994. Available at American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
\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'', 27th Edition, Volume 1, 1990. Available at the Environmental Measurements Laboratory, U.S. Department of Energy (DOE), 376 Hudson Street, New York, NY 10014-
  3621.

[[Page 371]]

 
\9\ ``Determination of Ra-226 and Ra-228 (Ra-02)'', January 1980, Revised June 1982. Available at Radiological Sciences Institute Center 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/g of uranium conversion factor must be used. This conservative factor is based on the 1:1 activity ratio of U-234 to U-238 that
  is characteristic of naturally occurring uranium.


[[Page 372]]

    (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 where 
 is the standard deviation of the net counting rate of the 
sample).
    (1) To determine compliance with Sec. 141.15(a) the detection limit 
shall not exceed 1 pCi/1. To determine compliance with Sec. 141.15(b) 
the detection limit shall not exceed 3 pCi/1.
    (2) To determine compliance with Sec. 141.16 the detection limits 
shall not exceed the concentrations listed in Table B.

Table B--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 Secs. 141.15 and 141.16, 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]



Sec. 141.26  Monitoring frequency for radioactivity in community water systems.

    (a) Monitoring requirements for gross alpha particle activity, 
radium-226 and radium-228.
    (1) Initial sampling to determine compliance with Sec. 141.15 shall 
begin within two years of the effective date of these regulations and 
the analysis shall be completed within three years of the effective date 
of these regulations. Compliance shall be based on the analysis of an 
annual composite of four consecutive quarterly samples or the average of 
the analyses of four samples obtained at quarterly intervals.
    (i) A gross alpha particle activity measurement may be substituted 
for the required radium-226 and radium-228 analysis Provided, That the 
measured gross alpha particle activity does not exceed 5 pCi/1 at a 
confidence level of 95 percent (1.65 where  is the 
standard deviation of the net counting rate of the sample). In 
localities where radium-228 may be present in drinking water, it is 
recommended that the State require radium-226 and/or radium-228 analyses 
when the gross alpha particle activity exceeds 2 pCi/1.
    (ii) When the gross alpha particle activity exceeds 5 pCi/1, the 
same or an equivalent sample shall be analyzed for radium-226. If the 
concentration of radium-226 exceeds 3 pCi/1 the same or an equivalent 
sample shall be analyzed for radium-228.
    (2) For the initial analysis required by paragraph (a)(1) of this 
section, data acquired within one year prior to the effective date of 
this part may be substituted at the discretion of the State.
    (3) Suppliers of water shall monitor at least once every four years 
following the procedure required by paragraph (a)(1) of this section. At 
the discretion of the State, when an annual record taken in conformance 
with paragraph (a)(1) of this section has established that the average 
annual concentration is less than half the maximum contaminant levels 
established by Sec. 141.15,

[[Page 373]]

analysis of a single sample may be substituted for the quarterly 
sampling procedure required by paragraph (a)(1) of this section.
    (i) More frequent monitoring shall be conducted when ordered by the 
State in the vicinity of mining or other operations which may contribute 
alpha particle radioactivity to either surface or ground water sources 
of drinking water.
    (ii) A supplier of water shall monitor in conformance with paragraph 
(a)(1) of this section within one year of the introduction of a new 
water source for a community water system. More frequent monitoring 
shall be conducted when ordered by the State in the event of possible 
contamination or when changes in the distribution system or treatment 
processing occur which may increase the concentration of radioactivity 
in finished water.
    (iii) A community water system using two or more sources having 
different concentrations of radioactivity shall monitor source water, in 
addition to water from a free-flowing tap, when ordered by the State.
    (iv) Monitoring for compliance with Sec. 141.15 after the initial 
period need not include radium-228 except when required by the State, 
Provided, That the average annual concentration of radium-228 has been 
assayed at least once using the quarterly sampling procedure required by 
paragraph (a)(1) of this section.
    (v) Suppliers of water shall conduct annual monitoring of any 
community water system in which the radium-226 concentration exceeds 3 
pCi/1, when ordered by the State.
    (4) If the average annual maximum contaminant level for gross alpha 
particle activity or total radium as set forth in Sec. 141.15 is 
exceeded, the supplier of a community water system shall give notice to 
the State pursuant to Sec. 141.31 and notify the public as required by 
Sec. 141.32. Monitoring at quarterly intervals shall be continued until 
the annual average concentration no longer exceeds the maximum 
contaminant level or until a monitoring schedule as a condition to a 
variance, exemption or enforcement action shall become effective.
    (b) Monitoring requirements for manmade radioactivity in community 
water systems.
    (1) Within two years of the effective date of this part, systems 
using surface water sources and serving more than 100,000 persons and 
such other community water systems as are designated by the State shall 
be monitored for compliance with Sec. 141.16 by analysis of a composite 
of four consecutive quarterly samples or analysis of four quarterly 
samples. Compliance with Sec. 141.16 may be assumed without further 
analysis if the average annual concentration of gross beta particle 
activity is less than 50 pCi/1 and if the average annual concentrations 
of tritium and strontium-90 are less than those listed in table A, 
Provided, That if both radionuclides are present the sum of their annual 
dose equivalents to bone marrow shall not exceed 4 millirem/year.
    (i) If the gross beta particle activity exceeds 50 pCi/1, an 
analysis of the sample must be performed to identify the major 
radioactive constituents present and the appropriate organ and total 
body doses shall be calculated to determine compliance with Sec. 141.16.
    (ii) Suppliers of water shall conduct additional monitoring, as 
ordered by the State, to determine the concentration of man-made 
radioactivity in principal watersheds designated by the State.
    (iii) At the discretion of the State, suppliers of water utilizing 
only ground waters may be required to monitor for man-made 
radioactivity.
    (2) For the initial analysis required by paragraph (b)(1) of this 
section data acquired within one year prior to the effective date of 
this part may be substituted at the discretion of the State.
    (3) After the initial analysis required by paragraph (b)(1) of this 
section suppliers of water shall monitor at least every four years 
following the procedure given in paragraph (b)(1) of this section.
    (4) Within two years of the effective date of these regulations the 
supplier of any community water system designated by the State as 
utilizing waters contaminated by effluents from nuclear facilities shall 
initiate quarterly monitoring for gross beta particle and iodine-131 
radioactivity and annual

[[Page 374]]

monitoring for strontium-90 and tritium.
    (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. If the gross beta 
particle activity in a sample exceeds 15 pCi/1, the same or an 
equivalent sample shall be analyzed for strontium-89 and cesium-134. If 
the gross beta particle activity exceeds 50 pCi/1, an analysis of the 
sample must be performed to identify the major radioactive constituents 
present and the appropriate organ and total body doses shall be 
calculated to determine compliance with Sec. 141.16.
    (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) The State may allow the substitution of environmental 
surveillance data taken in conjunction with a nuclear facility for 
direct monitoring of manmade radioactivity by the supplier of water 
where the State determines such data is applicable to a particular 
community water system.
    (5) If the average annual maximum contaminant level for man-made 
radioactivity set forth in Sec. 141.16 is exceeded, the operator of a 
community water system shall give notice to the State pursuant to 
Sec. 141.31 and to the public as required by Sec. 141.32. Monitoring at 
monthly intervals shall be continued until the concentration no longer 
exceeds the maximum contaminant level or until a monitoring schedule as 
a condition to a variance, exemption or enforcement action shall become 
effective.

[41 FR 28404, July 9, 1976]



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 Secs. 141.21 
through 141.27, 141.41 and 141.42, samples may be considered only if 
they have been analyzed by a laboratory certified by the State except 
that measurements for turbidity, free chlorine residual, temperature and 
pH 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]



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 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. 141.30  Total trihalomethanes sampling, analytical and other requirements.

    (a) Community water system which serve a population of 10,000 or 
more individuals and which add a disinfectant (oxidant) to the water in 
any part of the drinking water treatment process

[[Page 375]]

shall analyze for total trihalomethanes in accordance with this section. 
For systems serving 75,000 or more individuals, sampling and analyses 
shall begin not later than 1 year after the date of promulgation of this 
regulation. For systems serving 10,000 to 74,999 individuals, sampling 
and analyses shall begin not later than 3 years after the date of 
promulgation of this regulation. For the purpose of this section, 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. All samples taken within an established 
frequency shall be collected within a 24-hour period.
    (b)(1) For all community water systems utilizing surface water 
sources in whole or in part, and for all community water systems 
utilizing only ground water sources that have not been determined by the 
State to qualify for the monitoring requirements of paragraph (c) of 
this section, analyses for total trihalomethanes shall be performed at 
quarterly intervals on at least four water samples for each treatment 
plant used by the system. At least 25 percent of the samples shall be 
taken at locations within the distribution system reflecting the maximum 
residence time of the water in the system. The remaining 75 percent 
shall be taken at representative locations in the distribution system, 
taking into account number of persons served, different sources of water 
and different treatment methods employed. The results of all analyses 
per quarter shall be arithmetically averaged and reported to the State 
within 30 days of the system's receipt of such results. Results shall 
also be reported to EPA until such monitoring requirements have been 
adopted by the State. All samples collected shall be used in the 
computation of the average, unless the analytical results are 
invalidated for technical reasons. Sampling and analyses shall be 
conducted in accordance with the methods listed in paragraph (e) of this 
section.
    (2) Upon the written request of a community water system, the 
monitoring frequency required by paragraph (b)(1) of this section may be 
reduced by the State to a minimum of one sample analyzed for TTHMs per 
quarter taken at a point in the distribution system reflecting the 
maximum residence time of the water in the system, upon a written 
determination by the State that the data from at least 1 year of 
monitoring in accordance with paragraph (b)(1) of this section and local 
conditions demonstrate that total trihalomethane concentrations will be 
consistently below the maximum contaminant level.
    (3) If at any time during which the reduced monitoring frequency 
prescribed under this paragraph applies, the results from any analysis 
exceed 0.10 mg/l of TTHMs and such results are confirmed by at least one 
check sample taken promptly after such results are received, or if the 
system makes any significant change to its source of water or treatment 
program, the system shall immediately begin monitoring in accordance 
with the requirements of paragraph (b)(1) of this section, which 
monitoring shall continue for at least 1 year before the frequency may 
be reduced again. At the option of the State, a system's monitoring 
frequency may and should be increased above the minimum in those cases 
where it is necessary to detect variations of TTHM levels within the 
distribution system.
    (c)(1) Upon written request to the State, a community water system 
utilizing only ground water sources may seek to have the monitoring 
frequency required by paragraph (b)(1) of this section reduced to a 
minimum of one sample for maximum TTHM potential per year for each 
treatment plant used by the system taken at a point in the distribution 
system reflecting maximum residence time of the water in the system. The 
system shall submit the results of at least one sample for maximum TTHM 
potential using the procedure specified in paragraph (g) of this 
section. A sample must be analyzed from each treatment plant used by the 
system and be taken at a point in the distribution system reflecting the 
maximum residence time of the water in

[[Page 376]]

the system. The system's monitoring frequency may only be reduced upon a 
written determination by the State that, based upon the data submitted 
by the system, the system has a maximum TTHM potential of less than 0.10 
mg/l and that, based upon an assessment of the local conditions of the 
system, the system is not likely to approach or exceed the maximum 
contaminant level for total TTHMs. The results of all analyses shall be 
reported to the State within 30 days of the system's receipt of such 
results. Results shall also be reported to EPA until such monitoring 
requirements have been adopted by the State. All samples collected shall 
be used for determining whether the system must comply with the 
monitoring requirements of paragraph (b) of this section, unless the 
analytical results are invalidated for technical reasons. Sampling and 
analyses shall be conducted in accordance with the methods listed in 
paragraph (e) of this section.
    (2) If at any time during which the reduced monitoring frequency 
prescribed under paragraph (c)(1) of this section applies, the results 
from any analysis taken by the system for maximum TTHM potential are 
equal to or greater than 0.10 mg/l, and such results are confirmed by at 
least one check sample taken promptly after such results are received, 
the system shall immediately begin monitoring in accordance with the 
requirements of paragraph (b) of this section and such monitoring shall 
continue for at least one year before the frequency may be reduced 
again. In the event of any significant change to the system's raw water 
or treatment program, the system shall immediately analyze an additional 
sample for maximum TTHM potential taken at a point in the distribution 
system reflecting maximum residence time of the water in the system for 
the purpose of determining whether the system must comply with the 
monitoring requirements of paragraph (b) of this section. At the option 
of the State, monitoring frequencies may and should be increased above 
the minimum in those cases where this is necessary to detect variation 
of TTHM levels within the distribution system.
    (d) Compliance with Sec. 141.12 shall be determined based on a 
running annual average of quarterly samples collected by the system as 
prescribed in paragraph (b)(1) or (2) of this section. If the average of 
samples covering any 12 month period exceeds the Maximum Contaminant 
Level, the supplier of water shall report to the State pursuant to 
Sec. 141.31 and notify the public pursuant to Sec. 141.32. Monitoring 
after public notification shall be at a frequency designated by the 
State and shall continue until a monitoring schedule as a condition to a 
variance, exemption or enforcement action shall become effective.
    (e) Sampling and analyses made pursuant to this section shall be 
conducted by one of the total trihalomethane methods as directed in 
Sec. 141.24(e), and the Technical Notes on Drinking Water Methods, EPA-
600/R-94-173, October 1994, which is available from NTIS, PB-104766. 
Samples for TTHM shall be dechlorinated upon collection to prevent 
further production of trihalomethanes, according to the procedures 
described in the methods, except acidification is not required if only 
THMs or TTHMs are to be determined. Samples for maximum TTHM potential 
should not be dechlorinated or acidified, and should be held for seven 
days at 25  deg.C (or above) prior to analysis.
    (f) Before a community water system makes any significant 
modifications to its existing treatment process for the purposes of 
achieving compliance with Sec. 141.12, such system must submit and 
obtain State approval of a detailed plan setting forth its proposed 
modification and those safeguards that it will implement to ensure that 
the bacteriological quality of the drinking water served by such system 
will not be adversely affected by such modification. Each system shall 
comply with the provisions set forth in the State-approved plan. At a 
minimum, a State approved plan shall require the system modifying its 
disinfection practice to:
    (1) Evaluate the water system for sanitary defects and evaluate the 
source water for biological quality;
    (2) Evaluate its existing treatment practices and consider 
improvements

[[Page 377]]

that will minimize disinfectant demand and optimize finished water 
quality throughout the distribution system;
    (3) Provide baseline water quality survey data of the distribution 
system. Such data should include the results from monitoring for 
coliform and fecal coliform bacteria, fecal streptococci, standard plate 
counts at 35  deg.C and 20  deg.C, phosphate, ammonia nitrogen and total 
organic carbon. Virus studies should be required where source waters are 
heavily contaminated with sewage effluent;
    (4) Conduct additional monitoring to assure continued maintenance of 
optimal biological quality in finished water, for example, when 
chloramines are introduced as disinfectants or when pre-chlorination is 
being discontinued. Additional monitoring should also be required by the 
State for chlorate, chlorite and chlorine dioxide when chlorine dioxide 
is used. Standard plate count analyses should also be required by the 
State as appropriate before and after any modifications;
    (5) Consider inclusion in the plan of provisions to maintain an 
active disinfectant residual throughout the distribution system at all 
times during and after the modification.
    (g) The water sample for determination of maximum total 
trihalomethane potential is taken from a point in the distribution 
system that reflects maximum residence time. Procedures for sample 
collection and handling are given in the methods. No reducing agent is 
added to ``quench'' the chemical reaction producing THMs at the time of 
sample collection. The intent is to permit the level of THM precursors 
to be depleted and the concentration of THMs to be maximized for the 
supply being tested. Four experimental parameters affecting maximum THM 
production are pH, temperature, reaction time and the presence of a 
disinfectant residual. These parameters are dealt with as follows: 
Measure the disinfectant residual at the selected sampling point. 
Proceed only if a measurable disinfectant residual is present. Collect 
triplicate 40 ml water samples at the pH prevailing at the time of 
sampling, and prepare a method blank according to the methods. Seal and 
store these samples together for seven days at 25  deg.C or above. After 
this time period, open one of the sample containers and check for 
disinfectant residual. Absence of a disinfectant residual invalidates 
the sample for further analysis. Once a disinfectant residual has been 
demonstrated, open another of the sealed samples and determine total THM 
concentration using an approved analytical method.
    (h) The requirements in paragraphs (a) through (g) of this section 
apply to subpart H community water systems which serve a population of 
10,000 or more until December 16, 2001. The requirements in paragraphs 
(a) through (g) of this section apply to community water systems which 
use only ground water not under the direct influence of surface water 
that add a disinfectant (oxidant) in any part of the treatment process 
and serve a population of 10,000 or more until December 16, 2003. After 
December 16, 2003, this section is no longer applicable.

[44 FR 68641, Nov. 29, 1979, as amended at 45 FR 15545, 15547, Mar. 11, 
1980; 58 FR 41345, Aug. 3, 1993; 59 FR 62469, Dec. 5, 1994; 60 FR 34085, 
June 29, 1995; 63 FR 69464, Dec. 16, 1998]



       Subpart D--Reporting, Public Notification 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

[[Page 378]]

which would normally receive such notification from the supplier.
    (d) The water supply system, within ten days of completion of each 
public notification required pursuant to Sec. 141.32, shall submit to 
the State a representative copy of each type of notice distributed, 
published, posted, and/or made available to the persons served by the 
system and/or 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]



Sec. 141.32  Public notification.

    The requirements in this section are effective April 28, 1989. The 
requirements of Sec. 141.36 apply until April 28, 1989.
    (a) Maximum contaminant levels (MCLs), maximum residual disinfectant 
levels (MRDLs). The owner or operator of a public water system which 
fails to comply with an applicable MCL or treatment technique 
established by this part or which fails to comply with the requirements 
of any schedule prescribed pursuant to a variance or exemption, shall 
notify persons served by the system as follows:
    (1) Except as provided in paragraph (a)(3) of this section, the 
owner or operator of a public water system must give notice:
    (i) By publication in a daily newspaper of general circulation in 
the area served by the system as soon as possible, but in no case later 
than 14 days after the violation or failure. If the area served by a 
public water system is not served by a daily newspaper of general 
circulation, notice shall instead be given by publication in a weekly 
newspaper of general circulation serving the area; and
    (ii) By mail delivery (by direct mail or with the water bill), or by 
hand delivery, not later than 45 days after the violation or failure. 
The State may waive mail or hand delivery if it determines that the 
owner or operator of the public water system in violation has corrected 
the violation or failure within the 45-day period. The State must make 
the waiver in writing and within the 45-day period; and
    (iii) For violations of the MCLs of contaminants or MRDLs of 
disinfectants that may pose an acute risk to human health, by furnishing 
a copy of the notice to the radio and television stations serving the 
area served by the public water system as soon as possible but in no 
case later than 72 hours after the violation. The following violations 
are acute violations:
    (A) Any violations specified by the State as posing an acute risk to 
human health.
    (B) Violation of the MCL for nitrate or nitrite as defined in 
Sec. 141.62 and determined according to Sec. 141.23(i)(3).
    (C) Violation of the MCL for total coliforms, when fecal coliforms 
or E. coli are present in the water distribution system, as specified in 
Sec. 141.63(b).
    (D) Occurrence of a waterborne disease outbreak, as defined in 
Sec. 141.2, in an unfiltered system subject to the requirements of 
subpart H of this part, after December 30, 1991 (see Sec. 141.71(b)(4)).
    (E) Violation of the MRDL for chlorine dioxide as defined in 
Sec. 141.65 and determined according to Sec. 141.133(c)(2).
    (2) Except as provided in paragraph (a)(3) of this section, 
following the initial notice given under paragraph (a)(1) of this 
section, the owner or operator of the public water system must give 
notice at least once every three months by mail delivery (by direct mail 
or with the water bill) or by hand delivery, for as long as the 
violation or failure exists.
    (3)(i) In lieu of the requirements of paragraphs (a) (1) and (2) of 
this section, the owner or operator of a community water system in an 
area that is not served by a daily or weekly newspaper of general 
circulation must give notice by hand delivery or by continuous posting 
in conspicuous places within the area served by the system. Notice by 
hand delivery or posting must begin as soon as possible, but no later 
than 72 hours after the violation

[[Page 379]]

or failure for acute violations (as defined in paragraph (a)(1)(iii) of 
this section), or 14 days after the violation or failure (for any other 
violation). Posting must continue for as long as the violation or 
failure exists. Notice by hand delivery must be repeated at least every 
three months for as long as the violation or failure exists.
    (ii) In lieu of the requirements of paragraphs (a) (1) and (2) of 
this section, the owner or operator of a non-community water system may 
give notice by hand delivery or by continuous posting in conspicuous 
places within the area served by the system. Notice by hand delivery or 
posting must begin as soon as possible, but no later than 72 hours after 
the violation or failure for acute violations (as defined in paragraph 
(a)(1)(iii) of this section), or 14 days after the violation or failure 
(for any other violation). Posting must continue for as long as the 
violation or failure exists. Notice by hand delivery must be repeated at 
least every three months for as long as the violation or failure exists.
    (b) Other violations, variances, exemptions. The owner or operator 
of a public water system which fails to perform monitoring required by 
section 1445(a) of the Act (including monitoring required by the 
National Primary Drinking Water Regulations (NPDWRs) of this part), 
fails to comply with a testing procedure established by this part, is 
subject to a variance granted under section 1415(a)(1)(A) or 1415(a)(2) 
of the Act, or is subject to an exemption under section 1416 of the Act, 
shall notify persons served by the system as follows:
    (1) Except as provided in paragraph (b)(3) or (b)(4) of this 
section, the owner or operator of a public water system must give notice 
within three months of the violation or granting of a variance or 
exemption by publication in a daily newspaper of general circulation in 
the area served by the system. If the area served by a public water 
system is not served by a daily newspaper of general circulation, notice 
shall instead be given by publication in a weekly newspaper of general 
circulation serving the area.
    (2) Except as provided in paragraph (b)(3) or (b)(4) of this 
section, following the initial notice given under paragraph (b)(1) of 
this section, the owner or operator of the public water system must give 
notice at least once every three months by mail delivery (by direct mail 
or with the water bill) or by hand delivery, for as long as the 
violation exists. Repeat notice of the existence of a variance or 
exemption must be given every three months for as long as the variance 
or exemption remains in effect.
    (3)(i) In lieu of the requirements of paragraphs (b)(1) and (b)(2) 
of this section, the owner or operator of a community water system in an 
area that is not served by a daily or weekly newspaper of general 
circulation must give notice, within three months of the violation or 
granting of the variance or exemption, by hand delivery or by continuous 
posting in conspicuous places with the area served by the system. 
Posting must continue for as long as the violation exists or a variance 
or exemption remains in effect. Notice by hand delivery must be repeated 
at least every three months for as long as the violation exists or a 
variance or exemption remains in effect.
    (ii) In lieu of the requirements of paragraphs (b)(1) and (b)(2) of 
this section, the owner or operator of a non-community water system may 
give notice, within three months of the violation or the granting of the 
variance or exemption, by hand delivery or by continuous posting in 
conspicuous places within the area served by the system. Posting must 
continue for as long as the violation exists, or a variance or exemption 
remains in effect. Notice by hand delivery must be repeated at least 
every three months for as long as the violation exists or a variance or 
exemption remains in effect.
    (4) In lieu of the requirements of paragraphs (b)(1), (b)(2), and 
(b)(3) of this section, the owner or operator of a public water system, 
at the discretion of the State, may provide less frequent notice for 
minor monitoring violations as defined by the State, if EPA has approved 
the State's application for a program revision under Sec. 142.16. Notice 
of such violations must be given no less frequently than annually.
    (c) Notice to new billing units. The owner or operator of a 
community

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water system must give a copy of the most recent public notice for any 
outstanding violation of any maximum contaminant level, or any maximum 
residual disinfectant level, or any treatment technique requirement, or 
any variance or exemption schedule to all new billing units or new 
hookups prior to or at the time service begins.
    (d) General content of public notice. Each notice required by this 
section must provide a clear and readily understandable explanation of 
the violation, any potential adverse health effects, the population at 
risk, the steps that the public water system is taking to correct such 
violation, the necessity for seeking alternative water supplies, if any, 
and any preventive measures the consumer should take until the violation 
is corrected. Each notice shall be conspicuous and shall not contain 
unduly technical language, unduly small print, or similar problems that 
frustrate the purpose of the notice. Each notice shall include the 
telephone number of the owner, operator, or designee of the public water 
system as a source of additional information concerning the notice. 
Where appropriate, the notice shall be multi-lingual.
    (e) Mandatory health effects language. When providing the 
information on potential adverse health effects required by paragraph 
(d) of this section in notices of violations of maximum contaminant 
levels or treatment technique requirements, or notices of the granting 
or the continued existence of exemptions or variances, or notices of 
failure to comply with a variance or exemption schedule, the owner or 
operator of a public water system shall include the language specified 
below for each contaminant. (If language for a particular contaminant is 
not specified below at the time notice is required, this paragraph does 
not apply.)
    (1) Trichloroethylene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
trichloroethylene is a health concern at certain levels of exposure. 
This chemical is a common metal cleaning and dry cleaning fluid. It 
generally gets into drinking water by improper waste disposal. This 
chemical has been shown to cause cancer in laboratory animals such as 
rats and mice when the animals are exposed at high levels over their 
lifetimes. Chemicals that cause cancer in laboratory animals also may 
increase the risk of cancer in humans who are exposed at lower levels 
over long periods of time. EPA has set forth the enforceable drinking 
water standard for trichloroethylene at 0.005 parts per million (ppm) to 
reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. Drinking water which meets this 
standard is associated with little to none of this risk and should be 
considered safe.
    (2) Carbon tetrachloride. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
carbon tetrachloride is a health concern at certain levels of exposure. 
This chemical was once a popular household cleaning fluid. It generally 
gets into drinking water by improper waste disposal. This chemical has 
been shown to cause cancer in laboratory animals such as rats and mice 
when the animals are exposed at high levels over their lifetimes. 
Chemicals that cause cancer in laboratory animals also may increase the 
risk of cancer in humans who are exposed at lower levels over long 
periods of of time. EPA has set the enforceable drinking water standard 
for carbon tetrachloride at 0.005 parts per million (ppm) to reduce the 
risk of cancer or other adverse health effects which have been observed 
in laboratory animals. Drinking water which meets this standard is 
associated with little to none of this risk and should be considered 
safe.
    (3) 1,2-Dichloroethane. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 1,2-
dichloroethane is a health concern at certain levels of exposure. This 
chemical is used as a cleaning fluid for fats, oils, waxes, and resins. 
It generally gets into drinking water from improper waste disposal. This 
chemical has been shown to cause cancer in laboratory animals such as 
rats and mice when the animals are exposed at high levels over their 
lifetimes. Chemicals that cause cancer in laboratory animals also may 
increase the risk of cancer in

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humans who are exposed at lower levels over long periods of time. EPA 
has set the enforceable drinking water standard for 1,2-dichloroethane 
at 0.005 parts per million (ppm) to reduce the risk of cancer or other 
adverse health effects which have been observed in laboratory animals. 
Drinking water which meets this standard is associated with little to 
none of this risk and should be considered safe.
    (4) Vinyl chloride. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that vinyl 
chloride is a health concern at certain levels of exposure. This 
chemical is used in industry and is found in drinking water as a result 
of the breakdown of related solvents. The solvents are used as cleaners 
and degreasers of metals and generally get into drinking water by 
improper waste disposal. This chemical has been associated with 
significantly increased risks of cancer among certain industrial workers 
who were exposed to relatively large amounts of this chemical during 
their working careers. This chemical has also been shown to cause cancer 
in laboratory animals when the animals are exposed at high levels over 
their lifetimes. Chemicals that cause increased risk of cancer among 
exposed industrial workers and in laboratory animals also may increase 
the risk of cancer in humans who are exposed at lower levels over long 
periods of time. EPA has set the enforceable drinking water standard for 
vinyl chloride at 0.002 part per million (ppm) to reduce the risk of 
cancer or other adverse health effects which have been observed in 
humans and laboratory animals. Drinking water which meets this standard 
is associated with little to none of this risk and should be considered 
safe.
    (5) Benzene. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that benzene is a 
health concern at certain levels of exposure. This chemical is used as a 
solvent and degreaser of metals. It is also a major component of 
gasoline. Drinking water contamination generally results from leaking 
undergound gasoline and petroleum tanks or improper waste disposal. This 
chemical has been associated with significantly increased risks of 
leukemia among certain industrial workers who were exposed to relatively 
large amounts of this chemical during their working careers. This 
chemical has also been shown to cause cancer in laboratory animals when 
the animals are exposed at high levels over their lifetimes. Chemicals 
that cause increased risk of cancer among exposed industrial workers and 
in laboratory animals also may increase the risk of cancer in humans who 
are exposed at lower levels over long periods of time. EPA has set the 
enforceable drinking water standard for benzene at 0.005 parts per 
million (ppm) to reduce the risk of cancer or other adverse health 
effects which have been observed in humans and laboratory animals. 
Drinking water which meets this standard is associated with little to 
none of this risk and should be considered safe.
    (6) 1,1-Dichloroethylene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 1,1-
dichloroethylene is a health concern at certain levels of exposure. This 
chemical is used in industry and is found in drinking water as a result 
of the breakdown of related solvents. The solvents are used as cleaners 
and degreasers of metals and generally get into drinking water by 
improper waste disposal. This chemical has been shown to cause liver and 
kidney damage in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals which 
cause adverse effects in laboratory animals also may cause adverse 
health effects in humans who are exposed at lower levels over long 
periods of time. EPA has set the enforceable drinking water standard for 
1,1-dichloroethylene at 0.007 parts per million (ppm) to reduce the risk 
of these adverse health effects which have been observed in laboratory 
animals. Drinking water which meets this standard is associated with 
little to none of this risk and should be considered safe.
    (7) Para-dichlorobenzene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that para-
dichlorobenzene is a health concern at certain levels of exposure. This

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chemical is a component of deodorizers, moth balls, and pesticides. It 
generally gets into drinking water by improper waste disposal. This 
chemical has been shown to cause liver and kidney damage in laboratory 
animals such as rats and mice when the animals are exposed to high 
levels over their lifetimes. Chemicals which cause adverse effects in 
laboratory animals also may cause adverse health effects in humans who 
are exposed at lower levels over long periods of time. EPA has set the 
enforceable drinking water standard for para-dichlorobenzene at 0.075 
parts per million (ppm) to reduce the risk of these adverse health 
effects which have been observed in laboratory animals. Drinking water 
which meets this standard is associated with little to none of this risk 
and should be considered safe.
    (8) 1,1,1-Trichloroethane. The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that the 1,1,1-trichloroethane is a health concern at certain levels of 
exposure. This chemical is used as a cleaner and degreaser of metals. It 
generally gets into drinking water by improper waste disposal. This 
chemical has been shown to damage the liver, nervous system, and 
circulatory system of laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Some industrial 
workers who were exposed to relatively large amounts of this chemical 
during their working careers also suffered damage to the liver, nervous 
system, and circulatory system. Chemicals which cause adverse effects 
among exposed industrial workers and in laboratory animals also may 
cause adverse health effects in humans who are exposed at lower levels 
over long periods of time. EPA has set the enforceable drinking water 
standard for 1,1,1-trichloroethane at 0.2 parts per million (ppm) to 
protect against the risk of these adverse health effects which have been 
observed in humans and laboratory animals. Drinking water which meets 
this standard is associated with little to none of this risk and should 
be considered safe.
    (9) Fluoride.
    [Note: EPA is not specifying language that must be included in a 
public notice for a violation of the fluoride maximum contaminant level 
in this section because Sec. 143.5 of this part includes the necessary 
information. See paragraph (f) of this section.]
    (10) Microbiological contaminants (for use when there is a violation 
of the treatment technique requirements for filtration and disinfection 
in subpart H or subpart P of this part). The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that the presence of microbiological contaminants are a health concern 
at certain levels of exposure. If water is inadequately treated, 
microbiological contaminants in that water may cause disease. Disease 
symptoms may include diarrhea, cramps, nausea, and possibly jaundice, 
and any associated headaches and fatigue. These symptoms, however, are 
not just associated with disease-causing organisms in drinking water, 
but also may be caused by a number of factors other than your drinking 
water. EPA has set enforceable requirements for treating drinking water 
to reduce the risk of these adverse health effects. Treatment such as 
filtering and disinfecting the water removes or destroys microbiological 
contaminants. Drinking water which is treated to meet EPA requirements 
is associated with little to none of this risk and should be considered 
safe.
    (11) Total coliforms (To be used when there is a violation of 
Sec. 141.63(a), and not a violation of Sec. 141.63(b)). The United 
States Environmental Protection Agency (EPA) sets drinking water 
standards and has determined that the presence of total coliforms is a 
possible health concern. Total coliforms are common in the environment 
and are generally not harmful themselves. The presence of these bacteria 
in drinking water, however, generally is a result of a problem with 
water treatment or the pipes which distribute the water, and indicates 
that the water may be contaminated with organisms that can cause 
disease. Disease symptoms may include diarrhea, cramps, nausea, and 
possibly jaundice, and any associated headaches and fatigue. These 
symptoms, however, are not just associated with disease-causing 
organisms in drinking water, but also may be caused

[[Page 383]]

by a number of factors other than your drinking water. EPA has set an 
enforceable drinking water standard for total coliforms to reduce the 
risk of these adverse health effects. Under this standard, no more than 
5.0 percent of the samples collected during a month can contain these 
bacteria, except that systems collecting fewer than 40 samples/month 
that have one total coliform-positive sample per month are not violating 
the standard. Drinking water which meets this standard is usually not 
associated with a health risk from disease-causing bacteria and should 
be considered safe.
    (12) Fecal Coliforms/E. coli (To be used when there is a violation 
of Sec. 141.63(b) or both Sec. 141.63 (a) and (b)). The United States 
Environmental Protection Agency (EPA) sets drinking water standards and 
has determined that the presence of fecal coliforms or E. coli is a 
serious health concern. Fecal coliforms and E. coli are generally not 
harmful themselves, but their presence in drinking water is serious 
because they usually are associated with sewage or animal wastes. The 
presence of these bacteria in drinking water is generally a result of a 
problem with water treatment or the pipes which distribute the water, 
and indicates that the water may be contaminated with organisms that can 
cause disease. Disease symptoms may include diarrhea, cramps, nausea, 
and possibly jaundice, and associated headaches and fatigue. These 
symptoms, however, are not just associated with disease-causing 
organisms in drinking water, but also may be caused by a number of 
factors other than your drinking water. EPA has set an enforceable 
drinking water standard for fecal coliforms and E. coli to reduce the 
risk of these adverse health effects. Under this standard all drinking 
water samples must be free of these bacteria. Drinking water which meets 
this standard is associated with little or none of this risk and should 
be considered safe. State and local health authorities recommend that 
consumers take the following precautions: [To be inserted by the public 
water system, according to instructions from State or local 
authorities].
    (13) Lead. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that lead is a health 
concern at certain exposure levels. Materials that contain lead have 
frequently been used in the construction of water supply distribution 
systems, and plumbing systems in private homes and other buildings. The 
most commonly found materials include service lines, pipes, brass and 
bronze fixtures, and solders and fluxes. Lead in these materials can 
contaminate drinking water as a result of the corrosion that takes place 
when water comes into contact with those materials. Lead can cause a 
variety of adverse health effects in humans. At relatively low levels of 
exposure, these effects may include interference with red blood cell 
chemistry, delays in normal physical and mental development in babies 
and young children, slight deficits in the attention span, hearing, and 
learning abilities of children, and slight increases in the blood 
pressure of some adults. EPA's national primary drinking water 
regulation requires all public water systems to optimize corrosion 
control to minimize lead contamination resulting from the corrosion of 
plumbing materials. Public water systems serving 50,000 people or fewer 
that have lead concentrations below 15 parts per billion (ppb) in more 
than 90% of tap water samples (the EPA ``action level'') have optimized 
their corrosion control treatment. Any water system that exceeds the 
action level must also monitor their source water to determine whether 
treatment to remove lead in source water is needed. Any water system 
that continues to exceed the action level after installation of 
corrosion control and/or source water treatment must eventually replace 
all lead service lines contributing in excess of 15 (ppb) of lead to 
drinking water. Any water system that exceeds the action level must also 
undertake a public education program to inform consumers of ways they 
can reduce their exposure to potentially high levels of lead in drinking 
water.
    (14) Copper. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that copper is a health 
concern at certain exposure levels. Copper, a reddish-brown metal, is 
often used to plumb residential and commercial

[[Page 384]]

structures that are connected to water distribution systems. Copper 
contaminating drinking water as a corrosion byproduct occurs as the 
result of the corrosion of copper pipes that remain in contact with 
water for a prolonged period of time. Copper is an essential nutrient, 
but at high doses it has been shown to cause stomach and intestinal 
distress, liver and kidney damage, and anemia. Persons with Wilson's 
disease may be at a higher risk of health effects due to copper than the 
general public. EPA's national primary drinking water regulation 
requires all public water systems to install optimal corrosion control 
to minimize copper contamination resulting from the corrosion of 
plumbing materials. Public water systems serving 50,000 people or fewer 
that have copper concentrations below 1.3 parts per million (ppm) in 
more than 90% of tap water samples (the EPA ``action level'') are not 
required to install or improve their treatment. Any water system that 
exceeds the action level must also monitor their source water to 
determine whether treatment to remove copper in source water is needed.
    (15) Asbestos. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that asbestos 
fibers greater than 10 micrometers in length are a health concern at 
certain levels of exposure. Asbestos is a naturally occurring mineral. 
Most asbestos fibers in drinking water are less than 10 micrometers in 
length and occur in drinking water from natural sources and from 
corroded asbestos-cement pipes in the distribution system. The major 
uses of asbestos were in the production of cements, floor tiles, paper 
products, paint, and caulking; in transportation-related applications; 
and in the production of textiles and plastics. Asbestos was once a 
popular insulating and fire retardent material. Inhalation studies have 
shown that various forms of asbestos have produced lung tumors in 
laboratory animals. The available information on the risk of developing 
gastrointestinal tract cancer associated with the ingestion of asbestos 
from drinking water is limited. Ingestion of intermediate-range 
chrysotile asbestos fibers greater than 10 micrometers in length is 
associated with causing benign tumors in male rats. Chemicals that cause 
cancer in laboratory animals also may increase the risk of cancer in 
humans who are exposed over long periods of time. EPA has set the 
drinking water standard for asbestos at 7 million long fibers per liter 
to reduce the potential risk of cancer or other adverse health effects 
which have been observed in laboratory animals. Drinking water which 
meets the EPA standard is associated with little to none of this risk 
and should be considered safe with respect to asbestos.
    (16) Barium. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that barium is a health 
concern at certain levels of exposure. This inorganic chemical occurs 
naturally in some aquifers that serve as sources of ground water. It is 
also used in oil and gas drilling muds, automotive paints, bricks, tiles 
and jet fuels. It generally gets into drinking water after dissolving 
from naturally occurring minerals in the ground. This chemical may 
damage the heart and cardiovascular system, and is associated with high 
blood pressure in laboratory animals such as rats exposed to high levels 
during their lifetimes. In humans, EPA believes that effects from barium 
on blood pressure should not occur below 2 parts per million (ppm) in 
drinking water. EPA has set the drinking water standard for barium at 2 
parts per million (ppm) to protect against the risk of these adverse 
health effects. Drinking water that meets the EPA standard is associated 
with little to none of this risk and is considered safe with respect to 
barium.
    (17) Cadmium. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that cadmium is a 
health concern at certain levels of exposure. Food and the smoking of 
tobacco are common sources of general exposure. This inorganic metal is 
a contaminant in the metals used to galvanize pipe. It generally gets 
into water by corrosion of galvanized pipes or by improper waste 
disposal. This chemical has been shown to damage the kidney in animals 
such as rats and mice when the animals are exposed at high levels over

[[Page 385]]

their lifetimes. Some industrial workers who were exposed to relatively 
large amounts of this chemical during working careers also suffered 
damage to the kidney. EPA has set the drinking water standard for 
cadmium at 0.005 parts per million (ppm) to protect against the risk of 
these adverse health effects. Drinking water that meets the EPA standard 
is associated with little to none of this risk and is considered safe 
with respect to cadmium.
    (18) Chromium. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that chromium is 
a health concern at certain levels of exposure. This inorganic metal 
occurs naturally in the ground and is often used in the electroplating 
of metals. It generally gets into water from runoff from old mining 
operations and improper waste disposal from plating operations. This 
chemical has been shown to damage the kidney, nervous system, and the 
circulatory system of laboratory animals such as rats and mice when the 
animals are exposed at high levels. Some humans who were exposed to high 
levels of this chemical suffered liver and kidney damage, dermatitis and 
respiratory problems. EPA has set the drinking water standard for 
chromium at 0.1 parts per million (ppm) to protect against the risk of 
these adverse health effects. Drinking water that meets the EPA standard 
is associated with little to none of this risk and is considered safe 
with respect to chromium.
    (19) Mercury. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that mercury is a 
health concern at certain levels of exposure. This inorganic metal is 
used in electrical equipment and some water pumps. It usually gets into 
water as a result of improper waste disposal. This chemical has been 
shown to damage the kidney of laboratory animals such as rats when the 
animals are exposed at high levels over their lifetimes. EPA has set the 
drinking water standard for mercury at 0.002 parts per million (ppm) to 
protect against the risk of these adverse health effects. Drinking water 
that meets the EPA standard is associated with little to none of this 
risk and is considered safe with respect to mercury.
    (20) Nitrate. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that nitrate 
poses an acute health concern at certain levels of exposure. Nitrate is 
used in fertilizer and is found in sewage and wastes from human and/or 
farm animals and generally gets into drinking water from those 
activities. Excessive levels of nitrate in drinking water have caused 
serious illness and sometimes death in infants under six months of age. 
The serious illness in infants is caused because nitrate is converted to 
nitrite in the body. Nitrite interferes with the oxygen carrying 
capacity of the child's blood. This is an acute disease in that symptoms 
can develop rapidly in infants. In most cases, health deteriorates over 
a period of days. Symptoms include shortness of breath and blueness of 
the skin. Clearly, expert medical advice should be sought immediately if 
these symptoms occur. The purpose of this notice is to encourage parents 
and other responsible parties to provide infants with an alternate 
source of drinking water. Local and State health authorities are the 
best source for information concerning alternate sources of drinking 
water for infants. EPA has set the drinking water standard at 10 parts 
per million (ppm) for nitrate to protect against the risk of these 
adverse effects. EPA has also set a drinking water standard for nitrite 
at 1 ppm. To allow for the fact that the toxicity of nitrate and nitrite 
are additive, EPA has also established a standard for the sum of nitrate 
and nitrite at 10 ppm. Drinking water that meets the EPA standard is 
associated with little to none of this risk and is considered safe with 
respect to nitrate.
    (21) Nitrite. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that nitrite 
poses an acute health concern at certain levels of exposure. This 
inorganic chemical is used in fertilizers and is found in sewage and 
wastes from humans and/or farm animals and generally gets into drinking 
water as a result of those activities. While excessive levels of nitrite 
in drinking water have not been observed,

[[Page 386]]

other sources of nitrite have caused serious illness and sometimes death 
in infants under six months of age. The serious illness in infants is 
caused because nitrite interferes with the oxygen carrying capacity of 
the child's blood. This is an acute disease in that symptoms can develop 
rapidly. However, in most cases, health deteriorates over a period of 
days. Symptoms include shortness of breath and blueness of the skin. 
Clearly, expert medical advice should be sought immediately if these 
symptoms occur. The purpose of this notice is to encourage parents and 
other responsible parties to provide infants with an alternate source of 
drinking water. Local and State health authorities are the best source 
for information concerning alternate sources of drinking water for 
infants. EPA has set the drinking water standard at 1 part per million 
(ppm) for nitrite to protect against the risk of these adverse effects. 
EPA has also set a drinking water standard for nitrate (converted to 
nitrite in humans) at 10 ppm and for the sum of nitrate and nitrite at 
10 ppm. Drinking water that meets the EPA standard is associated with 
little to none of this risk and is considered safe with respect to 
nitrite.
    (22) Selenium. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that selenium is 
a health concern at certain high levels of exposure. Selenium is also an 
essential nutrient at low levels of exposure. This inorganic chemical is 
found naturally in food and soils and is used in electronics, photocopy 
operations, the manufacture of glass, chemicals, drugs, and as a 
fungicide and a feed additive. In humans, exposure to high levels of 
selenium over a long period of time has resulted in a number of adverse 
health effects, including a loss of feeling and control in the arms and 
legs. EPA has set the drinking water standard for selenium at 0.05 parts 
per million (ppm) to protect against the risk of these adverse health 
effects. Drinking water that meets the EPA standard is associated with 
little to none of this risk and is considered safe with respect to 
selenium.
    (23) Acrylamide. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that acrylamide 
is a health concern at certain levels of exposure. Polymers made from 
acrylamide are sometimes used to treat water supplies to remove 
particulate contaminants. Acrylamide has been shown to cause cancer in 
laboratory animals such as rats and mice when the animals are exposed at 
high levels over their lifetimes. Chemicals that cause cancer in 
laboratory animals also may increase the risk of cancer in humans who 
are exposed over long periods of time. Sufficiently large doses of 
acrylamide are known to cause neurological injury. EPA has set the 
drinking water standard for acrylamide using a treatment technique to 
reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. This treatment technique limits the 
amount of acrylamide in the polymer and the amount of the polymer which 
may be added to drinking water to remove particulates. Drinking water 
systems which comply with this treatment technique have little to no 
risk and are considered safe with respect to acrylamide.
    (24) Alachlor. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that alachlor is 
a health concern at certain levels of exposure. This organic chemical is 
a widely used pesticide. When soil and climatic conditions are 
favorable, alachlor may get into drinking water by runoff into surface 
water or by leaching into ground water. This chemical has been shown to 
cause cancer in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals that 
cause cancer in laboratory animals also may increase the risk of cancer 
in humans who are exposed over long periods of time. EPA has set the 
drinking water standard for alachlor at 0.002 parts per million (ppm) to 
reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. Drinking water that meets this 
standard is associated with little to none of this risk and is 
considered safe with respect to alachlor.

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    (25) Aldicarb. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that aldicarb is 
a health concern at certain levels of exposure. Aldicarb is a widely 
used pesticide. Under certain soil and climatic conditions (e.g., sandy 
soil and high rainfall), aldicarb may leach into ground water after 
normal agricultural applications to crops such as potatoes or peanuts or 
may enter drinking water supplies as a result of surface runoff. This 
chemical has been shown to damage the nervous system in laboratory 
animals such as rats and dogs exposed to high levels. EPA has set the 
drinking water standard for aldicarb at 0.003 parts per million (ppm) to 
protect against the risk of adverse health effects. Drinking water that 
meets the EPA standard is associated with little to none of this risk 
and is considered safe with respect to aldicarb.
    (26) Aldicarb sulfoxide. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
aldicarb sulfoxide is a health concern at certain levels of exposure. 
Aldicarb is a widely used pesticide. Aldicarb sulfoxide in ground water 
is primarily a breakdown product of aldicarb. Under certain soil and 
climatic conditions (e.g., sandy soil and high rainfall), aldicarb 
sulfoxide may leach into ground water after normal agricultural 
applications to crops such as potatoes or peanuts or may enter drinking 
water supplies as a result of surface runoff. This chemical has been 
shown to damage the nervous system in laboratory animals such as rats 
and dogs exposed to high levels. EPA has set the drinking water standard 
for aldicarb sulfoxide at 0.004 parts per million (ppm) to protect 
against the risk of adverse health effects. Drinking water that meets 
the EPA standard is associated with little to none of this risk and is 
considered safe with respect to aldicarb sulfoxide.
    (27) Aldicarb sulfone. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
aldicarb sulfone is a health concern at certain levels of exposure. 
Aldicarb is a widely used pesticide. Aldicarb sulfone is formed from the 
breakdown of aldicarb and is considered for registration as a pesticide 
under the name aldoxycarb. Under certain soil and climatic conditions 
(e.g., sandy soil and high rainfall), aldicarb sulfone may leach into 
ground water after normal agricultural applications to crops such as 
potatoes or peanuts or may enter drinking water supplies as a result of 
surface runoff. This chemical has been shown to damage the nervous 
system in laboratory animals such as rats and dogs exposed to high 
levels. EPA has set the drinking water standard for aldicarb sulfone at 
0.002 parts per million (ppm) to protect against the risk of adverse 
health effects. Drinking water that meets the EPA standard is associated 
with little to none of this risk and is considered safe with respect to 
aldicarb sulfone.
    (28) Atrazine. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that atrazine is 
a health concern at certain levels of exposure. This organic chemical is 
a herbicide. When soil and climatic conditions are favorable, atrazine 
may get into drinking water by runoff into surface water or by leaching 
into ground water. This chemical has been shown to affect offspring of 
rats and the heart of dogs. EPA has set the drinking water standard for 
atrazine at 0.003 parts per million (ppm) to protect against the risk of 
these adverse health effects. Drinking water that meets the EPA standard 
is associated with little to none of this risk and is considered safe 
with respect to atrazine.
    (29) Carbofuran. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that carbofuran 
is a health concern at certain levels of exposure. This organic chemical 
is a pesticide. When soil and climatic conditions are favorable, 
carbofuran may get into drinking water by runoff into surface water or 
by leaching into ground water. This chemical has been shown to damage 
the nervous and reproductive systems of laboratory animals such as rats 
and mice exposed at high levels over their lifetimes. Some humans who 
were exposed to relatively large amounts of this chemical during

[[Page 388]]

their working careers also suffered damage to the nervous system. 
Effects on the nervous system are generally rapidly reversible. EPA has 
set the drinking water standard for carbofuran at 0.04 parts per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water that meets the EPA standard is associated with little to 
none of this risk and is considered safe with respect to carbofuran.
    (30) Chlordane. The United States Environmental Protection Agency 
(EPA sets drinking water standards and has determined that chlordane is 
a health concern at certain levels of exposure. This organic chemical is 
a pesticide used to control termites. Chlordane is not very mobile in 
soils. It usually gets into drinking water after application near water 
supply intakes or wells. This chemical has been shown to cause cancer in 
laboratory animals such as rats and mice when the animals are exposed at 
high levels over their lifetimes. Chemicals that cause cancer in 
laboratory animals also may increase the risk of cancer in humans who 
are exposed over long periods of time. EPA has set the drinking water 
standard for chlordane at 0.002 parts per million (ppm) to reduce the 
risk of cancer or other adverse health effects which have been observed 
in laboratory animals. Drinking water that meets the EPA standard is 
associated with little to none of this risk and is considered safe with 
respect to chlordane.
    (31) Dibromochloropropane (DBCP). The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that DBCP is a health concern at certain levels of exposure. This 
organic chemical was once a popular pesticide. When soil and climatic 
conditions are favorable, dibromochloropropane may get into drinking 
water by runoff into surface water or by leaching into ground water. 
This chemical has been shown to cause cancer in laboratory animals such 
as rats and mice when the animals are exposed at high levels over their 
lifetimes. Chemicals that cause cancer in laboratory animals also may 
increase the risk of cancer in humans who are exposed over long periods 
of time. EPA has set the drinking water standard for DBCP at 0.0002 
parts per million (ppm) to reduce the risk of cancer or other adverse 
health effects which have been observed in laboratory animals. Drinking 
water that meets the EPA standard is associated with little to none of 
this risk and is considered safe with respect to DBCP.
    (32) o-Dichlorobenzene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that o-
dichlorobenzene is a health concern at certain levels of exposure. This 
organic chemical is used as a solvent in the production of pesticides 
and dyes. It generally gets into water by improper waste disposal. This 
chemical has been shown to damage the liver, kidney and the blood cells 
of laboratory animals such as rats and mice exposed to high levels 
during their lifetimes. Some industrial workers who were exposed to 
relatively large amounts of this chemical during working careers also 
suffered damage to the liver, nervous system, and circulatory system. 
EPA has set the drinking water standard for o-dichlorobenzene at 0.6 
parts per million (ppm) to protect against the risk of these adverse 
health effects. Drinking water that meets the EPA standard is associated 
with little to none of this risk and is considered safe with respect to 
o-dichlorobenzene.
    (33) cis-1,2-Dichloroethylene. The United States Environmental 
Protection Agency (EPA) establishes drinking water standards and has 
determined that cis-1,2-dichloroethylene is a health concern at certain 
levels of exposure. This organic chemical is used as a solvent and 
intermediate in chemical production. It generally gets into water by 
improper waste disposal. This chemical has been shown to damage the 
liver, nervous system, and circulatory system of laboratory animals such 
as rats and mice when exposed at high levels over their lifetimes. Some 
humans who were exposed to relatively large amounts of this chemical 
also suffered damage to the nervous system. EPA has set the drinking 
water standard for cis-1,2-dichloroethylene at 0.07 parts per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water that meets the EPA standard is associated with little

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to none of this risk and is considered safe with respect to cis-1,2-
dichloroethylene.
    (34) trans-1,2-Dichloroethylene. The United States Environmental 
Protection Agency (EPA) establishes drinking water standards and has 
determined that trans-1,2-dichloroethylene is a health concern at 
certain levels of exposure. This organic chemical is used as a solvent 
and intermediate in chemical production. It generally gets into water by 
improper waste disposal. This chemical has been shown to damage the 
liver, nervous system, and the circulatory system of laboratory animals 
such as rats and mice when exposed at high levels over their lifetimes. 
Some humans who were exposed to relatively large amounts of this 
chemical also suffered damage to the nervous system. EPA has set 
drinking water standard for trans-1,2-dichloroethylene at 0.1 parts per 
million (ppm) to protect against the risk of these adverse health 
effects. Drinking water that meets the EPA standard is associated with 
little to none of this risk and is considered safe with respect to 
trans-1,2-dichloroethylene.
    (35) 1,2-Dichloropropane. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 1,2-
dichloropropane is a health concern at certain levels of exposure. This 
organic chemical is used as a solvent and pesticide. When soil and 
climatic conditions are favorable, 1,2-dichloropropane may get into 
drinking water by runoff into surface water or by leaching into ground 
water. It may also get into drinking water through improper waste 
disposal. This chemical has been shown to cause cancer in laboratory 
animals such as rats and mice when the animals are exposed at high 
levels over their lifetimes. Chemicals that cause cancer in laboratory 
animals also may increase the risk of cancer in humans who are exposed 
over long periods of time. EPA has set the drinking water standard for 
1,2-dichloropropane at 0.005 parts per million (ppm) to reduce the risk 
of cancer or other adverse health effects which have been observed in 
laboratory animals. Drinking water that meets the EPA standard is 
associated with little to none of this risk and is considered safe with 
respect to 1,2-dichloropropane.
    (36) 2,4-D. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that 2,4-D is a health 
concern at certain levels of exposure. This organic chemical is used as 
a herbicide and to control algae in reservoirs. When soil and climatic 
conditions are favorable, 2,4-D may get into drinking water by runoff 
into surface water or by leaching into ground water. This chemical has 
been shown to damage the liver and kidney of laboratory animals such as 
rats exposed at high levels during their lifetimes. Some humans who were 
exposed to relatively large amounts of this chemical also suffered 
damage to the nervous system. EPA has set the drinking water standard 
for 2,4-D at 0.07 parts per million (ppm) to protect against the risk of 
these adverse health effects. Drinking water that meets the EPA standard 
is associated with little to none of this risk and is considered safe 
with respect to 2,4-D.
    (37) Epichlorohydrin. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
epichlorohydrin is a health concern at certain levels of exposure. 
Polymers made from epichlorohydrin are sometimes used in the treatment 
of water supplies as a flocculent to remove particulates. 
Epichlorohydrin generally gets into drinking water by improper use of 
these polymers. This chemical has been shown to cause cancer in 
laboratory animals such as rats and mice when the animals are exposed at 
high levels over their lifetimes. Chemicals that cause cancer in 
laboratory animals also may increase the risk of cancer in humans who 
are exposed over long periods of time. EPA has set the drinking water 
standard for epichlorohydrin using a treatment technique to reduce the 
risk of cancer or other adverse health effects which have been observed 
in laboratory animals. This treatment technique limits the amount of 
epichlorohydrin in the polymer and the amount of the polymer which may 
be added to drinking water as a flocculent to remove particulates. 
Drinking water systems which

[[Page 390]]

comply with this treatment technique have little to no risk and are 
considered safe with respect to epichlorohydrin.
    (38) Ethylbenzene. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined ethylbenzene is a 
health concern at certain levels of exposure. This organic chemical is a 
major component of gasoline. It generally gets into water by improper 
waste disposal or leaking gasoline tanks. This chemical has been shown 
to damage the kidney, liver, and nervous system of laboratory animals 
such as rats exposed to high levels during their lifetimes. EPA has set 
the drinking water standard for ethylbenzene at 0.7 part per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water that meets the EPA standard is associated with little to 
none of this risk and is considered safe with respect to ethylbenzene.
    (39) Ethylene dibromide (EDB). The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that EDB is a health concern at certain levels of exposure. This organic 
chemical was once a popular pesticide. When soil and climatic conditions 
are favorable, EDB may get into drinking water by runoff into surface 
water or by leaching into ground water. This chemical has been shown to 
cause cancer in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals that 
cause cancer in laboratory animals also may increase the risk of cancer 
in humans who are exposed over long periods of time. EPA has set the 
drinking water standard for EDB at 0.00005 part per million (ppm) to 
reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. Drinking water that meets this 
standard is associated with little to none of this risk and is 
considered safe with respect to EDB.
    (40) Heptachlor. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that heptachlor 
is a health concern at certain levels of exposure. This organic chemical 
was once a popular pesticide. When soil and climatic conditions are 
favorable, heptachlor may get into drinking water by runoff into surface 
water or by leaching into ground water. This chemical has been shown to 
cause cancer in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals that 
cause cancer in laboratory animals also may increase the risk of cancer 
in humans who are exposed over long periods of time. EPA has set the 
drinking water standards for heptachlor at 0.0004 part per million (ppm) 
to reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. Drinking water that meets this 
standard is associated with little to none of this risk and is 
considered safe with respect to heptachlor.
    (41) Heptachlor epoxide. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
heptachlor epoxide is a health concern at certain levels of exposure. 
This organic chemical was once a popular pesticide. When soil and 
climatic conditions are favorable, heptachlor expoxide may get into 
drinking water by runoff into surface water or by leaching into ground 
water. This chemical has been shown to cause cancer in laboratory 
animals such as rats and mice when the animals are exposed at high 
levels over their lifetimes. Chemicals that cause cancer in laboratory 
animals also may increase the risk of cancer in humans who are exposed 
over long periods of time. EPA has set the drinking water standards for 
heptachlor epoxide at 0.0002 part per million (ppm) to reduce the risk 
of cancer or other adverse health effects which have been observed in 
laboratory animals. Drinking water that meets this standard is 
associated with little to none of this risk and is considered safe with 
respect to heptachlor epoxide.
    (42) Lindane. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that lindane is a 
health concern at certain levels of exposure. This organic chemical is 
used as a pesticide. When soil and climatic conditions are favorable, 
lindane may get

[[Page 391]]

into drinking water by runoff into surface water or by leaching into 
ground water. This chemical has been shown to damage the liver, kidney, 
nervous system, and immune system of laboratory animals such as rats, 
mice and dogs exposed at high levels during their lifetimes. Some humans 
who were exposed to relatively large amounts of this chemical also 
suffered damage to the nervous system and circulatory system. EPA has 
established the drinking water standard for lindane at 0.0002 part per 
million (ppm) to protect against the risk of these adverse health 
effects. Drinking water that meets the EPA standard is associated with 
little to none of this risk and is considered safe with respect to 
lindane.
    (43) Methoxychlor. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that methoxychlor 
is a health concern at certain levels of exposure. This organic chemical 
is used as a pesticide. When soil and climatic conditions are favorable, 
methoxychlor may get into drinking water by runoff into surface water or 
by leaching into ground water. This chemical has been shown to damage 
the liver, kidney, nervous system, and reproductive system of laboratory 
animals such as rats exposed at high levels during their lifetimes. It 
has also been shown to produce growth retardation in rats. EPA has set 
the drinking water standard for methoxychlor at 0.04 part per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water that meets the EPA standard is associated with little to 
none of this risk and is considered safe with respect to methoxychlor.
    (44) Monochlorobenzene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
monochlorobenzene is a health concern at certain levels of exposure. 
This organic chemical is used as a solvent. It generally gets into water 
by improper waste disposal. This chemical has been shown to damage the 
liver, kidney and nervous system of laboratory animals such as rats and 
mice exposed to high levels during their lifetimes. EPA has set the 
drinking water standard for monochlorobenzene at 0.1 part per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water that meets the EPA standard is associated with little to 
none of this risk and is considered safe with respect to 
monochlorobenzene.
    (45) Polychlorinated biphenyls (PCBs). The United States 
Environmental Protection Agency (EPA) sets drinking water standards and 
has determined that polychlorinated biphenyls (PCBs) are a health 
concern at certain levels of exposure. These organic chemicals were once 
widely used in electrical transformers and other industrial equipment. 
They generally get into drinking water by improper waste disposal or 
leaking electrical industrial equipment. This chemical has been shown to 
cause cancer in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals that 
cause cancer in laboratory animals also may increase the risk of cancer 
in humans who are exposed over long periods of time. EPA has set the 
drinking water standard for PCBs at 0.0005 part per million (ppm) to 
reduce the risk of cancer or other adverse health effects which have 
been observed in laboratory animals. Drinking water that meets this 
standard is associated with little to none of this risk and is 
considered safe with respect to PCBs.
    (46) Pentachlorophenol. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
pentachlorophenol is a health concern at certain levels of exposure. 
This organic chemical is used as a wood preservative, herbicide, 
disinfectant, and defoliant. It generally gets into drinking water by 
runoff into surface water or leaching into ground water. This chemical 
has been shown to produce adverse reproductive effects and to damage the 
liver and kidneys of laboratory animals such as rats exposed to high 
levels during their lifetimes. Some humans who were exposed to 
relatively large amounts of this chemical also suffered damage to the 
liver and kidneys. This chemical has been shown to cause cancer in 
laboratory animals such as rats and mice when the animals are exposed to 
high levels over their lifetimes. Chemicals that cause

[[Page 392]]

cancer in laboratory animals also may increase the risk of cancer in 
humans who are exposed over long periods of time. EPA has set the 
drinking water standard for pentachlorophenol at 0.001 parts per million 
(ppm) to protect against the risk of cancer or other adverse health 
effects. Drinking water that meets the EPA standard is associated with 
little to none of this risk and is considered safe with respect to 
pentachlorophenol.
    (47) Styrene. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that styrene is a 
health concern at certain levels of exposure. This organic chemical is 
commonly used to make plastics and is sometimes a component of resins 
used for drinking water treatment. Styrene may get into drinking water 
from improper waste disposal. This chemical has been shown to damage the 
liver and nervous system in laboratory animals when exposed at high 
levels during their lifetimes. EPA has set the drinking water standard 
for styrene at 0.1 part per million (ppm) to protect against the risk of 
these adverse health effects. Drinking water that meets the EPA standard 
is associated with little to none of this risk and is considered safe 
with respect to styrene.
    (48) Tetrachloroethylene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
tetrachloroethylene is a health concern at certain levels of exposure. 
This organic chemical has been a popular solvent, particularly for dry 
cleaning. It generally gets into drinking water by improper waste 
disposal. This chemical has been shown to cause cancer in laboratory 
animals such as rats and mice when the animals are exposed at high 
levels over their lifetimes. Chemicals that cause cancer in laboratory 
animals also may increase the risk of cancer in humans who are exposed 
over long periods of time. EPA has set the drinking water standard for 
tetrachloroethylene at 0.005 part per million (ppm) to reduce the risk 
of cancer or other adverse health effects which have been observed in 
laboratory animals. Drinking water that meets this standard is 
associated with little to none of this risk and is considered safe with 
respect to tetrachloroethylene.
    (49) Toluene. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that toluene is a 
health concern at certain levels of exposure. This organic chemical is 
used as a solvent and in the manufacture of gasoline for airplanes. It 
generally gets into water by improper waste disposal or leaking 
underground storage tanks. This chemical has been shown to damage the 
kidney, nervous system, and circulatory system of laboratory animals 
such as rats and mice exposed to high levels during their lifetimes. 
Some industrial workers who were exposed to relatively large amounts of 
this chemical during working careers also suffered damage to the liver, 
kidney and nervous system. EPA has set the drinking water standard for 
toluene at 1 part per million (ppm) to protect against the risk of 
adverse health effects. Drinking water that meets the EPA standard is 
associated with little to none of this risk and is considered safe with 
respect to toluene.
    (50) Toxaphene. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that toxaphene is 
a health concern at certain levels of exposure. This organic chemical 
was once a pesticide widely used on cotton, corn, soybeans, pineapples 
and other crops. When soil and climatic conditions are favorable, 
toxaphene may get into drinking water by runoff into surface water or by 
leaching into ground water. This chemical has been shown to cause cancer 
in laboratory animals such as rats and mice when the animals are exposed 
at high levels over their lifetimes. Chemicals that cause cancer in 
laboratory animals also may increase the risk of cancer in humans who 
are exposed over long periods of time. EPA has set the drinking water 
standard for toxaphene at 0.003 part per million (ppm) to reduce the 
risk of cancer or other adverse health effects which have been observed 
in laboratory animals. Drinking water that meets this standard is 
associated with little to none of this risk and is considered safe with 
respect to toxaphene.

[[Page 393]]

    (51) 2,4,5-TP. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that 2,4,5-TP is 
a health concern at certain levels of exposure. This organic chemical is 
used as a herbicide. When soil and climatic conditions are favorable, 
2,4,5-TP may get into drinking water by runoff into surface water or by 
leaching into ground water. This chemical has been shown to damage the 
liver and kidney of laboratory animals such as rats and dogs exposed to 
high levels during their lifetimes. Some industrial workers who were 
exposed to relatively large amounts of this chemical during working 
careers also suffered damage to the nervous system. EPA has set the 
drinking water standard for 2,4,5-TP at 0.05 part per million (ppm) to 
protect against the risk of these adverse health effects. Drinking water 
that meets the EPA standard is associated with little to none of this 
risk and is considered safe with respect to 2,4,5-TP.
    (52) Xylenes. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that xylene is a 
health concern at certain levels of exposure. This organic chemical is 
used in the manufacture of gasoline for airplanes and as a solvent for 
pesticides, and as a cleaner and degreaser of metals. It usually gets 
into water by improper waste disposal. This chemical has been shown to 
damage the liver, kidney and nervous system of laboratory animals such 
as rats and dogs exposed to high levels during their lifetimes. Some 
humans who were exposed to relatively large amounts of this chemical 
also suffered damage to the nervous system. EPA has set the drinking 
water standard for xylene at 10 parts per million (ppm) to protect 
against the risk of these adverse health effects. Drinking water that 
meets the EPA standard is associated with little to none of this risk 
and is considered safe with respect to xylene.
    (53) Antimony. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that antimony is 
a health concern at certain levels of exposure. This inorganic chemical 
occurs naturally in soils, ground water and surface waters and is often 
used in the flame retardant industry. It is also used in ceramics, 
glass, batteries, fireworks and explosives. It may get into drinking 
water through natural weathering of rock, industrial production, 
municipal waste disposal or manufacturing processes. This chemical has 
been shown to decrease longevity, and altered blood levels of 
cholesterol and glucose in laboratory animals such as rats exposed to 
high levels during their lifetimes. EPA has set the drinking water 
standard for antimony at 0.006 parts per million (ppm) to protect 
against the risk of these adverse health effects. Drinking water which 
meets the EPA standard is associated with little to none of this risk 
and should be considered safe with respect to antimony.
    (54) Beryllium. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that beryllium is 
a health concern at certain levels of exposure. This inorganic metal 
occurs naturally in soils, ground water and surface waters and is often 
used in electrical equipment and electrical components. It generally 
gets into water from runoff from mining operations, discharge from 
processing plants and improper waste disposal. Beryllium compounds have 
been associated with damage to the bones and lungs and induction of 
cancer in laboratory animals such as rats and mice when the animals are 
exposed at high levels over their lifetimes. There is limited evidence 
to suggest that beryllium may pose a cancer risk via drinking water 
exposure. Therefore, EPA based the health assessment on noncancer 
effects with an extra uncertainty factor to account for possible 
carcinogenicity. Chemicals that cause cancer in laboratory animals also 
may increase the risk of cancer in humans who are exposed over long 
periods of time. EPA has set the drinking water standard for beryllium 
at 0.004 part per million (ppm) to protect against the risk of these 
adverse health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to beryllium.

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    (55) Cyanide. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that cyanide is a 
health concern at certain levels of exposure. This inorganic chemical is 
used in electroplating, steel processing, plastics, synthetic fabrics 
and fertilizer products. It usually gets into water as a result of 
improper waste disposal. This chemical has been shown to damage the 
spleen, brain and liver of humans fatally poisoned with cyanide. EPA has 
set the drinking water standard for cyanide at 0.2 parts per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water which meets the EPA standard is associated with little to 
none of this risk and should be considered safe with respect to cyanide.
    (56) [Reserved]
    (57) Thallium. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that thallium is 
a health concern at certain high levels of exposure. This inorganic 
metal is found naturally in soils and is used in electronics, 
pharmaceuticals, and the manufacture of glass and alloys. This chemical 
has been shown to damage the kidney, liver, brain and intestines of 
laboratory animals when the animals are exposed at high levels over 
their lifetimes. EPA has set the drinking water standard for thallium at 
0.002 parts per million (ppm) to protect against the risk of these 
adverse health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to thallium.
    (58) Benzo[a]pyrene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
benzo[a]pyrene is a health concern at certain levels of exposure. 
Cigarette smoke and charbroiled meats are common source of general 
exposure. The major source of benzo[a]pyrene in drinking water is the 
leaching from coal tar lining and sealants in water storage tanks. This 
chemical has been shown to cause cancer in animals such as rats and mice 
when the animals are exposed at high levels. EPA has set the drinking 
water standard for benzo[a]pyrene at 0.0002 parts per million (ppm) to 
protect against the risk of cancer. Drinking water which meets the EPA 
standard is associated with little to none of this risk and should be 
considered safe with respect to benzo[a]pyrene.
    (59) Dalapon. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that dalapon is a 
health concern at certain levels of exposure. This organic chemical is a 
widely used herbicide. It may get into drinking water after application 
to control grasses in crops, drainage ditches and along railroads. This 
chemical has been shown to cause damage to the kidney and liver in 
laboratory animals when the animals are exposed to high levels over 
their lifetimes. EPA has set the drinking water standard for dalapon at 
0.2 parts per million (ppm) to protect against the risk of these adverse 
health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to dalapon.
    (60) Dichloromethane. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
dichloromethane (methylene chloride) is a health concern at certain 
levels of exposure. This organic chemical is a widely used solvent. It 
is used in the manufacture of paint remover, as a metal degreaser and as 
an aerosol propellant. It generally gets into drinking water after 
improper discharge of waste disposal. This chemical has been shown to 
cause cancer in laboratory animals such as rats and mice when the 
animals are exposed at high levels over their lifetimes. Chemicals that 
cause cancer in laboratory animals also may increase the risk of cancer 
in humans who are exposed over long periods of time. EPA has set the 
drinking water standard for dichloromethane at 0.005 parts per million 
(ppm) to reduce the risk of cancer or other adverse health effects which 
have been observed in laboratory animals. Drinking water which meets 
this standard is associated with little to none of this risk

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and should be considered safe with respect to dichloromethane.
    (61) Di (2-ethylhexyl)adipate. The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that di(2-ethylhexyl)adipate is a health concern at certain levels of 
exposure. Di(2-ethylhexyl)adipate is a widely used plasticizer in a 
variety of products, including synthetic rubber, food packaging 
materials and cosmetics. It may get into drinking water after improper 
waste disposal. This chemical has been shown to damage liver and testes 
in laboratory animals such as rats and mice exposed to high levels. EPA 
has set the drinking water standard for di(2-ethylhexyl)adipate at 0.4 
parts per million (ppm) to protect against the risk of adverse health 
effects. Drinking water which meets the EPA standards is associated with 
little to none of this risk and should be considered safe with respect 
to di(2-ethylhexyl)adipate.
    (62) Di(2-ethylhexyl)phthalate. The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that di(2-ethylhexyl)phthalate is a health concern at certain levels of 
exposure. Di(2-ethylhexyl)phthalate is a widely used plasticizer, which 
is primarily used in the production of polyvinyl chloride (PVC) resins. 
It may get into drinking water after improper waste disposal. This 
chemical has been shown to cause cancer in laboratory animals such as 
rats and mice exposed to high levels over their lifetimes. EPA has set 
the drinking water standard for di(2-ethylhexyl)phthalate at 0.006 parts 
per million (ppm) to reduce the risk of cancer or other adverse health 
effects which have been observed in laboratory animals. Drinking water 
which meets the EPA standard is associated with little to none of this 
risk and should be considered safe with respect to di(2-
ethylhexyl)phthalate.
    (63) Dinoseb. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that dinoseb is a 
health concern at certain levels of exposure. Dinoseb is a widely used 
pesticide and generally gets into drinking water after application on 
orchards, vineyards and other crops. This chemical has been shown to 
damage the thyroid and reproductive organs in laboratory animals such as 
rats exposed to high levels. EPA has set the drinking water standard for 
dinoseb at 0.007 parts per million (ppm) to protect against the risk of 
adverse health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to dinoseb.
    (64) Diquat. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that diquat is a health 
concern at certain levels of exposure. This organic chemical is a 
herbicide used to control terrestrial and aquatic weeds. It may get into 
drinking water by runoff into surface water. This chemical has been 
shown to damage the liver, kidney and gastrointestinal tract and causes 
cataract formation in laboratory animals such as dogs and rats exposed 
at high levels over their lifetimes. EPA has set the drinking water 
standard for diquat at 0.02 parts per million (ppm) to protect against 
the risk of these adverse health effects. Drinking water which meets the 
EPA standard is associated with little to none of this risk and should 
be considered safe with respect to diquat.
    (65) Endothall. The United States Environmental Protection Agency 
(EPA) has determined that endothall is a health concern at certain 
levels of exposure. This organic chemical is a herbicide used to control 
terrestrial and aquatic weeds. It may get into water by runoff into 
surface water. This chemical has been shown to damage the liver, kidney, 
gastrointestinal tract and reproductive system of laboratory animals 
such as rats and mice exposed at high levels over their lifetimes. EPA 
has set the drinking water standard for endothall at 0.1 parts per 
million (ppm) to protect against the risk of these adverse health 
effects. Drinking water which meets the EPA standard is associated with 
little to none of this risk and should be considered safe with respect 
to endothall.
    (66) Endrin. The United States Environmental Protection Agency (EPA) 
sets drinking water standards and has determined that endrin is a health 
concern at certain levels of exposure. This

[[Page 396]]

organic chemical is a pesticide no longer registered for use in the 
United States. However, this chemical is persistent in treated soils and 
accumulates in sediments and aquatic and terrestrial biota. This 
chemical has been shown to cause damage to the liver, kidney and heart 
in laboratory animals such as rats and mice when the animals are exposed 
at high levels over their lifetimes. EPA has set the drinking water 
standard for endrin at 0.002 parts per million (ppm) to protect against 
the risk of these adverse health effects which have been observed in 
laboratory animals. Drinking water that meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to endrin.
    (67) Glyphosate. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that glyphosate 
is a health concern at certain levels of exposure. This organic chemical 
is a herbicide used to control grasses and weeds. It may get into 
drinking water by runoff into surface water. This chemical has been 
shown to cause damage to the liver and kidneys in laboratory animals 
such as rats and mice when the animals are exposed at high levels over 
their lifetimes. EPA has set the drinking water standard for glyphosate 
at 0.7 parts per million (ppm) to protect against the risk of these 
adverse health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to glyphosate.
    (68) Hexachlorobenzene. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
hexachlorobenzene is a health concern at certain levels of exposure. 
This organic chemical is produced as an impurity in the manufacture of 
certain solvents and pesticides. This chemical has been shown to cause 
cancer in laboratory animals such as rats and mice when the animals are 
exposed to high levels during their lifetimes. Chemicals that cause 
cancer in laboratory animals also may increase the risk of cancer in 
humans who are exposed over long periods of time. EPA has set the 
drinking water standard for hexachlorobenzene at 0.001 parts per million 
(ppm) to protect against the risk of cancer and other adverse health 
effects. Drinking water which meets the EPA standard is associated with 
little to none of this risk and should be considered safe with respect 
to hexachlorobenzene.
    (69) Hexachlorocyclopentadiene. The United States Environmental 
Protection Agency (EPA) establishes drinking water standards and has 
determined that hexachlorocyclopentadiene is a health concern at certain 
levels of exposure. This organic chemical is used as an intermediate in 
the manufacture of pesticides and flame retardants. It may get into 
water by discharge from production facilities. This chemical has been 
shown to damage the kidney and the stomach of laboratory animals when 
exposed at high levels over their lifetimes. EPA has set the drinking 
water standard for hexachlorocyclopentadiene at 0.05 parts per million 
(ppm) to protect against the risk of these adverse health effects. 
Drinking water which meets the EPA standard is associated with little to 
none of this risk and should be considered safe with respect to 
hexachlorocyclopentadiene.
    (70) Oxamyl. The United States Environmental Protection Agency (EPA) 
establishes drinking water standards and has determined that oxamyl is a 
health concern at certain levels of exposure. This organic chemical is 
used as a pesticide for the control of insects and other pests. It may 
get into drinking water by runoff into surface water or leaching into 
ground water. This chemical has been shown to damage the kidneys of 
laboratory animals such as rats when exposed at high levels over their 
lifetimes. EPA has set the drinking water standard for oxamyl at 0.2 
parts per million (ppm) to protect against the risk of these adverse 
health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to oxamyl.
    (71) Picloram. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that picloram is 
a health concern at certain levels of exposure.

[[Page 397]]

This organic chemical is used as a pesticide for broadleaf weed control. 
It may get into drinking water by runoff into surface water or leaching 
into ground water as a result of pesticide application and improper 
waste disposal. This chemical has been shown to cause damage to the 
kidneys and liver in laboratory animals such as rats when the animals 
are exposed at high levels over their lifetimes. EPA has set the 
drinking water standard for picloram at 0.5 parts per million (ppm) to 
protect against the risk of these adverse health effects. Drinking water 
which meets the EPA standard is associated with little to none of this 
risk and should be considered safe with respect to picloram.
    (72) Simazine. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that simazine is 
a health concern at certain levels of exposure. This organic chemical is 
a herbicide used to control annual grasses and broadleaf weeds. It may 
leach into ground water or runs off into surface water after 
application. This chemical may cause cancer in laboratory animals such 
as rats and mice exposed at high levels during their lifetimes. 
Chemicals that cause cancer in laboratory animals also may increase the 
risk of cancer in humans who are exposed over long periods of time. EPA 
has set the drinking water standard for simazine at 0.004 parts per 
million (ppm) to reduce the risk of cancer or other adverse health 
effects. Drinking water which meets the EPA standard is associated with 
little to none of this risk and should be considered safe with respect 
to simazine.
    (73) 1,2,4-Trichlorobenzene. The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that 1,2,4-trichlorobenzene is a health concern at certain levels of 
exposure. This organic chemical is used as a dye carrier and as a 
precursor in herbicide manufacture. It generally gets into drinking 
water by discharges from industrial activities. This chemical has been 
shown to cause damage to several organs, including the adrenal glands. 
EPA has set the drinking water standard for 1,2,4-trichlorobenzene at 
0.07 parts per million (ppm) to protect against the risk of these 
adverse health effects. Drinking water which meets the EPA standard is 
associated with little to none of this risk and should be considered 
safe with respect to 1,2,4-trichlorobenzene.
    (74) 1,1,2-Trichloroethane. The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
1,1,2-trichloroethane is a health concern at certain levels of exposure. 
This organic chemical is an intermediate in the production of 1,1-
dichloroethylene. It generally gets into water by industrial discharge 
of wastes. This chemical has been shown to damage the kidney and liver 
of laboratory animals such as rats exposed to high levels during their 
lifetimes. EPA has set the drinking water standard for 1,1,2-
trichloroethane at 0.005 parts per million (ppm) to protect against the 
risk of these adverse health effects. Drinking water which meets the EPA 
standard is associated with little to none of this risk and should be 
considered safe with respect to 1,1,2-trichloroethane.
    (75) 2,3,7,8-TCDD (Dioxin). The United States Environmental 
Protection Agency (EPA) sets drinking water standards and has determined 
that dioxin is a health concern at certain levels of exposure. This 
organic chemical is an impurity in the production of some pesticides. It 
may get into drinking water by industrial discharge of wastes. This 
chemical has been shown to cause cancer in laboratory animals such as 
rats and mice when the animals are exposed at high levels over their 
lifetimes. Chemicals that cause cancer in laboratory animals also may 
increase the risk of cancer in humans who are exposed over long periods 
of time. EPA has set the drinking water standard for dioxin at 
0.00000003 parts per million (ppm) to reduce the risk of cancer or other 
adverse health effects which have been observed in laboratory animals. 
Drinking water which meets this standard is associated with little to 
none of this risk and should be considered safe with respect to dioxin.
    (76) Chlorine. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that chlorine is 
a health

[[Page 398]]

concern at certain levels of exposure. Chlorine is added to drinking 
water as a disinfectant to kill bacteria and other disease-causing 
microorganisms and is also added to provide continuous disinfection 
throughout the distribution system. Disinfection is required for surface 
water systems. However, at high doses for extended periods of time, 
chlorine has been shown to affect blood and the liver in laboratory 
animals. EPA has set a drinking water standard for chlorine to protect 
against the risk of these adverse effects. Drinking water which meets 
this EPA standard is associated with little to none of this risk and 
should be considered safe with respect to chlorine.
    (77) Chloramines. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that chloramines 
are a health concern at certain levels of exposure. Chloramines are 
added to drinking water as a disinfectant to kill bacteria and other 
disease-causing microorganisms and are also added to provide continuous 
disinfection throughout the distribution system. Disinfection is 
required for surface water systems. However, at high doses for extended 
periods of time, chloramines have been shown to affect blood and the 
liver in laboratory animals. EPA has set a drinking water standard for 
chloramines to protect against the risk of these adverse effects. 
Drinking water which meets this EPA standard is associated with little 
to none of this risk and should be considered safe with respect to 
chloramines.
    (78) Chlorine dioxide. The United States Environmental Protection 
Agency (EPA) sets drinking water standards and has determined that 
chlorine dioxide is a health concern at certain levels of exposure. 
Chlorine dioxide is used in water treatment to kill bacteria and other 
disease-causing microorganisms and can be used to control tastes and 
odors. Disinfection is required for surface water systems. However, at 
high doses, chlorine dioxide-treated drinking water has been shown to 
affect blood in laboratory animals. Also, high levels of chlorine 
dioxide given to laboratory animals in drinking water have been shown to 
cause neurological effects on the developing nervous system. These 
neurodevelopmental effects may occur as a result of a short-term 
excessive chlorine dioxide exposure. To protect against such potentially 
harmful exposures, EPA requires chlorine dioxide monitoring at the 
treatment plant, where disinfection occurs, and at representative points 
in the distribution system serving water users. EPA has set a drinking 
water standard for chlorine dioxide to protect against the risk of these 
adverse effects.

    Note: In addition to the language in this introductory text of 
paragraph (e)(78), systems must include either the language in paragraph 
(e)(78)(i) or (e)(78)(ii) of this section. Systems with a violation at 
the treatment plant, but not in the distribution system, are required to 
use the language in paragraph (e)(78)(i) of this section and treat the 
violation as a nonacute violation. Systems with a violation in the 
distribution system are required to use the language in paragraph 
(e)(78)(ii) of this section and treat the violation as an acute 
violation.

    (i) The chlorine dioxide violations reported today are the result of 
exceedances at the treatment facility only, and do not include 
violations within the distribution system serving users of this water 
supply. Continued compliance with chlorine dioxide levels within the 
distribution system minimizes the potential risk of these violations to 
present consumers.
    (ii) The chlorine dioxide violations reported today include 
exceedances of the EPA standard within the distribution system serving 
water users. Violations of the chlorine dioxide standard within the 
distribution system may harm human health based on short-term exposures. 
Certain groups, including pregnant women, infants, and young children, 
may be especially susceptible to adverse effects of excessive exposure 
to chlorine dioxide-treated water. The purpose of this notice is to 
advise that such persons should consider reducing their risk of adverse 
effects from these chlorine dioxide violations by seeking alternate 
sources of water for human consumption until such exceedances are 
rectified. Local and State health authorities are the best sources for 
information concerning alternate drinking water.

[[Page 399]]

    (79) Disinfection byproducts and treatment technique for DBPs. The 
United States Environmental Protection Agency (EPA) sets drinking water 
standards and requires the disinfection of drinking water. However, when 
used in the treatment of drinking water, disinfectants react with 
naturally-occurring organic and inorganic matter present in water to 
form chemicals called disinfection byproducts (DBPs). EPA has determined 
that a number of DBPs are a health concern at certain levels of 
exposure. Certain DBPs, including some trihalomethanes (THMs) and some 
haloacetic acids (HAAs), have been shown to cause cancer in laboratory 
animals. Other DBPs have been shown to affect the liver and the nervous 
system, and cause reproductive or developmental effects in laboratory 
animals. Exposure to certain DBPs may produce similar effects in people. 
EPA has set standards to limit exposure to THMs, HAAs, and other DBPs.
    (80) Bromate. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that bromate is a 
health concern at certain levels of exposure. Bromate is formed as a 
byproduct of ozone disinfection of drinking water. Ozone reacts with 
naturally occurring bromide in the water to form bromate. Bromate has 
been shown to produce cancer in rats. EPA has set a drinking water 
standard to limit exposure to bromate.
    (81) Chlorite. The United States Environmental Protection Agency 
(EPA) sets drinking water standards and has determined that chlorite is 
a health concern at certain levels of exposure. Chlorite is formed from 
the breakdown of chlorine dioxide, a drinking water disinfectant. 
Chlorite in drinking water has been shown to affect blood and the 
developing nervous system. EPA has set a drinking water standard for 
chlorite to protect against these effects. Drinking water which meets 
this standard is associated with little to none of these risks and 
should be considered safe with respect to chlorite.
    (f) Public notices for fluoride. Notice of violations of the maximum 
contaminant level for fluoride, notices of variances and exemptions from 
the maximum contaminant level for fluoride, and notices of failure to 
comply with variance and exemption schedules for the maximum contaminant 
level for fluoride shall consist of the public notice prescribed in 
Sec. 143.5(b), plus a description of any steps which the system is 
taking to come into compliance.
    (g) Public notification by the State. The State may give notice to 
the public required by this section on behalf of the owner or operator 
of the public water system if the State complies with the requirements 
of this section. However, the owner or operator of the public water 
system remains legally responsible for ensuring that the requirements of 
this section are met.

[52 FR 41546, Oct. 28, 1987, as amended at 54 FR 15188, Apr. 17, 1989; 
54 FR 27527, 27566, June 29, 1989; 55 FR 25064, June 19, 1990; 56 FR 
3587, Jan. 30, 1991; 56 FR 26548, June 7, 1991; 56 FR 30279, July 1, 
1991; 57 FR 31843, July 17, 1992; 59 FR 34323, July 1, 1994; 60 FR 
33932, June 29, 1995; 63 FR 69464, 69515, Dec. 16, 1998]



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 bacteriological 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

[[Page 400]]

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.



Sec. 141.34  [Reserved]



Sec. 141.35  Reporting and public notification for certain unregulated contaminants.

    (a) The requirements of this section only apply to the contaminants 
listed in Sec. 141.40.
    (b) The owner or operator of a community water system or non-
transient, non-community water system who is required to monitor under 
Sec. 141.40 shall send a copy of the results of such monitoring within 
30 days of receipt and any public notice under paragraph (d) of this 
section to the State.
    (c) The State, or the community water system or non-transient, non-
community water system if the State has not adopted regulations 
equivalent to Sec. 141.40, shall furnish the following information to 
the Administrator for each sample analyzed under Sec. 141.40:
    (1) Results of all analytical methods, including negatives;
    (2) Name and address of the system that supplied the sample;
    (3) Contaminant(s);
    (4) Analytical method(s) used;
    (5) Date of sample;
    (6) Date of analysis.
    (d) The owner or operator shall notify persons served by the system 
of the availability of the results of sampling conducted under 
Sec. 141.40 by including a notice in the first set of water bills issued 
by the system after the receipt of the results or written notice within 
three months. The notice shall identify a person and supply the 
telephone number to contact for information on the monitoring results. 
For surface water systems, public notification is required only after 
the first quarter's monitoring and must include a statement that 
additional monitoring will be conducted for three more quarters with the 
results available upon request.

[52 FR 25714, July 8, 1987; 53 FR 25110, July 1, 1988]



  Subpart E--Special Regulations, Including Monitoring Regulations and 
                         Prohibition on Lead Use



Sec. 141.40  Special monitoring for inorganic and organic contaminants.

    (a) All community and non-transient, non-community water systems 
shall monitor for the contaminants listed in paragraph (e) in this 
section by date specified in table 1:

               Table 1--Monitoring Schedule by System Size
------------------------------------------------------------------------
                                            Monitoring to begin no later
         Number of persons served                      than--
------------------------------------------------------------------------
Over 10,000...............................  Jan. 1, 1988.
3,300 to 10,000...........................  Jan. 1, 1989.
Less than 3,300...........................  Jan. 1, 1991.
------------------------------------------------------------------------

    (b) Surface water systems shall sample at points in the distribution 
system representative of each water source or at entry points to the 
distribution system after any application of treatment. The minimum 
number of samples is one year of quarterly samples per water source.
    (c) Ground water systems shall sample at points of entry to the 
distribution system representative of each well after any application of 
treatment. The minimum number of samples is one sample per entry point 
to the distribution system.
    (d) The State may require confirmation samples for positive or 
negative results.
    (e) Community water systems and non-transient, non-community water 
systems shall monitor for the following contaminants except as provided 
in paragraph (f) of this section:

(1) Chloroform
(2) Bromodichloromethane
(3) Chlorodibromomethane
(4) Bromoform
(5) Dibromomethane
(6) m-Dichlorobenzene

[[Page 401]]

(7) [Reserved]
(8) 1,1-Dichloropropene
(9) 1,1-Dichloroethane
(10) 1,1,2,2-Tetrachloroethane
(11) 1,3-Dichloropropane
(12) Chloromethane
(13) Bromomethane
(14) 1,2,3-Trichloropropane
(15) 1,1,1,2-Tetrachloroethane
(16) Chloroethane
(17) 2,2-Dichloropropane
(18) o-Chlorotoluene
(19) p-Chlorotoluene
(20) Bromobenzene
(21) 1,3-Dichloropropene
    (f) [Reserved]
    (g) Analysis for the unregulated contaminants listed under 
paragraphs (e) and (j) of this section shall be conducted using EPA 
Methods 502.2 or 524.2, or their equivalent as determined by EPA, except 
analysis for bromodichloromethane, bromoform, chlorodibromomethane and 
chloroform under paragraph (e) of this section also may be conducted by 
EPA Method 551, and analysis for 1,2,3-trichloropropane also may be 
conducted by EPA Method 504.1. A source for the EPA methods is 
referenced at Sec. 141.24(e).
    (h) Analysis under this section shall only be conducted by 
laboratories certified under Sec. 141.24(f)(17).
    (i) Public water systems may use monitoring data collected any time 
after January 1, 1983 to meet the requirements for unregulated 
monitoring, provided that the monitoring program was consistent with the 
requirements of this section. In addition, the results of EPA's Ground 
Water Supply Survey may be used in a similar manner for systems supplied 
by a single well.
    (j) Monitoring for the following compounds is required at the 
discretion of the State:
    (1) 1,2,4-Trimethylbenzene;
    (2) 1,2,3-Trichlorobenzene;
    (3) n-Propylbenzene;
    (4) n-Butylbenzene;
    (5) Naphthalene;
    (6) Hexachlorobutadiene;
    (7) 1,3,5-Trimethylbenzene;
    (8) p-Isopropyltoluene;
    (9) Isopropylbenzene;
    (10) Tert-butylbenzene;
    (11) Sec-butylbenzene;
    (12) Fluorotrichloromethane;
    (13) Dichlorodifluoromethane;
    (14) Bromochloromethane.
    (k) Instead of performing the monitoring required by this section, a 
community water system or non-transient non-community water system 
serving fewer than 150 service connections may send a letter to the 
State stating that the system is available for sampling. This letter 
must be sent to the State no later than January 1, 1991. The system 
shall not send such samples to the State, unless requested to do so by 
the State.
    (l) All community and non-transient, non-community water systems 
shall repeat the monitoring required in Sec. 141.40 no less frequently 
than every five years from the dates specified in Sec. 141.40(a). 
Systems serving 10,000 or fewer persons are not required to monitor for 
the contaminants in this section after December 31, 1998.
    (m) States or public water systems may composite up to five samples 
when monitoring for substances in Sec. 141.40 (e) and (j) of this 
section.
    (n) Monitoring of the contaminants listed in Sec. 141.40(n) (11) and 
(12) shall be conducted as follows:
    (1) Each community and non-transient, non-community water system 
shall take four consecutive quarterly samples at each sampling point for 
each contaminant listed in paragraph (n)(11) of this section and report 
the results to the State. Monitoring must be completed by December 31, 
1995.
    (2) Each community and non-transient non-community water system 
shall take one sample at each sampling point for each contaminant listed 
in paragraph (n)(12) of this section and report the results to the 
States. Monitoring must be completed by December 31, 1995.
    (3) Each community and non-transient non-community water system may 
apply to the State for a waiver from the requirements of paragraph (n) 
(1) and (2) of this section.
    (4) The State may grant a waiver for the requirement of paragraph 
(n)(1) of this section based on the criteria specified in 
Sec. 141.24(h)(6). The State may grant a waiver from the requirement of 
paragraph (n)(2) of this section if previous analytical results indicate 
contamination would not occur, provided

[[Page 402]]

this data was collected after January 1, 1990.
    (5) 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.
    (6) 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.
    (7) 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).
    (8) The State may require a confirmation sample for positive or 
negative results.
    (9) 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. Compositing of samples must 
be done in the laboratory and the composite sample must be analyzed 
within 14 days of collection. 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.
    (10) Instead of performing the monitoring required by this section, 
a community water system or non-transient non-community water system 
serving fewer than 150 service connections may send a letter to the 
State stating that the system is available for sampling. This letter 
must be sent to the State by January 1, 1994. The system shall not send 
such samples to the State, unless requested to do so by the State.
    (11) Systems shall monitor for the unregulated organic contaminants 
listed below, using the method(s) identified below and using the 
analytical test procedures contained in Technical Notes on Drinking 
Water Methods, EPA-600/R-94-173, October 1994, which is available at 
NTIS, PB95-104766. Method 6610 shall be followed in accordance with the 
Standard Methods for the Examination of Water and Wastewater 18th 
Edition Supplement, 1994, American Public Health Association. 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 from the American Public Health Association, 1015 
Fifteenth Street NW, Washington, DC 20005. Copies may be inspected at 
EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or 
at the Office of the Federal Register, 800 North Capitol Street, NW., 
Suite 700, Washington, DC. A source for EPA methods 505, 507, 508, 
508.1, 515.2, 525.2 and 531.1 is referenced at Sec. 141.24(e).

------------------------------------------------------------------------
               Contaminants                            Method
------------------------------------------------------------------------
aldicarb..................................  531.1, 6610.
aldicarb sulfone..........................  531.1, 6610.
aldicarb sulfoxide........................  531.1, 6610.
aldrin....................................  505, 508, 525.2, 508.1.
butachlor.................................  507, 525.2.
carbaryl..................................  531.1, 6610.
dicamba...................................  515.2, 555, 515.1.
dieldrin..................................  505, 508, 525.2, 508.1.
3-hydroxycarbofuran.......................  531.1, 6610.
methomyl..................................  531.1, 6610.
metolachlor...............................  507, 525.2, 508.1.
metribuzin................................  507, 525.2, 508.1.
propachlor................................  508, 525.2, 508.1.
------------------------------------------------------------------------

    (12) Systems shall monitor for sulfate, an unregulated inorganic 
contaminant, by using the methods listed at Sec. 143.4(b).

[52 FR 25715, July 8, 1987; 53 FR 25110, July 1, 1988, as amended at 56 
FR 3592, Jan. 30, 1991; 57 FR 31845, July 17, 1992; 59 FR 34323, July 1, 
1994; 59 FR 62469, Dec. 5, 1994; 64 FR 1498, Jan. 8, 1999]

[[Page 403]]



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 
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) Each public water system shall identify and provide notice to 
persons that may be affected by lead contamination of their drinking 
water where such contamination results from either or both of the 
following:

[[Page 404]]

    (i) The lead content in the construction materials of the public 
water distribution system,
    (ii) Corrosivity of the water supply sufficient to cause leaching of 
lead.
    Notice shall be provided notwithstanding the absence of a violation 
of any national drinking water standard. The manner and form of notice 
are specified in Sec. 141.34 of this part.
    (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) Enforcement of public notice requirements. The requirements of 
paragraph (a)(2) of this section, shall apply in all States effective 
June 19, 1988.
    (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, and
    (2) When used with respect to pipes and pipe fittings refers to 
pipes and pipe fittings containing not more than 8.0 percent lead.

[52 FR 20674, June 2, 1987]



    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
(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]

[[Page 405]]

    (b) MCLGs for the following contaminants are as indicated:

------------------------------------------------------------------------
                  Contaminant                          MCLG (mg/l)
------------------------------------------------------------------------
Antimony......................................                     0.006
Asbestos......................................    7 Million fibers/liter
                                                 (longer than 10 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
------------------------------------------------------------------------


[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]



Sec. 141.52  Maximum contaminant level goals for microbiological contaminants.

    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.
------------------------------------------------------------------------


[54 FR 27527, 27566, June 29, 1989; 55 FR 25064, June 19, 1990; 63 FR 
69515, Dec. 16, 1998]



Sec. 141.53  Maximum contaminant level goals for disinfection byproducts.

    MCLGs for the following disinfection byproducts are as indicated:

------------------------------------------------------------------------
                                                                  MCLG
                    Disinfection byproduct                       (mg/L)
------------------------------------------------------------------------
Chloroform....................................................   Zero
Bromodichloromethane..........................................   Zero
Bromoform.....................................................   Zero
Bromate.......................................................   Zero
Dichloroacetic acid...........................................   Zero
Trichloroacetic acid..........................................      0.3
Chlorite......................................................      0.8
Dibromochloromethane..........................................      0.06
------------------------------------------------------------------------


[63 FR 69465, Dec. 16, 1998]



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]



Subpart G--National Revised 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.

[56 FR 3593, Jan. 30, 1991, as amended at 57 FR 31846, July 17, 1992; 59 
FR 34324, July 1, 1994]



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

[[Page 406]]

 
 (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), 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     ........  ........

[[Page 407]]

 
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
 (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)--(15) of 
this section apply to community water systems and non-transient, non-
community water systems.

[[Page 408]]

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

    (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
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
Nitrate.................................................           5,7,9
Nitrite.................................................             5,7
Selenium................................................   1,2 \3\,6,7,9
Thallium................................................             1,5
------------------------------------------------------------------------
\1\ BAT only if influent Hg concentrations 10g/1.
\2\ BAT for Chromium III only.
\3\ BAT for Selenium IV only.

                          Key to BATS in Table

1=Activated Alumina
2=Coagulation/Filtration
3=Direct and Diatomite Filtration
4=Granular Activated Carbon
5=Ion Exchange
6=Lime Softening
7=Reverse Osmosis
8=Corrosion Control
9=Electrodialysis
10=Chlorine
11=Ultraviolet

[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]



Sec. 141.63  Maximum contaminant levels (MCLs) for microbiological contaminants.

    (a) The MCL is based on the presence or absence of total coliforms 
in a sample, rather than coliform density.
    (1) For a system which 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 which collects fewer than 40 samples/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) 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 Sec. 141.32, this is a violation that may 
pose an acute risk to health.
    (c) 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.
    (d) 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:
    (1) Protection of wells from contamination by coliforms by 
appropriate placement and construction;
    (2) Maintenance of a disinfectant residual throughout the 
distribution system;

[[Page 409]]

    (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, 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 
subpart H, or disinfection of ground water 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.

[54 FR 27566, June 29, 1989; 55 FR 25064, June 19, 1990]



Sec. 141.64  Maximum contaminant levels for disinfection byproducts.

    (a) The maximum contaminant levels (MCLs) for disinfection 
byproducts are as follows:

------------------------------------------------------------------------
                                                                MCL (mg/
                    Disinfection byproduct                         L)
------------------------------------------------------------------------
Total trihalomethanes (TTHM)..................................     0.080
Haloacetic acids (five) (HAA5)................................     0.060
Bromate.......................................................     0.010
Chlorite......................................................     1.0
------------------------------------------------------------------------

    (b) Compliance dates. (1) CWSs and NTNCWSs. Subpart H systems 
serving 10,000 or more persons must comply with this section beginning 
December 16, 2001. 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 section beginning December 16, 2003.
    (2) A system that is installing GAC or membrane technology to comply 
with this section may apply to the State for an extension of up to 24 
months past the dates in paragraphs (b)(1) of this section, but not 
beyond December 16, 2003. In granting the extension, States must set a 
schedule for compliance and may specify any interim measures that the 
system must take. Failure to meet the schedule or interim treatment 
requirements constitutes a violation of a National Primary Drinking 
Water Regulation.
    (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 
contaminant levels for disinfection byproducts identified in paragraph 
(a) of this section:

------------------------------------------------------------------------
         Disinfection byproduct             Best available technology
------------------------------------------------------------------------
TTHM...................................  Enhanced coagulation or
                                          enhanced softening or GAC10,
                                          with chlorine as the primary
                                          and residual disinfectant
HAA5...................................  Enhanced coagulation or
                                          enhanced softening or GAC10,
                                          with chlorine as the primary
                                          and residual disinfectant.
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.
------------------------------------------------------------------------


[63 FR 69465, Dec. 16, 1998]



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 December 16, 2001. 
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 December 16, 2003.
    (2) Transient NCWSs. Subpart H systems serving 10,000 or more 
persons and using chlorine dioxide as a disinfectant or oxidant must 
comply with the chlorine dioxide MRDL beginning December 16, 2001. 
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 December 16, 2003.

[[Page 410]]

    (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]



                 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.

[54 FR 27527, June 29, 1989, as amended at 63 FR 69516, Dec. 16, 1998]



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) 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 Secs. 141.72(b) and 141.73 by June 29, 1993.

[[Page 411]]

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 
Secs. 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)(4) 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 
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

[[Page 412]]

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 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 Secs. 141.12 and 141.30 until December 17, 2001. 
After December 17, 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 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)(4) 
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]



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

[[Page 413]]

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 beginnng 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.
    (3) The residual disinfectant concentration in the water entering 
the distribution system, measured as specified in Sec. 141.74 (a)(5) 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)(5) 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)(3), 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.

[[Page 414]]

[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)(3) 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)(5) 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)(5) 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)(3), 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 transported and analyzed 
for HPC by a certified laboratory under the requisite time and 
temperature conditions specified in Sec. 141.74(a)(3) 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.



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

[[Page 415]]

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)(4) 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)(4) 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)(4) and (c)(1).
    (3) Beginning December 17, 2001, systems serving at least 10,000 
people must meet the turbidity requirements in Sec. 141.173(a).
    (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)(4) 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)(4) 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)(4) 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)(4) 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 December 
17, 2001, systems serving at least 10,000 people must meet the 
requirements for other filtration technologies in Sec. 141.173(b).

[54 FR 27527, June 29, 1989, as amended at 63 FR 69516, Dec. 16, 1998]



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 the requirements of Secs. 141.71, 141.72, 
and 141.73. Measurements for pH, temperature, turbidity, and residual 
disinfectant concentrations must be conducted by a party approved by the 
State. Measurements 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 HPC and fecal coliforms, any laboratory certified for total 
coliform analysis by EPA is deemed certified for HPC and fecal coliform 
analysis. The following procedures shall be performed 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

[[Page 416]]

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 Street, SW., 
Washington, DC 20460 or at the Office of the Federal Register, 800 North 
Capitol Street, NW., suite 700, Washington, DC.
    (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 and by using analytical test 
procedures contained in Technical Notes on Drinking Water Methods, EPA-
600/R-94-173, October 1994, which is available at NTIS PB95-104766.

------------------------------------------------------------------------
            Organism                 Methodology         Citation \1\
------------------------------------------------------------------------
Total Coliforms \2\............  Total Coliform      9221A, B, C
                                  Fermentation
                                  Technique 3,4,5.
                                 Total Coliform      9222A, B, C
                                  Membrane Filter
                                  Technique.
                                 ONPG-Mug Test \6\.  9223
Fecal Coliforms \2\............  Fecal Coliform      9221E
                                  Procedure \7\.
                                 Fecal Coliform      9222D
                                  Membrane Filter
                                  Procedure.
Heterotrophic bacteria \2\.....  Pour Plate method.  9215B
Turbidity......................  Nephelometric       2130B
                                  Method.
                                 Nephelometric       180.1 \8\
                                  Method.
                                 Great Lakes         Method 2 \9\
                                  Instruments.
------------------------------------------------------------------------
\1\ Except where noted, all methods refer to the 18th edition of
  Standard Methods for the Examination of Water and Wastewater, 1992,
  American Public Health Association, 1015 Fifteenth Street NW,
  Washington, D.C. 20005.
\2\ The time from sample collection to initiation of analysis may not
  exceed 8 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 coliforms, 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\ The ONPG-MUG Test is also known as the Autoanalysis Colilert System.
 
\7\ A-1 Broth may be held up to three months in a tightly closed
  screwcap tube at 4  deg.C.
\8\ ``Methods for the Determination of Inorganic Substances in
  Environmental Samples'', EPA-600/R-93-100, August 1993. Available at
  NTIS, PB94-121811.
\9\ GLI Method 2, ``Turbidity'', November 2, 1992, Great Lakes
  Instruments, Inc., 8855 North 55th Street, Milwaukee, Wisconsin 53223.

    (2) Public water systems must measure residual disinfectant 
concentrations with one of the analytical methods in the following 
table. The methods are contained in the 18th edition of Standard Methods 
for the Examination of Water and Wastewater, 1992. Other analytical test 
procedures are contained in Technical Notes on Drinking Water Methods, 
EPA-600/R-94-173, October 1994, which is available at NTIS PB95-104766. 
If approved by the State, residual disinfectant concentrations for free 
chlorine and combined chlorine also may be measured by using DPD 
colorimetric test kits. 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 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.

------------------------------------------------------------------------
           Residual                Methodology            Methods
------------------------------------------------------------------------
Free Chlorine.................  Amperometric       4500-Cl D
                                 Titration.

[[Page 417]]

 
                                DPD Ferrous        4500-Cl F
                                 Titrimetric.
                                DPD Colorimetric.  4500-Cl G
                                Syringaldazine     4500-Cl H
                                 (FACTS).
Total Chlorine................  Amperometric       4500-Cl D
                                 Titration.
                                Amperometric       4500-Cl E
                                 Titration (low
                                 level
                                 measurement).
                                DPD Ferrous        4500-Cl F
                                 Titrimetric.
                                DPD Colorimetric.  4500-Cl G
                                Iodometric         4500-Cl I
                                 Electrode.
Chlorine Dioxide..............  Amperometric       4500-ClO2 C
                                 Titration.
                                DPD Method.......  4500-ClO2 D
                                Amperometric       4500-ClO2 E
                                 Titration.
Ozone.........................  Indigo Method....  4500-O3 B
------------------------------------------------------------------------

    (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

[[Page 418]]

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).

  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                                             9.0
                                                                   6.5    7.0    7.5    8.0    8.5
----------------------------------------------------------------------------------------------------------------
 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

[[Page 419]]

 
1.4................................................         41       49     58     70     85    103        123
1.6................................................         42       50     59     72     87    105        126
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                                             9.0
                                                                   6.5    7.0    7.5    8.0    8.5
----------------------------------------------------------------------------------------------------------------
 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                                                  25  deg.C
                                                  deg.C   5  deg.C  10  deg.C  15  deg.C  20  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 420]]


[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. 142.72(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) 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, except that 
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)(3) 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 421]]

time and temperature conditions specified by paragraph (a)(3) 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) 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, except that 
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)(3) 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)(3) 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]

[[Page 422]]



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:
    (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

[[Page 423]]

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)(3) 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.
    (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 
inform the State as soon as possible, but no later than the end of the 
next business day.
    (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

[[Page 424]]

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)(3) 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.
    (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 
inform the State as soon as possible, but no

[[Page 425]]

later than the end of the next business day.
    (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.



                  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) The requirements set forth in Secs. 141.86 to 141.91 shall take 
effect on July 7, 1991. The requirements set forth in Secs. 141.80 to 
141.85 shall take effect on December 7, 1992.
    (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.
    (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 Secs. 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. Any system exceeding the lead 
action level

[[Page 426]]

shall implement the public education requirements contained in 
Sec. 141.85.
    (h) Monitoring and analytical requirements. Tap water monitoring for 
lead 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 Secs. 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 Secs. 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]



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 
following criteria:
    (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). 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 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 six-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).

[[Page 427]]

    (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, large systems 
shall complete the following corrosion control treatment steps 
(described in the referenced portions of Secs. 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, l998.
    (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 Secs. 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 it exceeds one of the action 
levels.
    (2) Step 2: Within 12 months after 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 such system 
exceeds the lead or copper action level,
    (ii) For small systems, within 24 months after 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.

[[Page 428]]

    (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]



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 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

[[Page 429]]

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 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 shall maintain 
water quality parameter values at or above minimum values or within 
ranges designated by the State under paragraph (f) of this section in 
each sample collected under Sec. 141.87(d). If the water quality 
parameter value of any

[[Page 430]]

sample is below the minimum value or outside the range designated by the 
State, then the system is out of compliance with this paragraph. As 
specified in Sec. 141.87(d), the system may take a confirmation sample 
for any water quality parameter value no later than 3 days after the 
first sample. If a confirmation sample is taken, the result must be 
averaged with the first sampling result and the average must be used for 
any compliance determinations under this paragraph. States have 
discretion to delete results of obvious sampling errors from this 
calculation.
    (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.



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 Secs. 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)) within 6 
months after exceeding the lead or copper action level.
    (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 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

[[Page 431]]

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
    (iii) The technical aspects of a State's determination would be 
indefensible in an expected Federal enforcement action taken against a 
system.



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

[[Page 432]]

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) A 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 based upon a materials evaluation, including the evaluation 
required under Sec. 141.86(a). The first year of lead service line 
replacement shall begin on the date the action level was exceeded in tap 
sampling referenced in paragraph (a) of this section.
    (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 the entire service line (up to the 
building inlet) unless it demonstrates to the satisfaction of the State 
under paragraph (e) of this section that it controls less than the 
entire service line. In such cases, the system shall replace the portion 
of the line which the State determines is under the system's control. 
The system shall notify the user served by the line that the system will 
replace the portion of the service line under its control and shall 
offer to replace the building owner's portion of the line, but is not 
required to bear the cost of replacing the building owner's portion of 
the line. For buildings where only a portion of the lead service line is 
replaced, the water system shall inform the resident(s) that the system 
will collect a first flush tap water sample after partial replacement of 
the service line is completed if the resident(s) so desire. In cases 
where the resident(s) accept the offer, the system shall collect the 
sample and report the results to the resident(s) within 14 days 
following partial lead service line replacement.
    (e) A water system is presumed to control the entire lead service 
line (up to the building inlet) unless the system demonstrates to the 
satisfaction of the State, in a letter submitted under 
Sec. 141.90(e)(4), that it does not have any of the following forms of 
control over the entire line (as defined by state statutes, municipal 
ordinances, public service contracts or other applicable legal 
authority): authority to set standards for construction, repair, or 
maintenance of the line, authority to replace, repair, or maintain the 
service line, or ownership of the service line. The State shall review 
the information supplied by the system and determine whether the system 
controls less than the entire service line and, in such cases, shall 
determine the extent of the system's control. The State's determination 
shall be in writing and explain the basis for its decision.
    (f) 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.
    (g) 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) of this section.
    (h) 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]

[[Page 433]]



Sec. 141.85  Public education and supplemental monitoring requirements.

    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 paragraphs (a) and (b) of this 
section in accordance with the requirements in paragraph (c) of this 
section.
    (a) Content of written materials. A water system shall include the 
following text in all of the printed materials it distributes through 
its lead public education program. Any additional information presented 
by a system shall be consistent with the information below and be in 
plain English that can be understood by laypersons.
    (1) Introduction. The United States Environmental Protection Agency 
(EPA) and [insert name of water supplier] are concerned about lead in 
your drinking water. Although most homes have very low levels of lead in 
their drinking water, some homes in the community have lead levels above 
the EPA action level of 15 parts per billion (ppb), or 0.015 milligrams 
of lead per liter of water (mg/L). Under Federal law we are required to 
have a program in place to minimize lead in your drinking water by 
[insert date when corrosion control will be completed for your system]. 
This program includes corrosion control treatment, source water 
treatment, and public education. We are also required to replace each 
lead service line that we control if the line contributes lead 
concentrations of more than 15 ppb after we have completed the 
comprehensive treatment program. If you have any questions about how we 
are carrying out the requirements of the lead regulation please give us 
a call at [insert water system's phone number]. This brochure explains 
the simple steps you can take to protect you and your family by reducing 
your exposure to lead in drinking water.
    (2) Health effects of lead. Lead is a common metal found throughout 
the environment in lead-based paint, air, soil, household dust, food, 
certain types of pottery porcelain and pewter, and water. Lead can pose 
a significant risk to your health if too much of it enters your body. 
Lead builds up in the body over many years and can cause damage to the 
brain, red blood cells and kidneys. The greatest risk is to young 
children and pregnant women. Amounts of lead that won't hurt adults can 
slow down normal mental and physical development of growing bodies. In 
addition, a child at play often comes into contact with sources of lead 
contamination--like dirt and dust--that rarely affect an adult. It is 
important to wash children's hands and toys often, and to try to make 
sure they only put food in their mouths.
    (3) Lead in drinking water. (i) Lead in drinking water, although 
rarely the sole cause of lead poisoning, can significantly increase a 
person's total lead exposure, particularly the exposure of infants who 
drink baby formulas and concentrated juices that are mixed with water. 
The EPA estimates that drinking water can make up 20 percent or more of 
a person's total exposure to lead.
    (ii) Lead is unusual among drinking water contaminants in that it 
seldom occurs naturally in water supplies like rivers and lakes. Lead 
enters drinking water primarily as a result of the corrosion, or wearing 
away, of materials containing lead in the water distribution system and 
household plumbing. These materials include lead-based solder used to 
join copper pipe, brass and chrome plated brass faucets, and in some 
cases, pipes made of lead that connect your house to the water main 
(service lines). In 1986, Congress banned the use of lead solder 
containing greater than 0.2% lead, and restricted the lead content of 
faucets, pipes and other plumbing materials to 8.0%.
    (iii) When water stands in lead pipes or plumbing systems containing 
lead for several hours or more, the lead may dissolve into your drinking 
water. This means the first water drawn from the tap in the morning, or 
later in the afternoon after returning from work or school, can contain 
fairly high levels of lead.
    (4) Steps you can take in the home to reduce exposure to lead in 
drinking water. (i) Despite our best efforts mentioned earlier to 
control water corrosivity and remove lead from the water supply, lead 
levels in some homes or buildings can be high. To find out whether you

[[Page 434]]

need to take action in your own home, have your drinking water tested to 
determine if it contains excessive concentrations of lead. Testing the 
water is essential because you cannot see, taste, or smell lead in 
drinking water. Some local laboratories that can provide this service 
are listed at the end of this booklet. For more information on having 
your water tested, please call [insert phone number of water system].
    (ii) If a water test indicates that the drinking water drawn from a 
tap in your home contains lead above 15 ppb, then you should take the 
following precautions:
    (A) Let the water run from the tap before using it for drinking or 
cooking any time the water in a faucet has gone unused for more than six 
hours. The longer water resides in your home's plumbing the more lead it 
may contain. Flushing the tap means running the cold water faucet until 
the water gets noticeably colder, usually about 15-30 seconds. If your 
house has a lead service line to the water main, you may have to flush 
the water for a longer time, perhaps one minute, before drinking. 
Although toilet flushing or showering flushes water through a portion of 
your home's plumbing system, you still need to flush the water in each 
faucet before using it for drinking or cooking. Flushing tap water is a 
simple and inexpensive measure you can take to protect your family's 
health. It usually uses less than one or two gallons of water and costs 
less than [insert a cost estimate based on flushing two times a day for 
30 days] per month. To conserve water, fill a couple of bottles for 
drinking water after flushing the tap, and whenever possible use the 
first flush water to wash the dishes or water the plants. If you live in 
a high-rise building, letting the water flow before using it may not 
work to lessen your risk from lead. The plumbing systems have more, and 
sometimes larger pipes than smaller buildings. Ask your landlord for 
help in locating the source of the lead and for advice on reducing the 
lead level.
    (B) Try not to cook with, or drink water from the hot water tap. Hot 
water can dissolve more lead more quickly than cold water. If you need 
hot water, draw water from the cold tap and heat it on the stove.
    (C) Remove loose lead solder and debris from the plumbing materials 
installed in newly constructed homes, or homes in which the plumbing has 
recently been replaced, by removing the faucet strainers from all taps 
and running the water from 3 to 5 minutes. Thereafter, periodically 
remove the strainers and flush out any debris that has accumulated over 
time.
    (D) If your copper pipes are joined with lead solder that has been 
installed illegally since it was banned in 1986, notify the plumber who 
did the work and request that he or she replace the lead solder with 
lead-free solder. Lead solder looks dull gray, and when scratched with a 
key looks shiny. In addition, notify your State [insert name of 
department responsible for enforcing the Safe Drinking Water Act in your 
State] about the violation.
    (E) Determine whether or not the service line that connects your 
home or apartment to the water main is made of lead. The best way to 
determine if your service line is made of lead is by either hiring a 
licensed plumber to inspect the line or by contacting the plumbing 
contractor who installed the line. You can identify the plumbing 
contractor by checking the city's record of building permits which 
should be maintained in the files of the [insert name of department that 
issues building permits]. A licensed plumber can at the same time check 
to see if your homes's plumbing contains lead solder, lead pipes, or 
pipe fittings that contain lead. The public water system that delivers 
water to your home should also maintain records of the materials located 
in the distribution system. If the service line that connects your 
dwelling to the water main contributes more than 15 ppb to drinking 
water, after our comprehensive treatment program is in place, we are 
required to replace the line. If the line is only partially controlled 
by the [insert name of the city, county, or water system that controls 
the line], we are required to provide you with information on how to 
replace your portion of the service line, and offer to replace that 
portion of the line at your expense and take a follow-up tap water 
sample

[[Page 435]]

within 14 days of the replacement. Acceptable replacement alternatives 
include copper, steel, iron, and plastic pipes.
    (F) Have an electrician check your wiring. If grounding wires from 
the electrical system are attached to your pipes, corrosion may be 
greater. Check with a licensed electrician or your local electrical code 
to determine if your wiring can be grounded elsewhere. DO NOT attempt to 
change the wiring yourself because improper grounding can cause 
electrical shock and fire hazards.
    (iii) The steps described above will reduce the lead concentrations 
in your drinking water. However, if a water test indicates that the 
drinking water coming from your tap contains lead concentrations in 
excess of 15 ppb after flushing, or after we have completed our actions 
to minimize lead levels, then you may want to take the following 
additional measures:
    (A) Purchase or lease a home treatment device. Home treatment 
devices are limited in that each unit treats only the water that flows 
from the faucet to which it is connected, and all of the devices require 
periodic maintenance and replacement. Devices such as reverse osmosis 
systems or distillers can effectively remove lead from your drinking 
water. Some activated carbon filters may reduce lead levels at the tap, 
however all lead reduction claims should be investigated. Be sure to 
check the actual performance of a specific home treatment device before 
and after installing the unit.
    (B) Purchase bottled water for drinking and cooking.
    (iv) You can consult a variety of sources for additional 
information. Your family doctor or pediatrician can perform a blood test 
for lead and provide you with information about the health effects of 
lead. State and local government agencies that can be contacted include:
    (A) [insert the name of city or county department of public 
utilities] at [insert phone number] can provide you with information 
about your community's water supply, and a list of local laboratories 
that have been certified by EPA for testing water quality;
    (B) [insert the name of city or county department that issues 
building permits] at [insert phone number] can provide you with 
information about building permit records that should contain the names 
of plumbing contractors that plumbed your home; and
    (C) [insert the name of the State Department of Public Health] at 
[insert phone number] or the [insert the name of the city or county 
health department] at [insert phone number] can provide you with 
information about the health effects of lead and how you can have your 
child's blood tested.
    (v) The following is a list of some State approved laboratories in 
your area that you can call to have your water tested for lead. [Insert 
names and phone numbers of at least two laboratories].
    (b) Content of broadcast materials. A water system shall include the 
following information in all public service announcements submitted 
under its lead public education program to television and radio stations 
for broadcasting:
    (1) Why should everyone want to know the facts about lead and 
drinking water? Because unhealthy amounts of lead can enter drinking 
water through the plumbing in your home. That's why I urge you to do 
what I did. I had my water tested for [insert free or $ per sample]. You 
can contact the [insert the name of the city or water system] for 
information on testing and on simple ways to reduce your exposure to 
lead in drinking water.
    (2) To have your water tested for lead, or to get more information 
about this public health concern, please call [insert the phone number 
of the city or water system].
    (c) Delivery of a public education program. (1) In communities where 
a significant proportion of the population speaks a language other than 
English, public education materials shall be communicated in the 
appropriate language(s).
    (2) A community water system that fails to meet the lead action 
level on the basis of tap water samples collected in accordance with 
Sec. 141.86 shall, within 60 days:

[[Page 436]]

    (i) Insert notices in each customer's water utility bill containing 
the information in paragraph (a) of this section, along with the 
following alert on the water bill itself in large print: ``SOME HOMES IN 
THIS COMMUNITY HAVE ELEVATED LEAD LEVELS IN THEIR DRINKING WATER. LEAD 
CAN POSE A SIGNIFICANT RISK TO YOUR HEALTH. PLEASE READ THE ENCLOSED 
NOTICE FOR FURTHER INFORMATION.''
    (ii) Submit the information in paragraph (a) of this section to the 
editorial departments of the major daily and weekly newspapers 
circulated throughout the community.
    (iii) Deliver pamphlets and/or brochures that contain the public 
education materials in paragraphs (a) (2) and (4) of this section to 
facilities and organizations, including the following:
    (A) Public schools and/or local school boards;
    (B) City or county health department;
    (C) Women, Infants, and Children and/or Head Start Program(s) 
whenever available;
    (D) Public and private hospitals and/or clinics;
    (E) Pediatricians;
    (F) Family planning clinics; and
    (G) Local welfare agencies.
    (iv) Submit the public service announcement in paragraph (b) of this 
section to at least five of the radio and television stations with the 
largest audiences that broadcast to the community served by the water 
system.
    (3) A community water system shall repeat the tasks contained in 
paragraphs (c)(2) (i), (ii) and (iii) of this section every 12 months, 
and the tasks contained in paragraphs (c)(2)(iv) of this section every 6 
months for as long as the system exceeds the lead action level.
    (4) Within 60 days after it exceeds the lead action level, a non-
transient non-community water system shall deliver the public education 
materials contained in paragraphs (a) (1), (2), and (4) 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.
    (5) A non-transient non-community water system shall repeat the 
tasks contained in paragraph (c)(4) of this section at least once during 
each calendar year in which the system exceeds the lead action level.
    (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.
    (d) 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.

[56 FR 26548, June 7, 1991; 57 FR 28788, June 29, 1992]



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

[[Page 437]]

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 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.
    (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.
    (8) Any water system whose sampling pool does not consist 
exclusively of tier 1 sites shall demonstrate in a letter submitted to 
the State under Sec. 141.90(a)(2) why a review of the information listed 
in paragraph (a)(2) of this section was inadequate to locate a 
sufficient number of tier l sites. Any community water system which 
includes tier 3 sampling sites in its sampling pool shall demonstrate in 
such a letter why it was unable to locate a sufficient number of tier l 
and tier 2 sampling sites.
    (9) 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 demonstrate 
in a letter submitted to the State under Sec. 141.90(a)(4) why the 
system was unable to locate a sufficient number of such sites. Such a 
water system shall collect first draw samples from all of the sites 
identified as being served by such lines.

[[Page 438]]

    (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), 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 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 days after the 
sample is collected. If the sample is not acidified immediately after 
collection, then the sample must stand in the original container for at 
least 28 hours after acidification. 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.
    (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 below 
(``standard monitoring''). A system conducting reduced monitoring under 
paragraph (d)(4) of this section may collect one sample from the number 
of sites specified in the second column below during each monitoring 
period specified in paragraph (d)(4) of this section.

------------------------------------------------------------------------
                                           No. of sites    No. of sites
     System size (No. people served)         (standard       (reduced
                                            monitoring)     monitoring)
------------------------------------------------------------------------
>100,000................................             100              50
10,001-100,000..........................              60              30
3,301 to 10,000.........................              40              20
501 to 3,300............................              20              10
101 to 500..............................              10               5
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

[[Page 439]]

    (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.
    (ii) Any water system that 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 request that the State 
allow the system to reduce the frequency of monitoring to once per year 
and to reduce the number of lead and copper samples in accordance with 
paragraph (c) of this section. The State shall review the information 
submitted by the water system and shall make its decision in writing, 
setting forth the basis for its determination. 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.
    (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 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 request that the State 
allow the system to reduce the frequency of monitoring from annually to 
once every three years. The State shall review the information submitted 
by the water system and shall make its decision in writing, setting 
forth the basis for its determination. 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 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.
    (v) 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 
(d) of this section. Such 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

[[Page 440]]

level. Any water system subject to the reduced monitoring frequency that 
fails to operate within the range of values for the water quality 
parameters specified by the State under Sec. 141.82(f) shall resume tap 
water 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.
    (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.

[56 FR 26548, June 7, 1991; 56 FR 32113, July 15, 1991; 57 FR 28788, 
June 29, 1992]



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 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) 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

[[Page 441]]

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) At each entry point to the distribution system, one sample every 
two weeks (bi-weekly) 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).
    (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 during each monitoring period specified in 
Sec. 141.86(d)(3). Any small or medium-size system shall conduct such 
monitoring during each monitoring period specified in Sec. 141.86(d)(3) 
in which the system exceeds the lead or copper action level. The system 
may take a confirmation sample for any water quality parameter value no 
later than 3 days after the first sample. If a confirmation sample is 
taken, the result must be averaged with the first sampling result and 
the average must be used for any compliance determinations under 
Sec. 141.82(g). States have discretion to delete results of obvious 
sampling errors from this calculation.
    (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) 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. 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) from annually to every 
three years.
    (3) A water system that conducts sampling annually shall collect 
these samples evenly throughout the year so as to reflect seasonal 
variability.

[[Page 442]]

    (4) Any water system subject to the reduced monitoring frequency 
that fails to operate within the range of values for the water quality 
parameters specified by the State in Sec. 141.82(f) shall resume tap 
water sampling in accordance with the number and frequency requirements 
in paragraph (d) 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         Biweekly
                                       rate and concentration   distribution system.
                                       (if alkalinity
                                       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          orthophosphate or
 Control.                              silica \3\, calcium
                                       \4\.
                                     ---------------------------------------------------------------------------
                                      pH, alkalinity dosage    Entry point(s) to         Biweekly
                                       rate and concentration   distribution system.
                                       (if alkalinity
                                       adjusted as part of
                                       corrosion control),
                                       inhibitor dosage rate
                                       and inhibitor residual
                                       \5\.
 
----------------------------------------------------------------------------------------------------------------
Reduced Monitoring..................  pH, alkalinity,          Taps....................  Every 6 months at a
                                       orthophosphate or                                  reduced number of
                                       silica \3\, calcium                                sites
                                       \4\.
                                     ---------------------------------------------------------------------------
                                      pH, alkalinity dosage    Entry point(s) to         Biweekly
                                       rate and concentration   distribution system.
                                       (if alkalinity
                                       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.

[56 FR 26548, June 7, 1991; 57 FR 28788, June 29, 1992, as amended at 59 
FR 33862, June 30, 1994]



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 
requirements regarding sample location, number of samples, and 
collection methods specified in Sec. 141.23(a) (1)-(4) (inorganic 
chemical sampling). (Note: The timing of sampling for lead and copper 
shall be in accordance with paragraphs (b) and (c) of this section, and 
not dates specified in Sec. 141.23(a) (1) and (2)).
    (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

[[Page 443]]

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 within six months after the exceedance.
    (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 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.
    (ii) A water system using surface water (or a combination of surface 
and groundwater) shall collect samples once during each year, the first 
annual monitoring period to begin on the date on 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 
groundwater which demonstrates that finished drinking water entering the 
distribution system has been maintained below the maximum permissible 
lead and/or 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 may reduce the monitoring 
frequency for lead and/or copper to once during each nine-year 
compliance cycle (as that term is defined in Sec. 141.2).
    (2) A water system using surface water (or a combination of surface 
and ground waters) which 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 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).
    (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]



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).
    (1) Analyses under this section 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 EPA Environmental Monitoring and Support Laboratory 
or

[[Page 444]]

equivalent samples provided by the State; 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 method detection limits according to the procedures in 
appendix B of part 136 of this title as follows:
    (A) Lead: 0.001 mg/L (only if source water compositing is done under 
Sec. 141.23(a)(4)); and
    (B) Copper: 0.001 mg/L or 0.020 mg/L when atomic absorption direct 
aspiration is used (only if source water compositing is done under 
Sec. 141.23(a)(4)).
    (iv) Be currently certified by EPA or the State to perform analyses 
to the specifications described in paragraph (a)(2) 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]



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) A water system 
shall report the information specified below for all tap water samples 
within the first 10 days following the end of each applicable monitoring 
period specified in Secs. 141.86 and 141.87 and 141.88 (i.e., every six-
months, annually, or every 3 years).
    (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) A certification that each first draw sample collected by the 
water system is one-liter in volume and, to the best of their knowledge, 
has stood motionless in the service line, or in the interior plumbing of 
a sampling site, for at least six hours;
    (iii) Where residents collected samples, a certification that each 
tap sample collected by the residents was taken after the water system 
informed them of proper sampling procedures specified in 
Sec. 141.86(b)(2);
    (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));
    (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;
    (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).
    (2) By the applicable date in Sec. 141.86(d)(1) for commencement of 
monitoring, each community water system

[[Page 445]]

which does not complete its targeted sampling pool with tier 1 sampling 
sites meeting the criteria in Sec. 141.86(a)(3) shall send a letter to 
the State justifying its selection of tier 2 and/or tier 3 sampling 
sites under Sec. 141.86 (a)(4) and/or (a)(5).
    (3) By the applicable date in Sec. 141.86(d)(1) for commencement of 
monitoring, each non-transient, non-community water system which does 
not complete its sampling pool with tier 1 sampling sites meeting the 
criteria in Sec. 141.86(a)(6) shall send a letter to the State 
justifying its selection of sampling sites under Sec. 141.86(a)(7).
    (4) By the applicable date in Sec. 141.86(d)(1) for commencement of 
monitoring, each water system with lead service lines that is not able 
to locate the number of sites served by such lines required under 
Sec. 141.86(a)(9) shall send a letter to the State demonstrating why it 
was unable to locate a sufficient number of such sites based upon the 
information listed in Sec. 141.86(a)(2).
    (5) Each water system that requests that the State reduce the number 
and frequency of sampling shall provide the information required under 
Sec. 141.86(d)(4).
    (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) Within 12 months after a system exceeds the lead action level in 
sampling referred to in Sec. 141.84(a), the system shall demonstrate in 
writing to the State that it has conducted a material evaluation, 
including the evaluation in Sec. 141.86(a), to identify the initial 
number of lead service lines in its distribution system, and shall 
provide the State with the system's schedule for replacing annually at 
least 7 percent of the initial number of lead service lines in its 
distribution system.
    (2) Within 12 months after 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(f)) 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

[[Page 446]]

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 (a) of 
this section (or the percentage specified by the State under 
Sec. 141.84(f)).
    (3) The annual letter submitted to the State under paragraph (e)(2) 
of this section shall contain the following information:
    (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) As soon as practicable, but in no case later than three months 
after a system exceeds the lead action level in sampling referred to in 
Sec. 141.84(a), any system seeking to rebut the presumption that it has 
control over the entire lead service line pursuant to Sec. 141.84(d) 
shall submit a letter to the State describing the legal authority (e.g., 
state statutes, municipal ordinances, public service contracts or other 
applicable legal authority) which limits the system's control over the 
service lines and the extent of the system's control.
    (f) Public education program reporting requirements. By December 
31st of each year, any water system that is subject to the public 
education requirements in Sec. 141.85 shall submit a letter to the State 
demonstrating that the system has delivered the public education 
materials that meet the content requirements in Sec. 141.85 (a) and (b) 
and the delivery requirements in Sec. 141.85(c). This information shall 
include a list of all the newspapers, radio stations, television 
stations, facilities and organizations to which the system delivered 
public education materials during the previous year. The water system 
shall submit the letter required by this paragraph annually for as long 
as it exceeds the lead action level.
    (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 
Secs. 141.86, 141.87 and 141.88 during which the samples are collected.

[56 FR 26548, June 7, 1991; 57 FR 28789, June 29, 1992, as amended at 59 
FR 33864, June 30, 1994]



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 Secs. 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.

[[Page 447]]

    (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 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

    Source: 63 FR 69466, Dec. 16, 1998, unless otherwise noted.



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 Secs. 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

[[Page 448]]

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 December 16, 2001. 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 December 16, 2003.
    (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 and chlorite in this 
subpart beginning December 16, 2001. 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 and 
chlorite in this subpart beginning December 16, 2003.
    (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.



Sec. 141.131  Analytical requirements.

    (a) General. (1) Systems must use only the analytical method(s) 
specified in this section, or otherwise approved by EPA for monitoring 
under this subpart, to demonstrate compliance with the requirements of 
this subpart. These methods are effective for compliance monitoring 
February 16, 1999.
    (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, 401 M Street, SW, 
Washington, DC 20460, or at the Office of the Federal Register, 800 
North Capitol Street, NW, Suite 700, Washington DC. 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 Method 300.1 is titled USEPA Method 
300.1, Determination of Inorganic Anions in Drinking Water by Ion 
Chromatography, Revision 1.0, USEPA, 1997, EPA/600/R-98/118 (available 
through NTIS, PB98-169196); also available from: Chemical Exposure 
Research Branch, Microbiological & Chemical Exposure Assessment Research 
Division, National Exposure Research Laboratory, U.S. Environmental 
Protection Agency, Cincinnati, OH 45268, Fax Number: 513-569-7757, Phone 
number: 513-569-7586. Standard Methods 4500-Cl D, 4500-Cl E, 4500-Cl F, 
4500-Cl G, 4500-Cl H, 4500-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 
Edition, American Public Health Association, 1995; copies may be 
obtained from

[[Page 449]]

the American Public Health Association, 1015 Fifteenth Street, NW, 
Washington, DC 20005. 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, American 
Public Health Association, 1996; copies may be obtained from the 
American Public Health Association, 1015 Fifteenth Street, NW, 
Washington, DC 20005. ASTM Method D 1253-86 shall be followed in 
accordance with the Annual Book of ASTM Standards, Volume 11.01, 
American Society for Testing and Materials, 1996 edition; copies may be 
obtained from the American Society for Testing and Materials, 100 Barr 
Harbor Drive, West Conshohoken, PA 19428.
    (b) Disinfection byproducts. (1) Systems must measure disinfection 
byproducts by the methods (as modified by the footnotes) listed in the 
following table:

                                            Approved Methods for Disinfection Byproduct Compliance Monitoring
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                  Byproduct measured \1\
              Methodology \2\                EPA method              Standard method             -------------------------------------------------------
                                                                                                      TTHM          HAA5      Chlorite \4\     Bromate
--------------------------------------------------------------------------------------------------------------------------------------------------------
P&T/GC/ElCD & PID.........................     \3\502.2                                                     X
P&T/GC/MS.................................        524.2                                                     X
LLE/GC/ECD................................        551.1                                                     X
LLE/GC/ECD................................               6251 B                                                           X
SPE/GC/ECD................................        552.1                                                                   X
LLE/GC/ECD................................        552.2                                                                   X
Amperometric Titration....................               4500-ClO2 E                                                                    X
IC........................................        300.0                                                                                 X
IC........................................        300.1                                                                                 X             X
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ X indicates method is approved for measuring specified disinfection byproduct.
\2\ 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 extractor; IC = ion chromatography.
\3\ If TTHMs are the only analytes being measured in the sample, then a PID is not required.
\4\ Amperometric titration 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).

    (2) Analysis under this section for disinfection byproducts must be 
conducted by laboratories that have received certification by EPA or the 
State. To receive certification to conduct analyses for the contaminants 
in Sec. 141.64(a), the laboratory must carry out annual analyses of 
performance evaluation (PE) samples approved by EPA or the State. In 
these analyses of PE samples, the laboratory must achieve quantitative 
results 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 data 
between a maximum and minimum acceptance limit of +/-50% and +/-15% of 
the study mean.
    (c) Disinfectant residuals. (1) Systems must measure residual 
disinfectant concentrations for free chlorine, combined chlorine 
(chloramines), and chlorine dioxide by the methods listed in the 
following table:

                                            Approved Methods for Disinfectant Residual Compliance Monitoring
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                   Residual Measured \1\
                                                                                                 -------------------------------------------------------
             Methodology                    Standard  method                 ASTM method              Free        Combined        Total       Chlorine
                                                                                                    chlorine      chlorine      chlorine       dioxide
--------------------------------------------------------------------------------------------------------------------------------------------------------
Amperometric Titration..............  4500-Cl D                     D 1253-86                               X             X             X
Low Level Amperometric Titration....  4500-Cl E                                                                                         X
DPD Ferrous Titrimetric.............  4500-Cl F                                                             X             X             X
DPD Colorimetric....................  4500-Cl G                                                             X             X             X

[[Page 450]]

 
Syringaldazin e (FACTS).............  4500-Cl H                                                             X
Iodometric Electrode................  4500-Cl I                                                                                         X
DPD.................................  4500-ClO2 D                                                                                                     X
Amperometric Method II..............  4500-ClO2 E                                                                                                     X
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ X indicates method is approved for measuring specified disinfectant residual.

    (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. 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 Method 300.0 or EPA Method 300.1.
    (3) Total Organic Carbon (TOC). Standard Method 5310 B (High-
Temperature Combustion Method) or Standard Method 5310 C (Persulfate-
Ultraviolet or Heated-Persulfate Oxidation Method) or Standard Method 
5310 D (Wet-Oxidation Method). TOC samples may not be filtered prior to 
analysis. TOC samples must either be analyzed or must be acidified to 
achieve pH less than 2.0 by minimal addition of phosphoric or sulfuric 
acid as soon as practical after sampling, not to exceed 24 hours. 
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 (High-
Temperature Combustion Method) or Standard Method 5310 C (Persulfate-
Ultraviolet or Heated-Persulfate Oxidation Method) or Standard Method 
5310 D (Wet-Oxidation Method). Prior to analysis, DOC samples must be 
filtered through a 0.45 m pore-diameter filter. 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. DOC samples must be filtered through 
the 0.45 m pore-diameter filter prior to acidification. DOC 
samples must either be analyzed or must be acidified to achieve pH less 
than 2.0 by minimal addition of phosphoric or sulfuric acid as soon as 
practical after sampling, not to exceed 48 hours. Acidified DOC samples 
must be analyzed within 28 days.
    (ii) Ultraviolet Absorption at 254 nm (UV254). Method 
5910 B (Ultraviolet Absorption Method). 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 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.

[[Page 451]]

    (5) pH. All methods allowed in Sec. 141.23(k)(1) for measuring pH.



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(f)(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 or subpart M of this part 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 MCL, 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
                                                                        system meets reduced monitoring criteria
                                                                        in paragraph (c) 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.
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 MCL, 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
                                                                        system meets criteria in paragraph (c)
                                                                        of this section for reduced monitoring.
----------------------------------------------------------------------------------------------------------------
\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(f)(5) of this chapter.

    (ii) Systems may reduce monitoring, except as otherwise provided, in 
accordance with the following table:

[[Page 452]]



                                 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 mg/L and HAA5       quarter at distribution system location
 average TOC level, before any             annual average 4.0 mg/L.           eq>0.030 mg/L.
Subpart H system serving from 500 to      TTHM annual average 0.040 mg/L and HAA5       at distribution system location
 annual average TOC level, before any      annual average 4.0 mg/L.           eq>0.030 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 mg/L and HAA5       at distribution system location
 chemical disinfectant and serving at      annual average 0.030 mg/L.               month of warmest water temperature
System using only ground water not under  TTHM annual average 0.040 mg/L and HAA5       year monitoring cycle at distribution
 chemical disinfectant and serving fewer   annual average 0.030 mg/L for two        residence time during month of warmest
                                           consecutive years OR TTHM    water temperature, with the three-year
                                           annual average 0.020 mg/L and HAA5       quarter in which system qualifies for
                                           annual average 0.015 mg/L for one year.
----------------------------------------------------------------------------------------------------------------

    (iii) 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 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 in the 
quarter immediately following the quarter in which the system exceeds 
0.060 mg/L and 0.045 mg/L for TTHMs and HAA5, respectively.
    (iv) 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

[[Page 453]]

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.
    (ii) Reduced monitoring. Systems required to analyze for bromate may 
reduce 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 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 upon 
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.
    (c) Monitoring requirements for disinfectant residuals. (1) Chlorine 
and chloramines. (i) Routine monitoring. Systems must measure the 
residual disinfectant level at the same points in the distribution 
system and at the same time as total coliforms are sampled, as specified 
in Sec. 141.21. Subpart H systems 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 454]]

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.



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's failure 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's 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, 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

[[Page 455]]

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). 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, 
in addition to reporting to the State pursuant to Sec. 141.134. If a PWS 
fails to complete four consecutive quarters' monitoring, compliance with 
the MCL for the last four-quarter compliance period must be based on an 
average of the available data.
    (ii) For systems monitoring less frequently than quarterly, 
compliance must be based on an average of samples taken that year under 
the provisions of Sec. 141.132(b)(1). If the average of these samples 
exceeds the MCL, the system must increase monitoring to once per quarter 
per treatment plant.
    (iii) Systems on a reduced monitoring schedule whose annual average 
exceeds the MCL will revert to routine monitoring immediately. These 
systems will not be considered in violation of the MCL until they have 
completed one year of routine monitoring.
    (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 Sec. 141.32, 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 Sec. 141.32, 
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 of quarterly averages 
covering any consecutive four-quarter period exceeds the MRDL, the 
system is in violation of the MRDL and must notify the public pursuant 
to Sec. 141.32, 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 must notify the public pursuant to the procedures for acute health 
risks in Sec. 141.32(a)(1)(iii)(E). 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 Sec. 141.32(a)(1)(iii)(E).
    (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

[[Page 456]]

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 Sec. 141.32(e)(78). 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).
    (d) Disinfection byproduct precursors (DBPP). Compliance must be 
determined as specified by Sec. 141.135(b). 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.



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 TTHM and HAA5      (1) The number of samples taken
 under the requirements of Secs.          during the last quarter.
 141.132(b) on a quarterly or more
 frequent basis.
                                         (2) The location, date, and
                                          result of each sample taken
                                          during the last quarter.
                                         (3) The arithmetic average of
                                          all samples taken in the last
                                          quarter.
                                         (4) The annual arithmetic
                                          average of the quarterly
                                          arithmetic averages of this
                                          section for the last four
                                          quarters.
                                         (5) Whether the MCL was
                                          exceeded.
System monitoring for TTHMs and HAA5     (1) The number of samples taken
 under the requirements of Secs.          during the last year.
 141.132(b) less frequently than
 quarterly (but at least annually).
                                         (2) The location, date, and
                                          result of each sample taken
                                          during the last quarter.
                                         (3) The arithmetic average of
                                          all samples taken over the
                                          last year.
                                         (4) Whether the MCL was
                                          exceeded.
System monitoring for TTHMs and HAA5     (1) The location, date, and
 under the requirements of Sec.           result of the last sample
 141.132(b) less frequently than          taken.
 annually.
                                         (2) Whether the MCL was
                                          exceeded.
System monitoring for chlorite under     (1) The number of samples taken
 the requirements of Sec.  141.132(b).    each month for the last 3
                                          months.
                                         (2) The location, date, and
                                          result of each sample taken
                                          during the last quarter.
                                         (3) For each month in the
                                          reporting period, the
                                          arithmetic average of all
                                          samples taken in the month.
                                         (4) Whether the MCL was
                                          exceeded, and in which month
                                          it was exceeded.
System monitoring for bromate under the  (1) The number of samples taken
 requirements of Sec.  141.132(b).        during the last quarter.
                                         (2) The location, date, and
                                          result of each sample taken
                                          during the last quarter.

[[Page 457]]

 
                                         (3) The arithmetic average of
                                          the monthly arithmetic
                                          averages of all samples taken
                                          in the last year.
                                         (4) Whether the MCL was
                                          exceeded.
------------------------------------------------------------------------

    (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        (1) The number of samples taken
 chloramines under the requirements of    during each month of the last
 Sec.  141.132(c).                        quarter.
                                         (2) The monthly arithmetic
                                          average of all samples taken
                                          in each month for the last 12
                                          months.
                                         (3) The arithmetic average of
                                          all monthly averages for the
                                          last 12 months.
                                         (4) Whether the MRDL was
                                          exceeded.
System monitoring for chlorine dioxide   (1) The dates, results, and
 under the requirements of Sec.           locations of samples taken
 141.132(c).                              during the last quarter.
                                         (2) Whether the MRDL was
                                          exceeded.
                                         (3) Whether the MRDL was
                                          exceeded in any two
                                          consecutive daily samples and
                                          whether the resulting
                                          violation was acute 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\
------------------------------------------------------------------------
System monitoring monthly or quarterly   (1) The number of paired
 for TOC under the requirements of Sec.   (source water and treated
  141.132(d) and required to meet the     water, prior to continuous
 enhanced coagulation or enhanced         disinfection) samples taken
 softening requirements in Sec.           during the last quarter.
 141.135(b)(2) or (3).
                                         (2) The location, date, and
                                          result of each paired sample
                                          and associated alkalinity
                                          taken during the last quarter.
                                         (3) 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.
                                         (4) Calculations for
                                          determining compliance with
                                          the TOC percent removal
                                          requirements, as provided in
                                          Sec.  141.135(c)(1).
                                         (5) 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.
System monitoring monthly or quarterly   (1) The alternative compliance
 for TOC under the requirements of Sec.   criterion that the system is
  141.132(d) and meeting one or more of   using.
 the alternative compliance criteria in
 Sec.  141.135(a)(2) or (3).
                                         (2) The number of paired
                                          samples taken during the last
                                          quarter.
                                         (3) The location, date, and
                                          result of each paired sample
                                          and associated alkalinity
                                          taken during the last quarter.
                                         (4) The running annual
                                          arithmetic average based on
                                          monthly averages (or quarterly
                                          samples) of source water TOC
                                          for systems meeting a
                                          criterion in Secs.
                                          141.135(a)(2)(i) or (iii) or
                                          of treated water TOC for
                                          systems meeting the criterion
                                          in Sec.  141.135(a)(2)(ii).
                                         (5) 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).
                                         (6) 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).

[[Page 458]]

 
                                         (7) The running annual average
                                          for both TTHM and HAA5 for
                                          systems meeting the criterion
                                          in Sec.  141.135(a)(2)(iii) or
                                          (iv).
                                         (8) 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).
                                         (9) 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.



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 as required by 
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 16, 2005. Failure to install 
and operate these technologies by the date in the 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

[[Page 459]]

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 and 
calculated quarterly as an annual running 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 CaCO3
                                                                  ----------------------------------------------
                      Source-water TOC, mg/L                           0-60      60-120    >120 \3\
                                                                     (percent)       (percent)        (percent)
----------------------------------------------------------------------------------------------------------------
>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 systems meeting one of the alternative compliance criteria in paragraph (a)(3) of this section are
  not required to operate with enhanced softening.
\3\ Systems 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 systems for 
approval of alternative minimum TOC removal (Step 2) requirements under 
paragraph (b)(3) of this section must include, as a minimum, results of 
bench- or pilot-scale testing conducted under paragraph (b)(4)(i) of 
this section and 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 (as aluminum) (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

[[Page 460]]

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 (as aluminum) (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 (as aluminum) (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 (as aluminum) 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) 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, 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

[[Page 461]]

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.



 Subpart M--Information Collection Requriements (ICR) for Public Water 
                                 Systems

    Source: 61 FR 24368, May 14, 1996, unless otherwise noted.

    Effective Date Note: At 61 FR 24368, May 14, 1996, subpart M, 
consisting of Secs. 141.140 through 141.144, was added, effective June 
18, 1996 and will expire on Dec. 31, 2000.



Sec. 141.140  Definitions specific to subpart M.

    The following definitions apply only to the requirements of subpart 
M of this part and are arranged alphabetically.
    Distribution system means the components of a PWS that are under the 
control of that PWS located after the point where the finished water 
sample is taken and that provide distribution, storage, and/or booster 
disinfection of finished water.
    Distribution System Equivalent (DSE) sample means a sample collected 
from the distribution system for the purpose of comparing it with the 
``simulated distribution system (SDS) sample''. The DSE sample shall be 
selected using the following criteria:
    (1) No additional disinfectant added between the treatment plant and 
the site where the DSE sample is collected;
    (2) Approximate detention time of water is available; and
    (3) There is no blending with finished water from other treatment 
plants.
    Entry point to distribution system means a location following one or 
more finished water sample points but prior to the beginning of the 
distribution system.
    Finished water means water that does not undergo further treatment 
by a treatment plant other than maintenance of a disinfection residual.
    Haloacetic acids (five) (HAA5) means the sum of the concentration in 
micrograms per liter of the haloacetic acids mono-, di-, and 
trichloroacetic acid; mono-, and di-, bromoacetic acid, rounded to two 
significant figures.
    Haloacetic acids (six) (HAA6) means the concentration in micrograms 
per liter of the haloacetic acids mono-,    di-, and trichloroacetic 
acid; mono-, and di- bromoacetic acid; and bromochloroacetic acid, 
rounded to two significant figures.
    Haloacetonitriles (HAN) means the concentration in micrograms per 
liter of the haloacetonitriles dichloro-, trichloro-, bromochloro-, and 
dibromo- acetonitrile, rounded to two significant figures.
    Haloketones (HK) means the concentration in micrograms per liter of 
the haloketones 1,1-dichloropropanone and 1,1,1- trichloropropanone, 
rounded to two significant figures.
    Intake means the physical location at which the PWS takes water from 
a water resource. Thereafter, the water is under the control of that 
PWS.
    Notice of applicability means a notice sent by EPA to a PWS that 
indicates that EPA believes that the PWS must comply with some or all 
requirements of subpart M. The PWS is required to reply to this notice 
by providing information specified in the notice (e.g., retail and 
wholesale population served, types of water sources used, volume of 
water treated) by the date provided in subpart M.

[[Page 462]]

    Process train means some number of unit processes connected in 
series starting from the treatment plant influent and ending with 
finished water. A particular unit process may be in more than one 
process train.
    Purchased finished water means finished water purchased by one PWS 
from another PWS (the wholesaler). Purchased finished water includes 
both purchased finished water that is redisinfected and purchased 
finished water that is not.
    Simulated distribution system (SDS) sample means a finished water 
sample incubated at the temperature and detention time of a ``DSE 
sample'' collected from the distribution system. Analytical results of 
the SDS sample will be compared with the DSE sample to determine how 
well the SDS sample predicts disinfection byproduct formation in the 
actual distribution system sample.
    Total finished water means the flow (volume per unit of time) of 
finished water obtained from all treatment plants operated by a PWS and 
includes purchased finished water. This flow includes water entering the 
distribution system and water sold to another PWS.
    Treatment plant means the PWS components that have as their 
exclusive source of water a shared treatment plant influent and that 
deliver finished water to a common point which is located prior to the 
point at which finished water enters a distribution system or is 
diverted for sale to another PWS. For these components of the PWS to be 
considered part of one treatment plant, the PWS must be able to collect 
one representative treatment plant influent sample, either at a single 
sample point or by a composite of multiple influent samples, and there 
must exist a single sampling point where a representative sample of 
finished water can be collected. For the purpose of subpart M, a 
treatment plant is considered to include any site where a disinfectant 
or oxidant is added to water prior to the water entering the 
distribution system. Facilities in which ground water is disinfected 
prior to entering a distribution system, and facilities in which 
purchased finished water has a disinfectant added prior to entering a 
distribution system, are considered treatment plants.
    Treatment plant influent means water that represents the water 
quality challenge to a particular plant.
    Treatment system means all treatment plants operated by one PWS.
    Trihalomethanes (four) (THM4) means the sum of the concentration in 
micrograms per liter of the trihalomethanes chloroform, 
bromodichloromethane, dibromochloromethane, and bromoform, rounded to 
two significant figures.
    Unit process means a component of a treatment process train which 
serves any treatment purpose such as mixing or sedimentation for which 
design and operating information is requested in Sec. 141.142(a), Table 
6c, of this subpart.
    Water resource means a body of water before it passes through an 
intake structure. Examples of a water resource include a river, lake, or 
aquifer. For a PWS which purchases finished water, the water resource is 
the wholesale PWS which supplies the purchased finished water. Generally 
water resources are not under the direct control of a PWS.
    Watershed control practice means protection of a water resource from 
microbiological contamination prior to the water entering an intake. 
These protective measures might include, but are not limited to, a 
watershed control program approved under Sec. 141.71(b)(2) of this part, 
or land use restrictions.



Sec. 141.141  General requirements, applicability, and schedule for information collection.

    (a) General requirements. (1) The purpose of subpart M is to collect 
specified information from certain PWSs for a limited period of time. 
Accordingly, subpart M is of limited duration and is effective for a 
defined period (see Secs. 141.6(i) and 141.141(e) of this part). Since 
subpart M does not establish continuing obligations, a PWS that has 
completed all of its requirements at the required duration and frequency 
may discontinue its information collection efforts even if subpart M is 
still in effect.

[[Page 463]]

    (2) For the purpose of this subpart, a PWS shall make applicability 
determinations based on completion of data gathering, calculations, and 
treatment plant categorization specified in appendix A to paragraph (a) 
of this section.
    (3) For the purpose of this subpart, a PWS that uses multiple wells 
drawing from the same aquifer and has no central treatment plant is 
considered to have one treatment plant for those wells and shall conduct 
required monitoring under this specification. A PWS with multiple wells 
in one or more aquifers that are treated in the same treatment plant is 
considered to have one treatment plant for those wells and shall conduct 
required monitoring under this specification.
    (i) To the extent possible, the PWS should sample at the well with 
the largest flow and at the same well each month for the duration of 
required monitoring.
    (ii) A PWS must report information from Sec. 141.142(a) tables 6a 
through 6e of this subpart for each well that the PWS sampled.
    (4) For the purpose of this subpart, a PWS shall treat ground water 
sources that have been classified by the State as under the direct 
influence of surface water by May 14, 1996, as surface water sources. A 
PWS shall treat ground water sources that either have not been 
classified by the State (as under the direct influence of surface water 
or not) or have been classified by the State as ground water, by May 14, 
1996, as ground water sources.

                     Appendix A to 40 CFR 141.141(a)

    Purpose. The purpose of this appendix is to enable the PWS to assign 
proportional amounts of its retail and wholesale population served to 
specific treatment plants. The PWS shall then use these values to 
determine which specific requirements in subpart M that it must comply 
with and on what schedule.
    Period of applicability determination. For the purpose of this 
appendix, a PWS shall make applicability determinations based on 
population calculated as annual averages based on PWS records of 
treatment system or treatment plant operation during calendar year 1995.

--If a natural disaster made a treatment system or treatment plant 
inoperable for one or more calendar months in 1995, the applicability 
determination will be based on those months in 1995 during which the 
treatment system or treatment plant was in operation, plus the calendar 
months from 1994 that are representative of those months of 1995 during 
which the treatment system or treatment plant was inoperable. The total 
time period shall be 12 months.
--If the treatment system or treatment plant was not in operation during 
one or more calendar months during 1995 due to a seasonal reduction in 
demand for finished water, the months that the treatment system or 
treatment plant was not in operation are to be included in the 12 months 
of applicability determination with zero flow indicating no operation.
--If the treatment system or treatment plant was not in operation for 
one or more calendar months in 1995 due to construction and/or 
maintenance, the applicability determination will be based on those 
months in 1995 during which the treatment system or treatment plant was 
in operation, plus the calendar months from 1994 that correspond to 
those months of 1995 during which the treatment system or treatment 
plant was inoperable. The total time period shall be 12 months.
--Treatment systems or treatment plants whose total operational lifetime 
is fewer than 12 calendar months as of December 1995 are not required to 
comply with subpart M requirements.
--PWSs that purchase all their water from one or more other PWSs and do 
not further treat any of their water are not required to comply with 
subpart M requirements.

    Applicability determination. To determine applicability, the PWS is 
required to collect certain operational data and perform specified 
mathematical operations. All operational data and calculated values will 
be expressed as either ``F'' (for flow) or ``P'' (for population), with 
a one or two character subscript. Table A-1 contains a more detailed 
explanation.

       Table A-1.--: Appendix A Subscript Identification Protocol
General.
1. ``F'' indicates a flow value. The PWS must use million gallons per
 day (MGD) to express the flow throughout its calculations.
2. ``P'' indicates a population value, expressed as a number of people.
Subscripts.
1. ``PR'' is retail population, ``FW'' is wholesale flow, and ``FN'' is
 purchased finished water that is not further treated.

[[Page 464]]

 
2. Each ``F'' value (in Table A-2) or ``P'' value (in Table A-4) will
 have a two character designator.
    a. The first character in the subscript indicates the source type.
     Possible entries are ``S'' (for surface water or ground water under
     the direct influence of surface water), ``G'' (for ground water not
     under the direct influence of surface water), ``P'' (for finished
     water purchased from another PWS and further treated at the
     entrance to the distribution system, such as by redisinfection),
     and ``C'' (for combined, or the sum of all water treated by the
     PWS, including purchased water that is further treated at the
     entrance to the distribution system).
    b. The second character in the subscript indicates the specific
     identification of the treatment plant. This will be a number (e.g.,
     1, 2, 3, * * *, with # being a non-specific designator) and ``T''
     (for a Total).
 

    Data from operational records. The PWS shall determine the following 
information based on operational records.

--PR=Retail population served by the PWS
    =________ (number of people)
--FN=treated water bought from one or more other PWSs and not 
          further treated at the entry point to the distribution system
    =________ (MGD)
--FW= finished water sold to one or more other PWSs, 
          regardless of whether buying PWSs further treat the finished 
          water
    =________ (MGD)
--Flows from specific water resources to specific treatment plants. For 
each treatment plant operated by the PWS, the PWS must determine the 
flow from each water resource that provides water to the treatment 
plant. In the following table, the PWS must enter flow from each type of 
water resource into the appropriate block, using the subscript 
identification protocol in table A-1.

--FS=surface water treated at treatment plant ``#''
    =________ (MGD) (enter into Table A-2)
--FG=ground water treated at treatment plant ``#''
    =________ (MGD) (enter into Table A-2)
--FP=treated water bought from one or more other 
          PWSs and further treated at treatment plant ``#'' prior to the 
          entry point to the distribution system
    =________ (MGD) (enter into Table A-2)

                                         Table A-2.--Treated Flow Values
----------------------------------------------------------------------------------------------------------------
                                                          Sources of treated water (FLOW)
                                  ------------------------------------------------------------------------------
 Water resources (by type source)                                 Treatment plants
                                  ------------------------------------------------------------------------------
                                           #1                  #2                  #3                  #4
----------------------------------------------------------------------------------------------------------------
Surface water (S)................  (FS1)               (FS2)               (FS3)               (FS4)
Ground water (G).................  (FG1)               (FG2)               (FG3)               (FG4)
Purchased finished water that is   (FP1)               (FP2)               (FP3)               (FP4)
 further treated (P).
Combined (C).....................  (FC1)               (FC2)               (FC3)               (FC4)
----------------------------------------------------------------------------------------------------------------
Note: The FC# value is calculated by adding the FS#, FG#, and FP# values in the column above.

--FCT=finished water produced in all of the PWS's treatment 
          plants (calculated by adding the combined flows from each 
          treatment plant ( (FC)).
    =________ (MGD)

    Calculated values. The PWS must calculate the following values.

--Population equivalents. Divide the flow values in Table A-2 by the 
conversion factor K below (a PWS-specific per capita finished water 
usage rate) and enter in the corresponding box in Table A-3 below. For 
each treatment plant operated by the PWS, the PWS must determine the 
population served by each type of water resource that provides water to 
the treatment plant.

Conversion factor=K=(FCT+FNFW)/
          PR=________
For Table A-3, P=F/K, using F values from Table A-2 (e.g., 
          PS1=FS1/K).

                                       Table A-3: Population Served Values
----------------------------------------------------------------------------------------------------------------
                                               Population served by treated water (number of people)
                                  ------------------------------------------------------------------------------
 Water resources (by type source)                                 Treatment plants
                                  ------------------------------------------------------------------------------
                                           #1                  #2                  #3                  #4
----------------------------------------------------------------------------------------------------------------
Surface water (S)................  (PS1)               (PS2)               (PS3)               (PS4)
Ground water (G).................  (PG1)               (PG2)               (PG3)               (PG4)
Purchased finished water that is   (PP1)               (PP2)               (PP3)               (PP4)
 further treated (P).

[[Page 465]]

 
Combined (C).....................  (PC1)               (PC2)               (PC3)               (PC4)
----------------------------------------------------------------------------------------------------------------
Note: The PC# value is calculated by adding the PS#, PG#, and PP# values in the column above.

--PCT=number of people served by finished water produced in 
          all of the PWS's treatment plants (calculated by adding the 
          combined populations served by each treatment plant ( 
          (PC)))
    =________ (people)
    Note: A PWS that sells all its finished water and thus has no retail 
population must calculate the population served by the PWS by raising 
the PWS's average treated flow (in MGD) to the 0.95 power and 
multiplying the result by 7,700. As an equation, this would appear as:

PWS population served=7,700 (PWS's average treated flow in 
          MGD)0.95
    The PWS may then calculate the population served by each of its 
treatment plants by multiplying the PWS population served times the 
average treated flow from the treatment plant divided by the average 
treated flow for the PWS. As an equation, this would appear as:
[GRAPHIC] [TIFF OMITTED] TC15NO91.001

    Treatment plant categorization. A PWS must categorize its treatment 
plants to determine its specific compliance requirements by reviewing 
Table A-4 below.

                                     Table A-4.--Treatment Plant Categories
----------------------------------------------------------------------------------------------------------------
    Treatment plant category              PCT                 PC#                 PS#                 PG#
----------------------------------------------------------------------------------------------------------------
A...............................  100,000  100,000  1......  NA.
B...............................  100,000  100,000  Zero..............  NA.
C...............................  100,000  PC# is 100,000 and  1......  NA.
                                                       is largest PC# in
                                                       PWS.
D...............................  100,000  PC# is 100,000 and  Zero..............  NA.
                                                       is largest PC# in
                                                       PWS.
E...............................  100,000  100,000 and is not  1......  NA.
                                                       largest PC# in
                                                       PWS.
F...............................  100,000  100,000 and is not  Zero..............  NA.
                                                       largest PC# in
                                                       PWS.
G...............................  50,000-99,999 and   NA................  NA................  Largest PG#.
                                   PGT 
                                   50,000.
----------------------------------------------------------------------------------------------------------------
NA--not applicable.


    (b) Applicability.
    (1) Table 1 of this paragraph is a summary of treatment plant 
categorization under the provisions of appendix A to paragraph (a) of 
this section.

                                      Table 1.--Treatment Plant Categories
----------------------------------------------------------------------------------------------------------------
                                                        Treatment plant     Treatment plant     Treatment plant
    Treatment plant category         PWS combined          combined          surface water       ground water
                                   population served   population served   population served   population served
----------------------------------------------------------------------------------------------------------------
A...............................  100,000  100,000  1......  NA.
B...............................  100,000  100,000  zero..............  NA.
C...............................  100,000  Plant serves        1......  NA.
                                                       100,000 and is
                                                       largest plant.

[[Page 466]]

 
D...............................  100,000  Plant serves        zero..............  100,000.
                                                       100,000 and is
                                                       largest plant.
E...............................  100,000  Plant serves        1......  NA.
                                                       100,000 and is
                                                       not largest plant
                                                       in PWS.
F...............................  100,000  Plant serves        zero..............  100,000.
                                                       100,000 and is
                                                       not largest plant
                                                       in PWS.
G...............................  50,000-99,999 and   NA................  NA................  Largest ground
                                                                                    water plant.
                                   50,000 served by
                                   ground water.
----------------------------------------------------------------------------------------------------------------
NA-not applicable.

    (2) Table 2 of this paragraph specifies applicability for 
requirements contained in Secs. 141.142, 141.143, and 141.144 of this 
part, based on treatment plant categorization determined under the 
provisions of appendix A to paragraph (a) of this section.

                                                            Table 2--Subpart M Applicability
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                         Categories of treatment plants1
                Subpart M Requirements                 -------------------------------------------------------------------------------------------------
                                                              A             B             C             D             E             F             G
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                       Sec.  141.142.--DBP and Related Monitoring
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1a and 1b.......................................            X             X             X             X             X             X   ............
Table 22..............................................            X             X             X             X             X             X   ............
Table 32..............................................            X             X             X             X             X             X   ............
Table 4a and 4b2......................................            X             X             X             X             X             X   ............
Table 5a and 5b2......................................            X             X             X             X             X             X   ............
Table 6...............................................            X             X             X             X             X             X   ............
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                        Sec.  141.143--Microbiological Monitoring
--------------------------------------------------------------------------------------------------------------------------------------------------------
Treatment plant influent monitoring...................            X   ............            X   ............            X   ............  ............
Finished water monitoring3............................            X   ............            X   ............            X   ............  ............
 
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                              Sec.  141.144--Applicability Monitoring and Treatment Studies
--------------------------------------------------------------------------------------------------------------------------------------------------------
Treatment study applicability monitoring..............            X             X             X             X   ............  ............            X
Pilot-scale treatment studies4........................            X             X   ............  ............  ............  ............  ............
Bench- or pilot-scale treatment studies4..............            X             X             X             X   ............  ............           X
--------------------------------------------------------------------------------------------------------------------------------------------------------
1 As determined by Appendix A to paragraph (a) of this section.
2 Table 2 required only for treatment plants using chloramines. Table 3 required only for treatment plants using hypochlorite solution. Table 4a and 4b
  required only for treatment plants using ozone. Table 5a and 5b required only for treatment plants using chlorine dio xide.
3 Only required for a PWS that, during any of the first twelve months of monitoring at the treatment plant influent, detects 10 or more Giardia cysts,
  or 10 or more Cryptosporidium oocysts, or one or more total culturable viruses in one liter of water; or calculates a numerical value of the Giardia
  or Cryptosporidium concentration equal to or greater than 1000 per 100 liters or virus concentration equal to or greater than 100 per 100 liters; or
  detects no pathogens in the sample and calculates a numerical value of the detection limit for Giardia or Cryptosporidium concentration equal to or
  greater than 1000 per 100 liters or virus concentration equal to or greater than 100 per 100 liters.
4 Pilot-scale treatment studies are required for treatment plants that serve a population of 500,000 or greater. Bench- or pilot-scale treatment studies
  are required for treatment plants that serve a population of fewer than 500,000.

    (c) Disinfection Byproduct and Related Monitoring. A PWS must comply 
with the monitoring requirements in Sec. 141.142 of this subpart for 
treatment plants in treatment plant categories A, B, C, D, and E listed 
in table 1 in paragraph (b)(1) of this section. The PWS shall monitor 
monthly for 18 consecutive months at each treatment plant, even if a 
treatment plant was not used for one or more calendar months. When the 
treatment plant is not operating,

[[Page 467]]

the PWS shall file the report required under Sec. 141.142(c) of this 
subpart to indicate zero flow, and need only conduct treatment plant 
influent monitoring under the provisions of Sec. 141.142 of this 
subpart. A PWS must comply with the monitoring requirements in 
Sec. 141.142 of this subpart for treatment plants in treatment plant 
categories F listed in table 1 in paragraph (b)(1) of this section 
monthly for 18 consecutive months at each treatment plant, except if a 
treatment plant was not used for one or more calendar months. When the 
treatment plant is not operating, the PWS shall file the report required 
under Sec. 141.142(c) of this subpart to indicate zero flow, and is not 
required to conduct treatment plant influent monitoring under the 
provisions of Sec. 141.142 of this subpart.
    (d) Microbiological Monitoring. A PWS must comply with the 
monitoring requirements in Sec. 141.143 of this subpart for treatment 
plants in treatment plant categories A, C, and E listed in table 1 in 
paragraph (b)(1) of this section and table 3 of this paragraph. The PWS 
shall conduct 18 consecutive months of microbiological monitoring at 
each treatment plant, even if it is not operated each calendar month.

     Table 3.--Microbiological Monitoring Requirements for Subpart M
------------------------------------------------------------------------
                                         Treatment plant category
                                 ---------------------------------------
                                                A, C and E
        Microbial sample         ---------------------------------------
                                    Treatment plant
                                       influent       Finished water \1\
------------------------------------------------------------------------
Total culturable viruses........  1/month \2\.......  1/month.
Total coliforms.................  1/month...........  1/month.
Fecal coliforms or E. coli......  1/month...........  1/month.
Giardia.........................  1/month...........  1/month.\3\
Cryptosporidium.................  1/month...........  1/month.\3\
------------------------------------------------------------------------
\1\ Only required for a PWS that, during any of the first twelve months
  of monitoring at the treatment plant influent, detects 10 or more
  Giardia cysts, or 10 or more Cryptosporidium oocysts, or one or more
  total culturable viruses in one liter of water; or calculates a
  numerical value of the Giardia or Cryptosporidium concentration equal
  to or greater than 1000 per 100 liters or virus concentration equal to
  or greater than 100 per 100 liters; or detects no pathogens in the
  sample and calculates a numerical value of the detection limit for
  Giardia or Cryptosporidium concentration equal to or greater than 1000
  per 100 liters or virus concentration equal to or greater than 100 per
  100 liters. The PWS shall collect one sample of finished water during
  each month that the treatment plant is operated at each such treatment
  plant beginning in the first calendar month after the PWS learns of
  such a result. A PWS shall continue finished water monitoring monthly
  until 18 months of treatment plant influent monitoring has been
  completed.
\2\ A PWS may avoid virus monitoring if the PWS has monitored total
  coliforms, fecal coliforms, or E. coli in the source water for at
  least five days/week for any period of six consecutive months
  beginning after January 1, 1994, and 90% of all samples taken in that
  six-month period contained no greater than 100 total coliforms/100 ml,
  or 20 fecal coliforms/100 ml, or 20 E. coli/100 ml.
\3\ A PWS may avoid the requirement for finished water monitoring of
  Giardia and Cryptosporidium if the PWS notifies EPA that it will
  comply with the alternative monitoring requirements in Sec.
  141.143(a)(2)(iii). The PWS must still conduct finished water
  monitoring for all other microorganisms, except that Giardia and
  Cryptosporidium monitoring in the finished water is not required.

    (e) Disinfection Byproduct Precursor Removal Studies (Treatment 
Studies).
    (1) A PWS shall comply with treatment study applicability monitoring 
in paragraph (e)(2) of this section at each treatment plant in treatment 
plant categories A, B, C, D, and G listed in table 1 in paragraph (b)(1) 
of this section. A PWS shall comply with the treatment study 
requirements in Sec. 141.144 of this subpart at each such treatment 
plant, except for those treatment plants:
    (i) Meeting the source water quality, disinfection practice, or 
disinfection byproduct precursor removal practice criteria in paragraph 
(e)(3) of this section, for which no treatment study is required; or
    (ii) Meeting the common water resource criteria in paragraph (e)(4) 
of this section, for which several PWSs may conduct treatment studies 
jointly, in lieu of separately; or
    (iii) Meeting the common water resource criteria in paragraph (e)(5) 
of this section, for which a PWS may contribute funds towards research, 
in lieu of conducting a treatment study; or
    (iv) At which a previous treatment study that meets the criteria in 
paragraph (e)(6) of this section has already been conducted, for which a 
PWS may use the results of this previous treatment study, in lieu of 
conducting another treatment study; or
    (v) Operated by the PWS that use the same water resource, as 
classified by

[[Page 468]]

the procedure in paragraph (e)(4) of this section. The PWS is not 
required to conduct more than one treatment study for those treatment 
plants. If both pilot-scale and bench-scale treatment studies would 
otherwise be required for treatment plants on the same water resource, 
the PWS shall conduct a pilot-scale study. A PWS with multiple water 
resources shall conduct treatment studies for each treatment plant that 
uses different water resources.
    (2) Treatment study applicability monitoring.
    (i) PWSs shall monitor total organic carbon (TOC) monthly for 12 
months. Treatment plants using surface water shall monitor treatment 
plant influent. Treatment plants using ground water shall monitor 
finished water.
    (ii) Treatment study applicability monitoring for THM4 and HAA5 is 
only required by a PWS that intends to qualify for avoiding a treatment 
study under the provisions of paragraph (e)(3)(i) of this section.
    (iii) Total organic halides formed under the uniform formation 
conditions (UFCTOX) monitoring is only required by a PWS that intends to 
qualify for a joint treatment study under the provisions of paragraph 
(e)(4)(i)(A)(2) of this section or for the alternative to conducting a 
treatment study under the provisions of paragraph (e)(5) of this 
section.
    (3) Criteria under which no treatment study is required. A PWS 
identified in paragraph (e)(1) of this section is not required to 
conduct a treatment study at any treatment plant that satisfies any 
criteria in paragraphs (e)(3) (i) through (iv) of this section, provided 
that the PWS has also complied with the requirements in paragraph 
(e)(7)(i) of this section and EPA has approved the PWS's request to 
avoid the treatment study.
    (i) Treatment plants that use chlorine as both the primary and 
residual disinfectant and have, as an annual average of four quarterly 
averages, levels of less than 40

 g/l for THM4 and less than 30  g/l for HAA5. 
Quarterly averages are the arithmetic average of the four distribution 
system samples collected under the requirements of Sec. 141.142(a)(1) of 
this subpart.
    (ii) Treatment plants using surface water that do not exceed a TOC 
annual average of 4.0 mg/l in the treatment plant influent, measured in 
accordance with Secs. 141.141(f)(4) and 141.144(a) of this subpart and 
calculated by averaging the initial 12 monthly TOC samples.
    (iii) Treatment plants using only ground water not under the direct 
influence of surface water that do not exceed a TOC annual average of 
2.0 mg/l in the finished water, measured in accordance with 
Secs. 141.141(f)(4) and 141.144(a) of this subpart and calculated by 
averaging the initial 12 monthly TOC samples.
    (iv) Treatment plants that already use full scale membrane or GAC 
technology. For a treatment plant that already uses full-scale GAC or 
membrane technology capable of achieving precursor removal, a PWS shall 
conduct monitoring and submit full-scale plant data required for 
disinfection byproduct and related monitoring by Sec. 141.142(a) of this 
subpart, ensuring that the GAC or membrane processes are included in the 
process train being monitored. For a treatment plant to be considered to 
have membrane technology to achieve precursor removal, the PWS shall 
have used nanofiltration or reverse osmosis membranes. GAC capable of 
removing precursors is defined as GAC with an empty bed contact time 
(EBCT) of 15 minutes or greater, with a time between carbon reactivation 
or replacement of no more than nine months. PWSs that operate treatment 
plants that use GAC with either an EBCT of less than 15 minutes or a 
replacement or reactivation frequency for GAC longer than nine months 
may submit a request to avoid treatment studies under the provisions of 
paragraph (e)(7)(i) of this section by including data demonstrating 
effective DBP precursor removal.
    (4) Criteria under which joint treatment studies are allowed. (i) 
PWSs that use common water resources and have similar treatment trains 
may conduct joint treatment studies. A common water resource for all 
types of surface water resources requires the mean treatment plant 
influent TOC or UFCTOX of each of the cooperating

[[Page 469]]

treatment plants to be within 10% of the average of the mean treatment 
plant influent TOCs or UFCTOX of all the cooperating treatment plants. A 
common water resource for all types of ground water resources requires 
the mean treatment plant finished water TOC or UFCTOX of each of the 
cooperating treatment plants to be within 10% of the average of the mean 
treatment plant finished water TOCs or UFCTOX of all the cooperating 
treatment plants. The mean is calculated from the monthly TOC or UFCTOX 
monitoring data for the initial twelve months of monitoring under 
Sec. 141.144(a) of this subpart. Similar treatment trains means that, 
for example, softening plants may not conduct joint studies with 
conventional treatment plants. In addition, the applicable requirements 
in paragraphs (e)(4)(i) (A) through (C) of this section shall be met for 
the water resource to be considered a common water resource. If 
otherwise eligible, a PWS may choose to either perform a joint treatment 
study with other eligible systems or contribute funds to a cooperative 
research program, as described in paragraph (e)(5) of this section, as 
an alternative to conducting a treatment study.
    (A) River sources. Treatment plants with river intakes are 
considered to have a common water resource if the PWS meets either 
criteria in paragraphs (e)(4)(i)(A) (1) or (2) of this section.
    (1) The intakes are no more than 20 river miles apart and TOC at 
each treatment plant influent is within 10% of the mean TOC of all the 
treatment plant influents.
    (2) The intakes are at least 20, but no more than 200, river miles 
apart and the PWS demonstrates that the mean water resource UFCTOX is 
within 10% of the mean UFCTOX of all the treatment plant influents, 
based on UFCTOX analytical results of the same 12 consecutive months for 
all cooperating treatment plants.
    (B) Lake/reservoir. Treatment plants with lake or reservoir intakes 
are considered to have a common water resource if the same lake or 
reservoir serves all the cooperating treatment plants and TOC at each 
treatment plant influent is within 10% of the mean TOC of all the 
treatment plant influents.
    (C) Ground water not under the direct influence of surface water. 
Treatment plants with intakes from a single aquifer are considered to 
have a common water resource if treatment plant finished water TOC at 
each treatment plant is within 10% of the mean finished water TOC of all 
the treatment plants.
    (ii) PWSs that meet the requirements of paragraph (e)(4)(i) of this 
section shall conduct at least the number and type of joint studies 
noted in the following tables. Joint studies shall only be conducted 
among treatment plants in the same size category, i.e. a population 
served of either 500,000 or of 500,000. The maximum number of 
treatment plants with a population served 500,000 persons 
allowed to join together to conduct a study is three. The maximum number 
of treatment plants with a population served 500,000 persons allowed to 
join together to conduct a study is six.

 Joint Studies Requirement for Treatment Plants With a Population Served
                               of 500,000
------------------------------------------------------------------------
       Number of plants              Minimum studies to be conducted
------------------------------------------------------------------------
2.............................  1 pilot (GAC or membrane).
3.............................  1 pilot and 1 bench (GAC or membrane).
4.............................  2 pilots (GAC and/or membrane).
5.............................  2 pilots (GAC and/or membrane), 1 bench
                                 (GAC or membrane).
6.............................  2 pilots and 2 bench (GAC and/or
                                 membrane).
------------------------------------------------------------------------


 Joint Studies Requirement For Treatment Plants With a Population Served
                          of 500,000
------------------------------------------------------------------------
       Number of plants              Minimum studies to be conducted
------------------------------------------------------------------------
2.............................  1 pilot (GAC or membrane), 2 bench (GAC
                                 and/or membrane).
3.............................  2 pilots (GAC and/or membrane).
------------------------------------------------------------------------

    (5) Criteria under which an alternative to conducting a treatment 
study is allowed. In lieu of conducting the required treatment study, a 
PWS may apply to EPA to contribute funds to a cooperative research 
effort. The PWS shall submit an application to EPA Technical Support 
Division, ICR Precursor Removal Studies Coordinator, 26

[[Page 470]]

W. Martin Luther King Drive, Cincinnati, OH 45268. The application shall 
show that the treatment plant for which the waiver of the treatment 
study is sought uses a common water resource, as described in paragraph 
(e)(4) of this section, that is being studied by another PWS or 
cooperative of PWSs operating treatment plants in the same size 
category. A PWS operating treatment plants serving a population of fewer 
than 500,000 may also contribute to this fund if there is a common water 
resource (as defined in paragraph (e)(4) of this section) treatment 
plant serving 500,000 or more conducting a treatment study. If EPA 
approves the application, the PWS shall contribute funds in the amount 
specified in paragraph (e)(5)(i) of this section to the Disinfection 
Byproducts/Microbial Research Fund, to be administered by the American 
Water Works Association Research Foundation (AWWARF) under the direction 
of an independent research council, for use in a dedicated cooperative 
research program related to disinfectants, disinfection byproducts, and 
enhanced surface water treatment.
    (i) The PWS shall contribute $300,000 for a treatment plant with a 
population served of 500,000 or more. The PWS shall contribute $100,000 
for a treatment plant with a population served of fewer than 500,000.
    (ii) The PWS shall send the contribution to the address specified in 
EPA's approval letter not later than 90 days after EPA approves the PWS 
application for waiver of the treatment study.
    (6) Criteria under which a previous treatment study is acceptable 
(grandfathered studies). A PWS that has conducted studies of precursor 
removal that meet all the criteria in paragraphs (e)(6) (i) and (ii) of 
this section may use the results of that study in lieu of conducting 
another treatment study.
    (i) The PWS used analytical methods specified in table 7 of 
Sec. 141.142(b)(1) of this subpart and used the analytical and quality 
control procedures described in ``DBP/ICR Analytical Methods Manual'', 
EPA 814-B-96-002.
    (ii) The PWS followed a protocol similar to that specified and 
supplies the data specified in ``ICR Bench- and Pilot-scale Treatment 
Study Manual'' (EPA 814-B-96-003, April 1996).
    (7) Process for a PWS to obtain EPA approval of criteria 
applicability. A PWS wanting to avoid the requirements for a treatment 
study under the provisions of paragraphs (e) (3) through (6) of this 
section shall submit the applicable information in paragraphs (e)(7) (i) 
through (iv) of this section and in ``ICR Bench- and Pilot-scale 
Treatment Study Manual'' (EPA 814-B-96-003, April 1996) and all 
monitoring data required under Secs. 141.142(a) and 141.143(a) of this 
subpart to EPA, Technical Support Division, ICR Precursor Removal 
Studies Coordinator, 26 W. Martin Luther King Drive, Cincinnati, OH 
45268.
    (i) Approval of request to avoid treatment studies. A PWS that 
believes it qualifies to avoid the requirements for a treatment study 
under the provisions of paragraph (e)(3) (i) through (iii) of this 
section shall submit the information showing the applicable criterion 
for not conducting the study has been met not later than November 14, 
1997. A PWS wanting to avoid the requirements for a treatment study 
under the provisions of paragraph (e)(3)(iv) of this section shall 
submit the supporting information, including any pilot- or full-scale 
data showing effective precursor removal, not later than November 14, 
1997. A PWS that applies to avoid a treatment study under the provisions 
of paragraph (e) (4) through (6) of this section and subsequently 
qualifies to avoid a treatment study under the provisions of paragraph 
(e)(3) (i) through (iii) of this section may elect to avoid a treatment 
study under the provisions of paragraph (e)(3) (i) through (iii) of this 
section. If the PWS elects to avoid a treatment study under the 
provisions of paragraph (e)(3) (i) through (iii) of this section, the 
PWS shall notify all PWSs that were associated with the application to 
avoid a treatment study under the provisions of paragraph (e) (4) 
through (6) of this section.
    (ii) Approval of request to conduct joint studies. A PWS that 
believes it qualifies to avoid the requirements for a treatment study 
under the joint study provisions of paragraph (e)(4) of this section 
shall submit a letter of intent to EPA with the information in 
paragraphs (e)(7)(ii) (A) through (F) of this

[[Page 471]]

section for all treatment plants to be included in the joint study not 
later than May 14, 1997. The letter shall be signed by all PWSs planning 
to participate in the joint study. All PWSs shall submit a combined 
application for joint studies approval to EPA (including 12 months of 
treatment plant influent TOC or finished water TOC results or UFCTOX 
results, as appropriate, for each treatment plant to be included in the 
joint study) not later than November 14, 1997.
    (A) Data to support their common water resource designation.
    (B) Information to demonstrate that treatment plants have similar 
treatment trains.
    (C) Information that treatment plants are in the same size category.
    (D) The treatment plant influent TOC or finished water TOC results, 
or UFCTOX results, as appropriate, from the first six months of 
monitoring.
    (E) What studies will be conducted (i.e., combination of bench/pilot 
and GAC/membrane).
    (F) Any additional supporting data.
    (iii) Approval of request for alternative to treatment studies. A 
PWS that believes it qualifies to avoid the requirements for a treatment 
study under the provisions for an alternative in paragraph (e)(5) of 
this section shall submit a letter of intent expressing its intention to 
contribute funds to the cooperative research effort not later than May 
14, 1997. The letter shall identify the other treatment plants using the 
same water resource which will be conducting studies. Each PWS shall 
submit an application for approval of alternative to treatment studies 
to EPA (including 12 months of treatment plant influent TOC or finished 
water TOC results or UFCTOX results, as appropriate) not later than 
November 14, 1997. EPA shall notify the PWS whether a treatment study is 
required (because there is no other appropriately sized treatment plant 
using the same water resource conducting a treatment study) or if the 
PWS can avoid the study by contributing funds to the cooperative 
research effort specified in paragraph (e)(5) of this section.
    (iv) Approval of request to use grandfathered studies. A PWS that 
believes it qualifies to avoid the requirements for a treatment study 
under the grandfathered study provisions of paragraph (e)(6) of this 
section shall submit the following information not later than February 
14, 1997: a description of the study, the equipment used, the 
experimental protocol, the analytical methods, the quality assurance 
plan, and any reports resulting from the study. EPA shall review the 
information and inform the PWS whether or not the prior study meets the 
ICR requirements. Not later than November 14, 1997, the PWS must submit 
study data in the format specified in ``ICR Manual for Bench- and Pilot-
scale Treatment Studies'', EPA 814-B-96-003, April 1996. An approved 
grandfathered study can be justification for common water resource PWSs 
contributing to the cooperative research effort under the provisions of 
paragraph (e)(5) of this section, but may not be used as joint treatment 
studies unless it incorporates the requirements listed in 
Sec. 141.141(e)(4) of this section and the PWS submits written 
concurrence of the PWS which conducted the study.
    (f) Effective dates. (1) A PWS shall respond to the Notice of 
Applicability sent by EPA within 35 calendar days of receipt of that 
notice. The PWS's response to the Notice shall indicate what 
requirements in subpart M apply to each treatment plant operated by the 
PWS. If a PWS meets the applicability criteria in paragraph (b) of this 
section and has not received a Notice of Applicability from EPA by June 
28, 1996, that PWS must request a Notice of Applicability from EPA by 
contacting the ICR Utilities Coordinator, TSD, USEPA, 26 West Martin 
Luther King Drive, Cincinnati, OH 45268, not later than July 15, 1996.
    (2) A PWS required to monitor under both paragraphs (c) and (d) of 
this section shall begin monitoring to comply with the provisions of 
Sec. 141.142 (Disinfection Byproduct and Related Monitoring) and 
Sec. 141.143 (Microbiological Monitoring) of this subpart in the same 
month. The PWS must submit the sampling plans required by 
Secs. 141.142(c)(2)(ii) and 141.143(c)(3)(ii) of this subpart at the 
same time.
    (3) Disinfection Byproduct and Related Monitoring. A PWS operating a 
treatment plant required to comply with

[[Page 472]]

Sec. 141.142 of this subpart shall begin monitoring in the calendar 
month following approval of the DBP and related monitoring sampling plan 
submitted under the provisions of Sec. 141.142(c)(2)(ii) of this 
subpart. Once a PWS has begun monitoring, it shall continue to monitor 
for 18 consecutive months.
    (4) Microbiological Monitoring. A PWS operating a treatment plant 
identified in paragraph (d) of this section shall begin monitoring under 
the provisions of Sec. 141.143 of this subpart in the calendar month 
following approval of the sampling plan submitted under the provisions 
of Sec. 141.143(c)(3)(ii) of this subpart. Once a PWS has begun 
monitoring, it shall continue to monitor for 18 consecutive months.
    (5) DBP precursor removal studies. (i) TOC, UFCTOX, THM4, and HAA5 
monitoring. A PWS required to comply with Sec. 141.144 of this subpart 
shall begin TOC, UFCTOX, THM4, and HAA5 monitoring specified in 
paragraph (e)(2) of this section not later than August 14, 1996 and 
continue this monitoring for 12 consecutive months for TOC and UFCTOX 
and four consecutive quarters for THM4 and HAA5.
    (ii) A PWS required to conduct a disinfection byproduct precursor 
removal study (treatment study) under the provisions of paragraph (e)(1) 
of this section shall begin conducting such treatment studies not later 
than April 14, 1998 and submit the report(s) of the completed study to 
EPA not later than July 14, 1999.



Sec. 141.142  Disinfection byproduct and related monitoring.

    (a) Monitoring requirements. Samples taken under the provisions of 
this section shall be taken according to the procedures described in the 
``ICR Sampling Manual,'' EPA 814-B-96-001, April 1996. If a treatment 
plant configuration results in two required sampling points from any 
table in this section when in fact it is a single location, duplicate 
analyses are not required for the same location and time. A PWS that 
uses purchased finished water shall determine whether any monitoring of 
treatment plant influent is required under paragraphs (a) (2) through 
(5) of this section because of certain treatment (e.g., use of 
hypochlorite or chlorine dioxide) of the water provided by the selling 
PWS.
    (1) A PWS shall obtain a complete set of samples at the frequency 
and location noted in tables 1a and 1b of this section for treatment 
plants required to test under Sec. 141.141(b) of this subpart. Samples 
shall be taken according to the sampling plan approved under the 
provisions of paragraph (c)(2)(ii) of this section.
    (i) Samples of finished water shall be collected at a point after 
which all treatment processes for a particular treatment plant are 
complete (including the clearwell and final point of chlorination) and 
before the distribution system begins. A PWS that purchases finished 
water shall collect a sample before additional disinfectant is added to 
the purchased finished water. A PWS shall collect a sample of purchased 
finished water only if the PWS redisinfects the purchased finished 
water. A sample of finished water is a sample representing the final 
product water from a particular treatment plant.
    (ii) A sample of treatment plant influent for a PWS that treats 
untreated water shall be taken at a location at the upstream end of a 
treatment plant where waters from all intakes are blended prior to any 
treatment or chemical addition. For treatment plants that have multiple 
intakes and add chemicals at the intake, the sample of treatment plant 
influent shall be a flow proportional composite of intake samples 
collected before chemical addition and before pretreatment. If the 
intakes are expected to have the same source water quality, one 
representative intake sample may be taken. If a disinfectant is added at 
or before the intake (e.g., for zebra mussel control), the sample shall 
be taken in the vicinity of the intake so that the sample is not 
contaminated by the disinfectant. A sample of treatment plant influent 
for a PWS that treats purchased finished water is taken at a location 
just before the purchased finished water is treated. An intake sample is 
collected after the intake but before blending with waters from other 
intakes and before addition of chemicals or any treatment.

[[Page 473]]



     Table 1a.--Monthly Monitoring Requirements for Treatment Plants
------------------------------------------------------------------------
        Sampling point                     Monthly analyses 1
------------------------------------------------------------------------
Treatment plant influent for   pH, Alkalinity, Turbidity, Temperature,
 non-finished water.            Calcium and Total Hardness, TOC, UV 254,
                                Bromide, Ammonia.
Treatment plant influent for   pH, Alkalinity, Turbidity, Temperature,
 purchased finished water 2.    Calcium and Total Hardness, TOC, UV 254,
                                Disinfectant residual 3.
Before first point of oxidant  Chlorine demand test.
 addition.
Washwater return between       pH, Alkalinity, Turbidity, Temperature,
 washwater treatment plant      Calcium and Total hardness, TOC, UV 254,
 and point of addition to       Bromide, Ammonia, Disinfectant residual
 process train 4.               3 if disinfectant is used.
Additional water sources       pH, Alkalinity, Turbidity, Temperature,
 added to process train after   Calcium and Total hardness, TOC, UV 254,
 treatment plant influent.      Bromide, Ammonia, Disinfectant residual
 The sample point is before     3 if disinfectant is used.
 additional water is blended
 with the process train.
Before Filtration............  pH, Alkalinity, Turbidity, Temperature,
                                Calcium and Total Hardness, TOC, and UV
                                254.
After Filtration.............  pH, Alkalinity, Turbidity, Temperature,
                                Calcium and Total Hardness, TOC, and UV
                                254.
Before each Point of           pH, Alkalinity, Turbidity, Temperature,
 Disinfection 5.                Calcium and Total Hardness, TOC, and UV
                                254.
After every unit process that  Disinfectant Residual 3.
 is downstream from the
 addition of chlorine or
 chloramines.
Finished water sample point    pH, Alkalinity, Turbidity, Temperature,
 (Plant effluent).              Calcium and Total Hardness, TOC, UV 254,
                                Disinfectant Residual 3.
Entry point to distribution    pH, Alkalinity, Turbidity, Temperature,
 system 6.                      Calcium and Total Hardness, TOC, UV 254,
                                Disinfectant Residual 3.
------------------------------------------------------------------------
\1\ TOC: total organic carbon. UV 254 absorbance of
  ultraviolet light at 254 nanometers.
\2\ Samples of purchased finished water shall be taken prior to addition
  of any more disinfectant.
\3\ Free chlorine residual and total chlorine residual shall be measured
  in treatment systems using free chlorine. Total chlorine residual, but
  not free chlorine residual, shall be measured in treatment systems
  using chloramines as the residual disinfectant.
\4\ Washwater return shall be sampled prior to blending with the process
  train.
\5\ For utilities using ozone or chlorine dioxide, Tables 4 and 5,
  respectively, of this section, show additional monitoring requirements
  at this sampling point. Addition of ammonia for the purpose of
  converting free chlorine to chloramines is considered a point of
  disinfectant addition. PWSs that disinfect just before filtration may
  use the ``before filtration'' sampling point analytical results to
  meet the monitoring requirement for this point.
\6\ Entry point to distribution system only required for treatment
  plants that blend finished water with finished water from other
  treatment plant(s) prior to entry point of distribution system. For
  most treatment plants, the finished water sample point and the entry
  point to the distribution system are the same.


    Table 1b.--Quarterly Monitoring Requirements for Treatment Plants
------------------------------------------------------------------------
        Sampling point                    Quarterly analyses1
------------------------------------------------------------------------
Treatment plant influent for   TOX.
 non-finished water.
Treatment plant influent for   THM4, HAA67, HAN, CP, HK, CH, TOX.
 purchased finished water.
Washwater Return between       TOX.
 washwater treatment plant
 and point of addition to
 process train.
After filtration if            THM4, HAA67, HAN, CP, HK, CH, TOX.
 disinfectant is applied at
 any point in the treatment
 plant prior to filtration.
Finished water sample point    THM4, HAA67, HAN, CP, HK, CH, TOX.
 (Plant Effluent).
Entry point to distribution    THM4, HAA67, HAN, CP, HK, CH, TOX.
 system2.
SDS3.........................  THM4, HAA67, HAN, CP, HK, CH, TOX, pH,
                                Alkalinity, Turbidity, Temperature,
                                Calcium and Total Hardness, Disinfectant
                                Residual5.
Four monitoring points in      THM4, HAA67, HAN, CP, HK, CH, TOX, pH,
 distribution system4,6.        Alkalinity, Turbidity, Temperature,
                                Calcium and Total Hardness, Disinfectant
                                Residual5.
------------------------------------------------------------------------
\1\ TOC: total organic carbon. THM4: trihalomethane (four). HAA6:
  haloacetic acids (six). HAN: Haloacetonitriles. CP: chloropicrin. HK:
  haloketones. CH: chloral hydrate. TOX: total organic halide. For THM4,
  HAA6, HAN, and HK, analytical results for individual analytes shall be
  reported.
\2\ Entry point to distribution system only required for treatment
  plants that blend finished water with finished water from other
  treatment plant(s) prior to entry point of distribution system. For
  most treatment plants, the finished water sample point and the entry
  point to the distribution system are the same.
\3\ Simulated Distribution System (SDS) sample shall be collected at the
  finished water sampling point (or entry point to distribution system
  if finished water from two or more plants are blended prior to
  entering the distribution system) and analyzed using the method
  specified in Sec.  141.142. PWSs using purchased finished water are
  not required to take an SDS sample at treatment plants that use only
  purchased finished water.

[[Page 474]]

 
\4\ For each treatment plant, one distribution system equivalent sample
  location (known as DSE) shall be chosen to correspond to the SDS
  sample, one sample location shall be chosen to be representative of
  maximum residence time for the treatment plant, and the remaining two
  sample locations shall be representative of the average residence time
  in the distribution system for the treatment plant. PWSs using
  purchased finished water shall take three samples representing the
  average residence time in the distribution system for the treatment
  plant and one representing the maximum residence time for the
  treatment plant (no DSE sample required).
\5\ Free chlorine residual and total chlorine residual shall be measured
  in treatment systems using free chlorine. Total chlorine residual, but
  not free chlorine residual, shall be measured in treatment systems
  using chloramines as the residual disinfectant.
\6\ A PWS may use TTHM compliance monitoring locations and analytical
  results under Sec.  141.30 of this part to the extent that such
  locations and analytical results are consistent with the requirements
  of this section.
\7\ PWSs are encouraged to also analyze for the additional haloacetic
  acids bromodichloro-, chlorodibromo-, and tribromo-acetic acid, and
  report the results as part of the reports specified in paragraph
  (c)(1) of this section.

    (2) Additional requirements for PWSs using chloramines. For each 
treatment plant that uses chloramines for treatment or disinfection 
residual maintenance, a PWS shall also conduct the additional sampling 
identified in table 2 of this section. A PWS shall send samples of 
cyanogen chloride taken under the provisions of this paragraph for 
analysis to EPA, following the procedures contained in the ``ICR 
Sampling Manual,'' EPA 814-B-96-001, April 1996.

  Table 2.--Additional Quarterly Monitoring for Treatment Plants Using
                               Chloramines
------------------------------------------------------------------------
             Sampling point                     Quarterly analyses
------------------------------------------------------------------------
Treatment plant influent for purchased   Cyanogen Chloride\2\.
 finished water \1\.
Finished water sample point (plant       Cyanogen Chloride\2\.
 effluent).
Distribution system sample point         Cyanogen Chloride\2\.
 representing a maximum residence time
 in distribution system relative to the
 treatment plant.
------------------------------------------------------------------------
\1\ Applicable only when wholesale water provider is using chloramines.
\2\ EPA shall provide all analytical results to the PWS. The PWS shall
  report all results in its monthly report.

    (3) Additional requirements for PWSs using hypochlorite solutions. 
For each treatment plant that uses hypochlorite solutions for treatment 
or disinfection residual maintenance, a PWS shall also conduct the 
additional sampling identified in table 3 of this section.

  Table 3.--Additional Quarterly Monitoring for Treatment Plants Using
                         Hypochlorite Solutions
------------------------------------------------------------------------
             Sampling point                     Quarterly analyses
------------------------------------------------------------------------
Treatment plant influent for non-        Chlorate.
 finished water.
Treatment plant influent for purchased   Chlorate.
 finished water \1\.
Hypochlorite Stock Solution............  pH, Temperature, Free Residual
                                          Chlorine, Chlorate.
Finished Water Sample Point (Plant       Chlorate.
 Effluent).
------------------------------------------------------------------------
\1\ Applicable only when wholesale water provider is using hypochlorite
  solutions.

    (4) Additional requirements for PWSs using ozone. For each treatment 
plant that uses ozone for treatment, a PWS shall also conduct the 
additional sampling identified in tables 4a and 4b of this section. A 
PWS shall collect samples for bromate taken under the provisions of this 
paragraph in duplicate, with the PWS analyzing one aliquot and 
submitting the other aliquot for analysis to EPA, following the 
procedures contained in the ``ICR Sampling Manual,'' EPA 814-B-96-001, 
April 1996. A PWS shall submit samples for aldehydes taken under the 
provisions of this paragraph for analysis to EPA, following the 
procedures contained in the ``ICR Sampling Manual,'' EPA 814-B-96-001, 
April 1996.

   Table 4a.--Additional Monthly Monitoring for Treatment Plants Using
                                  Ozone
------------------------------------------------------------------------
             Sampling point                      Monthly analyses
------------------------------------------------------------------------
Ozone Contactor Influent...............  Bromide, bromate 2,3, and
                                          ammonia.
Each Ozone Contact Chamber Effluent \1\  Ozone residual.

[[Page 475]]

 
Ozone Contactor Effluent...............  Bromate\2\.
Finished Water Sample Point (Plant       Bromate\2\.
 Effluent).
------------------------------------------------------------------------
\1\ Each ozone contactor can be subdivided into its contact chambers.
  Measure ozone residual in effluent of all contact chambers until 0.05
  mg/l is measured in two consecutive chambers.
\2\ EPA shall provide all analytical results to the PWS. The PWS shall
  report all results in its monthly report.
\3\PWSs are not required to analyze a bromate sample at this location.
  However, PWSs are still required to submit a sample to EPA for
  analysis.


  Table 4b.--Additional Quarterly Monitoring for Treatment Plants Using
                                  Ozone
------------------------------------------------------------------------
             Sampling point                     Quarterly analyses
------------------------------------------------------------------------
Ozone Contactor Influent...............  Aldehydes \1\ and AOC/BDOC \2\.
Ozone Contactor Effluent...............  Aldehydes \1\ and AOC/BDOC \2\.
Finished Water Sample Point (Plant       Aldehydes \1\ and AOC/BDOC \2\.
 Effluent).
------------------------------------------------------------------------
\1\ EPA shall measure the following aldehydes: formaldehyde,
  acetaldehyde, propanal, butanal, pentanal, glyoxal, and methyl
  glyoxal. EPA may analyze for other aldehydes. EPA shall provide all
  analytical results to the PWS. The PWS shall report all results in its
  monthly report.
\2\ Analysis and submission of data for both assimilable organic carbon
  (AOC) and biodegradable organic carbon (BDOC) are optional. Analytical
  methods for AOC and BDOC are listed in ``DBP/ICR Analytical Methods
  Manual,'' EPA 814-B-96-002, April 1996.

    (5) Additional sampling requirements for PWSs using chlorine 
dioxide. For each treatment plant that uses chlorine dioxide for 
treatment or disinfection residual maintenance, a PWS shall also conduct 
the additional sampling identified in tables 5a and 5b of this section. 
A PWS shall collect samples for bromate taken under the provisions of 
this paragraph in duplicate, with the PWS analyzing one aliquot and 
submitting the other aliquot for analysis to EPA, following the 
procedures contained in the ``ICR Sampling Manual,'' EPA 814-B-96-001, 
April 1996. A PWS shall submit samples for aldehydes taken under the 
provisions of this paragraph for analysis to EPA, following the 
procedures contained in the ``ICR Sampling Manual,'' EPA 814-B-96-001, 
April 1996.

   Table 5a.--Additional Monthly Monitoring for Treatment Plants Using
                            Chlorine Dioxide
------------------------------------------------------------------------
             Sampling point                      Monthly analyses
------------------------------------------------------------------------
Treatment plant influent for purchased   Chlorine Dioxide Residual,
 finished water \1\.                      Chlorite, Chlorate.
Before first chlorine dioxide            Chlorate, bromate 2,3.
 application.
Before application of ferrous salts,     Chlorine Dioxide Residual,
 sulfur reducing agents, or GAC.          Chlorite, Chlorate, pH.
Finished water sample point (plant       Chlorine Dioxide Residual,
 effluent).                               Chlorite, Chlorate, Bromate
                                          \2\.
Three distribution system sampling       Chlorine Dioxide Residual,
 points (1 near first customer, 1 in      Chlorite, Chlorate, pH, and
 middle of distribution system, and 1     Temperature.
 representative of maximum residence
 time in the distribution system).
------------------------------------------------------------------------
\1\ Applicable only when wholesale water provider is using chlorine
  dioxide.
\2\ EPA shall provide all analytical results to the PWS. The PWS shall
  report all results in its monthly report.
\3\ PWSs are not required to analyze a bromate sample at this location.
  However, PWSs are still required to submit a sample to EPA for
  analysis.


  Table 5b.--Additional Quarterly Monitoring for Treatment Plants Using
                            Chlorine Dioxide
------------------------------------------------------------------------
             Sampling point                     Quarterly analyses
------------------------------------------------------------------------
Before First Chlorine Dioxide            Aldehydes \1\ and AOC/BDOC \2\.
 Application.
Before First Point of Downstream         Aldehydes \1\ and AOC/BDOC \2\.
 Chlorine/Chloramine Application After
 Chlorine Dioxide Addition.
Finished Water Sample Point (Plant       Aldehydes \1\ and AOC/BDOC \2\.
 Effluent).
------------------------------------------------------------------------
\1\EPA shall measure the following aldehydes: formaldehyde,
  acetaldehyde, propanal, butanal, pentanal, glyoxal, and methyl
  glyoxal. EPA may analyze for other aldehydes. EPA shall provide all
  analytical results to the PWS. The PWS shall report all results in its
  monthly report.
\2\ Analysis and submission of data for both assimilable organic carbon
  (AOC) and biodegradable organic carbon (BDOC) are optional. Analytical
  methods for AOC and BDOC are listed in ``DBP/ICR Analytical Methods
  Manual,'' EPA 814-B-96-002, April 1996.


[[Page 476]]

    (6) Additional requirements. A PWS shall also report the applicable 
information in tables 6a through 6e of this section. A PWS is required 
to provide the information in paragraphs (a)(6) (i) through (iii) of 
this section for each unit process listed in table 6c. The PWS may 
provide the information in paragraphs (a)(6) (iv) and (v) of this 
section for each unit process listed in table 6c. T10 and 
T50 tracer studies shall be conducted as specified in 
``Guidance Manual for Compliance with the Filtration and Disinfection 
Requirements for Public Water Systems using Surface Water Sources'', 
appendix C.
    (i) Unit process flow (MGD) at time of sampling.
    (ii) T10 (minutes). A PWS shall determine T10 
based on a one-time tracer study in the clearwell of all treatment 
plants required to conduct microbiological monitoring under the 
provisions of Sec. 141.141(d) of this subpart. The PWS may use results 
of a tracer study conducted to meet the requirements of subpart H 
(Filtration and Disinfection) of this part to meet this requirement. For 
subsequent T10 determinations, the PWS shall use a flow-
proportional interpolation of the clearwell tracer study. For unit 
processes other than a clearwell, a PWS shall either estimate 
T10 or use an interpolation of tracer study T10 
using multiple flows for each unit process in which a disinfectant 
residual exists.
    (iii) Chemicals in use at time of sampling. Report chemical name, 
chemical dose at time of sampling, and measurement formula. Measurement 
formulas (e.g., mg/l as Aluminum) shall be provided to determine the 
correct amount of the chemical compound being added.
    (iv) Short circuiting factor (optional). The short circuiting factor 
is an assumed value for the ratio of T10 to nominal contact 
time (volume divided by flow).
    (v) T50 (minutes) (optional). T50 should be 
reported only if based on a tracer study.

                                   Table 6a.--Public Water System Information
----------------------------------------------------------------------------------------------------------------
              Permanent data                                Design data                       Monthly data
----------------------------------------------------------------------------------------------------------------
Public Water System:
Utility Name                                ..........................................  Sampling Dates: From
Public Water Supply Identification Number                                                (date) To (date).
 (PWSID)                                                                                Retail population on day
Water Industry Data Base (WIDB) Number                                                   of sampling.
 [Optional]                                                                             Wholesale population on
Official Contact Person:                                                                 day of sampling.
  Name                                                                                  Monthly average Retail
  Mailing Address                                                                        flow (MGD).
  Phone Number [optional]                                                               Monthly average
  FAX Number [optional]                                                                  Wholesale flow (MGD).
ICR Contact Person:
  Name
  Mailing Address
  Phone Number [optional]
  FAX Number [optional]
  E-Mail Address [optional]
Treatment Plant: \1\
Plant name                                  Plant type (e.g., Conventional Filtration,  Hours of operation
ICR plant number assigned by EPA \2\         Direct Filtration, In-Line Filtration,      (hours per day)
PWSID number of treatment plant \3\          Two Stage Softening, Disinfection Only/    Sludge solids production
State approved (permitted) plant capacity    Groundwater, Other Groundwater treatment)   (lb/day)
 (MGD)                                                                                  Percent solids in sludge
Historical minimum water temperature (                                                   (%)
 deg.C)
Installed sludge handling capacity (lb/
 day)
Process Train:
Name                                        Process Train Type (e.g., Conventional
                                             Filtration, Direct Filtration, In-Line
                                             Filtration, Two Stage Softening,
                                             Disinfection Only/Groundwater, Other
                                             Groundwater treatment)
----------------------------------------------------------------------------------------------------------------
\1\ A PWS that operates more than one treatment plant shall report treatment plant information in this table for
  each treatment plant.
\2\ EPA shall assign ICR plant number after the PWS submits sampling plan.
\3\ PWSID of treatment plant if different from the PWSID reported in ``Public Water System''.


[[Page 477]]


                                      Table 6b.--Plant Influent Information
----------------------------------------------------------------------------------------------------------------
                       Permanent data                                            Monthly data
----------------------------------------------------------------------------------------------------------------
                                               Water Resource \1\
----------------------------------------------------------------------------------------------------------------
Name of resource:                                            If Reservoir/Lake: Mean Residence Time (days).
    Type of resource (One of the following):
        1  Flowing stream
        2  Reservoir/Lake
        3  Ground water classified as under the direct
         influence of surface water (GWUDI)
        4  Ground water
        5  Purchased finished water
        6  Non-Fresh (such as salt water)
----------------------------------------------------------------------------------------------------------------
                                            Intake-Surface Water \2\
----------------------------------------------------------------------------------------------------------------
Location of intake: \3\                                      Flow on day of sampling (MGD).
    Latitude (deg/min/sec)
    Longitude (deg/min/sec)
    Hydrologic unit code (8 digit), if known \4\
    Stream Reach Code (3 digit) (if known)
    River mile number (mile) (if known)
Is watershed control practiced? (yes/no)
----------------------------------------------------------------------------------------------------------------
                                            Intake-Ground Water \5\ 6
 
----------------------------------------------------------------------------------------------------------------
Location of intake:                                          Flow on day of sampling (MGD).
    Latitude (deg/min/sec)
    Longitude (deg/min/sec)
    Hydrological unit code (8 digit), if known \4\
Is wellhead protection practiced? (yes/no)
 
----------------------------------------------------------------------------------------------------------------
                                       Intake-Purchased Finished Water \7\
----------------------------------------------------------------------------------------------------------------
Name of supplying utility..................................  Flow on day of sampling (MGD).
PWSID of supplying utility
 
----------------------------------------------------------------------------------------------------------------
                                               Plant Influent \8\
----------------------------------------------------------------------------------------------------------------
                                                             Monthly average flow (MGD).
                                                             Flow at time of sampling (MGD).
----------------------------------------------------------------------------------------------------------------
\1\ Each treatment plant shall have at least one water resource. Each water resource shall have at least one
  intake. A treatment plant that uses more than one water resource shall report water resource information in
  this table for each water resource.
\2\ Intake-Surface Water describes the physical location of an intake structure located in a river, lake, or
  other surface water resource or, for ground water under the direct influence of surface water, the physical
  location of a well.
\3\ The location of the intake will allow cross referencing into other data bases containing information on
  possible contamination threats to the intake.
\4\ The hydrologic unit code will allow cross referencing into other data bases containing information on
  possible contamination threats to the intake.
\5\ An Intake-Ground Water describes the physical location of a well or well field (if multiple wells draw from
  a common aquifer.
\6\ A PWS is not required to report information for ground water that is not treated.
\7\ A PWS is required to report information for purchased finished water only if that water is further treated.
\8\ Multiple ``Intakes'' combine into one ``Plant Influent.'' Each treatment plant has only one treatment plant
  influent. The treatment plant influent shall mark the point in the treatment plant where the ``Plant
  Influent'' sample shall be collected as described in Tables 1, 2, 3 and 5 of this section.


                                       Table 6c.--Unit Process Information
----------------------------------------------------------------------------------------------------------------
                      Design data                                              Monthly data
----------------------------------------------------------------------------------------------------------------
                                           Presedimentation Basin \1\
 
----------------------------------------------------------------------------------------------------------------
Tube Settler Brand Name                                  Liquid volume (gallons).
Plate Settler Brand Name                                 Surface area (ft2).
Baffling type\2\                                         Projected Tube Settler Surface Area (ft\2\).
                                                         Projected Plate Settler Surface Area (ft2).
 
----------------------------------------------------------------------------------------------------------------

[[Page 478]]

 
                                               Ozone Contact Basin
 
----------------------------------------------------------------------------------------------------------------
Information for the complete ozone contact basin:        Information for the complete ozone contact basin:
    Type of Ozone Contactor (One of the following)         Ozone CT (mg min/l).10
      1  Bubble Diffusion                                  Ozone Giardia Inactivation (logs).
      2  Turbine                                           Ozone Virus Inactivation (logs).
    Number of Chambers                                     Ozone concentration in feed gas (% by weight).
Information for each ozone contact chamber:                Total Ozone Gas Flow Rate to Contactor (SCFM).3
    Chamber sequence number                                Type of feed gas used to generate ozone (one of the
    Liquid volume (ft3)                                   following).
    Surface area (ft2)                                         1  Air.
    Water/Ozone flow regime (one of the following)             2  Oxygen.
      1  Counter-current                                   Total Ozone Applied Dose (mg/l).
      2  Co-current                                      Information for each ozone contact chamber:
                                                           Percent ozone gas flow split to this chamber (%).
                                                           Hydrogen peroxide dose (mg/l).
 
----------------------------------------------------------------------------------------------------------------
                                            Washwater Return Point 8
 
----------------------------------------------------------------------------------------------------------------
Indicate which washwater treatment processes are being   Flow of returned washwater at time of sampling (MGD).
 used on day of sampling                                 24 hr average flow prior to sampling (MGD).
Is there treatment (yes/no):
    If yes:
        Plain sedimentation (yes/no)
        Coagulation/sedimentation (yes/no)
        Filtration (yes/no)
        Disinfection (yes/no)
        Other Treatment (Text)
 
----------------------------------------------------------------------------------------------------------------
                                                    Rapid Mix
 
----------------------------------------------------------------------------------------------------------------
Type of mixer (one of the following):                    Mean velocity gradient ``G'' (sec-1).4
                                                         Liquid volume (gallons).
    1  Mechanical
    2  Hydraulic
    3  Static
    4  Other
Baffling type 2
 
----------------------------------------------------------------------------------------------------------------
                                               Flocculation Basin
 
----------------------------------------------------------------------------------------------------------------
Type of mixer (one of the following):                    Mean velocity gradient ``G'' (sec-1) in each stage.4
                                                         Liquid volume of each stage (gallons).
    1  Mechanical
    2  Hydraulic
Number of stages
Baffling type 2
 
----------------------------------------------------------------------------------------------------------------
                                               Sedimentation Basin
 
----------------------------------------------------------------------------------------------------------------
Tube settler brand name                                  Liquid volume (gallons).
Plate settler brand name                                 Surface area (ft2).
Baffling type 2                                          Projected tube settler surface area (ft2).
                                                         Projected plate settler surface area (ft2).
 
----------------------------------------------------------------------------------------------------------------
                                            Solids Contact Clarifier
 
----------------------------------------------------------------------------------------------------------------
Brand name:                                              Liquid volume (gallons).
                                                         Surface area of settling zone (ft2).
                                                         Projected tube settler surface area (ft2).
                                                         Projected plate settler surface area (ft2).
    Type (check all that apply):
        Rectangular basin
        Upflow
        Reactor-clarifier
        Sludge blanket
Tube settler brand name
Plate settler brand name

[[Page 479]]

 
Baffling type 2
 
----------------------------------------------------------------------------------------------------------------
                                              Adsorption Clarifier
 
----------------------------------------------------------------------------------------------------------------
Brand Name                                               Liquid volume (gallons).
Baffling type 2                                          Surface area (ft2).
 
----------------------------------------------------------------------------------------------------------------
                                             Dissolved Air Flotation
 
----------------------------------------------------------------------------------------------------------------
Baffling type 2                                          Liquid volume (gallons).
                                                         Surface area (ft2).
                                                         Percent recycle rate (%).
                                                         Recycle stream pressure (psi).
 
----------------------------------------------------------------------------------------------------------------
                                               Recarbonation Basin
 
----------------------------------------------------------------------------------------------------------------
Baffling type 2                                          Liquid volume (gallons).
                                                         Surface area (ft2).
 
----------------------------------------------------------------------------------------------------------------
                                                   Filtration
 
----------------------------------------------------------------------------------------------------------------
Media Type (one of the following):                       Liquid volume (gallons).
                                                         Surface area (ft2).
                                                         Average filter run time (hr).
    1  Dual media (Anthracite/Sand)
    2  GAC over sand
    3  Tri media (Anthracite/Sand/Garnet)
    4  Sand
    5  Deep bed monomedia anthracite
    6  Deep bed monomedia GAC
    7  Greensand
    8  Other
Design depth of GAC (inch)
Type and manufacturer of activated carbon
Design media depth (inch)
Minimum water depth to top of media (ft)
Depth from top of media to top of backwash trough (ft)
 
----------------------------------------------------------------------------------------------------------------
                                              Slow Sand Filtration
 
----------------------------------------------------------------------------------------------------------------
Media type                                               Surface area (ft2).
Media depth                                              Average filter run length.
Media size                                               Cleaning method.
 
----------------------------------------------------------------------------------------------------------------
                                            Diatomaceous Earth Filter
 
----------------------------------------------------------------------------------------------------------------
                                                         Effective DE filter surface (ft2).
                                                         Precoat (lb/ft2).
                                                         Bodyfeed (mg/l).
                                                         Run length (hours).
 
----------------------------------------------------------------------------------------------------------------
                                 Granular Activated Carbon--Post-Filter Adsorber
 
----------------------------------------------------------------------------------------------------------------
Manufacturer of activated carbon                         Liquid volume (gallons).
Type of activated carbon                                 Surface area (ft2).
                                                         Carbon volume (ft3).
                                                         Empty bed contact time (minutes).
                                                         Operating reactivation frequency (days).
 
----------------------------------------------------------------------------------------------------------------

[[Page 480]]

 
                                                    Membranes
 
----------------------------------------------------------------------------------------------------------------
Model name:                                              Surface area (ft\2\).
  Type (one of the following):                           Percent recovery (%).
      1 Reverse osmosis                                  Operating pressure (psi).
      2 Nanofiltration                                   Operating flux (gpd/ft2).
      3 Ultrafiltration                                    Cleaning method (one of the following)
      4 Microfiltration                                    Hydraulic.
      5 Electrodialysis                                    Chemical.
Number of stages                                           Cleaning frequency (days).
Molecular weight cutoff (daltons)
Design flux (gpd/ft2)
Design pressure (psi)
 
----------------------------------------------------------------------------------------------------------------
                                                  Air Stripping
 
----------------------------------------------------------------------------------------------------------------
Packing height (ft)                                      Horizontal cross-section area (ft2).
Design air to water ratio (volume/volume)                Air flow (SCFM).3
Type of packing (Name)
Nominal size of packing (inch)
 
----------------------------------------------------------------------------------------------------------------
                                                  Ion Exchange
 
----------------------------------------------------------------------------------------------------------------
Resin (Name)                                             Liquid volume (gallons).
Resin manufacturer                                       Surface area (ft2).
Design exchange capacity (equ/ft3) 3
Bed depth (ft)
 
----------------------------------------------------------------------------------------------------------------
                                         Disinfection Contact Basin 5 6
 
----------------------------------------------------------------------------------------------------------------
Baffling type 2                                          Liquid volume (gallons).
                                                         Surface area (ft2).
 
----------------------------------------------------------------------------------------------------------------
                                                   Clearwell 7
 
----------------------------------------------------------------------------------------------------------------
Baffling type 2                                          Liquid volume (gallons).
Minimum liquid volume (gallons)                          Surface area (ft2).
Covered or Open
 
----------------------------------------------------------------------------------------------------------------
                                           Additional Water Sources 9
 
----------------------------------------------------------------------------------------------------------------
Type of water source:                                    Flow of additional source (MGD).6
    Purchased Finished water
    Untreated ground water
    Treated ground water
    Untreated surface water
    Treated surface water
    Other
 
----------------------------------------------------------------------------------------------------------------
                                                 Other Treatment
 
----------------------------------------------------------------------------------------------------------------
Purpose                                                  Surface area (ft2) [optional].
                                                         Liquid Volume (gallons) [optional].
----------------------------------------------------------------------------------------------------------------
1 A reservoir to which oxidants, disinfectants, or coagulants are added is considered a presedimentation basin.
2 Baffling type classified as one of the following: 1 (Unbaffled (mixed tank)), 2 (Poor (inlet/outlet only)), 3
  (Average (Inlet/Outlet and intermediate)), 4 (Superior (Serpentine)), or 5 (Perfect (Plug flow)). Information
  on classifying baffling types can be found in ``Guidance Manual for Compliance with the Filtration and
  Disinfection Requirements for Public Water Systems using Surface Water Sources'', Appendix C.
3 ``SCFM'' is standard cubic feet per minute. ``Equ/ft\3\'' is equivalents per cubic foot.
4 The mean velocity gradient is typically computed as G=square root of (P/uV) where P=power expended,
  u=viscosity, and V=liquid volume.
5 The disinfection contact basin shall have a stable liquid level.
6 Disinfection Contact Basin can be used to represent a pipe with a long contact time.
7 A clear well may have a variable liquid level.
8 The ``Washwater Return'' shall mark the point in the process train where washwater joins the main flow.
9 Additional water sources includes water that is added to the process train after the influent.
10 Ozone CT calculated using the procedure contained in ``Guidance Manual for Compliance with the Filtration and
  Disinfection Requirements for Public Water Systems using Surface Water Sources'', Appendix O, 1991.


[[Page 481]]


             Table 6d.--Additional Process Train Information
------------------------------------------------------------------------
            Design data                          Monthly data
------------------------------------------------------------------------
                          Disinfectant Addition
 
------------------------------------------------------------------------
                                     Disinfectants in use at time of
                                      sampling.
                                     Dose (mg/l).
                                     Chemical formula (e.g., mg/l as
                                      chlorine).
 
------------------------------------------------------------------------
            Finished Water Sample Point (Plant Effluent) 1, 2
 
------------------------------------------------------------------------
                                     Monthly average flow (MGD).
                                     Flow at time of sampling (MGD).
------------------------------------------------------------------------
\1\ This shall mark the end of a treatment plant.
\2\ Unless the finished water of this treatment plant is blended with
  finished water from another treatment plant, this point is also the
  entry point to the distribution system.


           Table 6e.--Finished Water Distribution Information
------------------------------------------------------------------------
            Design data                          Monthly data
------------------------------------------------------------------------
                 Entry Point to Distribution System \1\
 
------------------------------------------------------------------------
                                     Monthly average flow (MGD).
                                     Flow at time of sampling (MGD).
 
------------------------------------------------------------------------
                        Wholesale Information \2\
 
------------------------------------------------------------------------
Name of purchaser..................  Flow at time of sampling (MGD).
PWSID of purchaser
 
------------------------------------------------------------------------
                           Distribution System
 
------------------------------------------------------------------------
Typical maximum residence time       Maximum residence time (days).
 (days)
Average residence time (days)        Average residence time (days).
Design volume of distribution        Number of disinfection booster
 system storage (million gallon)      stations in operation at time of
                                      sampling:
Total surface area of open             Chlorine.
 reservoirs in distribution system     Chloramine.
 storage (ft\2\)                       Chlorine dioxide.
                                     Range of distribution system
                                      disinfectant dosages.
                                       Chlorine: High (mg/l) Low (mg/l).
                                       Chloramine: High (mg/l) Low (mg/
                                      l).
                                       Chlorine dioxide: High (mg/l) Low
                                      (mg/l).
------------------------------------------------------------------------
\1\ Multiple treatment plants can feed into one entry point to the
  distribution system. If there is only one treatment plant then
  ``Finished Water Sample Point (Plant Effluent)'' and ``Entry Point to
  Distribution System'' are the same.
\2\ The supplying public water system shall report ``Wholesale
  Information'' for each public water system which purchases finished
  water.

    (b) Analytical methods. (1) A PWS shall use the methods identified 
in table 7 of this section for conducting analyses required by this 
subpart.

                               Table 7.--Analytical Methods Approved for Subpart M
----------------------------------------------------------------------------------------------------------------
                                                                   Methodology \1\
              Analyte              -----------------------------------------------------------------------------
                                     40 CFR reference \2\        EPA method             Standard method \3\
----------------------------------------------------------------------------------------------------------------
pH, alkalinity, calcium hardness,   Sec.  141.23(k)(1)
 temperature.
Turbidity.........................  Sec.  141.74(a)(1)
Disinfectant residuals: free        Sec.  141.74(a)(2)     .....................  4500-Cl B \9\
 chlorine, total chlorine,
 chlorine dioxide, ozone.
Trihalomethanes: chloroform, bro..  Sec.  141.24(e)        551.1 \4\
modichloromethane, dibro..........
mochloromethane, bromoform........
Haloacetic acids: mono-, di-, and   .....................  552.1, \5\ 552.2 \4\   6251 B
 trichloroacetic acids; mono- and
 dibromoacetic acid;
 bromochloroacetic acid.
Chloral hydrate...................  .....................  551.1 \4\

[[Page 482]]

 
Haloacetonitriles: di- and          .....................  551.1 \4\
 trichloroacetonitrile;
 bromochloroacetonitrile;
 dibromoacetonitrile.
Haloketones: 1,1-                   .....................  551.1 \4\
 Dichloropropanone; 1,1,1-
 trichloropropanone.
Chloropicrin......................  .....................  551.1 \4\
Chlorite..........................  .....................  300.0 \6\
Chlorate..........................  .....................  300.0 \6\
Bromide...........................  .....................  300.0 \6\
Bromate...........................  .....................  300.0 \6\
Total Organic Halide (TOX)........  .....................  .....................  5320 B
Total Organic Carbon..............  .....................  .....................  5310 B, 5310 C, 5310 D
UV absorbance at 254 nm...........  .....................  .....................  5910
Simulated Distribution System Test  .....................  .....................  5710 C
 (SDS).
Total Hardness....................  .....................  .....................  2340 B,\7\ 2340 C
Ammonia...........................  Sec.  136.3, Table 1b  350.1 \6\              4500-NH3 D, 4500-NH3 G
                                     \8\
Chlorine Demand Test..............  .....................  .....................  2350 B
----------------------------------------------------------------------------------------------------------------
\1\ Analyses shall be conducted by using mandatory analytical and quality control procedures contained in ``DBP/
  ICR Analytical Methods Manual'', EPA 814-B-96-002.
\2\ Currently approved methodology for drinking water compliance monitoring is listed in Title 40 of the Code of
  Federal Regulations in the sections referenced in this column. The 18th and 19th editions of Standard Methods
  for the Examination of Water and Wastewater, American Public Health Association, 1015 Fifteenth Street NW,
  Washington, D.C. 20005, are equivalent for the methods cited in these sections. Therefore, either edition may
  be used.
\3\ Except where noted, all methods refer to the 19th edition of Standard Methods for the Examination of Water
  and Wastewater, American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005.
\4\ Analytical method reprinted in ``Reprints of EPA Methods for Chemical Analyses Under the Information
  Collection Rule'', EPA 814-B-96-006. Originally published in ``Methods for the Determination of Organic
  Compounds in Drinking Water--Supplement III,'' EPA/600/R-95/131, August 1995, PB95-261616.
\5\ Analytical method reprinted in ``Reprints of EPA Methods for Chemical Analyses Under the Information
  Collection Rule'', EPA 814-B-96-006. Originally published in ``Methods for the Determination of Organic
  Compounds in Drinking Water--Supplement II,'' EPA/600/R-92/129, August 1992, PB92-207703.
\6\ Analytical method reprinted in ``Reprints of EPA Methods for Chemical Analyses Under the Information
  Collection Rule'', EPA 814-B-96-006. Originally published in ``Methods for the Determination of Inorganic
  Substances in Environmental Samples,'' EPA/600/R-93/100, August 1993, PB94-121811.
\7\ The following methods, cited at Sec.  141.23(k)(1) of this part, can be used to determine calcium and
  magnesium concentrations for use in conjunction with Standard Method 2340 B: EPA Method 200.7, Standard Method
  3111 B, Standard Method 3120 B, or ASTM Method D511-93 B.
\8\ PWSs may use only the automated electrode method from Sec.  136.3, Table 1b.
\9\ Standard Method 4500-Cl B is approved only for determining free chlorine residual concentrations in
  hypochlorite stock solutions. This method may not be used for any other disinfectant residual analyses.

    (2) Analyses under this section shall be conducted by laboratories 
that have received approval from EPA to perform sample analysis for 
compliance with this rule. Laboratories that wish to become approved 
shall contact EPA in writing at USEPA, Technical Support Division, ICR 
Laboratory Coordinator, 26 W. Martin Luther King Drive, Cincinnati, OH 
45268 not later than November 14, 1996. Requirements for approval are 
included in ``DBP/ICR Analytical Methods Manual'', EPA 814-B-96-002.
    (c) Reporting. (1) A PWS shall report required data and information 
collected under the provisions of paragraph (a) of this section to EPA, 
using an EPA-specified computer readable format. A PWS shall submit a 
monthly report that indicates the analytical results of all samples 
collected, including quarterly samples taken in that same month, and all 
process train data. These reports shall be submitted on a diskette no 
later than the fourth month following sampling. In addition to the 
information in tables 1 through 6 in paragraph (a) of this section, 
reports shall include PWSID, ICR plant identification, sample date, 
analysis date, laboratory identification numbers, analytical methods 
used, sample identification numbers, quality assurance code, internal 
standards, surrogate standards, and preserved sample pH, if appropriate.
    (2) Additional Requirements. A PWS shall submit a DBP and related 
monitoring sampling plan for EPA approval, using software provided by 
EPA, for each treatment plant specified in Sec. 141.141(b)(2) of this 
subpart that indicates sampling point locations and monitoring to be 
conducted at each point, and process treatment train information. This 
sampling plan shall be submitted to EPA at the same time

[[Page 483]]

and on the same diskette as the microbiological sampling plan required 
by Sec. 141.143(c)(3) and no later than eight weeks after the PWS 
receives the Notice of ICR Final Applicability Determination from EPA, 
using the procedure specified in ``ICR Sampling Manual'', EPA 814-B-96-
001, April 1996.
    (3) All reports required by this section shall be submitted to USEPA 
(ICR4600), ICR Data Center, Room 1111 East Tower, 401 M Street SW., 
Washington, DC 20460.
    (4) The PWS shall keep all data for at least three years following 
data submission to EPA.
    (d) Incorporation by reference. The documents and methods listed in 
paragraphs (d) (1) and (2) of this section are incorporated by reference 
for purposes specified 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 inspected at USEPA, 
Drinking Water Docket (4101), 401 M Street SW., Washington, DC 20460, or 
at Office of the Federal Register, 800 North Capitol Street, NW., Suite 
700, Washington, DC.
    (1) ``Standard Methods for the Examination of Water and 
Wastewater,'' 19th edition, 1995. Available from the American Public 
Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005.
    (2) ``Guidance Manual for Compliance with the Filtration and 
Disinfection Requirements for Public Water Systems using Surface Water 
Sources'', Appendices C and O, 1991. Available from American Water Works 
Association, 6666 West Quincy Avenue, Denver, CO 80235.



Sec. 141.143  Microbial monitoring.

    (a) Monitoring requirements. (1) Parameters. A PWS shall sample for 
the following parameters for the period specified in Sec. 141.141(d) of 
this subpart and at the location specified and using the analytical 
methods specified in paragraphs (a)(2) and (b), respectively, of this 
section. For each sample, a PWS shall determine the densities of total 
coliforms, fecal coliforms or Escherichia coli, Giardia, 
Cryptosporidium, and total culturable viruses for each treatment plant 
required to monitor under the provisions of Sec. 141.141(b) of this 
subpart.
    (2) Monitoring locations. (i) A PWS shall collect one sample of the 
treatment plant influent at the frequency specified in Sec. 141.141(d) 
of this subpart.
    (A) A sample of treatment plant influent shall be taken at a 
location at the upstream end of a treatment plant where waters from all 
intakes are blended prior to any treatment or chemical addition.
    (B) For treatment plants that have multiple intakes and add 
chemicals at the intake, the PWS shall take an intake sample of the 
water resource with the poorest microbiological quality (or, if that 
cannot be determined, the water resource with the highest flow) 
collected before chemical addition and before pretreatment. If the 
intakes are expected to have the same source water quality, one 
representative intake sample may be taken. If a disinfectant is added at 
or before the intake (e.g., for zebra mussel control), the sample shall 
be taken in the vicinity of the intake in such manner that the sample is 
not contaminated by the disinfectant.
    (ii) A PWS that, during any of the first twelve months of monitoring 
at the treatment plant influent, detects 10 or more Giardia cysts, or 10 
or more Cryptosporidium oocysts, or one or more total culturable 
viruses, in one liter of water; or calculates a numerical value of the 
Giardia or Cryptosporidium concentration equal to or greater than 1000 
per 100 liters or virus concentration equal to or greater than 100 per 
100 liters; or detects no pathogens in the sample and calculates a 
numerical value of the detection limit for Giardia or Cryptosporidium 
concentration equal to or greater than 1000 per 100 liters or virus 
concentration equal to or greater than 100 per 100 liters; shall also 
collect one sample of finished water per month at each such treatment 
plant, beginning in the first calendar month after the PWS learns of 
such a result. The sample of finished water shall be collected at a 
point after which all treatment processes for a particular treatment 
plant are complete (including the clearwell and final point of 
disinfection) and before the distribution system begins. For each sample 
of finished

[[Page 484]]

water, PWSs shall determine the density of total coliforms, fecal 
coliforms or E. coli, Giardia, Cryptosporidium, and total culturable 
viruses. A PWS shall continue finished water monitoring monthly until 18 
months of treatment plant influent monitoring has been completed.
    (iii) In lieu of conducting finished water monitoring of Giardia and 
Cryptosporidium specified in paragraph (a)(2)(ii) of this section, a PWS 
may notify EPA in its response to the notice of applicability required 
by paragraph (c)(3)(i) of this section that the PWS will comply with the 
alternative monitoring requirements in paragraphs (a)(2)(iii) (A) and 
(B) of this section. The PWS shall still conduct finished water 
monitoring for all other microorganisms, except for Giardia and 
Cryptosporidium monitoring in the finished water.
    (A) The PWS measures the particle counts in the treatment plant 
influent, at points immediately prior to filtration and after filtration 
(but before the addition of post-filtration chemicals). Particle 
counting shall be conducted on the same treatment train as is sampled 
for monitoring conducted under the provisions of Sec. 141.142(a) of this 
subpart. Such samples shall be collected monthly during the entire 18-
month monitoring period, using the procedures contained in the ``ICR 
Sampling Manual'', EPA 814-B-96-001, April 1996. The PWS may use either 
grab or continuous particle counting. Particle counting shall be 
conducted during the same time as protozoa monitoring required by 
paragraph (a)(2)(iii)(B) of this section.
    (1) If grab sampling is conducted, the PWS shall collect 12 samples 
per location at the treatment plant influent, filter influent, and 
filter effluent, over either a 24-hour period or the duration of the 
filter run, whichever is shorter.
    (2) If continuous particle counting is conducted, the PWS shall 
collect 12 instrument readings per location, evenly spaced in time, at 
the treatment plant influent, filter influent, and filter effluent, over 
either a 24-hour period or the duration of the filter run, whichever is 
shorter.
    (3) For each sample, the PWS shall measure particle counts per 
milliliter in the size ranges of 3m-5m, 5m-
7m, 7m-10m, 10m-15m, and 
>15m, and shall report to EPA the mean value in each size range 
of the 12 values collected over the sampling period.
    (B) The PWS collects and analyzes at least four consecutive months 
of Giardia and Cryptosporidium samples at the same locations specified 
in paragraph (a)(2)(iii)(A) of this section, within the first 12 months 
of the 18 months of sampling. The PWS shall collect Giardia and 
Cryptosporidium samples during the same time period as it is conducting 
particle counting. The minimum sample volume for Giardia and 
Cryptosporidium analyses shall be 100 liters for treatment plant 
influent and 1,000 liters for water that has undergone any treatment. 
The PWS may use results of monitoring for Giardia and Cryptosporidium in 
the treatment plant influent specified in paragraph (a)(2) of this 
section to meet the requirements of this paragraph as long as such 
monitoring meets the requirements of both this paragraph and paragraph 
(a)(2) of this section.
    (iv) If a PWS has monitored total coliforms, fecal coliforms, or E. 
coli in the treatment plant influent for at least five days/week for any 
period of six consecutive months beginning after January 1, 1994 and 90% 
of all samples taken in that six-month period contained no greater than 
100 total coliforms/100 ml, or 20 fecal coliforms/100 ml, or 20 E. coli/
100 ml, the PWS may request to not conduct virus monitoring for that 
treatment plant, for the duration of the requirement. Even if approved, 
the PWS may subsequently be required to monitor under the criteria in 
paragraph (a)(2)(iv)(A) of this section. This request shall be submitted 
as part of the response to the notice of applicability required by 
paragraph (c)(3)(i) of this section.
    (A) If the PWS is subsequently required to monitor the finished 
water under the provisions of paragraph (a)(2)(ii) of this section, the 
PWS shall monitor, along with the other specified organisms, total 
culturable viruses, as specified in paragraph (a)(2)(i) of this section 
for treatment plant influent and as specified in paragraph (a)(2)(ii) of 
this section for finished water, until

[[Page 485]]

18 months of microbial monitoring is completed.
    (B) A PWS may use coliform data collected under Sec. 141.71(a)(1) of 
this part for this purpose but, if this is done, the PWS shall submit 
two separate monitoring reports. One report, to meet the requirements of 
Sec. 141.71(a)(1) of this part, shall continue to be submitted as 
required by subpart H of this part. The other report shall be submitted 
to meet the requirements of paragraph (c)(3) of this section.
    (C) If a PWS does not provide EPA with six months of suitable 
coliform results as part of its response to the notice of applicability, 
the PWS shall begin virus monitoring. If a PWS begins virus monitoring 
and subsequently provides EPA with six months of coliform results that 
are at or below the indicated density limit, and EPA approves the 
request to not conduct virus monitoring, the PWS may avoid subsequent 
treatment plant virus monitoring.
    (b) Analytical Methods. (1) A PWS shall use the methods listed in 
paragraphs (b)(1) (i) through (v) of this section for monitoring under 
this subpart.
    (i) Fecal coliforms--specified at Sec. 141.74(a)(1) of this part, 
except that whenever paired source water samples and finished water 
samples are to be collected, only the fecal coliform procedure (Standard 
Method 9221E), as specified in Sec. 141.74(a)(1) of this part, using EC 
Medium, can be used. The time between sample collection and initiation 
of sample analysis shall not exceed eight hours. Samples shall be 
chilled, but not frozen, and shipped at a temperature of less than 10 
deg.C. Samples not processed immediately at the laboratory shall be 
refrigerated. The laboratory must invalidate samples that arrive frozen 
or at a temperature greater than 10  deg.C.
    (ii) Total coliforms--specified at Sec. 141.74(a)(2) of this part. 
The time between sample collection and initiation of sample analysis 
shall not exceed eight hours. Samples shall be chilled, but not frozen, 
and shipped at a temperature of less than 10  deg.C. Samples not 
processed immediately at the laboratory shall be refrigerated. The 
laboratory must invalidate samples that arrive frozen or at a 
temperature greater than 10  deg.C.
    (iii) E. coli-- as specified by Sec. 141.21(f)(6) (i) through (iii) 
of this part, except that the density shall be reported. PWSs using the 
EC+MUG and ONPG-MUG tests shall use either a 5-tube or 10-tube 10-ml 
configuration, with serial dilutions of the original sample as needed, 
and report the Most Probable Number. PWSs may also use a commercial 
multi-test system for E. coli enumeration, as long as they use M-Endo 
medium for the initial isolation of the organisms, pick every colony on 
the plate with the appearance of a total coliform, and streak it for 
purification before subjecting the colony to a multi-test system. The 
time between sample collection and initiation of sample analysis, 
regardless of method used, shall not exceed eight hours. Samples shall 
be chilled, but not frozen, and shipped at a temperature of less than 10 
 deg.C. Samples not processed immediately at the laboratory shall be 
refrigerated. The laboratory must invalidate samples that arrive frozen 
or at a temperature greater than 10  deg.C.
    (iv) Giardia and Cryptosporidium-- ICR Protozoan Method, as 
described in ``ICR Microbial Laboratory Manual'', EPA 600/R-95/178, 
April 1996.
    (v) Total culturable viruses--Virus Monitoring Protocol, as 
described in ``ICR Microbial Laboratory Manual'', EPA 600/R-95/178, 
April 1996.
    (2) Laboratories. A PWS shall use EPA-approved laboratories to 
analyze for Giardia, Cryptosporidium, and total culturable viruses. A 
PWS shall use laboratories certified for microbiology analyses by either 
EPA or a State under the EPA or State drinking water program for the 
analysis of total coliforms, fecal coliforms, and E. coli. Laboratories 
that wish to become approved shall contact EPA in writing at USEPA, 
Technical Support Division, ICR Laboratory Coordinator, 26 W. Martin 
Luther King Drive, Cincinnati, OH 45268 not later than August 14, 1996. 
Laboratory approval criteria for Giardia, Cryptosporidium, and total 
culturable viruses are found in the ``ICR Microbial Laboratory Manual'', 
EPA 600/R-95/178, April 1996.
    (3) A PWS shall send EPA a virus archive sample prepared as 
described in

[[Page 486]]

Chapter VIII of ``ICR Microbial Laboratory Manual'', EPA 600/R-95/178, 
April 1996, for each water sample identified in paragraph (b)(3) (i) or 
(ii) of this section.
    (i) Samples of treatment plant influent and finished water, for 
every month after the PWS learns that viruses were detected in any 
previous sample of finished water.
    (ii) Samples of treatment plant influent and finished water, 
regardless of whether viruses are detected in the finished water, for 
every month after the PWS learns that a density of at least 10 viruses/L 
was detected in any previous treatment plant influent water sample.
    (iii) A PWS may arrange to have virus samples shipped directly to 
EPA by its virus laboratory for archiving.
    (iv) Samples shall be sent on dry ice to ICR Virus Archiving 
Coordinator following the procedures specified in ``ICR Microbial 
Laboratory Manual'', EPA 600/R-95/178, April 1996.
    (c) Reporting. (1) A PWS shall report data and information required 
under paragraphs (a) and (b) of this section using an EPA-specified 
computer readable format. A PWS shall submit a monthly report on a 
diskette, no later than the fourth month following sampling, that 
indicates the analytical results of all samples collected. Reports shall 
include PWSID, ICR plant identification, sample date, analysis date, 
laboratory identification numbers, analytical methods used, sample 
identification numbers, analytical batch numbers, quality assurance 
code, and processing batch numbers, if appropriate.
    (2)(i) For a PWS using the alternative to Giardia and 
Cryptosporidium monitoring in paragraph (a)(2)(iii) of this section, the 
PWS shall report to EPA the mean value in each size range of the 12 
particle counting values collected over the sampling period. In 
addition, during the four consecutive months when the PWS collects 
Giardia and Cryptosporidium samples specified in paragraph 
(a)(2)(iii)(B) of this section, the PWS shall report to EPA, for each 
measured site, the densities of Giardia and Cryptosporidium at each 
measured site. This information shall be submitted at the same time as 
the report required by paragraph (c)(1) of this section.
    (ii) A PWS that is not required to monitor for total culturable 
viruses under the provisions of paragraph (a)(2)(iv) of this section 
shall report to EPA the dates and results of all total coliform, fecal 
coliform, or E. coli monitoring used by the PWS to determine that 
additional virus monitoring is unnecessary. The report shall indicate 
all data collected during the six-month time period, and how the data 
were used to calculate compliance with this requirement.
    (3) Additional Requirements. A PWS shall submit a microbiological 
sampling plan for EPA approval, using software provided by EPA, for each 
treatment plant specified in Sec. 141.141(b) of this subpart that 
indicates sampling point locations and monitoring to be conducted at 
each point. This sampling plan shall be submitted to EPA at the same 
time and on the same diskette as the DBP and related monitoring sampling 
plan required by Sec. 141.142(c)(2) and no later than eight weeks after 
the PWS receives the Notice of ICR Final Applicability Determination 
from EPA, using the procedure specified in ``ICR Sampling Manual'', EPA 
814-B-96-001, April 1996.
    (4) All reports required by this section shall be submitted to USEPA 
(ICR4600), ICR Data Center, Room 1111 East Tower, 401 M Street SW., 
Washington, DC 20460.
    (5) The PWS shall keep all data for at least three years following 
data submission to EPA.



Sec. 141.144  Disinfection byproduct precursor removal studies.

    (a) TOC, UFCTOX, THM4, and HAA5 applicability monitoring. A PWS 
required to comply with this section shall conduct TOC, UFCTOX, THM4, 
and HAA5 monitoring specified in Sec. 141.141(e)(2) of this subpart. A 
PWS may use monitoring results from samples required by Sec. 141.142(a) 
of this subpart to meet this requirement to the extent that all 
requirements in each section are met.
    (b) Treatment study requirements. A PWS identified in 
Sec. 141.141(b) of this subpart shall conduct disinfection byproduct 
precursor removal studies (treatment studies). The treatment

[[Page 487]]

study shall use bench-and/or pilot-scale systems for at least one of the 
two appropriate candidate technologies (GAC or membrane processes) for 
the reduction of organic DBP precursors. The treatment studies shall be 
designed to yield representative performance data and allow the 
development of national treatment cost estimates for different levels of 
organic disinfection byproduct control. The treatment objective of the 
studies is the achievement of levels of byproducts less than 40 
 g/L TTHM and 30  g/L HAA5, as an annual average. The 
treatment study shall be conducted with the effluent from treatment 
processes already in place that remove disinfection byproduct precursors 
and TOC, to simulate the most likely treatment scenario. PWSs are 
permitted to optimize these processes or pilot additional processes 
appropriate for pretreatment for treatment studies. In order to minimize 
the formation of DBPs, the test water for both the bench- and pilot-
scale tests shall be obtained from a location before the first point at 
which oxidants or disinfectants that form halogenated disinfection 
byproducts are added. If the use of these oxidants or disinfectants 
precedes any full-scale treatment process that removes disinfection 
byproduct precursors, then bench- and pilot-scale treatment processes 
that represent these full-scale treatment processes are required prior 
to the GAC or membrane process. A PWS should exercise sound judgement in 
its selection of treatment process to study and the point at which to 
obtain water for study. Depending upon the type of treatment study, the 
study shall be conducted in accordance with the following criteria.
    (1) Bench-scale tests are continuous flow tests using rapid small 
scale column test (RSSCT) for GAC and small scale membrane test 
apparatus as specified in ``ICR Manual for Bench- and Pilot-scale 
Treatment Studies'' (EPA 814-B-96-003, April 1996).
    (i) GAC bench-scale testing shall include information on the 
experimental conditions and results necessary to adequately determine 
the scaled-up breakthrough curves under the conditions of each RSSCT. At 
least two empty bed contact times (EBCTs) shall be tested using the 
RSSCT. These RSSCT EBCTs shall be designed to represent a full-scale 
EBCT of 10 min and a full-scale EBCT of 20 min. Additional EBCTs may be 
tested. The RSSCT testing is described in the ``ICR Bench- and Pilot-
scale Treatment Study Manual'' (EPA 814-B-96-003, April 1996). The RSSCT 
tests at each EBCT shall be run quarterly to ascertain the impact of 
seasonal variation. Thus a total of four RSSCTs at each EBCT should be 
run. When seasonal variation is not significant, as is the case in most 
ground waters, the quarterly tests should be run to investigate other 
variables, as described in the ``ICR Bench- and Pilot-scale Treatment 
Study Manual'' (EPA 814-B-96-003, April 1996). The RSSCT shall be run 
until the effluent TOC concentration is at least 70% of the average 
influent TOC concentration or the effluent TOC reaches a plateau at 
greater than 50% of the influent TOC (i.e., the effluent TOC does not 
increase over a two-month full-scale-equivalent time period by more than 
10% of the average influent TOC concentration) or a RSSCT operation time 
that represents the equivalent of one year of full-scale operation, 
whichever is shorter. The average influent TOC is defined as the running 
average of the influent TOC at the time of effluent sampling. If, after 
completion of the first quarter RSSCTs, the PWS finds that the effluent 
TOC reaches 70% of the average influent TOC within 20 full-scale 
equivalent days on the EBCT=10 min test and within 30 full-scale 
equivalent days on the EBCT=20 min test, the last three quarterly tests 
shall be conducted using membrane bench-scale testing with only one 
membrane, as described in paragraph (b)(1)(ii) of this section.
    (ii) Membrane bench-scale testing shall include information on the 
experimental conditions and results necessary to determine the water 
quality produced by the membrane treatment and a preliminary estimate of 
productivity. The testing procedures and monitoring and reporting 
requirements are described in the ``ICR Bench- and Pilot-scale Treatment 
Study Manual'' (EPA 814-B-96-003, April 1996). A minimum of two 
different membrane types with nominal molecular weight cutoffs

[[Page 488]]

of less than 1000 shall be investigated. Membrane tests shall be 
conducted quarterly over one year to determine the seasonal variation. 
Thus, a total of four bench-scale tests with each membrane shall be run. 
If seasonal variation is not significant, as is the case of most ground 
waters, the quarterly tests should be run to evaluate the impact of 
other variables, such as pretreatment, or additional membranes could be 
tested. Alternatively, a PWS may choose to conduct a long-term, single 
element study using a single membrane type in lieu of evaluating two 
membranes in four quarterly short-term tests, using the protocol in the 
``ICR Bench- and Pilot-scale Treatment Study Manual'' (EPA 814-B-96-003, 
April 1996).
    (2) A PWS shall conduct pilot-scale testing as continuous flow 
tests. For GAC, the PWS shall use GAC of particle size representative of 
that used in full-scale practice, a pilot GAC column with a minimum 
inner diameter of 2.0 inches, and hydraulic loading rate (volumetric 
flow rate/column cross-sectional area) representative of that used in 
full-scale practice. The PWS shall design a pilot-scale membrane system 
as a staged array of elements as described in ``ICR Manual for Bench- 
and Pilot-scale Treatment Studies'', EPA 814-B-96-003, April 1996.
    (i) GAC pilot-scale testing. (A) The pilot testing procedures and 
monitoring and reporting requirements are prescribed in the ``ICR Bench- 
and Pilot-scale Treatment Study Manual'' (EPA 814-B-96-003, April 1996).
    (B) At least two EBCTs shall be tested, EBCT=10 min and EBCT=20 min, 
using the pilot-scale plant. Additional EBCTs may be tested.
    (C) The pilot tests at each EBCT shall continue until the effluent 
TOC concentration is at least 70% of the average influent TOC 
concentration on two consecutive TOC sample dates that are at least two 
weeks apart or the effluent TOC reaches a plateau at greater than 50% of 
the influent TOC (i.e., the effluent TOC does not increase over a two-
month period by more than 10% of the average influent TOC 
concentration). If either of these criteria is met for the 20-minute 
EBCT prior to six months run time, a second pilot test at each EBCT 
shall be conducted following the same sampling requirements. In all 
cases the maximum length of the pilot study (one or two tests) is one 
year. The average influent TOC is defined as the running average of the 
influent TOC at the time of sampling. The pilot-scale testing shall be 
timed to capture seasonal variation. If seasonal variation is not 
significant, as is the case with most ground waters, the pilot-scale 
test runs shall be designed to evaluate the impact of other variables, 
such as pretreatment.
    (ii) Membrane pilot-scale testing.
    (A) The membrane pilot testing procedures and monitoring and 
reporting requirements are prescribed in the ``ICR Bench- and Pilot-
scale Treatment Study Manual'' (EPA 814-B-96-003, April 1996).
    (B) The membrane test system shall be designed to yield information 
on loss of productivity (fouling), pretreatment requirements, cleaning 
requirements, and permeate quality and operated at a recovery 
representative of full-scale operation.
    (C) The pilot-scale testing shall be run for one year.
    (3) Chlorination under simulated distribution system (SDS) 
conditions shall be used prior to the measurement of THM4, HAA6, TOX, 
and chlorine demand. These conditions are described in ``ICR Manual for 
Bench- and Pilot-scale Treatment Studies'' (EPA 814-B-96-003, April 
1996) and represent the average conditions in the distribution system at 
that time with regard to holding time, temperature, pH, and chlorine 
residual. If chlorine is not used as the final disinfectant in practice, 
then a chlorine dose shall be set to yield a free chlorine residual of 
1.0 to 0.5 mg/l after a holding time, temperature, and pH equal to those 
representative of the distribution system averages.
    (c) Analytical Methods. All analyses required by paragraphs (a) and 
(b) of this section shall be conducted using the methods and the 
mandatory analytical and quality control procedures contained in either 
``DBP/ICR Analytical Methods Manual'' (EPA 814-B-96-002, April 1996) or 
``ICR Manual for Bench- and Pilot-scale Treatment Studies'' (EPA 814-B-
96-003, April 1996).

[[Page 489]]

In addition, TOC analyses required by paragraph (a) of this section 
shall be conducted by a laboratory approved under the provisions of 
Sec. 141.142(b)(2) of this subpart.
    (d) Reporting. (1) TOC and UFCTOX reporting. A PWS shall submit the 
monthly results of 12 months of TOC or UFCTOX monitoring required by 
paragraph (a)(1) of this section and the annual average of those monthly 
results not later than October 14, 1997. This report is not required to 
be submitted electronically. Although a PWS may use monitoring results 
from samples required by Sec. 141.142(a) of this subpart to meet this 
requirement, it shall submit separate reports to meet this reporting 
requirement and the reporting requirement in Sec. 141.142(c)(1) of this 
subpart.
    (2) A PWS shall report all data collected under the provisions of 
paragraph (b) of this section. In addition, a PWS shall report the 
information for water resource and full-scale and pilot- or bench-scale 
pretreatment processes that precede the bench/pilot systems. These data 
and information shall be reported in the format specified in ``ICR 
Manual for Bench- and Pilot-scale Treatment Studies'' (EPA 814-B-96-003, 
April 1996) not later than July 14, 1999.
    (3) All reports required by this section shall be submitted to 
USEPA, Technical Support Division, ICR Precursor Removal Studies 
Coordinator, 26 West Martin Luther King Drive, Cincinnati, OH 45268.



                 Subpart O--Consumer Confidence Reports

    Source: 63 FR 44526, Aug. 19, 1998, unless otherwise noted.

    Effective Date Note: At 63 FR 44526, Aug. 19, 1998, subpart O was 
added. This subpart contains information collection requirements and 
will not become effective until approval has been given by the Office of 
Management and Budget.



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 level prescribed by 
Sec. 141.24(h)(18) for the contaminants listed in Sec. 141.61(c), 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 Secs. 141.153 and 
141.154, and must be designed to achieve an equivalent level of public 
information and education as would be achieved under this subpart.
    (f) For purpose of Secs. 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.



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

[[Page 490]]

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 which contains data on a contaminant for which EPA has 
set a treatment technique or an action level must include one or both of 
the following definitions as applicable:
    (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.
    (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 an MCL, action 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 Secs. 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.

[[Page 491]]

    (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 Secs. 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 and total 
coliforms, 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 a sampling point: the 
highest average of any of the sampling points and the range of all 
sampling points expressed in the same units as 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 
sampling points: the average and range of detection expressed in the 
same units as the MCL.

    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 Secs. 141.73 or 141.173: The 
highest single measurement and the lowest monthly percentage of samples 
meeting the turbidity limits specified in Secs. 141.73 or 141.173 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:
    (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: The total number of positive samples; and
    (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

[[Page 492]]

sources for that contaminant listed in appendix B to this subpart which 
are most applicable to the system.
    (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 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 C 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 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 which fail to take one or more actions prescribed 
by Secs. 141.80(d), 141.81, 141.82, 141.83 or 141.84, the report must 
include the applicable language of appendix C to this subpart for lead, 
copper, or both.
    (4) Treatment techniques for Acrylamide and Epichlorohydrin 
prescribed by subpart K of this part. For systems

[[Page 493]]

which violate the requirements of subpart K of this part, the report 
must include the relevant language from appendix C to this subpart.
    (5) Recordkeeping of compliance data.
    (6) Special monitoring requirements prescribed by Secs. 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 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

[[Page 494]]

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.

[63 FR 44526, Aug. 19, 1998, as amended at 63 FR 69516, Dec. 16, 1998; 
64 FR 34733, June 29, 1999]



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) A system which detects arsenic at levels above 25 ``g/
l, but below the MCL:
    (1) Must include in its report a short informational statement about 
arsenic, using language such as: EPA is reviewing the drinking water 
standard for arsenic because of special concerns that it may not be 
stringent enough. Arsenic is a naturally-occurring mineral known to 
cause cancer in humans at high concentrations.
    (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.
    (2) May write its own educational statement, but only in 
consultation with the Primacy Agency.
    (d) Systems which detect lead above the action level in more than 
5%, and up to and including 10%, of homes sampled:
    (1) Must include a short informational statement about the special 
impact of lead on children using language such as: Infants and young 
children are typically more vulnerable to lead in drinking water than 
the general population. It is possible that lead levels at your home may 
be higher than at other homes in the community as a result of materials 
used in your home's plumbing. If you are concerned about elevated lead 
levels in your home's water, you may wish to have your water tested and 
flush your tap for 30 seconds to 2 minutes before using tap water. 
Additional information is available from the Safe Drinking Water Hotline 
(800-426-4791).
    (2) May write its own educational statement, but only in 
consultation with the Primacy Agency.
    (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 prescribed by paragraph (73) of appendix C to subpart 
O.

[63 FR 44526, Aug. 19, 1998, as amended at 63 FR 69475, Dec. 16, 1998; 
64 FR 34733, June 29, 1999]



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

[[Page 495]]

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 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 5 years.

 Appendix A to Subpart O--Converting MCL Compliance Values for Consumer 
                           Confidence Reports

                                   Key

                             AL=Action Level

                      MCL=Maximum Contaminant Level

                   MCLG=Maximum Contaminant Level Goal

                      MFL=million fibers per liter

  mrem/year=millirems per year (a measure of radiation absorbed by the 
                                  body)

                    NTU=Nephelometric Turbidity Units

         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 (g/l)

             ppt=parts per trillion, or nanograms per liter

            ppq=parts per quadrillion, or picograms per liter

                         TT=Treatment Technique

[[Page 496]]



----------------------------------------------------------------------------------------------------------------
                                      MCL in compliance                                              MCLG in CCR
            Contaminant                  units (mg/L)      multiply by . . .     MCL in CCR units       units
----------------------------------------------------------------------------------------------------------------
   Microbiological Contaminants
1. Total Coliform Bacteria........  .....................  .................  (systems that collect            0
                                                                               40 or more samples
                                                                               per month) 5% of
                                                                               monthly samples are
                                                                               positive; (systems
                                                                               that collect fewer
                                                                               than 40 samples per
                                                                               month) 1 positive
                                                                               monthly sample.
2. Fecal coliform and E. coli.....  .....................  .................  A routine sample and             0
                                                                               a repeat sample are
                                                                               total coliform
                                                                               positive, and one is
                                                                               also fecal coliform
                                                                               or E. coli positive.
3. Turbidity......................  .....................  .................  TT (NTU).............          n/a
 
     Radioactive Contaminants
 
4. Beta/photon emitters...........  4 mrem/yr............  .................  4 mrem/yr............            0
5. Alpha emitters.................  15 pCi/l.............  .................  15 pCi/l.............            0
6. Combined radium................  5 pCi/l..............  .................  5 pCi/l..............            0
 
      Inorganic Contaminants
 
7. Antimony.......................  .006.................               1000  6 ppb................            6
8. Arsenic........................  .05..................               1000  50 ppb...............          n/a
9. Asbestos.......................  7 MFL................  .................  7 MFL................            7
10. Barium........................  2....................  .................  2 ppm................            2
11. Beryllium.....................  .004.................               1000  4 ppb................            4
12. Cadmium.......................  .005.................               1000  5 ppb................            5
13. Chromium......................  .1...................               1000  100 ppb..............          100
14. Copper........................  AL=1.3...............  .................  AL=1.3 ppm...........          1.3
15. Cyanide.......................  .2...................               1000  200 ppb..............          200
16. Fluoride......................  4....................  .................  4 ppm................            4
17. Lead..........................  AL=.015..............               1000  AL=15 ppb............            0
18. Mercury (inorganic)...........  .002.................               1000  2 ppb................            2
19. Nitrate (as Nitrogen).........  10...................  .................  10 ppm...............           10
20. Nitrite (as Nitrogen).........  1....................  .................  1 ppm................            1
21. Selenium......................  .05..................               1000  50 ppb...............           50
22. Thallium......................  .002.................               1000  2 ppb................          0.5
 
  Synthetic Organic Contaminants
     including Pesticides and
            Herbicides
 
23. 2,4-D.........................  .07..................               1000  70 ppb...............           70
24. 2,4,5-TP [Silvex].............  .05..................               1000  50 ppb...............           50
25. Acrylamide....................  .....................  .................  TT...................            0
26. Alachlor......................  .002.................               1000  2 ppb................            0
27. Atrazine......................  .003.................               1000  3 ppb................            3
28. Benzo(a)pyrene [PAH]..........  .0002................          1,000,000  200 ppt..............            0
29. Carbofuran....................  .04..................               1000  40 ppb...............           40
30. Chlordane.....................  .002.................               1000  2 ppb................            0
31. Dalapon.......................  .2...................               1000  200 ppb..............          200
32. Di(2-ethylhexyl)adipate.......  .4...................               1000  400 ppb..............          400
33. Di(2-ethylhexyl) phthalate....  .006.................               1000  6 ppb................            0
34. Dibromochloropropane..........  .0002................          1,000,000  200 ppt..............            0
35. Dinoseb.......................  .007.................               1000  7 ppb................            7
36. Diquat........................  .02..................               1000  20 ppb...............           20
37. Dioxin [2,3,7,8-TCDD].........  .00000003............      1,000,000,000  30 ppq...............            0
38. Endothall.....................  .1...................               1000  100 ppb..............          100
39. Endrin........................  .002.................               1000  2 ppb................            2
40. Epichlorohydrin...............  .....................  .................  TT...................            0
41. Ethylene dibromide............  .00005...............          1,000,000  50 ppt...............            0
42. Glyphosate....................  .7...................               1000  700 ppb..............          700
43. Heptachlor....................  .0004................          1,000,000  400 ppt..............            0
44. Heptachlor epoxide............  .0002................          1,000,000  200 ppt..............            0
45. Hexachlorobenzene.............  .001.................               1000  1 ppb................            0
46. Hexachloro-cyclopentadiene....  .05..................               1000  50 ppb...............           50
47. Lindane.......................  .0002................          1,000,000  200 ppt..............          200
48. Methoxychlor..................  .04..................               1000  40 ppb...............           40
49. Oxamyl [Vydate]...............  .2...................               1000  200 ppb..............          200
50. PCBs [Polychlorinated           .0005................          1,000,000  500 ppt..............            0
 biphenyls].
51. Pentachlorophenol.............  .001.................               1000  1 ppb................            0
52. Picloram......................  .5...................               1000  500 ppb..............          500

[[Page 497]]

 
53. Simazine......................  .004.................               1000  4 ppb................            4
54. Toxaphene.....................  .003.................               1000  3 ppb................            0
 
   Volatile Organic Contaminants
 
55. Benzene.......................  .005.................               1000  5 ppb................            0
56. Carbon tetrachloride..........  .005.................               1000  5 ppb................            0
57. Chlorobenzene.................  .1...................               1000  100 ppb..............          100
58. o-Dichlorobenzene.............  .6...................               1000  600 ppb..............          600
59. p-Dichlorobenzene.............  .075.................               1000  75 ppb...............           75
60. 1,2-Dichloroethane............  .005.................               1000  5 ppb................            0
61. 1,1-Dichloroethylene..........  .007.................               1000  7 ppb................            7
62. cis-1,2-Dichloroethylene......  .07..................               1000  70 ppb...............           70
63. trans-1,2-Dichloroethylene....  .1...................               1000  100 ppb..............          100
64. Dichloromethane...............  .005.................               1000  5 ppb................            0
65. 1,2-Dichloropropane...........  .005.................               1000  5 ppb................            0
66. Ethylbenzene..................  .7...................               1000  700 ppb..............          700
67. Styrene.......................  .1...................               1000  100 ppb..............          100
68. Tetrachloroethylene...........  .005.................               1000  5 ppb................            0
69. 1,2,4-Trichlorobenzene........  .07..................               1000  70 ppb...............           70
70. 1,1,1-Trichloroethane.........  .2...................               1000  200 ppb..............          200
71. 1,1,2-Trichloroethane.........  .005.................               1000  5 ppb................            3
72. Trichloroethylene.............  .005.................               1000  5 ppb................            0
73. TTHMs [Total trihalomethanes].  .10..................               1000  100 ppb..............          n/a
74. Toluene.......................  1....................  .................  1 ppm................            1
75. Vinyl Chloride................  .002.................               1000  2 ppb................            0
76. Xylenes.......................  10...................  .................  10 ppm...............           10
----------------------------------------------------------------------------------------------------------------


[63 FR 44526, Aug. 19, 1998; 64 FR 34733, June 29, 1999]

             Appendix B to Subpart O--Regulated Contaminants

                                   Key

                             AL=Action Level

                      MCL=Maximum Contaminant Level

                   MCLG=Maximum Contaminant Level Goal

                      MFL=million fibers per liter

  mrem/year=millirems per year (a measure of radiation absorbed by the 
                                  body)

                    NTU=Nephelometric Turbidity Units

         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 (g/l)

             ppt=parts per trillion, or nanograms per liter

            ppq=parts per quadrillion, or picograms per liter

                         TT=Treatment Technique

[[Page 498]]



----------------------------------------------------------------------------------------------------------------
                                                                                     Major sources in drinking
          Contaminant (units)                MCLG                 MCL                          water
----------------------------------------------------------------------------------------------------------------
      Microbiological Contaminants
 
1. Total Coliform Bacteria.............             0  (systems that collect 40   Naturally present in the
                                                        or more samples per        environment.
                                                        month) 5% of monthly
                                                        samples are positive;
                                                        (systems that collect
                                                        fewer than 40 samples
                                                        per month) 1 positive
                                                        monthly sample.
2. Fecal coliform and E. coli..........             0  A routine sample and a     Human and animal fecal waste.
                                                        repeat sample are total
                                                        coliform positive, and
                                                        one is also fecal
                                                        coliform or E. coli
                                                        positive.
3. Turbidity...........................           n/a  TT.......................  Soil runoff.
 
        Radioactive Contaminants
 
4. Beta/photon emitters (mrem/yr)......             0  4........................  Decay of natural and man-made
                                                                                   deposits.
5. Alpha emitters (pCi/l)..............             0  15.......................  Erosion of natural deposits.
6. Combined radium (pCi/l).............             0  5........................  Erosion of natural deposits.
 
         Inorganic Contaminants
 
7. Antimony (ppb)......................             6  6........................  Discharge from petroleum
                                                                                   refineries; fire retardants;
                                                                                   ceramics; electronics;
                                                                                   solder.
8. Arsenic (ppb).......................           n/a  50.......................  Erosion of natural deposits;
                                                                                   Runoff from orchards; Runoff
                                                                                   from glass and electronics
                                                                                   production wastes.
9. Asbestos (MFL)......................             7  7........................  Decay of asbestos cement water
                                                                                   mains; Erosion of natural
                                                                                   deposits.
10. Barium (ppm).......................             2  2........................  Discharge of drilling wastes;
                                                                                   Discharge from metal
                                                                                   refineries; Erosion of
                                                                                   natural deposits.
11. Beryllium (ppb)....................             4  4........................  Discharge from metal
                                                                                   refineries and coal-burning
                                                                                   factories; Discharge from
                                                                                   electrical, aerospace, and
                                                                                   defense industries.
12. Cadmium (ppb)......................             5  5........................  Corrosion of galvanized pipes;
                                                                                   Erosion of natural deposits;
                                                                                   Discharge from metal
                                                                                   refineries; runoff from waste
                                                                                   batteries and paints.
13. Chromium (ppb).....................           100  100......................  Discharge from steel and pulp
                                                                                   mills; Erosion of natural
                                                                                   deposits.
14. Copper (ppm).......................           1.3  AL=1.3...................  Corrosion of household
                                                                                   plumbing systems; Erosion of
                                                                                   natural deposits; Leaching
                                                                                   from wood preservatives.
15. Cyanide (ppb)......................           200  200......................  Discharge from steel/metal
                                                                                   factories; Discharge from
                                                                                   plastic and fertilizer
                                                                                   factories.
16. Fluoride (ppm).....................             4  4........................  Erosion of natural deposits;
                                                                                   Water additive which promotes
                                                                                   strong teeth; Discharge from
                                                                                   fertilizer and aluminum
                                                                                   factories.
17. Lead (ppb).........................             0  AL=15....................  Corrosion of household
                                                                                   plumbing systems; Erosion of
                                                                                   natural deposits.
18. Mercury [inorganic] (ppb)..........             2  2........................  Erosion of natural deposits;
                                                                                   Discharge from refineries and
                                                                                   factories; Runoff from
                                                                                   landfills; Runoff from
                                                                                   cropland.
19. Nitrate [as Nitrogen] (ppm)........            10  10.......................  Runoff from fertilizer use;
                                                                                   Leaching from septic tanks,
                                                                                   sewage; Erosion of natural
                                                                                   deposits.
20. Nitrite [as Nitrogen] (ppm)........             1  1........................  Runoff from fertilizer use;
                                                                                   Leaching from septic tanks,
                                                                                   sewage; Erosion of natural
                                                                                   deposits.
21. Selenium (ppb).....................            50  50.......................  Discharge from petroleum and
                                                                                   metal refineries; Erosion of
                                                                                   natural deposits; Discharge
                                                                                   from mines.
22. Thallium (ppb).....................           0.5  2........................  Leaching from ore-processing
                                                                                   sites; Discharge from
                                                                                   electronics, glass, and drug
                                                                                   factories.
 

[[Page 499]]

 
     Synthetic Organic Contaminants
  including Pesticides and Herbicides
 
23. 2,4-D (ppb)........................            70  70.......................  Runoff from herbicide used on
                                                                                   row crops.
24. 2,4,5-TP [Silvex] (ppb)............            50  50.......................  Residue of banned herbicide.
25. Acrylamide.........................             0  TT.......................  Added to water during sewage/
                                                                                   wastewater treatment.
26. Alachlor (ppb).....................             0  2........................  Runoff from herbicide used on
                                                                                   row crops.
27. Atrazine (ppb).....................             3  3........................  Runoff from herbicide used on
                                                                                   row crops.
28. Benzo(a)pyrene [PAH] (nanograms/l).             0  200......................  Leaching from linings of water
                                                                                   storage tanks and
                                                                                   distribution lines.
29. Carbofuran (ppb)...................            40  40.......................  Leaching of soil fumigant used
                                                                                   on rice and alfalfa.
30. Chlordane (ppb)....................             0  2........................  Residue of banned termiticide.
31. Dalapon (ppb)......................           200  200......................  Runoff from herbicide used on
                                                                                   rights of way.
32. Di(2-ethylhexyl) adipate (ppb).....           400  400......................  Discharge from chemical
                                                                                   factories.
33. Di(2-ethylhexyl) phthalate (ppb)...             0  6........................  Discharge from rubber and
                                                                                   chemical factories.
34. Dibromochloropropane (ppt).........             0  200......................  Runoff/leaching from soil
                                                                                   fumigant used on soybeans,
                                                                                   cotton, pineapples, and
                                                                                   orchards.
35. Dinoseb (ppb)......................             7  7........................  Runoff from herbicide used on
                                                                                   soybeans and vegetables.
36. Diquat (ppb).......................            20  20.......................  Runoff from herbicide use.
37. Dioxin [2,3,7,8-TCDD] (ppq)........             0  30.......................  Emissions from waste
                                                                                   incineration and other
                                                                                   combustion; Discharge from
                                                                                   chemical factories.
38. Endothall (ppb)....................           100  100......................  Runoff from herbicide use.
39. Endrin (ppb).......................             2  2........................  Residue of banned insecticide.
40. Epichlorohydrin....................             0  TT.......................  Discharge from industrial
                                                                                   chemical factories; An
                                                                                   impurity of some water
                                                                                   treatment chemicals.
41. Ethylene dibromide (ppt)...........             0  50.......................  Discharge from petroleum
                                                                                   refineries.
42. Glyphosate (ppb)...................           700  700......................  Runoff from herbicide use.
43. Heptachlor (ppt)...................             0  400......................  Residue of banned termiticide.
44. Heptachlor epoxide (ppt)...........             0  200......................  Breakdown of heptachlor.
45. Hexachlorobenzene (ppb)............             0  1........................  Discharge from metal
                                                                                   refineries and agricultural
                                                                                   chemical factories.
46. Hexachlorocyclopentadiene (ppb)....            50  50.......................  Discharge from chemical
                                                                                   factories.
47. Lindane (ppt)......................           200  200......................  Runoff/leaching from
                                                                                   insecticide used on cattle,
                                                                                   lumber, gardens.
48. Methoxychlor (ppb).................            40  40.......................  Runoff/leaching from
                                                                                   insecticide used on fruits,
                                                                                   vegetables, alfalfa,
                                                                                   livestock.
49. Oxamyl [Vydate](ppb)...............           200  200......................  Runoff/leaching from
                                                                                   insecticide used on apples,
                                                                                   potatoes and tomatoes.
50. PCBs [Polychlorinated biphenyls]                0  500......................  Runoff from landfills;
 (ppt).                                                                            Discharge of waste chemicals.
51. Pentachlorophenol (ppb)............             0  1........................  Discharge from wood preserving
                                                                                   factories.
52. Picloram (ppb).....................           500  500......................  Herbicide runoff.
53. Simazine (ppb).....................             4  4........................  Herbicide runoff.
54. Toxaphene (ppb)....................             0  3........................  Runoff/leaching from
                                                                                   insecticide used on cotton
                                                                                   and cattle.
 
     Volatile Organic Contaminants
 
55. Benzene (ppb)......................             0  5........................  Discharge from factories;
                                                                                   Leaching from gas storage
                                                                                   tanks and landfills.
56. Carbon tetrachloride (ppb).........             0  5........................  Discharge from chemical plants
                                                                                   and other industrial
                                                                                   activities.
57. Chlorobenzene (ppb)................           100  100......................  Discharge from chemical and
                                                                                   agricultural chemical
                                                                                   factories.
58. o-Dichlorobenzene (ppb)............           600  600......................  Discharge from industrial
                                                                                   chemical factories.
59. p-Dichlorobenzene (ppb)............            75  75.......................  Discharge from industrial
                                                                                   chemical factories.
60. 1,2-Dichloroethane (ppb)...........             0  5........................  Discharge from industrial
                                                                                   chemical factories.
61. 1,1-Dichloroethylene (ppb).........             7  7........................  Discharge from industrial
                                                                                   chemical factories.
62. cis-1,2-Dichloroethylene (ppb).....            70  70.......................  Discharge from industrial
                                                                                   chemical factories.
63. trans-1,2-Dichloroethylene (ppb)...           100  100......................  Discharge from industrial
                                                                                   chemical factories.
64. Dichloromethane (ppb)..............             0  5........................  Discharge from pharmaceutical
                                                                                   and chemical factories.

[[Page 500]]

 
65. 1,2-Dichloropropane (ppb)..........             0  5........................  Discharge from industrial
                                                                                   chemical factories.
66. Ethylbenzene (ppb).................           700  700......................  Discharge from petroleum
                                                                                   refineries.
67. Styrene (ppb)......................           100  100......................  Discharge from rubber and
                                                                                   plastic factories; Leaching
                                                                                   from landfills.
68. Tetrachloroethylene (ppb)..........             0  5........................  Leaching from PVC pipes;
                                                                                   Discharge from factories and
                                                                                   dry cleaners.
69. 1,2,4-Trichlorobenzene (ppb).......            70  70.......................  Discharge from textile-
                                                                                   finishing factories.
70. 1,1,1-Trichloroethane (ppb)........           200  200......................  Discharge from metal
                                                                                   degreasing sites and other
                                                                                   factories.
71. 1,1,2-Trichloroethane (ppb)........             3  5........................  Discharge from industrial
                                                                                   chemical factories.
72. Trichloroethylene (ppb)............             0  5........................  Discharge from metal
                                                                                   degreasing sites and other
                                                                                   factories.
73. TTHMs [Total trihalomethanes] (ppb)           n/a  100......................  By-product of drinking water
                                                                                   chlorination.
74. Toluene (ppm)......................             1  1........................  Discharge from petroleum
                                                                                   factories.
75. Vinyl Chloride (ppb)...............             0  2........................  Leaching from PVC piping;
                                                                                   Discharge from plastics
                                                                                   factories.
76. Xylenes (ppm)......................            10  10.......................  Discharge from petroleum
                                                                                   factories; Discharge from
                                                                                   chemical factories.
----------------------------------------------------------------------------------------------------------------


[63 FR 44526, Aug. 19, 1998; 64 FR 34733, June 29, 1999]

            Appendix C to Subpart O--Health Effects Language

                      Microbiological Contaminants

    (1) Total Coliform. 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.
    (2) Fecal coliform/E.Coli. Fecal coliforms and 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, and people with 
severely compromised immune systems.
    (3) Turbidity. 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

    (4) Beta/photon emitters. 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.
    (5) Alpha emitters. 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.
    (6) Combined Radium 226/228. Some people who drink water containing 
radium 226 or 228 in excess of the MCL over many years may have an 
increased risk of getting cancer.

                         Inorganic Contaminants

    (7) Antimony. 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.
    (8) Arsenic. 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.
    (9) Asbestos. 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.
    (10) Barium. Some people who drink water containing barium in excess 
of the MCL over many years could experience an increase in their blood 
pressure.
    (11) Beryllium. Some people who drink water containing beryllium 
well in excess of the MCL over many years could develop intestinal 
lesions.
    (12) Cadmium. Some people who drink water containing cadmium in 
excess of the MCL over many years could experience kidney damage.
    (13) Chromium. Some people who use water containing chromium well in 
excess of the MCL over many years could experience allergic dermatitis.
    (14) Copper. Copper is an essential nutrient, but some people who 
drink water containing copper in excess of the action level

[[Page 501]]

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.
    (15) Cyanide. 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. 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. Children may get mottled teeth.
    (17) Lead. 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.
    (18) Mercury (inorganic). Some people who drink water containing 
inorganic mercury well in excess of the MCL over many years could 
experience kidney damage.
    (19) Nitrate. 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.
    (20) Nitrite. 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.
    (21) Selenium. 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. 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.

   Synthetic Organic Contaminants Including Pesticides and Herbicides

    (23) 2,4-D. 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.
    (24) 2,4,5-TP (Silvex). Some people who drink water containing 
silvex in excess of the MCL over many years could experience liver 
problems.
    (25) Acrylamide. 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.
    (26) Alachlor. 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.
    (27) Atrazine. 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.
    (28) Benzo(a)pyrene (PAH). 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.
    (29) Carbofuran. 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.
    (30) Chlordane. 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.
    (31) Dalapon. Some people who drink water containing dalapon well in 
excess of the MCL over many years could experience minor kidney changes.
    (32) Di (2-ethylhexyl) adipate. Some people who drink water 
containing di (2-ethylhexyl) adipate well in excess of the MCL over many 
years could experience general toxic effects or reproductive 
difficulties.
    (33) Di (2-ethylhexyl) phthalate. Some people who drink water 
containing di (2-ethylhexyl) phthalate 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.
    (34) Dibromochloropropane (DBCP). Some people who drink water 
containing DBCP in excess of the MCL over many years could experience 
reproductive difficulties and may have an increased risk of getting 
cancer.
    (35) Dinoseb. Some people who drink water containing dinoseb well in 
excess of the MCL over many years could experience reproductive 
difficulties.
    (36) Dioxin (2,3,7,8-TCDD). 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.
    (37) Diquat. Some people who drink water containing diquat in excess 
of the MCL over many years could get cataracts.
    (38) Endothall. Some people who drink water containing endothall in 
excess of the MCL over many years could experience problems with their 
stomach or intestines.

[[Page 502]]

    (39) Endrin. Some people who drink water containing endrin in excess 
of the MCL over many years could experience liver problems.
    (40) Epichlorohydrin. 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.
    (41) Ethylene dibromide. 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. 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. 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. 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. 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) Hexachlorocyclopentadiene. 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. 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. Some people who drink water containing 
methoxychlor in excess of the MCL over many years could experience 
reproductive difficulties.
    (49) Oxamyl [Vydate]. Some people who drink water containing oxamyl 
in excess of the MCL over many years could experience slight nervous 
system effects.
    (50) PCBs [Polychlorinated biphenyls]. Some people who drink water 
containing 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.
    (51) Pentachlorophenol. 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.
    (52) Picloram. Some people who drink water containing picloram in 
excess of the MCL over many years could experience problems with their 
liver.
    (53) Simazine. Some people who drink water containing simazine in 
excess of the MCL over many years could experience problems with their 
blood.
    (54) Toxaphene. 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.

                      Volatile Organic Contaminants

    (55) Benzene. 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. 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. Some people who drink water containing 
chlorobenzene in excess of the MCL over many years could experience 
problems with their liver or kidneys.
    (58) o-Dichlorobenzene. 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. 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. 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. 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. 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-Dicholoroethylene. 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. 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.

[[Page 503]]

    (65) 1,2-Dichloropropane. 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. 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. 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. 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) 1,2,4-Trichlorobenzene. 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.
    (70) 1,1,1,-Trichloroethane. 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.
    (71) 1,1,2-Trichloroethane. 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.
    (72) Trichloroethylene. 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.
    (73) TTHMs [Total Trihalomethanes]. Some people who drink water 
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.
    (74) Toluene. 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.
    (75) Vinyl Chloride. Some people who drink water containing vinyl 
chloride in excess of the MCL over many years may have an increased risk 
of getting cancer.
    (76) Xylenes. Some people who drink water containing xylenes in 
excess of the MCL over many years could experience damage to their 
nervous system.



             Subpart P--Enhanced Filtration and Disinfection

    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 December 17, 2001 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 
Secs. 141.71 and 141.171 and the disinfection requirements in 
Secs. 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 
Secs. 141.72 and 141.172.
    (c) Systems are not permitted to begin construction of uncovered 
finished water storage facilities beginning February 16, 1999.

[[Page 504]]



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 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 
Secs. 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 Secs. 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 Secs. 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 Secs. 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 16, 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.

[[Page 505]]

    (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 16, 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 Secs. 141.12 and 141.30 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 16, 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 16, 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 16, 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 March 16, 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

[[Page 506]]

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 16, 
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 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 ( (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 ((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;

[[Page 507]]

    (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.
    (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.



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 17, 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.



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

[[Page 508]]

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 or direct 
filtration must report monthly to the State the information specified in 
paragraphs (a) and (b) of this section beginning December 17, 2001. 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 December 17, 2001. 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.

[[Page 509]]

    (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 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.



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.

[[Page 510]]

 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.
142.64  Variances and exemptions from the requirements of part 141, 
          subpart H--Filtration and Disinfection.

                        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.

[[Page 511]]

    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.
    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

[[Page 512]]

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 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
    (3) Public water systems owned or maintained by a Federal agency 
where the Administrator has waived compliance with national primary 
drinking water regulations pursuant to section 1447(b) of the Act.
    (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]



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

[[Page 513]]

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 
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 Secs. 141.32 and 
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.

[[Page 514]]

    (c) Has established and will maintain record keeping and reporting 
of its activities under paragraphs (a), (b) and (d) in compliance with 
Secs. 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 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) 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]



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

[[Page 515]]

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.
    (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 Secs. 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

[[Page 516]]

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 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]

    Effective Date Note: This section contains information collection 
and recordkeeping requirements and will not become effective until 
approval has been given by the Office of Management and Budget.



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 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;

[[Page 517]]

    (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 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.

[[Page 518]]

    (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 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 18 months 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]



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

[[Page 519]]

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 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 which makes 
possible comparison with the limits specified in Secs. 141.63, 141.71, 
and 141.72 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 Secs. 141.71, 
141.73, 141.173 and 141.175 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

[[Page 520]]

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 Secs. 141.72 and 141.74 of this chapter and the 
reporting requirements of Secs. 141.75 and 141.175 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 or subpart P of this 
chapter, must be made in writing and kept at 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; and
    (8) Section 141.75(b)(2)(iv)--Any decision to allow reduced 
reporting by a filtered public water system.
    (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.

[[Page 521]]

    (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 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.

[[Page 522]]

    (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.
    (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).

[[Page 523]]

    (6) Records of analysis for other than microbiological contaminants 
(including total coliform, fecal coliform, and heterotrophic plate 
count), residual 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 of this chapter.
    (i) Records of systems consulting with the State concerning a 
modification to disinfection practice under Sec. 141.172(c) of this 
chapter, including the status of the consultation.
    (ii) Records of decisions that a system using alternative filtration 
technologies, as allowed under Sec. 141.173(b) 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. 141.175 of this chapter.
    (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 CFR, part 141, subpart I for the control of lead and 
copper:
    (i) Section 141.82(b)--decisions to require a water system to 
conduct corrosion control treatment studies;
    (ii) Section 141.82(d)--designations of optimal corrosion control 
treatment;
    (iii) Section 141.82(f)--designations of optimal water quality 
parameters;
    (iv) Section 141.82(h)--decisions to modify a public water system's 
optimal

[[Page 524]]

corrosion control treatment or water quality parameters;
    (v) Section 141.83(b)(2)--determinations of source water treatment; 
and
    (vi) Section 141.83(b)(4)--designations of maximum permissible lead 
and copper concentrations in source water.
    (vii) Section 141.84(e)--determinations that a system does not 
control entire lead service lines.
    (viii) Section 141.84(f)--determinations establishing a shorter lead 
service line replacement schedule than required by Sec. 141.84.
    (9) Records of reports and any other information submitted by PWSs 
under Sec. 141.90;
    (10) Records of state activities, and the results thereof, to verify 
compliance with State determinations issued under Secs. 141.82(f), 
141.82(h), 141.83(b)(2), and 141.83(b)(4) and compliance with lead 
service line replacement schedules under Sec. 141.84.
    (11) Records of each system's currently applicable or most recently 
designated monitoring requirements. If, for the records identified in 
Secs. 142.14(d)(8)(i) through 142.14(d)(8)(viii) above, no change is 
made to State decision during a 12 year retention period, the State 
shall maintain 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 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(f)(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(f)(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.
    (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) 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, as amended at 54 FR 27537, June 29, 1989; 55 
FR 25065, June 19, 1990; 56 FR 3595, Jan. 30, 1991; 56 FR 26562, June 7, 
1991; 63 FR 69475, 69519, Dec. 16, 1998]



Sec. 142.15  Reports by States.

    Each State which has primary enforcement responsibility shall submit 
to the Administrator the following information:

[[Page 525]]

    (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;
    (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.
    (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) The results of monitoring for unregulated contaminants shall be 
reported quarterly.
    (4) States shall report to EPA by May 15, August 15, November 15 and 
February 15 of each year 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 the name and PWS identification number 
of:
    (i) Each public water system which exceeded the lead and copper 
action levels and the date upon which the exceedance occurred;

[[Page 526]]

    (ii) 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;
    (iii) 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);
    (iv) 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;
    (v) 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);
    (vi) Each public water system for which the State has specified 
maximum permissible source water levels under Sec. 141.83(b)(4); and
    (vii) 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).
    (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. 141.16(b)(3) of this chapter.
    (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, as amended at 43 FR 5373, Feb. 8, 1978; 54 
FR 27539, June 29, 1989; 55 FR 52140, Dec. 20, 1989; 55 FR 25065, June 
19, 1990; 56 FR 3595, Jan. 30, 1991; 56 FR 26562, June 7, 1991; 63 FR 
69520, Dec. 16, 1998]



Sec. 142.16  Special primacy requirements.

    (a) State public notification requirements. If a State exercises the 
option specified in Sec. 141.32(b)(4) to authorize less frequent notice 
for minor monitoring violations, it must adopt a program revision 
enforceable under State authorities which promulgates rules specifying 
either: (1) Which monitoring violations are minor and the frequency of 
public notification for such violations; or (2) criteria for determining 
which monitoring violations are minor and the frequency of public 
notification.
    (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 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

[[Page 527]]

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.
    (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

[[Page 528]]

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.
    (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

[[Page 529]]

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 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.

[[Page 530]]

    (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) Sections 141.82(d), 141.82(f), 141.82(h)--Designating optimal 
corrosion control treatment methods, optimal water quality parameters 
and modifications thereto.
    (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 of PWS demonstrations of limited control over 
lead service lines.
    (e) An application for approval of a State program revision which 
adopts the requirements specified in Secs. 141.11, 141.23, 141.24, 
141.32, 141.40, 141.61 and 141.62 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 Secs. 141.23, 141.24, and 141.40, 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 Secs. 141.24(f)(8), 141.24(h)(6), 
and 141.40(n)(4).
    (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

[[Page 531]]

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. 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, 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 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

[[Page 532]]

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 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.

[54 FR 15188, Apr. 17, 1989, as amended at 54 FR 27539, June 29, 1989; 
55 FR 25065, June 19, 1990; 56 FR 3595, Jan. 30, 1991; 56 FR 26563, June 
7, 1991; 57 FR 31847, July 17, 1992; 59 FR 33864, June 30, 1994; 63 FR 
44535, Aug. 19, 1998; 63 FR 69475, 69520, Dec. 16, 1998; 64 FR 34733, 
June 29, 1999]



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

[[Page 533]]

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 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 
Secs. 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;

[[Page 534]]

    (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 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.

[[Page 535]]

    (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 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

[[Page 536]]

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;
    (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:

[[Page 537]]

    (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 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

[[Page 538]]

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 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

[[Page 539]]

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 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]


[[Page 540]]





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.
    (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:

[[Page 541]]

    (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 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

[[Page 542]]

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 
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

[[Page 543]]

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.
    (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

[[Page 544]]

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 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 responsibile 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

[[Page 545]]

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 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 Secs. 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 Secs. 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

[[Page 546]]

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 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

[[Page 547]]

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 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                        .......................

[[Page 548]]

 
(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                        .......................
(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
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 >10g/1.
2 BAT for Chromium III only.
3 BAT for Selenium IV only.

                          Key to BATS in Table

1=Activated Alumina
2=Coagulation/Filtration (not BAT for systems 500 service connections)

[[Page 549]]

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

    (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 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 Secs. 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 Secs. 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 Secs. 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 
Secs. 141.61 (a) and (c) and 141.62, or an exemption from the 
requirements of Secs. 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 Secs. 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 103.35, 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

[[Page 550]]

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 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 Secs. 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]



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 the effective date of this section relating 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.

[54 FR 27568, June 29, 1989, as amended at 56 FR 1557, Jan. 15, 1991]



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]



                        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.

[[Page 551]]

    (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 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

[[Page 552]]

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]



  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

[[Page 553]]

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:
    (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

[[Page 554]]

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.



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 Secs. 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

[[Page 555]]

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 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

[[Page 556]]

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 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

[[Page 557]]

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.

            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.

[[Page 558]]



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.
143.5  Compliance with secondary maximum contaminant level and public 
          notification for fluoride.

    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 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]

[[Page 559]]



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 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. 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, which is available at NTIS PB95-104766.

----------------------------------------------------------------------------------------------------------------
          Contaminant               EPA             ASTM \3\                    SM4                  Other
----------------------------------------------------------------------------------------------------------------
Aluminum......................    \2\ 200.7  ......................  3120B...................
                                  \2\ 200.8  ......................  3113B...................
                                  \2\ 200.9  ......................  3111D...................
Chloride......................    \1\ 300.0  D4327-91..............  4110....................
                                                                     4500-Cl--D..............
Color.........................  ...........  ......................  2120B...................
Foaming Agents................  ...........  ......................  5540C...................
Iron..........................    \2\ 200.7  ......................  3120B...................
                                  \2\ 200.9  ......................  3111B...................
                                                                     3113B...................
Manganese.....................     \2\200.7  ......................  3120B...................
                                  \2\ 200.8  ......................  3111B...................
                                  \2\ 200.9  ......................  3113B...................
Odor..........................  ...........  ......................  2150B...................
Silver........................    \2\ 200.7  ......................  3120B...................  I-3720-85 \5\
                                  \2\ 200.8  ......................  3111B...................
                                  \2\ 200.9  ......................  3113B...................
Sulfate.......................    \1\ 300.0  D4327-91..............  4110....................
                                  \1\ 375.2  ......................  4500-SO 4-F.............
                                                                     4500-SO 4-C,D...........
TDS...........................  ...........  ......................  2540C...................
Zinc..........................    \2\ 200.7  ......................  3120B...................
                                  \2\ 200.8  ......................  3111B ..................
----------------------------------------------------------------------------------------------------------------
Footnotes:
\1\ ``Methods for the Determination of Inorganic Substances in Environmental Samples'', EPA-600/R-93-100, August
  1993. Available at NTIS, PB94-121811.
\2\ ``Methods for the Determination of Metals in Environmental Samples--Supplement I'', EPA-600/R-94-111, May
  1994. Available at NTIS, PB94-184942.
\3\ The procedures shall be done in accordance with the Annual Book of ASTM Standards, 1994, Vols. 11.01 and
  11.02, American Society for Testing and Materials. 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
  from the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103. Copies may be
  inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of the
  Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.

[[Page 560]]

 
\4\ The procedures shall be done in accordance with the 18th edition of Standard Methods for the Examination of
  Water and Wastewater, 1992, American Public Health Association. 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 from the American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20005. Copies
  may be inspected at EPA's Drinking Water Docket, 401 M Street, SW., Washington, DC 20460; or at the Office of
  the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\5\ Available from Books and Open-File Reports Section, U.S. Geological Survey, Federal Center, Box 25425,
  Denver, CO 80225-0425.


[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]



Sec. 143.5  Compliance with secondary maximum contaminant level and public notification for fluoride.

    (a) Community water systems, as defined in 40 CFR 141.2(e)(i) of 
this title, that exceed the secondary maximum contaminant level for 
fluoride as determined by the last single sample taken in accordance 
with the requirements of Sec. 141.23 of this title or any equivalent 
state law, but do not exceed the maximum contaminant level for flouride 
as specified by Sec. 141.62 of this title or any equivalent state law, 
shall provivde the notice described in paragraph (b) of all billing 
units annually, all new billing units at the time service begins, and 
the state public health officer.
    (b) The notice required by paragraph (a) shall contain the following 
language including the language necessary to replace the superscripts:

                              Public Notice

    Dear User,
    The U.S. Environmental Protection Agency requires that we send you 
this notice on the level of fluoride in your drinking water. The 
drinking water in your community has a fluoride concentration of \1\ 
milligrams per liter (mg/l).
    Federal regulations require that fluoride, which occurs naturally in 
your water supply, not exceed a concentration of 4.0 mg/l in drinking 
water. This is an enforceable standard called a Maximum Contaminant 
Level (MCL), and it has been established to protect the public health. 
Exposure to drinking water levels above 4.0 mg/l for many years may 
result in some cases of crippling skeletal fluorosis, which is a serious 
bone disorder.
    Federal law also requires that we notify you when monitoring 
indicates that the fluoride in your drinking water exceeds 2.0 mg/l. 
This is intended to alert families about dental problems that might 
affect children under nine years of age. The fluoride concentration of 
your water exceeds this federal guideline.
    Fluoride in children's drinking water at levels of approximately 1 
mg/l reduces the number of dental cavities. However, some children 
exposed to levels of fluoride greater than about 2.0 mg/l may develop 
dental fluorosis. Dental fluorosis, in its moderate and severe forms, is 
a brown staining and/or pitting of the permanent teeth.
    Because dental fluorosis occurs only when developing teeth (before 
they erupt from the gums) are exposed to elevated fluoride levels, 
households without children are not expected to be affected by this 
level of fluoride. Families with children under the age of nine are 
encouraged to seek other sources of drinking water for their children to 
avoid the possibility of staining and pitting.
    Your water supplier can lower the concentration of fluoride in your 
water so that you will still receive the benefits of cavity prevention 
while the possibility of stained and pitted teeth is minimized. Removal 
of fluoride may increase your water costs. Treatment systems are also 
commercially available for home use. Information on such systems is 
available at the address given below. Low fluoride bottled drinking 
water that would meet all standards is also commercially available.
    For further information, contact \2\ at your water system.

    \1\ PWS shall insert the compliance result which triggered 
notification under this part.
    \2\ PWS shall insert the name, address, and telephone number of a 
contact person at the PWS.


    (c) The effective date of this section is May 2, 1986.

[51 FR 11412, Apr. 2, 1986; 51 FR 24329, July 3, 1986, as amended at 52 
FR 41550, Oct. 28, 1987]



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.

[[Page 561]]

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  [Reserved]
144.16  Waiver of requirement by Director.
144.17  Records.

        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.

    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.



                      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

[[Page 562]]

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.
    (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.
    (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.

[[Page 563]]

    (g) Scope of the permit or rule requirement. The UIC Permit Program 
regulates underground injections by five classes of wells (see 
definition of ``well injection,'' Sec. 144.3). The five 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 142 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). Class V wells will be inventoried and 
assessed and regulatory action will be established at a later date.

In the meantime, if remedial action appears necessary, an individual 
permit may be required (Sec. 144.25) or the Director must require 
remedial action or closure by order (Sec. 144.12(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, even 
if it has not been ``identified.'' The Director may also designate 
``exempted aquifers'' using criteria in Sec. 146.04. 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 in Sec. 144.7. Aquifers which do not fit the definition 
of ``underground sources of drinking water'' are not ``exempted 
aquifers.'' They are simply not subject to the special protection 
afforded USDWs.
    (1) Specific inclusions. The following wells are included among 
those types by 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 septic tank or cesspool used by generators of hazardous 
waste, or by owners or operators of hazardous waste management 
facilities, to dispose of fluids containing hazardous waste.
    (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 which is not used for emplacement of fluids 
underground.
    (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

[[Page 564]]

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]



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 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.
    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.''

[[Page 565]]

    Drilling mud means a heavy suspension used in drilling an 
``injection well,'' introduced down the drill pipe and through the drill 
bit.
    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 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''
    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.

[[Page 566]]

    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 into or out of a formation through a borehole or well penetrating 
that formation.
    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.
    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.).
    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.
    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.
    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.

[[Page 567]]

    USDW means ``underground source of drinking water.''
    Well means a bored, drilled or driven shaft, or a dug hole, whose 
depth is greater than the largest surface dimension.
    Well injection means the subsurface 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.

[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]



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]



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).

[[Page 568]]

    (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.
    (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 Classes I, II, III, or 
IV.

[48 FR 14189, Apr. 1, 1983, as amended at 52 FR 20676, June 2, 1987]



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, except where 
exempted under paragraph (b) of this section, as an underground source 
of drinking water, all aquifers or parts of aquifers which meet the 
definition of an ``underground source of drinking water'' in Sec. 144.3. 
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 40 CFR 
146.04.

[[Page 569]]

    (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.
    (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 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.



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.
    (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.

[[Page 570]]

    (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 Secs. 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 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.
    (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

[[Page 571]]

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.



                 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 and III 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 Secs. 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.
    (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]

[[Page 572]]



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 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]



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:
    (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.

[[Page 573]]

    (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  [Reserved]



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]



        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 Secs. 144.25, 144.31, 144.33 or 144.34; after plugging and 
abandonment in accordance with an approved plugging and abandonment plan 
pursuant to Secs. 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 Secs. 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

[[Page 574]]

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 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 Secs. 144.25, 144.31, 144.33 or 144.34; after plugging and 
abandonment in accordance with an approved plugging and abandonment plan 
pursuant to Secs. 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 Secs. 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; 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]

[[Page 575]]



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 Secs. 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.

[49 FR 20181, May 11, 1984, as amended at 60 FR 33932, June 29, 1995]



Sec. 144.24  Class V wells.

    (a) A Class V injection well is authorized by rule until further 
requirements under future regulations become applicable.
    (b) Duration of well authorization by rule. Well authorization under 
this section expires upon the effective date of a permit issued pursuant 
to Secs. 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 Secs. 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]



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

[[Page 576]]

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 specified in paragraph (d) or (e) 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:
    (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 [Sec. 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. Except as provided in paragraph (e) of this section. 
(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.

[[Page 577]]

    (e) Deadlines for Class V Wells (EPA-administered programs only). 
(1) The owner or operator of a Class V well in which injection took 
place within one year after the date at which a UIC program authorized 
under the SDWA first became effective, and who failed to submit 
inventory for the well within the time specified in paragraph (d) of 
this section may resume injection 90 days after submittal of the 
inventory information to the Director unless the owner or operator 
receives notice that injection may not resume or may resume sooner.
    (2) The owner or operator of a Class V well in which injection 
started after the first anniversary date at which a UIC program 
authorized under the SDWA became effective, shall submit inventory 
information no later than one year after May 2, 1994.
    (3) The owner or operator of a Class V well in which injection will 
start after May 2, 1994, shall submit inventory information prior to 
starting injection.
    (4) The owner or operator of a Class V injection well prohibited 
from injecting for failure to submit inventory information for the well 
within the time specified in paragraphs (e) (2) and (3) of this section, 
may resume injection 90 days after submittal of the inventory 
information to the Director unless the owner or operator receives notice 
from the Director that injection may not resume or may resume sooner.

[48 FR 14189, Apr. 1, 1983, as amended at 49 FR 20182, May 11, 1984; 58 
FR 63896, Dec. 3, 1993]



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;
    (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 Secs. 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 
Secs. 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

[[Page 578]]

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 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 Secs. 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

[[Page 579]]

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 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 
Secs. 144.28(c) and 146.10, and a

[[Page 580]]

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 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

[[Page 581]]

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 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:

[[Page 582]]

    (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
    (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

[[Page 583]]

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.
    (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 permits shall 
provide the following information to the Director, using the application 
form provided by the Director.
    (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

[[Page 584]]

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.
    (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]



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

[[Page 585]]

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;
    (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;

[[Page 586]]

    (3) Operated by a single owner or operator; and
    (4) Used to inject other than hazardous waste.
    (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.



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
    (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 
Secs. 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

[[Page 587]]

rights, or any infringement of State or local law or regulations.



Sec. 144.36  Duration of permits.

    (a) Permits for Class I and Class 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. The Director shall review each issued Class II or III 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 Secs. 144.39, 144.40, and 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.



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.
    (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 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

[[Page 588]]

the date specified in the agreement mentioned in paragraph (b)(2) of 
this section.



Sec. 144.39  Modification or revocation and reisssuance 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 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, or 
Class III 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, or Class III wells may be modified during their 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).
    (b) Causes for modification or revocation and reissuance. The 
following are

[[Page 589]]

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 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]



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).



                      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

[[Page 590]]

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.
    (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

[[Page 591]]

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
    (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.
    (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 592]]

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 insure 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 it 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. 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 or III well permitted under this part 
shall establish prior to commencing injection or on a schedule 
determined by the Director, and thereafter maintain mechanical integrity 
as defined in Sec. 146.8 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, or III well 
lacks mechanical integrity pursuant to Sec. 146.8 of this chapter, he 
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 
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 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

[[Page 593]]

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]



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), Sec. 144.52 (a)(7) and (a)(9), and subpart G 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 Secs. 144.55 and 146.7
    (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:
    (A) The well has been plugged and abandoned in accordance with an 
approved plugging and abandonment plan pursuant to Secs. 144.51(o) and 
146.10 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

[[Page 594]]

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.
    (8) Mechanical integrity. A permit for any Class I, II or III 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. 146.08 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 (except as provided in Sec. 124.86(c) for UIC 
permits being processed under subpart E or F of part 124). 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]



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.
    (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

[[Page 595]]

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 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,

[[Page 596]]

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 Secs. 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 Secs. 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 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.

[[Page 597]]

    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 
Secs. 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.
    (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:

[[Page 598]]

    (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 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

[[Page 599]]

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 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).

[[Page 600]]

    (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
    (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

[[Page 601]]

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
    (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

[[Page 602]]

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 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

[[Page 603]]

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
    (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

[[Page 604]]

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
    (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.

[[Page 605]]

    (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 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

[[Page 606]]

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 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

[[Page 607]]

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.
    (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:

[[Page 608]]

                             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, 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:

[[Page 609]]

    (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 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.

[[Page 610]]

    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:

                                 [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

[[Page 611]]

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 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).

[[Page 612]]

    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 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

[[Page 613]]

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, 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

[[Page 614]]

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 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

[[Page 615]]

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]
[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.]

[[Page 616]]

    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]



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.

[[Page 617]]

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 
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.

[48 FR 14202, Apr. 1, 1983, as amended at 53 FR 37412, Sept. 26, 1988; 
59 FR 64345, Dec. 14, 1994]



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

[[Page 618]]

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); and
    (31) Section 124.17 (a) and (c)--(Response to comments).
    (b)(1) States need not implement provisions identical to the 
provisions listed in paragraphs (a) (1) through (31) 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).



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:

[[Page 619]]

    (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 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

[[Page 620]]

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 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.

[[Page 621]]

    (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 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.

[48 FR 14202, Apr. 1, 1983, as amended at 53 FR 37412, Sept. 26, 1988]



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. 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;

[[Page 622]]

    (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.



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. The 
program description shall include:
    (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.
    Note: States are encouraged to use uniform national forms 
established by the Administrator. If uniform national forms are used, 
they may be modified to include the State Agency's name, address, logo, 
and other similar information, as appropriate, in place of EPA's.
    (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 part 144;
    (2) The priorities (according to criteria set forth in 40 CFR 
146.09) for issuing permits, including the number

[[Page 623]]

of permits in each class of injection well which will be issued each 
year during the first five years of program operation;
    (3) A description of how the Director will implement the mechanical 
integrity testing requirements of 40 CFR 146.08, 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 and 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;
    (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 Secs. 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;
    (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.



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.

[[Page 624]]

    (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 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;

[[Page 625]]

    (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 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.

[[Page 626]]

    (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.



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:
    (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

[[Page 627]]

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.
    (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:

[[Page 628]]

    (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 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

[[Page 629]]

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.

     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.

     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.

    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.

    Editorial Note: 1. For a rule-related notice affecting part 146, see 
52 FR 26342, July 14, 1987.

    2. For a document removing the OMB control number wherever it 
appeared in part 146, see 58 FR 34370, June 25, 1993.



                      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.

[[Page 630]]

    (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.
    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.
    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.

[[Page 631]]

    Disposal well means a well used for the disposal of waste into a 
subsurface stratum.
    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).
    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.''
    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 
(Secs. 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

[[Page 632]]

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.
    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.).
    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.).
    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.
    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.
    USDW means ``underground source of drinking water.''
    Well means a bored, drilled or driven shaft, or a dug hole, whose 
depth is greater than the largest surface dimension.
    Well injection means the subsurface 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 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.

[[Page 633]]

    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]



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 40 CFR 144.8 to be an ``exempted aquifer'' if it meets the 
following criteria:
    (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.

(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]



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.
    (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

[[Page 634]]

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, or 
IV. 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 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.

[45 FR 42500, June 24, 1980, as amended at 46 FR 43161, Aug. 27, 1981; 
47 FR 4999, Feb. 3, 1982]



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,

[[Page 635]]

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)
=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;
    (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

[[Page 636]]

    (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 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]

[[Page 637]]



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-III wells.

    (a) Prior to abandoning Class I to 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 he 
is satisfied that such materials will prevent movement of fluids into or 
between underground sources of drinking water.
    (b) Placement of the cement plugs shall be accomplished by one of 
the following:
    (1) The Balance method;
    (2) The Dump Bailer method;
    (3) The Two-Plug method; or
    (4) An alternative method approved by the Director, which will 
reliably provide a comparable level of protection to underground sources 
of drinking water.
    (c) 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).
    (d) The plugging and abandonment plan required in 40 CFR 
144.52(a)(6) and 144.51(n) shall, in the case of a Class III project 
which underlies or is in an aquifer which has been exempted under 40 CFR 
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.

(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 5000, Feb. 3, 1982; 48 
FR 14293, Apr. 1, 1983]



      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;

[[Page 638]]

    (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.
    (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:

[[Page 639]]

    (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.
    (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

[[Page 640]]

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:
    (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;

[[Page 641]]

    (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
    (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]



     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.

[[Page 642]]

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 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

[[Page 643]]

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 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;

[[Page 644]]

    (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;
    (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

[[Page 645]]

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
    (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

[[Page 646]]

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 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;

[[Page 647]]

    (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;
    (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.

[[Page 648]]

    (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 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.

[[Page 649]]

    (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 Secs. 144.55 and 146.07.
    (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

[[Page 650]]

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;
    (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

[[Page 651]]

    (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.
    (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;

[[Page 652]]

    (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;
    (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,

[[Page 653]]

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;
    (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.

[[Page 654]]

    (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.
    (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

[[Page 655]]

    (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;
    (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

[[Page 656]]

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;
    (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 Secs. 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

[[Page 657]]

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;
    (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.

[[Page 658]]

    (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, 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.

[[Page 659]]

    (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 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.



PART 147--STATE 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.
147.60  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]

[[Page 660]]

                           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.

                             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. [Reserved]
147.901  EPA-administered program.
147.902  Aquifer exemptions. [Reserved]
147.903  Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.904  Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
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.

[[Page 661]]

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.
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 and V 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.

[[Page 662]]

                          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.
147.2152  Aquifer exemptions. [Reserved]
147.2153  Existing Class I, II (except enhanced recovery and hydrocarbon 
          storage) and III wells authorized by rule.
147.2154  Existing Class II enhanced recovery and hydrocarbon storage 
          wells authorized by rule.
147.2155  Requirements for all wells--area of review.

                            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.

                          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.

[[Page 663]]

                            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.
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--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.


[[Page 664]]


    Authority: 42 U.S.C. 300h; and 42 U.S.C. 6901 et seq.

    Source: 49 FR 20197, May 11, 1984, unless otherwise noted.



                      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.
    (b) The applicable UIC program for a State is either a State-
administered program approved by EPA, or a federally-administered 
program promulgated by EPA. In some cases, the UIC program may consist 
of a State-administered program applicable to some classes of wells and 
a federally-administered program applicable to other classes of wells. 
Approval of a State program is based upon a determination by the 
Administrator that the program meets the requirements of section 1422 or 
section 1425 of the Safe Drinking Water Act and the applicable 
provisions of parts 124, 144, and 146 of this chapter. A federally-
administered program is promulgated in those instances where the state 
has failed to submit a program for approval or where the submitted 
program does not meet the minimum statutory and regulatory requirements.
    (c) In the case of State programs approved by EPA pursuant to 
section 1422 of the SDWA, each State subpart describes the major 
elements of such programs, including State statutes and regulations, 
Statement of Legal Authority, Memorandum of Agreement, and Program 
Description. State 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 Office of the Federal Register Information Center, Room 8301, 
800 North Capitol Street, NW., suite 700, Washington, DC. Other State 
statutes and regulations containing standards and procedures that 
constitute elements of the State 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 State programs promulgated under section 1422 
that are to be administered by EPA, the State subpart makes applicable 
the provisions of parts 124, 144, and 146, and provides additional 
requirements pertinent to the specific State program.
    (e) Regulatory provisions incorporated by reference (in the case of 
approved State 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) The information requirements located in the following sections 
have been cleared by the Office of Management and Budget: Sections 
147.104, 147.304, 147.754, 147.904, 147.1154, 147.1354, 147.1454, 
147.1654, 147.1954, and 147.2154.
    The OMB clearance number is No. 2040-0042.



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

[[Page 665]]

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 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]

[[Page 666]]



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, 
Secs. 31.05.005 through 31.30.010 (1979 and Cum. Supp. 1984);
    (2) Alaska Statutes, Administrative Procedures Act, Title 44, 
Secs. 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.
    (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 Secs. 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 Secs. 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

[[Page 667]]

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 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 Secs. 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 668]]

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, is administered 
by EPA. The UIC program for Navajo Indian lands 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 is 
November 25, 1988.

[53 FR 43086, Oct. 25, 1988, as amended at 56 FR 9412, Mar. 6, 1991]



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;

[[Page 669]]

    (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]



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, Secs. 3000-3359 
(1989);
    (2) California Administrative Code, title 14, Secs. 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

[[Page 670]]

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.



                           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 Office of the Federal Register, 800 North Capitol 
Street NW., suite 700, Washington, DC.
    (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

[[Page 671]]

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 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 Secs. 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:


[[Page 672]]


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 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 Secs. 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;

[[Page 673]]

    (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 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, John F. 
Kennedy Federal Building, room 2203, Boston, Massachusetts, 02203, or at 
the Office of the Federal Register, 800 North Capitol Street NW., suite 
700, Washington, DC.
    (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).

[[Page 674]]

    (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]



Secs. 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]



Secs. 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 Office of the Federal 
Register, 800 North Capitol Street NW., suite 700, Washington, DC.
    (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]

[[Page 675]]



Secs. 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]



Secs. 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 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;

[[Page 676]]

    (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]



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.

[[Page 677]]

    (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 Secs. 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 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 Office of the Federal Register, 
800 North Capitol Street NW., suite 700, Washington, DC.
    (1) Oil and Gas and Deep Drilling Act of 1975, Official Code of 
Georgia Annotated (O.C.G.A.) Secs. 12-4-40 through 12-4-53 (1988);
    (2) Ground Water Use Act of 1972, O.C.G.A. Secs. 12-5-90 through 12-
5-107 (1988);
    (3) Water Well Standards Act of 1985, O.C.G.A. Secs. 12-5-120, 
through 12-5-138 (1988);
    (4) Georgia Administrative Procedure Act, O.C.G.A. Secs. 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. Secs. 12-5-20 
through 12-5-53 (1988);
    (6) Georgia Hazardous Waste Management Act, O.C.G.A. Secs. 12-8-60 
through 12-8-83 (1988);
    (7) Georgia Safe Drinking Water Act of 1977, O.C.G.A. Secs. 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).

[[Page 678]]

    (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]



Secs. 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]



Secs. 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);

[[Page 679]]

    (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 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

[[Page 680]]

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. 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:

[[Page 681]]

    (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 Office of the 
Federal Register, 800 North Capitol Street NW., suite 700, Washington, 
DC.
    (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).
    (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]

[[Page 682]]



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.
    (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, Forbes Field, Building 740, 
Topeka, Kansas, 66620. Copies may be inspected at the Environmental 
Protection Agency, Region VII, 726 Minnesota Avenue, Kansas City, 
Kansas, 66101, or at the Office of the Federal Register, 800 North 
Capitol Street, NW., suite 700, Washington, DC.
    (1) Chapter 28, Article 46, Underground Injection Control 
Regulations, Kansas Administrative Regulations Secs. 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 Secs. 28-43-1 through 28-43-10 (1986);
    (3) Kansas Statutes Annotated Secs. 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 Secs. 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]



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]



Secs. 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

[[Page 683]]

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. [Reserved]



Sec. 147.901  EPA-administered program.

    (a) Contents. The UIC program for the Commonwealth of Kentucky, 
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 in the remainder of Kentucky is June 25, 1984.

[53 FR 43087, Oct. 25, 1988, as amended at 56 FR 9415, Mar. 6, 1991]



Sec. 147.902  Aquifer exemptions. [Reserved]



Sec. 147.903  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. 147.904  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 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.

[[Page 684]]

    (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 Secs. 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 and the casing 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. 147.905  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);
    (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

[[Page 685]]

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 (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

[[Page 686]]

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 Office of the Federal Register, 800 North Capitol 
Street, NW., suite 700, Washington, DC.
    (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 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]

[[Page 687]]



Secs. 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]



Secs. 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 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]

[[Page 688]]



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 Secs. 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)

[[Page 689]]

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.



                          Supbart 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.
    (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.

[[Page 690]]

    (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 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



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

[[Page 691]]

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, Secs. 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);
    (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]

[[Page 692]]



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 Office of the Federal Register, 800 North Capitol Street, NW, 
Suite 700, Washington, D.C.
    (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.''
    (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 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 693]]

and operators, and EPA shall comply with these requirements.
    (b) Effective dates. The effective date for the UIC program on all 
lands in Montana, including all Indian lands, is June 25, 1984.

[52 FR 17681, May 11, 1987, as amended at 56 FR 9417, Mar. 6, 1991; 61 
FR 58933, Nov. 19, 1996]



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 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 Secs. 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.

[[Page 694]]

    (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.

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:

                          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.

[[Page 695]]

    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.
    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.

[[Page 696]]

    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.
    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.

[[Page 697]]

    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:
    (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

[[Page 698]]

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 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]

[[Page 699]]



                           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 Office of the Federal Register, 800 North Capitol Street NW., suite 
700, Washington, DC.
    (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]



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:


[[Page 700]]


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 Secs. 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) 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

[[Page 701]]

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 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)

[[Page 702]]

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 10-1-78), 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]

[[Page 703]]



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]



Sec. 147.1603  EPA-administered program--Indian lands.

    (a) Contents. The UIC program for all classes of wells on Indian 
lands in New Mexico 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 is November 25, 1988.

[53 FR 43089, Oct. 25, 1988]



                          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

[[Page 704]]

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 Secs. 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 Secs. 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 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 Secs. 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:

[[Page 705]]

    (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.
    (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 Office of the Federal Register, 800 
North Capitol Street, NW., suite 700, Washington, DC.

[[Page 706]]

    (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. Secs. 87-
83 through 87-99 (1989 and Cumm. Supp. 1989);
    (3) Water and Air Resources, N.C. GEN. STAT. Secs. 143-211 through 
143-215.10 (1987 and Cumm. Supp. 1989);
    (4) Solid Waste Management, N.C. GEN. STAT. Secs. 130A-290 through 
130A-309.03 (1989);
    (5) North Carolina Drinking Water Act, N.C. GEN. STAT. Secs. 130A-
311 through 130A-332 (1989);
    (6) Sanitary Sewage Systems, N.C. GEN. STAT. Secs. 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]



Secs. 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]



Secs. 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

[[Page 707]]

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 and V wells.

    The UIC program for Class I, III, IV, and V wells in the State of 
North Dakota, except those on Indian lands, is the program administered 
by the North Dakota Department of Health, approved by EPA pursuant to 
section 1422 of the SDWA. Notice of this approval was published in the 
Federal Register on September 21, 1984; the effective date of this 
program is October 5, 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 Dakota. This incorporation by 
reference was approved by the Director of the Federal Register effective 
October 5, 1984.
    (1) North Dakota Century Code Sections 38-12-01, 38-12-03 (1980);
    (2) North Dakota Century Code, Sections 61-28-02 and 61-28-06 
(1989);
    (3) North Dakota Administrative Code Sections 33-25-01-01 through 
33-25-01-18 (North Dakota State Health Department Underground Control 
Program) (1983);
    (4) North Dakota Administrative Code, Chapter 43-02-02 (Subsurface 
Mineral Exploration and Development) (August 1986), and Chapter 43-02-
02.1 (Underground Injection Control Program) (March 1, 1984);
    (5) North Dakota Administrative Code Sections 43-02-02-1-01 through 
43-02-02-1-18 (North Dakota Geological Survey--Undergound Injection 
Control Program) (1984);
    (b) Other laws. 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.

[49 FR 37066, Sept. 21, 1984, as amended at 56 FR 9418, Mar. 6, 1991]



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]

[[Page 708]]



                            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).
    (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.

[[Page 709]]

    (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 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

[[Page 710]]

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 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

[[Page 711]]

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, 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 Secs. 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

[[Page 712]]

provisions of Secs. 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 (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.

[[Page 713]]

    (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 Secs. 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.



                        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.

[[Page 714]]

    (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]



                       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,

[[Page 715]]

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.
    (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.

[[Page 716]]

    (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 Secs. 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 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

[[Page 717]]

that the owner or operator of an existing enhanced recovery or 
hydrocarbon storage well may not be in compliance with the requirement 
of Secs. 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.
    (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.

[[Page 718]]


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. [Reserved]



Sec. 147.2151  EPA-administered program.

    (a) Contents. The UIC program for the State of Tennessee, 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. 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]



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.



Sec. 147.2154  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 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 
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 Secs. 144.28(e) and 146.22, the owner or operator shall 
comply with paragraphs (b) (1) through (4)

[[Page 719]]

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) of this section, as needed to protect USDWs.



Sec. 147.2155  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 SS--Texas



Sec. 147.2200  State-administered program--Class I, III, IV, and V wells.

    Requirements for 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, is the State-administered program approved by EPA 
pursuant to section 1422 of the SDWA. Notice of this approval was 
published on January 6, 1982 (47 FR 618); the effective date of this 
program is February 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 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 sections 27.002, 27.011 
(Vernon Supp. 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 UIC program:
    (1) Texas Water Code Annotated, Chapter 5 (Vernon 1972 and Supp. 
1982);
    (2) Injection Well Act, Texas Water Code Annotated, Chapter 27 
(Vernon 1972 and Supp. 1982);
    (3) Rules of Texas Department of Water Resources, Chapter 27; Rules 
of Texas Water Development Board, Chapter 22.
    (c) The Memorandum of Agreement between EPA Region VI and the Texas 
Department of Water Resources, signed by the EPA Regional Administrator 
on October 11, 1981.
    (d) Statement of legal authority. ``Underground Injection Control 
Program--Attorney General's Statement for Class I, III, IV, and V 
Injection Wells,'' signed by the Attorney General of Texas, June 11, 
1981.
    (e) The Program Description and any other materials submitted as 
part of the application or as supplements thereto.
    (f) Certain Class V wells are under the UIC program of the Texas 
Railroad Commission approved on April 23, 1982, under the authorities 
cited in Sec. 147.2201 of this part.

[49 FR 20197, May 11, 1984, as amended at 53 FR 43091, Oct. 25, 1988]



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

[[Page 720]]

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 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

[[Page 721]]

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 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

[[Page 722]]

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 is administered by EPA. The program for wells 
on the lands of the Navajo and 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 (as well as for the program of the Navajo and 
Ute Mountain Ute) is November 25, 1988.

[53 FR 40391, Oct. 25, 1988, as amended at 56 FR 9420, Mar. 6, 1991] h



                           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).

[[Page 723]]

    (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]



Secs. 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.
    (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]



Secs. 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 this paragraph are hereby 
incorporated by reference and made a part of the applicable UIC program 
under the SDWA for the State of Washington. This incorporation by 
reference was approved by the Director of the Federal Register effective 
September 24, 1984.
    (1) Revised Code of Washington section 90.48.020, 90.48.080, 
90.48.160, and 90.48.162 (Bureau of National Affairs, 1983 Laws);
    (2) Washington Administrative Code sections 173-218-010 to 173-218-
110 (Bureau of National Affairs, 2/29/84);
    (3) Washington Administrative Code sections 344-12-001 to 344-12-262 
(1983 Ed.)
    (4) Washington Administrative Code Chapter 173-160 (reprinted May 
1988).

[[Page 724]]

    (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 May 14, 1984;
    (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;
    (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]



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, 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

[[Page 725]]

plug and abandon the well according to the approved plan and schedule.

[53 FR 43091, Oct. 25, 1988]



                        Subpart XX--West Virginia



Secs. 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]



Secs. 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 Office 
of the Federal Register, 800 North Capitol Street, NW., suite 700, 
Washington, DC.
    (1) Wisconsin Statutes Annotated Secs. 147.015, 147.02 and 147.04 
(West 1974 and Supp. 1983);
    (2) Chapter NR 112, Well Construction and Pump Installation, 
Wisconsin Administrative Code Secs. 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 Secs. 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 Secs. 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 
Secs. 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:
    (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);

[[Page 726]]

    (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 727]]

    (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 Office 
of the Federal Register, 800 North Capitol Street, NW., suite 700, 
Washington, DC.
    (1) Rules and Regulations of the Wyoming Oil and Gas Conservation 
Commission, including Rules of Practice 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

[[Page 728]]

(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 Secs. 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 729]]



            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]



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
------------------------------------------------------------------------
           Formation              Approx. depth           Location
------------------------------------------------------------------------
Powder River Basin, only        3,800 to 6,800     Two cylindrical
 approximately 0.4 square        feet from          volumes with centers
 miles of the Lance Formation    surface.           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.
------------------------------------------------------------------------

[64 FR 14803, Mar. 26, 1999]

[[Page 730]]



                            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).
    (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]

[[Page 731]]



                        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 
Street, SW., room E1101A, Washington, DC 20460; or the Office of the 
Federal Register, 800 North Capitol Street NW., suite 700, Washington, 
DC.
    (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.
    (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]

[[Page 732]]



                       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.
    (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]

[[Page 733]]



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.



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.

[[Page 734]]

    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.
    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.

[[Page 735]]

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 Secs. 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 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

[[Page 736]]

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.
    (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

[[Page 737]]

    (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 Secs. 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/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

[[Page 738]]

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:
    (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

[[Page 739]]

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.



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 Secs. 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

[[Page 740]]

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;
    (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.

[[Page 741]]



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
    (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

[[Page 742]]

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)



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.

[[Page 743]]

    (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 
Secs. 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 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.

[[Page 744]]

    (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.
    (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.

[[Page 745]]



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.
    (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:

[[Page 746]]

    (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.
    (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

[[Page 747]]

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, 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 the Indian lands of the Navajo, 
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.

[[Page 748]]

    (b) Effective date. The effective date for the UIC program on these 
lands is November 25, 1988.

[53 FR 43104, Oct. 25, 1988, as amended at 56 FR 9422, Mar. 6, 1991]



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 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 
Secs. 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 Secs. 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.

[[Page 749]]



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 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

[[Page 750]]

    (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.
    (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.

[[Page 751]]

    (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.

       Appendix A to Subpart HHH--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 752]]



--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                         Sec.                                                                              Well 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

[[Page 753]]

 
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
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

[[Page 754]]

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

[[Page 755]]

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

[[Page 756]]

 
                                       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 757]]



          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 Secs. 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 Secs. 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 758]]



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 759]]

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.



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.

[[Page 760]]

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.



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.

[[Page 761]]

    (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:
    (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;

[[Page 762]]

    (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 
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,

[[Page 763]]

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 
(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 Secs. 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 Secs. 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.

[[Page 764]]

    (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, 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

[[Page 765]]

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.
    (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) Effective November 4, 1998, the wastes specified in 40 CFR 
261.32 as EPA Hazardous Waste number K140, and in 40 CFR 261.33(f) as 
EPA Hazardous Waste number U408 are prohibited from injection.
    (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.

[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]



              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

[[Page 766]]

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 
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

[[Page 767]]

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 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 Secs. 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

[[Page 768]]

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
    (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

[[Page 769]]

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 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

[[Page 770]]

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 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;

[[Page 771]]

    (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).
    (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.

[[Page 772]]



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 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

[[Page 773]]

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 775]]



                              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.

  Material Approved for Incorporation by Reference
  Table of CFR Titles and Chapters
  Alphabetical List of Agencies Appearing in the CFR
  List of CFR Sections Affected

[[Page 777]]

            Material Approved for Incorporation by Reference

                      (Revised as of July 1, 1999)

  The Director of the Federal Register has approved under 5 U.S.C. 
552(a) and 1 CFR Part 51 the incorporation by reference of the following 
publications. This list contains only those incorporations by reference 
effective as of the revision date of this volume. Incorporations by 
reference found within a regulation are effective upon the effective 
date of that regulation. For more information on incorporation by 
reference, see the preliminary pages of this volume.


40 CFR (PARTS 136 TO 149)

ENVIRONMENTAL PROTECTION AGENCY
                                                                  40 CFR


American National Standards Institute

  11 West 42nd Street, New York, NY 10036; 
  Telephone: (212) 642-4900
American National Standard on Photographic           136.3(a) Table IB, 
  Processing Effluents, April 2, 1975.                            Note 9


American Public Health Association

  800 I Street NW., Washington, DC 20001-3710; 
  Telephone: (202) 777-APHA
    Standard Methods for the Examination of Water and Wastewater, Joint 
    Editorial Board, American Public Health Association, American 
    Waterworks Association, and Water Environment Control Federation:
18th Edition, 1992................................ 136.3, Tables IA, IB, 
                                                           IC, ID and IE
15th Edition, 1980................................   136.3(a) Table IB, 
                                                       Note 30; Table ID
14th Edition, 1975................................   136.3(a) Table IB, 
                                                         Notes 17 and 27
Selected Analytical Methods Approved and Cited by    136.3(a) Table IB, 
  the United States Environmental Protection         Note 10; Table IC, 
  Agency, Supplement to the 15th Edition of           Note 6; Table ID, 
  Standard Methods for the Examination of Water                   Note 6
  and Wastewater, 1981.


American Society for Testing and Materials

  100 Barr Harbor Drive, West Conshohocken, PA 
  19428-2959; Telephone: (610) 832-9585, FAX: 
  (610) 832-9555
Annual Book of ASTM Standards--Water, Section 11,   136.3(a) Tables IB, 
  Volumes 11.01 and 11.02, 1993.                          IC, ID, and IE
Annual Book of ASTM Standards, Water and           136.3, Tables IB, IC, 
  Environmental Technology, Section 11, Volumes               ID, and IE
  11.01 and 11.02, 1994.


AOAC International (Association of Official Analytical Chemists)

  481 N. Frederick Ave., Suite 500, Gaithersburg, 
  MD 20877-2407; Telephone: (301) 924-7077
Official Methods of Analysis of the Association of   136.3(a) Table IB, 
  Official Analytical Chemists, 15th Edition                      Note 3
  (1990).


Bran & Luebbe Analyzing Technologies, Inc.

  Elmsford, NY 10523

[[Page 778]]

Hydrogen Ion (pH) Automated Electrode Method,        136.3(a) Table IB, 
  Industrial Method Number 378-75WA, October 1976,               Note 21
  Bran & Luebbe (Techicon) Auto Analyzer II.


CEM Corporation

  P.O. Box 200, Matthews, North Carolina 28106-
  0200
Closed Vessel Microwave Digestion of Wastewater      136.3(a) Table IB, 
  Samples for Determination of Metals, April 16,                 Note 36
  1992.


Fisons Instruments, Inc

  32 Commerce Center, Cherry Hill Drive, Danvers, 
  MA 01923
Direct Current Plasma (DCP) Optical Emission         136.3(a) Table IB, 
  Spectrometric Method for Trace Elemental                       Note 34
  Analysis of Water and Wastes, Method AES0029, 
  1986, revised 1991.


Hach Chemical Company

  P.O. Box 389, Loveland, CO 80537
1, 10-Phenanthroline Method Using FerroVer Iron      136.3(a) Table IB, 
  Reagent for Water, Hach Method 8008, 1980.                     Note 22
Bicinchoninate Method for Copper, Method 8506,       136.3(a) Table IB, 
  Hach Handbook of Water Analysis, 1979.                         Note 19
Chemical Oxygen Demand, Method 8000, Hach Handbook   136.3(a) Table IB, 
  of Water Analysis, 1979.                                       Note 14
Nitrogen, Nitrite--Low Range, Diazotization Method   136.3(a) Table IB, 
  for Water and Wastewater, Hach Method 8507,                    Note 25
  1979.
Periodate Oxidation Method for Manganese, Method     136.3(a) Table IB, 
  8034, Hach Handbook for Water Analysis, 1979.                  Note 23
Zincon Method for Zinc, Method 8009, Hach Handbook   136.3(a) Table IB, 
  for Water Analysis, 1979.                                      Note 33


Journal of Chromatography

  Available from: Elsevier/North-Holland, Inc., 
  Journal Information Centre, 52 Vanderbilt 
  Avenue, New York, NY 10164
Direct Determination of Elemental Phosphorous by     136.3(a) Table IB, 
  Gas-Liquid Chromatography, by R.F. Addison and                 Note 28
  R.G. Ackman, Journal of Chromatography, Volume 
  47, No. 3, pp. 421-426, 1970.


National Council of the Paper Industry for Air and Stream Improvements, 
Inc.

  260 Madison Avenue, New York, NY 10016
An investigation of improved Procedures for          136.3(a) Table IB, 
  Measurement of Mill Effluent and Receiving Water               Note 18
  Color, NCASI Technical Bulletin No. 253, 
  December 1971.


Oceanography International Corporation

  512 West Loop, P.O. Box 2980, College Station, 
  TX 77840
OIC Chemical Oxygen Demand Method, 1978...........   136.3(a) Table IB, 
                                                                 Note 13


ORION Research Incorporated

  840 Memorial Dr., Cambridge, MA 02138
ORION Research Instruction Manual, Residual          136.3(a) Table IB, 
  Chlorine Electrode Model 97-70, 1977.                          Note 16


Perstorp Analytical Corporation

  1256 Stockton St., Helena, CA 94574
Nitrogen, Total Kjeldahl, Method PA1-Dk01, (Block   136.3(a), Table IB, 
  Digestion, Steam Distillation, Tritrimetric                    Note 39
  Detection), Revised December 22, 1994.
Nitrogen, Total Kjeldahl, Method PA1-Dk02, (Block   136.3(a), Table IB, 
  Digestion, Steam Distillation, Colorimetric                    Note 40
Detection), Revised December 22, 1994.
[[Page 779]]

Nitrogen, Total Kjeldahl, Method PA1-Dk03, (Block   136.3(a), Table IB, 
  Digestion, Steam Distillation, Automated FIA Gas               Note 41
  Diffusion), Revised December 22, 1994.


Technicon Industrial Systems

  Tarrytown, New York 10591
Ammonia, Automated Electrode Method, Industrial      136.3(a) Table IB, 
  Method Number 379-75WE, dated February 19, 1976,                Note 7
  Technicon Auto Analyzer II.


U.S. Environmental Protection Agency, ORD publications, CERI

  Cincinnati, OH 45268
Methods for Benzidine, Chlorinated Organic           136.3(a) Table IC, 
  Compounds, Pentachlorophenol and Pesticides in      Note 3; Table ID, 
  Water and Wastewater, U.S. Environmental                        Note 3
  Protection Agency, 1978.
Methods for Chemical Analysis of Water and Wastes,   136.3(a) Table IB, 
  U.S. Environmental Protection Agency, EPA-600/4-         Notes 1 and 4
  79-020, March 1979, or ``Methods for Chemical 
  Analysis of Water and Wastes,'' U.S. 
  Environmental Protection Agency, EPA-600/4-79-
  020, Revised March 1983.
Microbiological Methods for Monitoring the           136.3(a) Table IA, 
  Environment, Water and Wastes, U.S.                             Note 2
  Environmental Protection Agency, EPA-600/8-78-
  017, 1978.
Organochlorine Pesticides and PCBs in Wastewater            136.3(b)(33)
  Using Empore TM Disk, Revised October 28, 1994.
Prescribed Procedures for Measurement of             136.3(a) Table IE, 
  Radioactivity in Drinking Water, U.S.                           Note 1
  Environmental Protection Agency, EPA-600/4-80-
  032, 1980.


U.S. Environmental Protection Agency, Office of Water Resource Center

  Washington, DC 20460
Methods for Measuring the Acute Toxicity of                        136.3
  Effluents and Receiving Waters to Freshwater and 
  Marine Organisms, August 1993 (EPA 600/4-90/
  027F).
Errata (1999), Methods for Measuring the Acute                     136.3
  Toxicity of Effluents and Receiving Waters to 
  Freshwater and Marin Organisms, Fourth Edition, 
  August 1993 (EPA 600/4-90/027F).
Short-Term Methods for Estimating the Chronic                      136.3
  Toxicity of Effluents and Receiving Water to 
  Freshwater Organisms, Third Edition, July 1994 
  (EPA 600/4-91/002).
Errata (1999), Short-Term Methods for Estimating                   136.3
  the Chronic Toxicity of Effluents and Receiving 
  Water to Freshwater Organisms, Third Edition, 
  July 1994 (EPA 600/4-91/002).
Short-Term Methods for Estimating the Chronic                      136.3
  Toxicity of Effluents and Receiving Water to 
  Marine and Estuarine Organisms, Second Edition, 
  July 1994 (EPA 600/4-91/003.
Errata (1999), Short-Term Methods for Estimating                   136.3
  the Chronic Toxicity of Effluents and Receiving 
  Water to Marine and Estaurine Organisms, Second 
  Edition, July 1994 (EPA 600/4-91/003).
Method 1631, Revision B, Mercury in Water by                       136.3
  Oxidation, Purge and Trap, and Cold Vapor Atomic 
  Fluorescense Spectrometry, May 1999 (EPA-821-R-
  99-005).
Method 1664, Revision A, n-Hexane Extractable                      136.3
Material (HEM; Oil and Grease) and Silica Gel 
[[Page 780]]exane Extractable Material (SGT-HEM; 
  Non-polar material) by Extraction and 
  The following standard is available from: 
  National Technical Information Service, 5285 
  Port Royal Road, Springfield, VA 22161
EPA-821-B-98-016, Analytical Methods for the                       136.3
  Determination of Pollutants in Pharmaceutical 
  Manufacturing Industry Wastewater, July 1998.


U.S. Geological Survey

  Denver Federal Center, Box 25425, Denver, CO 
  80225
Methods for Collection and Analysis of Aquatic         136.3(a) Table IA
  Biological and Microbiological Samples, edited 
  by Britton, L.J. and P.E. Greason, Techniques of 
  Water-Resources Investigations of the U.S. 
  Geological Survey, Book 5, Chapter A1 (1989).
Methods for Determination of Inorganic Substances    136.3(a) Table IB, 
  in Water and Fluvial Sediments, N.W. Skougstad                  Note 8
  and others, editors, Techniques of Water-
  Resources Investigations of the U.S. Geological 
  Survey, Book 5, Chapter A1 (1979).
Methods for Determination of Inorganic Substances    136.3(a) Table IB, 
  in Water and Fluvial Sediments, M.J. Fishman and                Note 2
  Linda C. Friedman, Techniques of Water-Resources 
  Investigations of the U.S. Geological Survey, 
  Book 5, Chapter A1 (1989).
Methods for the Determination of Organic             136.3(a) Table IB, 
  Substances in Water and Fluvial Sediments,         Note 24; Table ID, 
  Wershaw, R.L., et al, Techniques of Water-                      Note 4
  Resources Investigations of the U.S. Geological 
  Survey, Book 5, Chapter A3 (1987).
Selected Methods of the U.S. Geological Survey of    136.3(a) Table IE, 
  Analysis of Wastewaters, by M.J. Fishman and                    Note 2
  Eugene Brown; U.S. Geological Survey Open File 
  Report 76-77 (1976).
Water Temperature--Influential Factors, Field        136.3(a) Table IB, 
  Measurement and Data Presentation, by H.H.                     Note 32
  Stevens, Jr., J. Ficke, and G.F. Smoot, 
  Techniques of Water-Resources Investigations of 
  the U.S. Geological Survey, Book 1, Chapter D1, 
  1975.


40 CFR (PART 141): WATER PROGRAMS
American Public Health Association, American Water Works Association, 
Water Pollution Control Federation

  Available from American Public Health 
  Association, 800 I Street NW., Washington, DC 
  20001-3710; Telephone: (202) 777-APHA
Selected Analytical Methods Approved and Cited by the United States 
  Environmental Protection Agency, Supplement to the 16th Edition of 
  Standards Methods for the Examination of Water and Wastewater, 1985:
  Methods 908C pp. 878-880; 908D pp. 880-882; 909C pp. 896-898;141.74(a) 
  872-876; 908B pp. 876-878; 908D pp. 880-882; 909A pp. 887-894; 909B 
  pp. 894-896; 907A pp. 864-866; 214A pp. 134-136; 408C pp. 303-306; 
  408D pp. 306-309; 408E pp. 309-310; 408F pp. 310-313; 410B pp. 322-
  323; 410C pp. 323-324; 212 pp. 126-127; 423 pp. 429-437.
  Methods 908, 908A, and 908B pp. 870-878; Method 908E pp. 882-141.21(f)
  Methods 909, 909A, and 909B pp. 886-896; Nutrient Agar p. 874; EC 
  Medium p. 879.
Standard Methods for the Examination of Water and Wastewater, 18th 
  Edition Supplement, 1994:
  Standard Methods for the Examination of Water and Wast141.21; 141.23; 
  Edition, 1992.                                   141.24; 141.74; 143.4
  Method 6610, Carbamate Pesticides Method................141.24; 141.40

[[Page 781]]

Standard Methods for the Examination of Water and                141.142
  Waste Water, 19th Edition, 1995.
Standard Methods for the Examination of Water and                 141.31
  Wastewater, 19th Edition, 1995; Supplement, 
  1996.


American Society for Testing and Materials

  100 Barr Harbor Drive, West Conshohocken, PA 
  19428-2959; Telephone: (610) 832-9585, FAX: 
  (610) 832-9555
ASTM D 511-88 Standard Test Methods for Calcium                   141.89
  and Magnesium in Water.
ASTM D 515-88 Standard Test Methods for Phosphorus                141.89
  in Water.
ASTM D 859-88 Standard Test Method for Silica in                  141.89
  Water.
ASTM D 1067-88 Standard Test Methods for Acidity                  141.89
  or Alkalinity of Water.
ASTM D 1125-82 Standard Test Methods for                          141.89
  Electrical Conductivity and Resistivity of 
  Water.
ASTM D 1293-84 Standard Test Methods for pH of                    141.89
  Water.
ASTM D 1688-90 Standard Test Methods for Copper in                141.89
  Water.
ASTM D 2459-75 Gamma Spectrometry in Water........          141.25(a)(6)
ASTM D 2907-75 Micro-quantities of Uranium in               141.25(a)(7)
  Water by Flourometry.
ASTM D 3559-85 Standard Test Methods for Lead in                  141.89
  Water.
ASTM D 4327-88 Standard Test Method for Anions in                 141.89
  Water by Ion Chromatography.
Annual Book of ASTM Standards, 1993, Volume 11....         141.23; 143.4
Annual Book of ASTM Standards 1994; Vol. 11.01,                   141.31
  1994 edition and 1996 edition.
Annual Book of ASTM Standards, 1994, Vol. 11:02...                141.25


American Water Works Association Research Foundation

  Customer Service, 6666 West Quincy Avenue, 
  Denver, CO 80235; Telephone: 303-794-7711
Guidance Manual for Compliance with the Filtration               141.142
  and Disinfection Requirements for Public Water 
  Systems Using Surface Water Sources, 1991, 
  Appendices C and O.
Methods for Chemical Analysis of Water and Wastes,                141.89
  EPA Environmental Monitoring and Support 
  Laboratory, Cincinnati, OH (EPA-600/4-79-020), 
  Revised March 1983, Procedures 239.2, 220.2, 
  220.1, 150.1, 150.2, 120.1, 215.2, 215.1, 310.1, 
  365.1, 365.3, 365.2, and 370.1 located at pp. 
  239.2-1 through 239.2-2 and metals -1 through 
  metals-19, 220.2-1 through 220.2-2 and metals-1 
  through metals-19, 220.1-1 through 220.1-2 and 
  metals-1 through metals-19, 150.1-1 through 
  150.1-3, 150.2-1 through 150.2-3, 120.1-1 
  through 120.1-3, 215.2-1 through 215.2-3, 215.1-
  1 through 215.1-2, 310.1-1 through 310.1-3, 
  365.1-1 through 365.1-9, 365.3-1 through 365.3-
  4, 365.2-1 through 365.2-6, and 370.1-1 through 
  370.1-5.
National Field Evaluation of a Defined Substrate    141.21(a); 141.74(a)
Method for the Simultaneous Enumeration of Total 
[[Page 782]]nd Escherichia coli from Drinking 
  Water: Comparison with the Standard Multiple 
National Field Evaluation of a Defined Substrate               141.21(f)
  Method for the Simultaneous Detection of Total 
  Coliforms and Escherichia coli from Drinking 
  Water: Comparison with Presence-Absence 
  Techniques, Stephen C. Edberg, Martin J. Allen, 
  Darwell B. Smith, and the National Collaborative 
  Study, which appears in Applied and appears in 
  Environmental Microbiology, Volume 55, No. 4 e 
  pages 1003-1008, April 1989, published by the er 
  American Society for Microbiology. Microbiology, 
Standard Methods for the Examination of Water and                 141.89
  Wastewater, 17th Edition, American Public Health 
  Association, American Water Works Association, 
  Water Pollution Control Federation, 1989, 
  Procedures 3113, 3111-B, 3120, 4500-H+, 2510, 
  3500-Ca-D, 3120, 2320, 4500-P-F, 4500-P-E, 4110, 
  4500-Si-D, 4500-Si-E, 4500-Si-F, and 2500 
  located at pp. 3-32 through 3-43, 3-20 through 
  3-23, 3-53 through 3-63, 4-94 through 4-102, 2-
  57 through 2-61, 3-85 through 3-87, 2-35 through 
  2-39, 4-178 through 4-181, 4-177 through 4-178, 
  4-2 through 4-6, 4-184 through 4-187, 4-188 
  through 4-191, and 2-80 through 2-81.


Analytical Technology, Inc. Orion

  529 Main St., Boston, MA 02129
Analytical Technology, Inc. Orion, Technical                      141.23
  Bulletin 601, Standard Method of Test for 
  Nitrate in Drinking Water, PN 221890-001, dated 
  July 1994.


Department of Commerce

  National Institute of Standard and Technology 
  (formerly National Bureau of Standards), 
  Washington, DC 20234
Handbook No. 69, Permissible Body Burdens and                  141.16(b)
  Maximum Permissible Concentrations of 
  Radionuclides in Air or Water for Occupational 
  Exposure, August 1963.


Department of Commerce

  National Technical Information Service, 5285 
  Port Royal Rd., Springfield, VA 22161; 
  Telephone: (703) 487-4650, FAX: (703) 487-4142
Interim Radiochemical Methodology for Drinking                    141.25
  Water, EPA 600/4-75-008 (revised), March 1976.
Prescribed Procedures for Measurement of                          141.25
  Radioactivity in Drinking Water, EPA 600/4-80-
  032, August 1980.
Radiochemical Analytical Procedures for Analysis                  141.25
  of Environmental Samples, March 1979.
Radiochemistry Procedures Manual, EPA 520/5-84-                   141.25
  006, December 1987.
Standard Methods for the Examination of Water and                 141.25
  Wastewater, 13th, 17th, 18th, and 19th Editions, 
  1971, 1989, 1992, and 1995.


Department of Energy

  Environmental Measurements Laboratory, 376 
  Hudson St., New York, NY 10014-3621
EML Procedures Manual, 27th Edition, Vol. 1, 1990.                141.25
HASL Procedures Manual HASL--300, 1978............          141.25(b)(2)


Environmental Protection Agency

  Environmental Monitoring & Support Laboratory 
  (EMSL), 25 W. St. Clair St., Cincinnati, OH 
  45268
Interim Radiochemical Methodology for Drinking                 141.25(a)
Water, EMSL, EPA-600/4-75-008.
[[Page 783]]

Microbiological Methods for Monitoring the                     141.21(f)
  Environment, Water and Wastes, U.S. EPA, 
  Environmental Monitoring and Support Laboratory 
  (EPA-600/8-78-017), December 1978; Part III, 
  Section B.2.1--2.6, pp. 108-112; Part III, 
  Section B.4.1--4.6.4, pp. 114-118.
  Office of Solid Waste and Emergency Response, 
  Waste Characterization Branch, Washington, DC 
  20460
  The above standards are also available at the 
  Office of Drinking Water, Criteria and Standards 
  Division, Environmental Protection Agency, 401 M 
  St., SW., Washington, DC 20460
  Available from: National Technical Information 
  Service, 5285 Port Royal Road, Springfield, VA 
  22161
Method 300.1 Determination of Inorganic Anions in                 141.31
  Drinking Water by Ion Chromatography, Revision 
  1.0, 1997 (EPA/600/R-98/118).
Methods for the Determination of Organic Compounds                141.31
  in Drinking Water, Supp. II, August 1992 (EPA 
  600/R-92-129).
Methods for the Determination of Organic Compounds                141.31
  in Drinking Water, Supp. III, August 1995 (EPA 
  600/R-95-131).
Methods for Determination of Inorganic Substances                9141.31
  in Environmental Samples, August 1993 (EPA 600/
  R-93-100).
  Pergamon Press, Ltd., Fairview Park, Elmsford, 
  NY 10523
Determination of Ozone in Water by the Indigo                  141.74(a)
  Method; A Submitted Standard Method, H. Bader 
  and J. Hoigne; Ozone Science and Engineering, 
  Volume 4, pp. 169-176, 1982.


Great Lakes Instruments, Inc.

  8855 North 55th Street, Milwaukee, WI 53223
Great Lakes Instruments, Method 2, Turbidity,                     141.74
  dated November 2, 1992.


Millipore Corporation

  Technical Services Department, 80 Ashby Road, 
  Bedford, MA 01730
Millipore Corporation, Method AN208, Colisure                     141.21
  Presence/Absence Test for Detection and 
  Identification of Coliform Bacteria and 
  Escherichia coli in Drinking Water, dated 
  February 28, 1994.


Radiological Sciences Institute Center for Laboratories and Research, 
New York State Department of Health

  Empire State Plaza, Albany, NY 12201
Determination of Ra-226 and Ra-228 (Ra-02),                       141.25
  January, 1980.


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
Determination of Radium 228 in Drinking Water,                    141.25
  August 1980.


Technicon Industrial Systems, c/o Bran & Luebbe

  1025 Busch Parkway, Buffalo Grove, IL 60089
Technicon Industrial Systems, Industrial Method                   141.23
  No. 129-71W, Fluoride in Water and Wastewater 
  dated December 1972, and Method No. 380-75WE, 
  Fluoride in Water and Wastewater, dated February 
  1976.


U.S. Geological Survey, Department of the Interior

  Books and Open-File Reports Section, Federal 
  Center, Box 25425, Denver, CO 80225

[[Page 784]]

Methods for Determination of Inorganic Substances                 141.89
  in Water and Fluvial Sediments, 3rd edition, 
  U.S. Department of Interior, U.S. Geological 
  Survey, 1989, Procedures I-1030-85, I-1601-85, 
  I-2601-85, I-2598-85, I-1700-85, and I-2700-85 
  located at pp. 55-56, 381-382, 383-385, 387-388, 
  415-416, and 417-419.


U.S. Geological Survey, Department of the Interior

  USGL Information Services, Box 25286, Federal 
  Center, Denver, CO 80225-0425
Methods for Determination of Radioactive                          141.25
  Substances in Water and Fluvial Sediments, 
  Chapter A5 in Book 5 of Techniques of Water-
  Resources Investigations of the United States 
  Geological Survey, 1977.


State Statutes and Regulations
(PART 147): STATE UNDERGROUND INJECTOR CONTROL PROGRAMS

Alabama: (1) Code of Alabama, section 9-17-1                   147.50(a)
  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 in 
  Alabama, and Oil and Gas Statutes of Alabama 
  with Oil and Gas Board Forms, 400-1-2, and 400-
  1-5-.04.
Alabama; (1) Alabama Water Pollution Control Act,              147.51(a)
  Code of Alabama 1975, Secs. 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).
Alaska: (1) Alaska Statutes, Alaska Oil and Gas               147.100(a)
  Conservation Act, Title 31, Sections 31.05.005 
  through 31.30.010 (1979 and Cumm. Supp. 1984); 
  (2) Alaska Statutes, Administrative Procedures 
  Act, Title 44, Sections 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).
Indiana: (1) Indiana Code, title 4, article 21.5,                147.750
  chapters 1 through 6 (1988); (2) West's 
  Annotated Indiana Code, title 13, article 8, 
  chapters 1 through 15 (1990 and Cumm. Supp. 
  1990); (3) Indiana Administrative Code, title 
  310, article 7, rules 1 through 3 (Cumm. Supp. 
  1991).
Arkansas: (1) Arkansas Water and Air Pollution                147.200(a)
Control Act, Act 472 of 1949 as amended, 
[[Page 785]]atutes Annotated Secs. 82-1901 
  through 82-1943 (1976); (2) Act 105 of 1939, 
California: (1) California Public Resources Code,             147.250(a)
  California Laws for Conservation of Petroleum 
  and Gas, Div. 3, Chapt. 1, sections 3000-3359 
  (1989); (2) California Administrative Code, 
  Title 14, section 1710 through 1724.10 (May 28,  
  1988). (1971 and Supp. 1981); Act 937 of 1979, 
Colorado: (1) Colorado Revised Statutes, 1989                 147.300(a)
  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 1; 
  Commission of the State of Colorado (revised de, 
  July 1989); (4) Oil and Gas Conservation gy, 
  Commission Revised Rules and Regulations in the 
  300, 400, 500, and 600 series, effective March n 
  20, 1989.. 2-39, revised July 1972); (5) 
Connecticut: (1) Connecticut General Statutes                 147.350(a)
  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).
Delaware: (1) Delaware Environmental Protection               147.400(a)
  Act (Environmental Control), 7 Delaware Code 
  Annotated, Chapter 60, Sections 6001 through 
  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.
Florida: (1) Florida Air and Water Pollution                  147.500(a)
  Control Act, Florida Statutes Annotated 
  Secs. 403.011-403.90 (1973 and Supp. 1983); (2) 
  Florida Administrative Code, Chapter 17-28, 
  Underground Injection Control (April 27, 1989).
Georgia: (1) Oil and Gas Deep Drilling Act of                 147.550(a)
1975, Official Code of Georgia Annotated 
[[Page 786]] sections 12-4-40 through 12-4-53 
  (1988); (2) Ground Water Use Act of 1972, 
Idaho: (1) Public Writings, Title 9, Chapter 3,               147.650(a)
  Idaho Code, Secs. 9-301 through 9-302 (Bobbs-
  Merrill 1979); (2) Crimes and Punishments, Title 
  18, Chapter 1, Idaho Code, Secs. 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, 22 
  Sec. 42-237(e); Sec. 42-238 (Bobbs-Merrill 1977 
  and Supp. 1984); Department of Water Resources-
  Water Resources Board, Title 42, Chapter 17, 
  Idaho Code, Secs. 42-1701, 42-1703, 42-1735 nt 
  (Bobbs-Merrill 1977), Sec. 42-1701A (Supp. 8-83 
  1984); (6) Director of Department of Water  of 
  Resources, Title 42, Chapter 18, Idaho Code, 5-
  Secs. 42-1801 through 42-1805 (Bobbs-Merrill nt 
  1977); (7) Waste Disposal and Injection Wells, 
  Title 42, Chapter 39, Idaho Code, Secs. 42-3901 
  through 42-3914 (Bobbs-Merrill 1977), Secs. 42-
  3915 through 42-3919 (Supp. 1984); (8) Idaho 
  Trade Secrets Act, Title 48, Chapter 8, Idaho 
  Code, Secs. 48-801 through 48-807 (Bobbs-Merrill 
  1977 and Supp. 1984); (9) Administrative 
  Procedure, Title 67, Chapter 52, Idaho Code, 
  Secs. 67-5201 through 67-5218 (Bobbs-Merrill 
  1980 and Supp. 1984); (10) Idaho Radiation 
  Control regulations (IRCR) Sec. 1-9002.70; 
  Secs. 1-9100 through 1-9110, Department of 
  Health and Welfare (May 1981); (11) Rules and 
  Regulations: Construction and Use of Injection 
  Wells, Idaho 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).
Illinois: (1) Illinois Environmental Protection               147.700(a)
  Act, Illinois ch. 111\1/2\, Secs. 1001-1051 
  (Smith-Hurd 1977 Revised Statutes and Supp. 
  1983), as amended by Public Act No. 83-431, 1983 
  Illinois Legislative Service, pages 2910-2916 
  (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.
Illinois: (1) Conservation of Oil and Gas, etc.,              147.701(a)
  Illinois Revised Statutes ch. 96\1/2\, 
  Secs. 5401-5457 (Smith-Hurd 1979 and Supp. 
  1983), as amended by Public Act No. 83-1074 1983 
  Illinois Legislative Service pages 7183-7185 
  (West); (2) Illinois Environmental Protection 
  Act, Illinois Revised Statutes ch. 111\1/2\, 
  Secs. 1001-1051 (Smith-Hurd 1977 and Supp. 
  1983), as amended by Public Act No. 83-431, 1983 
  Illinois Legislative Services pages 2910-2916 
  (West); (3) Illinois Revised Statutes ch. 100\1/
  2\, Secs. 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).
Indiana: (1) Indiana Code, title 4, article 21.5,                147.750
chapters 1 through 6 (1988); (2) West's 
[[Page 787]]ndiana Code, title 13, article 8, 
  chapters 1 through 15 (1990 and Cumm. Supp. 
Kansas: (1) Kansas Administrative Regulations,                147.850(a)
  Chapter 28, Article 46, Underground Injection 
  Control Regulations, Kansas Administrative 
  Regulations, sections 28-46-1 through 28-46-42 
  (1986 and Supp. 1987); (2) Kansas Administrative 
  Regulations, Chapter 28, Article 43, mm. Supp. 
  Construction, Operation, Monitoring and 
  Abandonment of Salt Solution Mining Wells, 
  sections 28-43-1 through 28-43-10 (1986); (3) 
  Kansas Statutes Annotated, sections 65-161, 65-
  164 through 65-166a, 65-171d (1980 and Cumm. 
  Supp. 1989).
Louisiana: (1) Louisiana Revised Statutes                     147.950(a)
  Annotated Secs. 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 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; (vi) 
  Amendment to Statewide Order No. 29-B (amendment 
  concerning disposal of nonhazardous oilfields 
  waste) (March 20, 1984, effective May 20, 1984); 
  (vii) Amendment to Statewide Order No. 29-B 
  (amendment concerning the adminstrative 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).
Maine: (1) Maine Revised Statutes Annotated title                147.100
  38, Secs. 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 (adopted 
  June 22, 1983, effective July 4, 1983).
Maryland: (1) Code of Maryland Regulations, Title            147.1050(a)
26, Subtitle 08, Chapter 07, promulgated and 
[[Page 788]]s of March 1, 1989; (2) Code of 
  Maryland Regulations, Title 26, Subtitle 08, 
Massachusetts: (1) Massachusetts General Laws                147.1100(a)
  Annotated ch. 21, Secs. 27, 43, and 44 (West 
  1981); (2) Code of Massachusetts Regulations, 
  title 310, Secs. 23.01-23.11 as amended April 
  26, 1982.1, promulgated and effective as of 
Mississippi: (1) Mississippi Air and Water                   147.1250(a)
  Pollution Control Law, Mississippi Code 
  Annotated Secs. 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 gulations, 
  Regulations (adopted February 11, 1982); (3) d 
  Mississippi Department of Natural Resources, f 
  Bureau of Pollution Control, State of le 08, 
  Mississippi Wastewater Permit Regulations for 
  National Pollutant Discharge Elimination System  
  (NPDES), Underground Injection Control (UIC),  
  and State Operating Permits (adopted May 1, of 
  1974; amended February 11, 1982).ubtitle 13, 
Mississippi: (1) (i) Mississippi Code Annotated              147.1251(a)
  (MCA), Section 5-9-9 (Supp. 1988); (ii) MCA, 
  Sections 53-1-1 through 53-1-47, inclusive and 
  Sections 53-1-71 through 53-1-77, inclusive 
  (1972 and Supp. 1988); (iii) MCA, Sections 53-3-
  1 through 53-3-165, inclusive (1972 and Supp. 
  1988); (2) State Oil and Gas Board Statewide 
  Rules and Regulations, Rules 1 through 65, 
  inclusive (Aug. 1, 1987, as amended, Sept. 17, 
  1987).
Missouri: (1) Revised Statutes of the State of               147.1300(a)
  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 50, 
  chapters 1 and 2 (June 1984); (3) Vernon's 
  Annotated Missouri Statutes, chapter 204, 
  sections 204.006 through 204.470 (1983 and Cumm. 
  Supp. 1990).
Montana: (1) Montana Statutory Requirements                  147.1350(a)
  Applicable to the Underground Injection Control 
  Program, August 1996; (2) Montana Regulatory 
  Requirements Applicable to the Underground 
  Injection Control Program, August 1996.
Nebraska: (1) Rules and Regulations of the                   147.1400(a)
  Nebraska Oil and Gas Conservation Commission, 
  Rules 1-6 (as published by the Commission, May 
  1981); (2) Revised Statutes of Nebraska, 
  sections 57-903 and 57-906 (Reissue 1988).
Nebraska: (1) Revised Statutes of Nebraska,                  147.1401(a)
  Nebraska Environmental Protection Act, 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.
Nevada: (1) (i) Nevada Revised Statutes (NRS)                147.1450(a)
VOlume 25, Chapter 445.131 through 445.354, 
[[Page 789]]1987; (ii) NRS Volume 29, Chapter 
  534A.010 through 534A.090, inclusive. 1987; 
New Hampshire: (1) New Hampshire Revised Statutes            147.1500(a)
  Annotated Sec. 149:8 III(a) (1978); (2) New 
  Hampshire Code of Administrative Rules, Part Wc 
  410 (Protection of Groundwaters of the State, 
  Secs. Ws 410.1 through Ws 410.16) (Issue Ws 3-
  82).190, inclusive. 1987; (2) (i) Nevada 
New Jersey: (1) New Jersey Statutes Annotated,               147.1550(a)
  Water Pollution Control Act, 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).ection 
New Mexico: (1) Oil and Gas Act, New Mexico                  147.1600(a)
  Statutes Annotated Secs. 70-2-1 through -36 
  (1978); (2) State of New Mexico Energy and 
  Mineral Department, Oil Conservation Division--
  Rules and Regulations (dated 10-1-78), Secs. B-
  3, I-701 through I-708, M-1100 through M-1121.
New Mexico: (1) New Mexico Water Quality Control             147.1601(a)
  Commission Regulations (WQCC 82-1) Secs. 1-100 
  through 5-300 (September 20, 1982).
North Carolina: (1) Administrative Procedure Act,            147.1700(a)
  N.C. GEN. STAT. sections 150B-1 through 150B-64 
  (1987 and Cumm. Supp. 1989); (2) North Carolina 
  Well Construction Act, N.C. GEN. STAT. sections 
  87-83 through 87-99 (1989 and Cumm. Supp. 1989); 
  (3) Water and Air Resources, N.C. GEN. STAT. 
  sections 143-211 through 143-215.10 (1987 and 
  Cumm. Supp. 1989); (4) Solid Waste Management, 
  N.C. GEN. STAT. sections 130A-290 through 130A-
  309.03 (1989); (5) North Carolina Drinking Water 
  Act, N.C. GEN. STAT. sections 130A-311 through  
  130A-332 (1989); (6) Sanitary Sewage Systems, gh 
  N.C. GEN. STAT. sections 130A-333 through 130A-
  335 (1989).A); (iii) NAC Regulations and Rules 
North Dakota: (1) North Dakota Century Code,                 147.1750(a)
  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)..
North Dakota: (1) North Dakota Century Code                  147.1751(a)
  sections 38-12-01, 39-12-03 (1980); sections 61-
  28-02, 61-28-06 (Supp. 1980); (2) North Dakota 
  Century Code, sections 61-28-02 and 61-28-06 
  (1989); (3) sections 43-02-02-01, 43-02-02-12, 
  43-02-02-16 through 43-02-02-26, 43-02-02-29, 
  43-02-02-31, 43-02-02-35 (1978); (4) North 
  Dakota Administrative Code, Chapter 43-02-02 
  (Subsurface Mineral Mineral Exploration and 
  Development) (August 1986), and Chapter 43-02-
  02.1 (Underground Injection Control Program) 
  (March 1, 1984).
Ohio: (1) Ohio Revised Code Annotated,                       147.1801(a)
Secs. 1509.01, 1509.03, 1509.221 (Supp. 1983); 
[[Page 790]]f the Division of Oil and Gas, Ohio 
  Administrative Code, Secs. 1501:9-7-01 through 
Oklahoma: (1) Oklahoma Statutes title 63 Secs. 1-            147.1850(a)
  901, 1-903 (1981); (2) Oklahoma Controlled 
  Industrial Waste Disposal Act, Oklahoma Statute 
  Annotated title 63 Secs. 1-2002, 1-2014 (West 
  Supp. 1983-1984).Ohio Revised Code Annotated, 
Oregon: (1) Oregon Revised Statutes, Title 16, Ch.           147.1900(a)
  164, sections 164.785; Title 36, Ch. 468, 
  sections 468.005, 468.065 to 468.070, 468.700 to 
  468.815; (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).
Rhode Island: (1) Rhode Island Gen. Laws Secs. 46-           147.2000(a)
  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).
South Carolina:(1) Pollution Control Act, S.C.               147.2050(a)
  Code Ann Secs. 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.
South Dakota: (1) South Dakota Codified Laws,                147.2100(a)
  Secs. 45-9-2, 45-9-4, 45-9-11, 45-9-13, 45-9-14, 
  5-9-15 (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.
Texas: (1) Injection Well Act, Texas Water Code                 147.2200
  Secs. 27.002, 27.011 (Vernon Supp. 1984).
Utah: (1) Utah Code Annotated, Utah Water                    147.2250(a)
  Pollution Control Act, Title 26, Chapter 11, 
  Sections 2, 8, and 10 (1989); (2) Utah 
  Administrative Code, Underground Injection 
  Control Regulations, section R448-7 (effective 
  as of January 2, 1990); (3) Underground 
  Injection Control Program (adopted January 20, 
  1990 and revised effective July 20, 1990) 
  (officially submitted to EPA by the Executive 
  Secretary of Utah Water Pollution Control 
  Committee on August 16, 1990).
Utah: (1) Utah Code Annotated, 1953, section 40-6-           147.2251(a)
  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.
Vermont: (1) Vt. Stat. Ann. tit. 10, sections                147.2300(a)
1251, 1259, 1263 (1973 and Supp. 1981), 
[[Page 791]]ate: July 1, 1982; (2) Vermont 
  Department of Water Resources and Environmental 
Washington: (1) Revised Code of Washington                   147.2400(a)
  Secs. 90.48.020, -.080, -.160, and -.162 (Bureau 
  of National Affairs, 1983 Laws); (2) Washington 
  Administrative Code Secs. 173-218-010 to 173-
  218-110 (Bureau of National Affairs 2/29/84); l 
  (3) Washington Administrative Code Secs. 344-12-
  001 to 344-12-262 (Bureau of National Affairs, 
  1983); (4) Washington Administrative Code, 
  Chapter 173-160 (reprinted May 1988).
Wisconsin: (1) Wisconsin Statutes Annotated,                 147.2500(a)
  sections 147.015, 147.02 and 147.04 (West 1974 
  and Supp. 1983); (2) Wisconsin Administrative 
  Code, Chapter NR 112, Well Construction and Pump 
  Installation, sections 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) 
  Wisconsin Administrative Code, Chapter NR 113, 
  Servicing Septic Tanks, Seepage Pits, Grease 
  Traps or Privies, sections NR 113.07 through 
  113.08 (1979), as amended by Natural Resources 
  Board Order No. WQ-25-82, approved by the 
  Natural Resources Board on August 25, 1982; (4) 
  Wisconsin Administrative Code, Chapter NR 181, 
  Hazardous Waste Management, sections NR 181.04 , 
  through 181.415 (1981), as amended June 1985; 
  (5) Wisconsin Administrative Code, Chapter NR 
  210, Sewage Treatment Works, Natural Resources , 
  Board Order No. WQ-25-82, section NR 210.05, d 
  approved by the Natural Resources Board on 
  August 25, 1982; (6) Wisconsin Administrative 
  Code, Chapter NR 214, Land Application and 
  Disposal of Liquid Industrial Wastes and By-
  products, sections NR 214.03 and 214.08 (1983).
Wyoming: (1) Wyoming Environmental Quality Act,              147.2550(a)
  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); (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).
Wyoming: (1) Rules and Regulations of the Wyoming            147.2551(a)
Oil and Gas Conservation Commission, including 
[[Page 792]]actice and Procedure, as published by 
  the Wyoming Oil and Gas Conservation Commission, 
Guam: (1) Water Resources Conservation Act,                  147.2600(a)
  Government Code of Guam Secs. 57021-57025, Pub. 
  L. 9-31 (March 9, 1967), as amended by Pub. L. 
  9-76 (July 29, 1967), as amended by Pub. L. 12-
  191 (December 30, 1974); (2) Water Pollution 0, 
  Control Act, Government Code of Guam Secs. 57042 
  and 57045, Pub. L. 9-76 (July 29, 1967), as 990 
  amended by Pub. L. 9-212 (August 5, 1968), as 
  amended by Pub. L. 10-31 (March 10, 1969), as 
  amended by Pub. L. 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).
Commonwealth of the Northern Mariana Islands: (1)            147.2800(a)
  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 8, 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.
Commonwealth of Puerto Rico: (1) Underground                    147.2650
  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.
Copies of these materials are available at the                          
  addreses provided in the regulations cited in 
  this table.



[[Page 793]]



                    Table of CFR Titles and Chapters




                      (Revised as of July 1, 1999)

                      Title 1--General Provisions

         I  Administrative Committee of the Federal Register 
                (Parts 1--49)
        II  Office of the Federal Register (Parts 50--299)
        IV  Miscellaneous Agencies (Parts 400--500)

                          Title 2--[Reserved]

                        Title 3--The President

         I  Executive Office of the President (Parts 100--199)

                           Title 4--Accounts

         I  General Accounting Office (Parts 1--99)
        II  Federal Claims Collection Standards (General 
                Accounting Office--Department of Justice) (Parts 
                100--299)

                   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  Advisory Committee on Federal Pay (Parts 1400--1499)
         V  The International Organizations Employees Loyalty 
                Board (Parts 1500--1599)
        VI  Federal Retirement Thrift Investment Board (Parts 
                1600--1699)
       VII  Advisory Commission on Intergovernmental Relations 
                (Parts 1700--1799)
      VIII  Office of Special Counsel (Parts 1800--1899)
        IX  Appalachian Regional Commission (Parts 1900--1999)
        XI  Armed Forces Retirement Home (Part 2100)
       XIV  Federal Labor Relations Authority, General Counsel of 
                the Federal Labor Relations Authority and Federal 
                Service Impasses Panel (Parts 2400--2499)
        XV  Office of Administration, Executive Office of the 
                President (Parts 2500--2599)
       XVI  Office of Government Ethics (Parts 2600--2699)
       XXI  Department of the Treasury (Parts 3100--3199)

[[Page 794]]

      XXII  Federal Deposit Insurance Corporation (Part 3201)
     XXIII  Department of Energy (Part 3301)
      XXIV  Federal Energy Regulatory Commission (Part 3401)
       XXV  Department of the Interior (Part 3501)
      XXVI  Department of Defense (Part 3601)
    XXVIII  Department of Justice (Part 3801)
      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 (Part 4301)
      XXXV  Office of Personnel Management (Part 4501)
        XL  Interstate Commerce Commission (Part 5001)
       XLI  Commodity Futures Trading Commission (Part 5101)
      XLII  Department of Labor (Part 5201)
     XLIII  National Science Foundation (Part 5301)
       XLV  Department of Health and Human Services (Part 5501)
      XLVI  Postal Rate Commission (Part 5601)
     XLVII  Federal Trade Commission (Part 5701)
    XLVIII  Nuclear Regulatory Commission (Part 5801)
         L  Department of Transportation (Part 6001)
       LII  Export-Import Bank of the United States (Part 6201)
      LIII  Department of Education (Parts 6300--6399)
       LIV  Environmental Protection Agency (Part 6401)
      LVII  General Services Administration (Part 6701)
     LVIII  Board of Governors of the Federal Reserve System (Part 
                6801)
       LIX  National Aeronautics and Space Administration (Part 
                6901)
        LX  United States Postal Service (Part 7001)
       LXI  National Labor Relations Board (Part 7101)
      LXII  Equal Employment Opportunity Commission (Part 7201)
     LXIII  Inter-American Foundation (Part 7301)
       LXV  Department of Housing and Urban Development (Part 
                7501)
      LXVI  National Archives and Records Administration (Part 
                7601)
      LXIX  Tennessee Valley Authority (Part 7901)
      LXXI  Consumer Product Safety Commission (Part 8101)
     LXXIV  Federal Mine Safety and Health Review Commission (Part 
                8401)
     LXXVI  Federal Retirement Thrift Investment Board (Part 8601)
    LXXVII  Office of Management and Budget (Part 8701)

                          Title 6--[Reserved]

                         Title 7--Agriculture

            Subtitle A--Office of the Secretary of Agriculture 
                (Parts 0--26)
            Subtitle B--Regulations of the Department of 
                Agriculture

[[Page 795]]

         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)
         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)
      XIII  Northeast Dairy Compact Commission (Parts 1300--1399)
       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)
      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, 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)

[[Page 796]]

    XXXIII  Office of Transportation, Department of Agriculture 
                (Parts 3300--3399)
     XXXIV  Cooperative State Research, Education, and Extension 
                Service, Department of 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)

                    Title 8--Aliens and Nationality

         I  Immigration and Naturalization Service, Department of 
                Justice (Parts 1--499)

                 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)
      XVII  Defense Nuclear Facilities Safety Board (Parts 1700--
                1799)

                      Title 11--Federal Elections

         I  Federal Election Commission (Parts 1--9099)

                      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)

[[Page 797]]

        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)
        XI  Federal Financial Institutions Examination Council 
                (Parts 1100--1199)
       XIV  Farm Credit System Insurance Corporation (Parts 1400--
                1499)
        XV  Department of the Treasury (Parts 1500--1599)
      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)

                    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--499)
         V  National Aeronautics and Space Administration (Parts 
                1200--1299)

                 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 Export Administration, Department of 
                Commerce (Parts 700--799)

[[Page 798]]

      VIII  Bureau of Economic Analysis, Department of Commerce 
                (Parts 800--899)
        IX  National Oceanic and Atmospheric Administration, 
                Department of Commerce (Parts 900--999)
        XI  Technology Administration, 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)

                    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  United States Customs Service, Department of the 
                Treasury (Parts 1--199)
        II  United States International Trade Commission (Parts 
                200--299)
       III  International Trade Administration, Department of 
                Commerce (Parts 300--399)

[[Page 799]]

                     Title 20--Employees' Benefits

         I  Office of Workers' Compensation Programs, Department 
                of Labor (Parts 1--199)
        II  Railroad Retirement Board (Parts 200--399)
       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  Employment Standards Administration, 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, 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  United States Information Agency (Parts 500--599)
       VII  Overseas Private Investment Corporation (Parts 700--
                799)
        IX  Foreign Service Grievance Board Regulations (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  Board for International Broadcasting (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)

[[Page 800]]

                          Title 23--Highways

         I  Federal Highway Administration, Department of 
                Transportation (Parts 1--999)
        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 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--999)
         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)
        XX  Office of Assistant Secretary for Housing--Federal 
                Housing Commissioner, Department of Housing and 
                Urban Development (Parts 3200--3899)
       XXV  Neighborhood Reinvestment Corporation (Parts 4100--
                4199)

[[Page 801]]

                           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--799)
         V  Bureau of Indian Affairs, Department of the Interior, 
                and Indian Health Service, Department of Health 
                and Human Services (Part 900)
        VI  Office of the Assistant Secretary-Indian Affairs, 
                Department of the Interior (Part 1001)
       VII  Office of the Special Trustee for American Indians, 
                Department of the Interior (Part 1200)

                      Title 26--Internal Revenue

         I  Internal Revenue Service, Department of the Treasury 
                (Parts 1--799)

           Title 27--Alcohol, Tobacco Products and Firearms

         I  Bureau of Alcohol, Tobacco and Firearms, Department of 
                the Treasury (Parts 1--299)

                   Title 28--Judicial Administration

         I  Department of Justice (Parts 0--199)
       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)

                            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)

[[Page 802]]

       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  Pension and Welfare Benefits 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  Minerals Management Service, Department of the 
                Interior (Parts 200--299)
       III  Board of Surface Mining and Reclamation Appeals, 
                Department of the Interior (Parts 300--399)
        IV  Geological Survey, Department of the Interior (Parts 
                400--499)
        VI  Bureau of Mines, Department of the Interior (Parts 
                600--699)
       VII  Office of Surface Mining Reclamation and Enforcement, 
                Department of the Interior (Parts 700--999)

                 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)
        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 International Investment, Department of the 
                Treasury (Parts 800--899)

                      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)

[[Page 803]]

       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)
       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)
      XXIX  Presidential Commission on the Assignment of Women in 
                the Armed Forces (Part 2900)

               Title 33--Navigation and Navigable Waters

         I  Coast Guard, Department of Transportation (Parts 1--
                199)
        II  Corps of Engineers, Department of the Army (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)
        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 Vocational and Adult Education, Department 
                of Education (Parts 400--499)
         V  Office of Bilingual Education and Minority Languages 
                Affairs, Department of Education (Parts 500--599)
        VI  Office of Postsecondary Education, Department of 
                Education (Parts 600--699)
       VII  Office of Educational Research and Improvement, 
                Department of Education (Parts 700--799)
        XI  National Institute for Literacy (Parts 1100--1199)
            Subtitle C--Regulations Relating to Education
       XII  National Council on Disability (Parts 1200--1299)

[[Page 804]]

                        Title 35--Panama Canal

         I  Panama Canal Regulations (Parts 1--299)

             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)
       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)
       XIV  Assassination Records Review Board (Parts 1400--1499)

             Title 37--Patents, Trademarks, and Copyrights

         I  Patent and Trademark Office, Department of Commerce 
                (Parts 1--199)
        II  Copyright Office, Library of Congress (Parts 200--299)
        IV  Assistant Secretary for Technology Policy, Department 
                of Commerce (Parts 400--499)
         V  Under Secretary for Technology, Department of Commerce 
                (Parts 500--599)

           Title 38--Pensions, Bonuses, and Veterans' Relief

         I  Department of Veterans Affairs (Parts 0--99)

                       Title 39--Postal Service

         I  United States Postal Service (Parts 1--999)
       III  Postal Rate Commission (Parts 3000--3099)

                  Title 40--Protection of Environment

         I  Environmental Protection Agency (Parts 1--799)
         V  Council on Environmental Quality (Parts 1500--1599)
       VII  Environmental Protection Agency and Department of 
                Defense; Uniform National Discharge Standards for 
                Vessels of the Armed Forces (Parts 1700--1799)

          Title 41--Public Contracts and Property Management

            Subtitle B--Other Provisions Relating to Public 
                Contracts

[[Page 805]]

        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, Department of Labor 
                (Parts 61-1--61-999)
            Subtitle C--Federal Property Management Regulations 
                System
       101  Federal Property Management Regulations (Parts 101-1--
                101-99)
       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)
            Subtitle D--Other Provisions Relating to Property 
                Management [Reserved]
            Subtitle E--Federal Information Resources Management 
                Regulations System
       201  Federal Information Resources Management Regulation 
                (Parts 201-1--201-99) [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 (Parts 303-1--303-2)
       304  Payment from a Non-Federal Source for Travel Expenses 
                (Parts 304-1--304-99)

                        Title 42--Public Health

         I  Public Health Service, Department of Health and Human 
                Services (Parts 1--199)
        IV  Health Care Financing Administration, Department of 
                Health and Human Services (Parts 400--499)
         V  Office of Inspector General-Health Care, Department of 
                Health and Human Services (Parts 1000--1999)

                   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 200--499)
        II  Bureau of Land Management, Department of the Interior 
                (Parts 1000--9999)

[[Page 806]]

       III  Utah Reclamation Mitigation and Conservation 
                Commission (Parts 10000--10005)

             Title 44--Emergency Management and Assistance

         I  Federal Emergency Management Agency (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)
       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)
         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  Office of Human Development Services, 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 on Fine Arts (Parts 2100--2199)
      XXII  Christopher Columbus Quincentenary Jubilee Commission 
                (Parts 2200--2299)
     XXIII  Arctic Research Commission (Part 2301)
      XXIV  James Madison Memorial Fellowship Foundation (Parts 
                2400--2499)
       XXV  Corporation for National and Community Service (Parts 
                2500--2599)

[[Page 807]]

                          Title 46--Shipping

         I  Coast Guard, Department of Transportation (Parts 1--
                199)
        II  Maritime Administration, Department of Transportation 
                (Parts 200--399)
       III  Coast Guard (Great Lakes Pilotage), Department of 
                Transportation (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)

           Title 48--Federal Acquisition Regulations System

         1  Federal Acquisition Regulation (Parts 1--99)
         2  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  United States 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  United States Information Agency (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)

[[Page 808]]

        34  Department of Education Acquisition Regulation (Parts 
                3400--3499)
        35  Panama Canal Commission (Parts 3500--3599)
        44  Federal Emergency Management Agency (Parts 4400--4499)
        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)
        54  Defense Logistics Agency, Department of Defense (Part 
                5452)
        57  African Development Foundation (Parts 5700--5799)
        61  General Services Administration Board of Contract 
                Appeals (Parts 6100--6199)
        63  Department of Transportation Board of Contract Appeals 
                (Parts 6300--6399)
        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  Research and Special Programs Administration, 
                Department of Transportation (Parts 100--199)
        II  Federal Railroad Administration, Department of 
                Transportation (Parts 200--299)
       III  Federal Highway Administration, Department of 
                Transportation (Parts 300--399)
        IV  Coast Guard, Department of Transportation (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, Department of 
                Transportation (Parts 1000--1399)
        XI  Bureau of Transportation Statistics, Department of 
                Transportation (Parts 1400--1499)

                   Title 50--Wildlife and Fisheries

         I  United States Fish and Wildlife Service, Department of 
                the Interior (Parts 1--199)

[[Page 809]]

        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)
        VI  Fishery Conservation and Management, National Oceanic 
                and Atmospheric Administration, Department of 
                Commerce (Parts 600--699)

                      CFR Index and Finding Aids

            Subject/Agency Index
            List of Agency Prepared Indexes
            Parallel Tables of Statutory Authorities and Rules
            List of CFR Titles, Chapters, Subchapters, and Parts
            Alphabetical List of Agencies Appearing in the CFR



[[Page 811]]





           Alphabetical List of Agencies Appearing in the CFR




                      (Revised as of July 1, 1999)

                                                  CFR Title, Subtitle or 
                     Agency                               Chapter

Administrative Committee of the Federal Register  1, I
Advanced Research Projects Agency                 32, I
Advisory Commission on Intergovernmental          5, VII
     Relations
Advisory Committee on Federal Pay                 5, IV
Advisory Council on Historic Preservation         36, VIII
African Development Foundation                    22, XV
  Federal Acquisition Regulation                  48, 57
Agency for International Development, United      22, II
     States
  Federal Acquisition Regulation                  48, 7
Agricultural Marketing Service                    7, I, IX, X, XI
Agricultural Research Service                     7, V
Agriculture Department
  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
  Cooperative State Research, Education, and      7, XXXIV
       Extension Service
  Economic Research Service                       7, XXXVII
  Energy, Office of                               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
  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                              32, VII
  Federal Acquisition Regulation Supplement       48, 53
Alcohol, Tobacco and Firearms, Bureau of          27, I
AMTRAK                                            49, VII
American Battle Monuments Commission              36, IV
American Indians, Office of the Special Trustee   25, VII
Animal and Plant Health Inspection Service        7, III; 9, I
Appalachian Regional Commission                   5, IX

[[Page 812]]

Architectural and Transportation Barriers         36, XI
     Compliance Board
Arctic Research Commission                        45, XXIII
Armed Forces Retirement Home                      5, XI
Army Department                                   32, V
  Engineers, Corps of                             33, II; 36, III
  Federal Acquisition Regulation                  48, 51
Assassination Records Review Board                36, XIV
Benefits Review Board                             20, VII
Bilingual Education and Minority Languages        34, V
     Affairs, Office of
Blind or Severely Disabled, Committee for         41, 51
     Purchase From People Who Are
Board for International Broadcasting              22, XIII
Census Bureau                                     15, I
Central Intelligence Agency                       32, XIX
Chief Financial Officer, Office of                7, XXX
Child Support Enforcement, Office of              45, III
Children and Families, Administration for         45, II, III, IV, X
Christopher Columbus Quincentenary Jubilee        45, XXII
     Commission
Civil Rights, Commission on                       45, VII
Civil Rights, Office for                          34, I
Coast Guard                                       33, I; 46, I; 49, IV
Coast Guard (Great Lakes Pilotage)                46, III
Commerce Department                               44, IV
  Census Bureau                                   15, I
  Economic Affairs, Under Secretary               37, V
  Economic Analysis, Bureau of                    15, VIII
  Economic Development Administration             13, III
  Emergency Management and Assistance             44, IV
  Export Administration, Bureau of                15, VII
  Federal Acquisition Regulation                  48, 13
  Fishery Conservation and Management             50, VI
  Foreign-Trade Zones Board                       15, IV
  International Trade Administration              15, III; 19, III
  National Institute of Standards and Technology  15, II
  National Marine Fisheries Service               50, II, IV, VI
  National Oceanic and Atmospheric                15, IX; 50, II, III, IV, 
       Administration                             VI
  National Telecommunications and Information     15, XXIII; 47, III
       Administration
  National Weather Service                        15, IX
  Patent and Trademark Office                     37, I
  Productivity, Technology and Innovation,        37, IV
       Assistant Secretary for
  Secretary of Commerce, Office of                15, Subtitle A
  Technology, Under Secretary for                 37, V
  Technology Administration                       15, XI
  Technology Policy, Assistant Secretary for      37, IV
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 Product Safety Commission                5, LXXI; 16, II
Cooperative State Research, Education, and        7, XXXIV
     Extension Service
Copyright Office                                  37, II
Corporation for National and Community Service    45, XII, XXV
Cost Accounting Standards Board                   48, 99
Council on Environmental Quality                  40, V
Customs Service, United States                    19, I
Defense Contract Audit Agency                     32, I
Defense Department                                5, XXVI; 32, Subtitle A; 
                                                  40, VII
  Advanced Research Projects Agency               32, I
  Air Force Department                            32, VII

[[Page 813]]

  Army Department                                 32, V; 33, II; 36, III, 
                                                  48, 51
  Defense Intelligence Agency                     32, I
  Defense Logistics Agency                        32, I, XII; 48, 54
  Engineers, Corps of                             33, II; 36, III
  Federal Acquisition Regulation                  48, 2
  National Imagery and Mapping Agency             32, I
  Navy Department                                 32, VI; 48, 52
  Secretary of Defense, Office of                 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
Drug Enforcement Administration                   21, II
East-West Foreign Trade Board                     15, XIII
Economic Affairs, Under Secretary                 37, V
Economic Analysis, Bureau of                      15, VIII
Economic Development Administration               13, III
Economic Research Service                         7, XXXVII
Education, Department of                          5, LIII
  Bilingual Education and Minority Languages      34, V
       Affairs, Office 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
  Vocational and Adult Education, Office of       34, IV
Educational Research and Improvement, Office of   34, VII
Elementary and Secondary Education, Office of     34, II
Employees' Compensation Appeals Board             20, IV
Employees Loyalty Board                           5, V
Employment and Training Administration            20, V
Employment Standards Administration               20, VI
Endangered Species Committee                      50, IV
Energy, Department of                             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                   5, LIV; 40, I, 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
  Administration, Office of                       5, XV
  Environmental Quality, Council on               40, V
  Management and Budget, Office of                25, III, LXXVII; 48, 99
  National Drug Control Policy, Office of         21, III
  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 Administration, Bureau of                  15, VII
Export-Import Bank of the United States           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

[[Page 814]]

Federal Aviation Administration                   14, I
  Commercial Space Transportation                 14, III
Federal Claims Collection Standards               4, II
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                       11, I
Federal Emergency Management Agency               44, I
  Federal Acquisition Regulation                  48, 44
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; 49, III
Federal Home Loan Mortgage Corporation            1, IV
Federal Housing Enterprise Oversight Office       12, XVII
Federal Housing Finance Board                     12, IX
Federal Labor Relations Authority, and General    5, XIV; 22, XIV
     Counsel of the Federal Labor Relations 
     Authority
Federal Law Enforcement Training Center           31, VII
Federal Maritime Commission                       46, IV
Federal Mediation and Conciliation Service        29, XII
Federal Mine Safety and Health Review Commission  5, LXXIV; 29, XXVII
Federal Pay, Advisory Committee on                5, IV
Federal Prison Industries, Inc.                   28, III
Federal Procurement Policy Office                 48, 99
Federal Property Management Regulations           41, 101
Federal Property Management Regulations System    41, Subtitle C
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
Fine Arts, Commission on                          45, XXI
Fiscal Service                                    31, II
Fish and Wildlife Service, United States          50, I, IV
Fishery Conservation and Management               50, VI
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
General Accounting Office                         4, I, II
General Services Administration                   5, LVII
  Contract Appeals, Board of                      48, 61
  Federal Acquisition Regulation                  48, 5
  Federal Property Management Regulations System  41, 101, 105
  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

[[Page 815]]

  Temporary Duty (TDY) Travel Allowances          41, 301
Geological Survey                                 30, IV
Government Ethics, Office of                      5, XVI
Government National Mortgage Association          24, III
Grain Inspection, Packers and Stockyards          7, VIII; 9, II
     Administration
Harry S. Truman Scholarship Foundation            45, XVIII
Health and Human Services, Department of          5, XLV; 45, Subtitle A
  Child Support Enforcement, Office of            45, III
  Children and Families, Administration for       45, II, III, IV, X
  Community Services, Office of                   45, X
  Family Assistance, Office of                    45, II
  Federal Acquisition Regulation                  48, 3
  Food and Drug Administration                    21, I
  Health Care Financing Administration            42, IV
  Human Development Services, Office of           45, XIII
  Indian Health Service                           25, V
  Inspector General (Health Care), Office of      42, V
  Public Health Service                           42, I
  Refugee Resettlement, Office of                 45, IV
Health Care Financing Administration              42, IV
Housing and Urban Development, Department of      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
  Inspector General, Office of                    24, XII
  Multifamily Housing Assistance Restructuring,   24, IV
       Office of
  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
Human Development Services, Office of             45, XIII
Immigration and Naturalization Service            8, I
Independent Counsel, Office of                    28, VII
Indian Affairs, Bureau of                         25, I, V
Indian Affairs, Office of the Assistant           25, VI
     Secretary
Indian Arts and Crafts Board                      25, II
Indian Health Service                             25, V
Information Agency, United States                 22, V
  Federal Acquisition Regulation                  48, 19
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
Institute of Peace, United States                 22, XVII
Inter-American Foundation                         5, LXIII; 22, X
Intergovernmental Relations, Advisory Commission  5, VII
     on
Interior Department
  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
  Minerals Management Service                     30, II
  Mines, Bureau of                                30, VI

[[Page 816]]

  National Indian Gaming Commission               25, III
  National Park Service                           36, I
  Reclamation, Bureau of                          43, I
  Secretary of the Interior, Office of            43, Subtitle A
  Surface Mining and Reclamation Appeals, Board   30, III
       of
  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 Development, United States        22, II; 48, 7
       Agency for
  Overseas Private Investment Corporation         5, XXXIII; 22, VII
International Fishing and Related Activities      50, III
International Investment, Office of               31, VIII
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
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                                5, XXVIII; 28, I
  Drug Enforcement Administration                 21, II
  Federal Acquisition Regulation                  48, 28
  Federal Claims Collection Standards             4, II
  Federal Prison Industries, Inc.                 28, III
  Foreign Claims Settlement Commission of the     45, V
       United States
  Immigration and Naturalization Service          8, I
  Offices of Independent Counsel                  28, VI
  Prisons, Bureau of                              28, V
  Property Management Regulations                 41, 128
Labor Department                                  5, XLII
  Benefits Review Board                           20, VII
  Employees' Compensation Appeals Board           20, IV
  Employment and Training Administration          20, V
  Employment Standards Administration             20, VI
  Federal Acquisition Regulation                  48, 29
  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
  Pension and Welfare Benefits Administration     29, XXV
  Public Contracts                                41, 50
  Secretary of Labor, Office of                   29, Subtitle A
  Veterans' Employment and Training, Office of    41, 61; 20, IX
       the Assistant Secretary for
  Wage and Hour Division                          29, V
  Workers' Compensation Programs, Office of       20, I
Labor-Management Standards, Office of             29, II, IV
Land Management, Bureau of                        43, II
Legal Services Corporation                        45, XVI
Library of Congress                               36, VII
  Copyright Office                                37, II
Management and Budget, Office of                  5, III, LXXVII; 48, 99
Marine Mammal Commission                          50, V
Maritime Administration                           46, II
Merit Systems Protection Board                    5, II
Micronesian Status Negotiations, Office for       32, XXVII
Mine Safety and Health Administration             30, I
Minerals Management Service                       30, II
Mines, Bureau of                                  30, VI

[[Page 817]]

Minority Business Development Agency              15, XIV
Miscellaneous Agencies                            1, IV
Monetary Offices                                  31, I
Multifamily Housing Assistance Restructuring,     24, IV
     Office of
National Aeronautics and Space Administration     5, LIX; 14, V
  Federal Acquisition Regulation                  48, 18
National Agricultural Library                     7, XLI
National Agricultural Statistics Service          7, XXXVI
National Archives and Records Administration      5, LXVI; 36, XII
  Information Security Oversight Office           32, XX
National Bureau of Standards                      15, II
National Capital Planning Commission              1, IV
National Commission for Employment Policy         1, IV
National Commission on Libraries and Information  45, XVII
     Science
National and Community Service, Corporation for   45, XII, XXV
National Council on Disability                    34, XII
National Credit Union Administration              12, VII
National Drug Control Policy, Office of           21, III
National Foundation on the Arts and the           45, XI
     Humanities
National Highway Traffic Safety Administration    23, II, III; 49, V
National Imagery and Mapping Agency               32, I
National Indian Gaming Commission                 25, III
National Institute for Literacy                   34, XI
National Institute of Standards and Technology    15, II
National Labor Relations Board                    5, LXI; 29, I
National Marine Fisheries Service                 50, II, IV, VI
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                       5, XLIII; 45, VI
  Federal Acquisition Regulation                  48, 25
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
     Administration
National Transportation Safety Board              49, VIII
National Weather Service                          15, IX
Natural Resources Conservation Service            7, VI
Navajo and Hopi Indian Relocation, Office of      25, IV
Navy Department                                   32, VI
  Federal Acquisition Regulation                  48, 52
Neighborhood Reinvestment Corporation             24, XXV
Northeast Dairy Compact Commission                7, XIII
Nuclear Regulatory Commission                     5, XLVIII; 10, I
  Federal Acquisition Regulation                  48, 20
Occupational Safety and Health Administration     29, XVII
Occupational Safety and Health Review Commission  29, XX
Offices of Independent Counsel                    28, VI
Operations Office                                 7, XXVIII
Overseas Private Investment Corporation           5, XXXIII; 22, VII
Panama Canal Commission                           48, 35
Panama Canal Regulations                          35, I
Patent and Trademark Office                       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                                       22, III
Pennsylvania Avenue Development Corporation       36, IX
Pension and Welfare Benefits Administration       29, XXV
Pension Benefit Guaranty Corporation              29, XL
Personnel Management, Office of                   5, I, XXXV; 45, VIII
  Federal Acquisition Regulation                  48, 17
  Federal Employees Group Life Insurance Federal  48, 21
     Acquisition Regulation
[[Page 818]]

  Federal Employees Health Benefits Acquisition   48, 16
       Regulation
Postal Rate 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 Commission on the Assignment of      32, XXIX
     Women in the Armed Forces
Presidential Documents                            3
Presidio Trust                                    36, X
Prisons, Bureau of                                28, V
Procurement and Property Management, Office of    7, XXXII
Productivity, Technology and Innovation,          37, IV
     Assistant Secretary
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
Regional Action Planning Commissions              13, V
Relocation Allowances                             41, 302
Research and Special Programs Administration      49, I
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
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                17, II
Selective Service System                          32, XVI
Small Business Administration                     13, I
Smithsonian Institution                           36, V
Social Security Administration                    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                                  22, I
  Federal Acquisition Regulation                  48, 6
Surface Mining and Reclamation Appeals, Board of  30, III
Surface Mining Reclamation and Enforcement,       30, VII
     Office of
Surface Transportation Board                      49, X
Susquehanna River Basin Commission                18, VIII
Technology Administration                         15, XI
Technology Policy, Assistant Secretary for        37, IV
Technology, Under Secretary for                   37, V
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                     5, L
  Coast Guard                                     33, I; 46, I; 49, IV
  Coast Guard (Great Lakes Pilotage)              46, III
  Commercial Space Transportation                 14, III
  Contract Appeals, Board of                      48, 63
  Emergency Management and Assistance             44, IV
  Federal Acquisition Regulation                  48, 12
  Federal Aviation Administration                 14, I
  Federal Highway Administration                  23, I, II; 49, III
  Federal Railroad Administration                 49, II
  Federal Transit Administration                  49, VI
  Maritime Administration                         46, II
  National Highway Traffic Safety Administration  23, II, III; 49, V
  Research and Special Programs Administration    49, I
  Saint Lawrence Seaway Development Corporation   33, IV

[[Page 819]]

  Secretary of Transportation, Office of          14, II; 49, Subtitle A
  Surface Transportation Board                    49, X
  Transportation Statistics Bureau                49, XI
Transportation, Office of                         7, XXXIII
Transportation Statistics Brureau                 49, XI
Travel Allowances, Temporary Duty (TDY)           41, 301
Treasury Department                               5, XXI; 12, XV; 17, IV
  Alcohol, Tobacco and Firearms, Bureau of        27, I
  Community Development Financial Institutions    12, XVIII
       Fund
  Comptroller of the Currency                     12, I
  Customs Service, United States                  19, I
  Engraving and Printing, Bureau of               31, VI
  Federal Acquisition Regulation                  48, 10
  Federal Law Enforcement Training Center         31, VII
  Fiscal Service                                  31, II
  Foreign Assets Control, Office of               31, V
  Internal Revenue Service                        26, I
  International Investment, 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
Utah Reclamation Mitigation and Conservation      43, III
     Commission
Veterans Affairs Department                       38, I
  Federal Acquisition Regulation                  48, 8
Veterans' Employment and Training, Office of the  41, 61; 20, IX
     Assistant Secretary for
Vice President of the United States, Office of    32, XXVIII
Vocational and Adult Education, Office of         34, IV
Wage and Hour Division                            29, V
Water Resources Council                           18, VI
Workers' Compensation Programs, Office of         20, I
World Agricultural Outlook Board                  7, XXXVIII

[[Page 821]]



List of CFR Sections Affected



All changes in this volume of the Code of Federal Regulations which were 
made by documents published in the Federal Register since January 1, 
1986, 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 and parts as well as 
sections for revisions.
Title 40 was established at 36 FR 12213, June 29, 1971. For the period 
before January 1, 1986, see the ``List of CFR Sections Affected, 1964-
1972 and 1973-1985'' published in six separate volumes.

                                  1986

40 CFR
                                                                   51 FR
                                                                    Page
Chapter I
136.3  (a) Tables IB and IE and (b) revised........................23693
136  Appendixes A, B, and C amended................................23702
141  Technical corrections..........................................4166
141.2  (v) added...................................................11410
141.6  (f) added...................................................11410
141.11  (c) revised................................................11410
141.23  (b) and (f)(10) revised; (f) footnotes 1 through 4 
        republished; (f) footnotes 5 through 7 and (g) added.......11410
    (f)(10) table corrected........................................24329
141.32  (a) amended................................................11411
141.60--141.62 (Subpart G)  Added..................................11411
142.61  Added......................................................11411
143  Authority citation revised....................................11412
143.3  Table amended...............................................11412
143.5  Added.......................................................11412
    (a) and (b) corrected..........................................24329
147.100  Revised...................................................16684

                                  1987

40 CFR
                                                                   52 FR
                                                                    Page
Chapter I
136.3  (a) Table IB amended; interim...............................33543
141  Authority citation revised.............................20674, 41546
    Nomenclature changes...........................................20674
141.2  (u) revised.................................................20674
    Amended; eff. 1-9-89...........................................25712
141.24  (g) added..................................................25712
141.32  (a) amended; eff. 1-9-89...................................25714
    Redesignated as 141.36 and introductory text added; eff. to 4-
22-89..............................................................41546
    Added; eff. 4-28-89............................................41546
141.34  Added......................................................41549
141.35  Added......................................................25714
141.36  Redesignated from 141.32 and introductory text added; eff. 
        to 4-28-89.................................................41546
141.40--141.43 (Subpart E)  Heading revised........................20674
141.40  Revised....................................................25715
141.43  Added......................................................20674
141.50  (b) revised; eff. 1-9-89...................................25716
141.60  Revised; eff. 1-9-89.......................................25716
141.61  Added; eff. 1-9-89.........................................25716
141.100--141.101 (Subpart J)  Added; eff. 1-9-89...................25716
142  Heading and authority citation revised........................20674
142.10  (a) revised................................................20675
142.30  (c), (d) and (e) removed...................................20675
142.31  Removed....................................................20675
142.41  (c)(6) revised.............................................20675
142.42  (c) redesignated as (d); new (c) added.....................20675
142.43  (b)(1), (c)(2), (f) and (g) revised........................20675
142.44  (a), (b) introductory text and (3), (c)(2) and (f) revised
                                                                   20675
142.45  Revised....................................................20675
142.53  (d) revised................................................20675
142.54  (d) revised................................................20675
142.55  (b) revised................................................20675
142.56  Added......................................................20676

[[Page 822]]

142.57  Added; eff. 1-9-89.........................................25716
142.62  Added; eff. 1-9-89.........................................25716
143.5  (a) and (b) introductory text revised.......................41550
144  Authority citation revised.............................20676, 45797
144.1  (a) and (d)(4) revised......................................20676
    (h) added......................................................45797
144.3  Amended.....................................................20676
144.6  (b)(1) revised..............................................20676
144.12  (b), (c)(2) and (e) revised................................20676
144.31  (g) revised................................................45797
    (a) amended....................................................46963
146  Test program approval extended to 7-14-88.....................26342
    Test program interim approval and requesty for comments.......41591, 
                                                                   44395
    Date paragraph corrected.......................................44520
147  Authority citation revised....................................17680
147.101  Revised...................................................17680
147.151  Revised...................................................17681
147.250  Introductory text revised.................................17681
147.251  Revised...................................................17681
147.301  Revised...................................................17681
147.651  Revised...................................................17681
147.801  Revised...................................................17681
147.1151  Revised..................................................17681
147.1351  Revised..................................................17681
147.1400  Introductory text revised................................17681
147.1401  Introductory text revised................................17681
147.1403  Added....................................................17681
147.1451  Revised..................................................17681
147.2101  Revised..................................................17682
149  Authority citation and heading revised; interim...............23986
149.1--149.3 (Subpart A)  Added; interim...........................23986
149.1--149.2 (Subpart A)  Heading removed; sections 149.1--149.2 
        redesignated as 149.100--149.101; interim..................23986
149.10--149.19 (Subpart B)  Heading removed; sections 149.10--
        149.19 redesignated as 149.102--149.111; interim...........23986
149.100--149.111 (Subpart B)  Heading added; interim...............23986
149.100--149.101  Redesignated from 149.1--149.2; interim..........23986
149.100  Amended...................................................23986
149.101  Amended...................................................23986
149.102--149.111  Redesignated from 149.10--149.19; interim........23986

                                  1988

40 CFR
                                                                   53 FR
                                                                    Page
Chapter I
141  Authority citation revised....................................37410
141.2  (d) and (h) revised.........................................37410
141.23  (f) introductory text, (1) through (5) and (9) revised; 
        footnotes 1 through 4 republished; footnote 8 added.........5146
141.24  (e) revised; footnotes 2 and 5 republished; footnote 6 
        added.......................................................5147
    (g)(1), (7) introductory text, (8) introductory text, (i)(A), 
(B)(1) and (2), and (ii) (A) and (B)(1) corrected; (g)(8)(v) 
correctly revised; (g)(15), (16), and (17) correctly removed; 
(g)(18) correctly redesignated as (g)(15); OMB number..............25110
141.35  (d) corrected..............................................25110
141.40  (a) Table 1, (b), (c), and (i) corrected; (k) correctly 
        revised; (m) correctly added...............................25110
141.60  (b) correctly revised......................................25111
141.61  (b) correctly revised......................................25111
141.100  (c) correctly revised; (d)(2) corrected...................25111
142  Authority citation revised....................................37410
142.2  (f) through (p) redesignated as (h) through (r); new (f) 
        and (g) added; new (i), (k), and (o) revised...............37410
142.3  (c) added...................................................37410
142.10  (b)(3) redesignated as (b)(3)(i); (b)(3)(ii) and (f) added
                                                                   37410
142.57  Correctly designated.......................................25111
142.62  Heading, (b), (c), (e), (f) introductory text, and (g) 
        introductory text and (5) correctly revised................25111
142.72--142.78 (Subpart H)  Added..................................37411
143  Authority citation revised....................................37412
143.2  (d) revised.................................................37412
143.4  (b) (3), (5), (6) and (11) revised...........................5147
144  Authority citation revised.............................28147, 37412
144.1  (f)(1)(vi) added............................................28147
144.3  Amended.....................................................37412

[[Page 823]]

144.39  (a) introductory text and (3) introductory text revised; 
        (b)(3) added...............................................28147
144.51  (j)(2)(ii) revised.........................................28147
144.52  (a) introductory text revised..............................28147
145  Authority citation revised....................................37412
145.1  (h) added...................................................37412
145.13  (e) added..................................................37412
145.21  (c) through (f) redesignated as (d) through (g); new added
                                                                   37412
145.52--145.58 (Subpart E) Added...................................37412
146  Authority citation revised.............................28148, 37414
    Test program interim approval and request for comments.........37294
    Test program approval extended to 3-27-89......................37296
146.3  Amended.....................................................37414
146.11  Revised....................................................28148
146.13  (d) added..................................................28148
146.61--146.73 (Subpart G) Added...................................28148
147  State withdrawal proceedings terminated.......................21450
    Petition denied................................................43080
    Authority citation revised....................................43086,
43104
147.50  Introductory text amended..................................43086
147.60  Added......................................................43086
147.151  Revised...................................................43086
147.200  Introductory text amended.................................43086
147.205  Added.....................................................43086
147.353  Added.....................................................43086
147.403  Added.....................................................43086
147.451  Revised...................................................43087
147.500  Introductory text amended.................................43087
147.501  Revised...................................................43087
147.553  Added.....................................................43087
147.601  Revised...................................................43087
147.700  Introductory text amended.................................43087
147.701  Introductory text amended.................................43087
147.703  Added.....................................................43087
147.751  Revised...................................................43087
147.901  Revised...................................................43087
147.951  Added.....................................................43087
147.1000  Introductory text amended................................43088
147.1001  Added....................................................43088
147.1053  Added....................................................43088
147.1100  Introductory text amended................................43088
147.1101  Added....................................................43088
147.1250  Introductory text amended................................43088
147.1251  Revised..................................................43088
147.1300  Introductory text amended................................43088
147.1303  Added....................................................43088
147.1450  Added....................................................39089
147.1451  Revised..................................................43088
147.1452  Removed and reserved.....................................43088
147.1500  Introductory text amended................................43088
147.1501  Added....................................................43088
147.1550  Introductory text amended................................43089
147.1551  Added....................................................43089
147.1600  Introductory text amended................................43089
147.1601  Introductory text amended................................43089
147.1603  Added....................................................43089
147.1651  Revised..................................................43089
147.1660  Removed..................................................43089
147.1703  Added....................................................43089
147.1750  Introductory text amended................................43089
147.1752  Added....................................................43089
147.1800  Introductory text amended................................43089
147.1805  Added....................................................43089
147.1850  Introductory text amended................................43090
147.1851  Introductory text amended................................43090
147.1852  Revised..................................................43090
147.1900  Heading revised; introductory text amended...............43090
147.1901  Added....................................................43090
147.1951  Revised..................................................43090
147.2000  Introductory text amended................................43090
147.2001  Added....................................................43090
147.2050  Heading revised; introductory text amended...............43090
147.2051  Added....................................................43090
147.2151  Revised..................................................43090
147.2200  Introductory text amended................................43091
147.2201  Introductory text amended................................43091
147.2205  Added....................................................43091
147.2250  Introductory text amended................................43091
147.2251  Introductory text amended................................43091
147.2253  Added....................................................43091

[[Page 824]]

147.2300  Heading revised; introductory text amended...............43091
147.2303  Added....................................................43091
147.2351  Revised..................................................43091
147.2403  Added....................................................43091
147.2404  Added....................................................43091
147.2453  Added....................................................43092
147.2550  Introductory text amended................................43092
147.2551  Introductory text amended................................43092
147.2553  Added....................................................43092
147.2554  Added....................................................43092
147.2600  Introductory text amended................................43092
147.2601  Added....................................................43093
147.2651  Revised..................................................43093
147.2701  Revised..................................................43093
147.2751  Revised..................................................43093
147.2801  Revised..................................................43093
147.2851  Revised..................................................43093
147.3000--147.3016 (Subpart HHH)  Added............................43104
147.3100--147.3109 (Subpart III) Added.............................43109
148  Added.........................................................28154
148.12  Added......................................................30918
    (b) revised....................................................41602
148.14  Added......................................................30918

                                  1989

40 CFR
                                                                   54 FR
                                                                    Page
Chapter I
141  Authority citation revised....................................27526
141.2  Amended; eff. 12-31-90......................................27526
    (d) and (h) redesignation removed; amended; eff. 12-31-90......27562
141.4  Revised; eff. 12-31-90......................................27562
141.13  Introductory text added; eff. 12-31-90.....................27527
141.14  Removed; eff. 12-31-90.....................................27562
    (b)(3) added...................................................30001
141.21  Revised; eff. 12-31-90.....................................27562
    (a) amended....................................................30001
141.22  Introductory text added; eff. 12-31-90.....................27527
141.31  (b) revised; eff. 12-31-90.................................27566
141.32  (a)(3) (i) and (ii) correctly revised......................15188
    (a)(1)(iii)(D) and (e)(10) added; eff. 12-31-90................27527
    (a)(1)(iii)(C), (e) (11) and (12) added; eff. 12-31-90.........27566
141.52  Added; eff. 12-31-90.......................................27527
    Table amended; eff. 12-31-90...................................27566
141.63  Added; eff. 12-31-90.......................................27566
141.70--141.75 (Subpart H)  Added; eff. 12-31-90...................27527
142  Authority citation revised.............................27537, 52137
142.2  Amended.....................................................52137
142.10  (b)(6)(v) correctly revised................................15188
    Introductory text, (a), and (d) revised........................52138
142.11  Introductory text and (a), (b) introductory text and (1) 
        through (6), and (c) through (e) redesignated as (a) 
        introductory text and (1), (a)(2) introductory text and 
        (2) (i) through (vi), and (a) (3) through (5); (b)(1) 
        through (3) redesignated from 142.12(a)(1) through (3); 
        heading, new (a) introductory text and (5) and (b)(3) 
        revised; (a)(6) added......................................52138
142.12  (a) (1) through (3) redesignated as 142.11 (b) (1) through 
        (3); section revised.......................................52138
142.13  (a) revised................................................52140
142.14  (a) introductory text, (1)(iii), (3) introductory text, 
        and (4) revised; (a)(4) redesignated as (a)(6); (a) (4) 
        added; eff. 12-31-90.......................................27537
    (a)(2) revised; (a)(5) added; eff. 12-31-90....................27567
142.15  (b) (3) and (4) and (e) added; eff. 12-31-90...............27539
    (b)(5) added; eff. 12-31-90....................................27567
    (a), (b), (c) (1), (2), and (d) revised; (b) (3), (4), (5) and 
(e) redesignated as (c)(1)(i) (A), (B), (ii), and (2)..............52140
142.16  Revised....................................................15188
    (b) added; eff. 12-31-90.......................................27539
    (c) added; eff. 12-31-90.......................................27567
142.17  Added......................................................52140
142.63  Added; eff. 12-31-90.......................................27568
142.64  Added; eff. 12-31-90.......................................27540
142.80--142.81 (Subpart I)  Added; eff. 12-31-90...................27540
144  Technical correction..........................................26198
144.1  (h) corrected...............................................21427
146  Test program interim approval and request for comments........34169
    Technical correction...........................................47451
147.1251  Revised...................................................8735

[[Page 825]]

147.1252  Revised...................................................8735
147.1253  Removed...................................................8735
147.1254  Removed...................................................8735
147.1651  (b) corrected............................................10616
148.10  (c)(4) removed; (c) (1) and (3) revised....................25422
148.11  (b)(4) removed; (b) (1) and (3) revised....................25422
148.14  Revised....................................................25423
    (b), (c), and (d) redesignated as (d), (e), and (g); new (g) 
introductory text revised; new (b), (c), and (f) added.............26647
    (a) revised....................................................35328
148.15  Added......................................................25423
    (b) redesignated as (e); new (e) introductory text revised; 
new (b), (c), and (d) added........................................26647
148.16  Added......................................................25423
    (b) redesignated as (c); new (c) introductory text revised; 
new (b) added......................................................26647
149.2  Revised......................................................6843
149.3  Revised......................................................6843

                                  1990

40 CFR
                                                                   55 FR
                                                                    Page
Chapter I
136.3  Table 1B amended; eff. 7-16-90..............................24534
    Tables IB and II amended; footnote 34 added....................33440
136.5  (e) revised.................................................33440
136  Appendix C amended............................................33440
    Appendix D added...............................................33442
141  Handbook availability..........................................4423
    Public meeting..................................................8948
    Technical corrections; eff. 12-31-90...........................25064
141.6  (a) revised; (g) added......................................30274
141.11  (b) introductory text revised; eff. 7-30-92................30274
141.12  (c) table revised..........................................30274
141.21  (a)(2), (3)(i), (iv), (4), (c)(1)(iii), (d)(1)(i), (e)(2), 
        (f)(3)(iv), (4), and (5) corrected; eff. 12-31-90..........25064
141.23  (a)(4)(i) introductory text, (i)(1), (k)(1) table, (2), 
        (4) table, and (5)(ii) table revised; (l) through (q) 
        added; eff. 7-30-92........................................30274
141.24  (e), (f), (h)(8), (12)(iv), (vi) and (vii), (13)(i), and 
        (g) introductory text revised; (h)(19) and (g)(8) added; 
        eff. 7-30-92...............................................30277
141.32  (e)(11) and (12) corrected; eff. 12-31-90..................25064
    (e)(16), (25) through (27), and (46) added; eff. 1-1-93........30279
141.50  (a)(15) added; (b) table amended; eff. 1-1-93..............30280
141.51  (b) table amended; eff. 1-1-93.............................30280
141.52  Corrected; eff. 12-31-90...................................25064
141.61  (c) table amended; eff. 1-1-93.............................30280
141.62  (b) table amended..........................................30280
    (b) table amended; eff. 1-1-93.................................30280
141.63  (d)(4) corrected; (d)(5) revised; eff. 12-31-90............25064
142  Handbook availability..........................................4423
    Technical corrections; eff. 12-31-90...........................25064
142.14  (a)(5)(ii)(A) and (G) corrected; eff. 12-31-90.............25065
142.15  (c)(2) corrected; eff. 12-31-90............................25065
142.16  (c) introductory text, (2)(i), (ii), (iii), (iv), (v), 
        (vi), (vii), (viii), (ix), and (x) corrected; eff. 12-31-
        90.........................................................25065
142.57  (b) revised; eff. 7-30-92..................................30281
143  Handbook availability..........................................4423
143.4  (b)(12) and (13) revised; eff. 7-30-92......................30281
145  Exemption approval............................................21191
    Exemption approval corrected...................................34017
148.1  (d) added...................................................22683
148.14  (d), (e), (f), and (g) redesignated as (e), (g), (h), and 
        (j); new (j) introductory text revised; new (d), (f), and 
        (i) added..................................................22683
148.15  (d) and (e) redesignated as (e) and (g); new (g) 
        introductory text revised; new (d) and (f) added...........22683
148.16  (c) redesignated as (g); new (g) introductory text 
        revised; new (c), (d), (e), and (f) added..................22683
    (c) and (f) revised............................................33694

                                  1991

40 CFR
                                                                   56 FR
                                                                    Page
Chapter I
136.3  (b) amended.................................................43702

[[Page 826]]

    (a) Tables IA through IE, (b), (c), (d) and (e) revised........50759
141.2  Amended; eff. 7-30-92........................................3578
    Amended; eff. 11-6-91..........................................26547
    Regulation at 56 FR 26547 effective date corrected to 12-7-92 
                                                                   32113
141.4  Existing text designated as (a); (b) added...................1557
    Technical correction...........................................61287
141.6  (a) revised; (g) added......................................30274
141.11  (b) introductory text revised; (b) table amended; eff. 7-
        30-92.......................................................3578
    (b) introductory text revised; eff. 11-6-91....................26548
    (b) introductory text revised; eff. 7-30-92....................30274
    Regulation at 56 FR 26548 effective date corrected to 12-7-92 
                                                                   32113
141.12  Revised; eff. 7-30-92.......................................3578
    Table amended..................................................30274
141.21  (f)(5) revised; (f)(6) redesignated as (f)(7); new (f)(6) 
        added........................................................642
    (f)(7) amended...................................................643
141.23  Revised; eff. 7-30-92.......................................3579
    (a)(4)(i) introductory text, (i)(1), (k)(1) table, (2), (4) 
table, and (5)(ii) table revised; (l) through (q) added; eff. 7-
30-92..............................................................30274
141.24  (a) introductory text, (e) and (f) revised; (h) added; 
        eff. 7-30-92................................................3583
    (e), (f), (g) introductory text, (h)(8), (12) (iv), (vi) and 
(vii), and (13)(i) revised; (g)(8) and (h)(19) added; eff. 7-30-92
                                                                   30277
141.32  (a)(1)(iii)(B) revised;(e)(15), (17) through (24), (28) 
        through (45) and (47) through (52) added; eff. 7-30-92......3587
    (e)(13) and (14) added; eff. 11-6-91...........................26548
    (e) (16), (25) through (27), and (46) added; eff. 1-1-93.......30279
    Regulation at 56 FR 26548 effective date corrected to 12-7-92 
                                                                   32113
141.40  Heading revised; (n) added; eff. 7-30-92....................3592
141.50  (a)(6) through (14) and (16) through (18) added; (b) table 
        amended; eff. 7-30-92.......................................3592
    (a)(15) added; (b) table amended; eff. 1-1-93..................30280
141.51  (b) table amended; eff. 7-30-92.............................3593
    (b) table amended; eff. 11-6-91................................26548
    (b) table amended; eff. 1-1-93.................................30280
    Regulation at 56 FR 26548 effective date corrected to 12-7-92 
                                                                   32113
141.60  Revised; eff. 7-30-92.......................................3593
141.61  Revised; eff. 7-30-92.......................................3593
    (c) table amended; eff. 1-1-93.................................30280
141.62  Revised; eff. 7-30-92.......................................3594
    (c) table amended; eff. in part 7-30-92 and 1-1-93.............30280
141.80--141.91 (Subpart I)  Added; 141.80--141.85 eff. 11-6-91; 
        141.86--141.91 eff. 6-6-91.................................26548
141.80  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92; (a)(2) corrected.....................................32113
141.81  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.82  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.83  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.84  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.85  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.86  Regulation at 56 FR 26548 effective date corrected to 7-7-
        91; (b)(2) corrected.......................................32113
141.87  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.88  Regulation at 56 FR 26548 effective date corrected to 12-
        7-92.......................................................32113
141.89  Regulation at 56 FR 26548 effective date corrected to 7-7-
        91.........................................................32113
141.90  Regulation at 56 FR 26548 effective date corrected to 7-7-
        91.........................................................32113
141.91  Regulation at 56 FR 26548 effective date corrected to 7-7-
        91.........................................................32113
141.110--141.111 (Subpart K) Added; eff. 7-30-92....................3594

[[Page 827]]

142.14  (a)(6), (c), (d) introductory text and (f) revised; (d)(4) 
        through (7) added; eff. 7-30-92.............................3595
    (d)(8) through (11) added......................................26562
    Regulation at 56 FR 26562 effective date corrected to 7-7-91 
                                                                   32113
142.15  (c)(3) added; eff. 7-30-92..................................3595
    (c)(4) added...................................................26562
    Regulation at 56 FR 26562 effective date corrected to 7-7-91 
                                                                   32113
142.16  (e) added; eff. 7-30-92.....................................3595
    (d) added......................................................26563
    Regulation at 56 FR 26563 effective date corrected to 7-7-91 
                                                                   32113
142.17  (a)(2) republished; eff. 7-3-91............................25050
142.18  Added; eff. 7-30-92.........................................3595
142.19  Added; eff. 11-6-91........................................26563
    Regulation at 56 FR 26563 effective date corrected to 12-7-92 
                                                                   32113
142.57  Revised; eff. 7-30-92.......................................3596
    (b) revised; eff. 7-30-92......................................30281
142.62  Revised; eff. 7-30-92.......................................3596
    Heading, (f) and (g) revised;(h)(7) added; eff. 11-6-91........26563
    Regulation at 56 FR 26563 effective date corrected to 12-7-92 
                                                                   32113
142.63  Existing text designated text as (a); (b) added.............1557
    Technical correction...........................................61287
142.201--142.208 (Subpart J) Added..................................3755
143.3  Table revised; eff. 7-30-92..................................3597
143.4  (b)(12) and (13) added; eff. 7-30-92.........................3597
    (b) (12) and (13) revised; eff. 7-30-92........................30281
147.50  (a)(1) and (2) revised......................................9411
147.60  (a) revised.................................................9411
147.100  (b) revised................................................9411
147.101  (a) revised................................................9412
147.151  (a) revised................................................9412
147.205  (a) revised................................................9412
147.250  (a)(1) and (2) revised.....................................9412
147.251  (a) revised................................................9412
147.300  Heading revised; text added................................9412
147.301  (a) revised................................................9413
147.350  Added......................................................9413
147.353  (a) revised................................................9413
147.400  Added......................................................9413
147.403  (a) revised................................................9413
147.451  (a) revised................................................9413
147.500  (a)(2) revised.............................................9414
147.501  (a) revised................................................9414
147.550  Added......................................................9414
    (a)(3) corrected...............................................14150
147.553  (a) revised................................................9414
147.601  (a) revised................................................9414
147.651  Heading and (a) revised....................................9414
147.703  (a) revised................................................9414
147.750  Added.....................................................41072
147.751  (a) revised.........................................9414, 41072
147.753  Heading revised...........................................41072
147.754  Removed...................................................41072
147.755  Removed...................................................41072
147.801  (a) revised................................................9415
147.850  (a) through (e) added......................................9415
147.860  (a) revised................................................9415
147.901  (a) revised................................................9415
147.950  Introductory text amended; (a)(2), (b)(1) revised; 
        (a)(3)(iv) through (vii), and (c)(3) added..................9415
147.951  (a) revised................................................9415
147.1000  (a) revised...............................................9415
147.1001  (a) revised...............................................9416
147.1050  Added.....................................................9416
147.1053  (a) revised...............................................9416
147.1101  (a) revised...............................................9416
147.1151  (a) revised...............................................9416
147.1201  (a) revised...............................................9416
147.1252  (a) revised...............................................9416
147.1300  (a)(2) revised; (a)(3) added..............................9416
147.1303  (a) revised...............................................9417
147.1351  (a) revised...............................................9417
147.1400  (a)(2) and (b)(1) revised.................................9417
147.1401  (a)(1), (2) and (b)(1) revised............................9417
147.1403  (a) revised...............................................9417
147.1451  (a) revised...............................................9417
147.1500  Introductory text revised.................................9417
147.1501  (a) revised...............................................9417
147.1550  (a)(1) and (2) revised....................................9417
147.1551  (a) revised...............................................9417
147.1651  (a) revised...............................................9417
147.1700  Added.....................................................9417
147.1703  (a) revised...............................................9418
147.1750  (a)(1), (2) and (b) revised; (a)(3) added.................9418
147.1751  (a)(2), (4) and (b)(3) revised............................9418
147.1752  (a) revised...............................................9418
147.1805  (a) revised...............................................9418
147.1900  Introductory text amended; (a)(2), (b)(1) and (2) 
        revised.....................................................9418

[[Page 828]]

147.1901  (a) revised...............................................9419
147.1951  (a) revised...............................................9419
147.2001  (a) revised...............................................9419
147.2051  (a) revised...............................................9419
147.2100  (a)(2) revised............................................9419
147.2101  Heading and (a) revised...................................9419
147.2151  (a) revised...............................................9419
147.2205  (a) revised...............................................9419
147.2250  Revised...................................................9419
147.2251  (a)(1) revised; (a)(2) and (d)(3) added...................9420
147.2253  (a) revised...............................................9420
147.2300  Introductory text revised.................................9420
147.2303  (a) revised...............................................9420
147.2351  Revised...................................................9420
147.2400  (a)(4) added..............................................9420
147.2403  (a) revised...............................................9420
147.2453  (a) revised...............................................9420
147.2500  (a) through (e) added.....................................9420
    (a) introductory text corrected................................14150
147.2550  (a)(1) revised; (b)(1) removed; (a)(5), (b)(2) and (3) 
        redesignated as (a)(6), (b)(1) and (2) and revised; new 
        (a)(5) and new (b)(3) added.................................9421
147.2551  Revised...................................................9421
147.2553  (a) revised...............................................9422
147.2601  (a) revised...............................................9422
147.2651  (a) revised...............................................9422
147.2701  (a) revised...............................................9422
147.2751  (a) revised...............................................9422
147.2801  (a) revised...............................................9422
147.2851  (a) revised...............................................9422
147.3000  (a) revised...............................................9422
147.3100  (a) revised...............................................9422
148  Extension.....................................................24138
148.10  (c) redesignated as (e); new (c), (d) and Tables A and B 
        added.......................................................3876
148.16  (c) revised.................................................3876

                                  1992

40 CFR
                                                                   57 FR
                                                                    Page
Chapter I
136.3  (a) Table 1B, (b) table amended.............................41833
141.2  Amended.....................................................31838
141.6  (g) amended.................................................22178
    (h) added......................................................31838
141.12  Table amended..............................................31838
141.21  (f)(7) redesignated as (f)(8); new (f)(7) added.............1852
    (f)(3)(ii) and (iv) amended;(f)(6)(iii) added; (f)(7) revised; 
eff. 7-10-92.......................................................24747
141.23  (k)(4) and (5) redesignated as (k)(5) and (6); (a)(4) 
        introductory text, (a)(4)(i) introductory text, Table, (c) 
        introductory text, (1), (i)(1), new (k)(5) and (6) 
        revised; (a)(4)(iii) and new (k)(4) added..................31838
141.24  (f) introductory text, (4), (5), (7), (10), (11), 
        introductory text, (12), (14) introductory text, (15) 
        introductory text, (16) introductory text, (17), (18), 
        (h)(10), (12)(ii), (iii), (iv), (vi), (vii), (viii), (18) 
        and (19)(i)(B) revised; (h)(12)(ix) through (xiv) added....31841
141.24  (h) introductory text amended; footnote 7 added............22178
141.32  (e)(53) through (75) added.................................31843
141.40  (e) through (h), (n)(11) and (12) revised; eff. 1-17-94....31845
141.50  (a)(19) through (23) added; (b) table amended; effective 
        in part 8-17-92 and 1-17-94................................31846
141.51  (b) table amended; eff. 1-17-94............................31846
141.60  (a)(3) and (b)(3) added....................................31846
141.61  (a)(19), (20), (21) and (c)(19) through (33) added; (b) 
        and (c) introductory text revised; effective in part 8-17-
        92 and 1-17-94.............................................31846
141.62  (b) introductory text and (c) revised; (b)(11) through 
        (b)(15) added; eff. 1-17-94................................31847
141.80  (a)(2) revised; eff. 12-7-92...............................28788
141.84  (g) revised; eff. 12-7-92..................................28788
141.85  (a)(1) amended;(a)(4)(iv)(B) revised;eff. 12-7-92..........28788
141.86  (a)(9) revised; (b)(2), (d)(1) table and (ii)(B) amended 
                                                                   28789
141.87  (e)(2) amended; (e)(4) revised.............................28788
141.88  (c) revised................................................28788
    (e)(2) amended.................................................28789
141.89  (a) table amended; (a) table footnotes 5, 6 and 7 and 
        (a)(4) revised.............................................28789
    (a) table amended..............................................31847
141.90  (c)(1) and (e)(2)(ii) revised..............................28789

[[Page 829]]

142.16  (e) introductory text and (2) revised; eff. 1-17-94........31847
142.62  (a) and (b) revised; eff. 1-17-94..........................31848
    (f), (g) introductory text and (h)(7) revised; eff. 7-30-92....28789
146  Test program approval..........................................1109
146.68  (d)(4) revised.............................................46294
147.2650  Revised..................................................33446
147.2651  Revised..................................................33447
148.1  (d) revised..................................................8088
    (d) revised....................................................31963
148.10  Table A amended.............................................8088
148.17  Added......................................................37263
    Regulation at 57 FR 37263 effective date corrected......39275, 41173

                                  1993

40 CFR
                                                                   58 FR
                                                                    Page
Chapter I
141.30  (e)(3) and (4) added; (e) amended..........................41345
144  OMB number....................................................34370
144.3  Amended.....................................................63895
144.11  Amended....................................................63895
144.17  Added......................................................63895
144.21  Introductory text, (a), (b) and (c) redesignated as (a), 
        (b), (d) and (e); new (a) and new (b) revised; new (c) 
        added......................................................63895
144.22  (a) revised; (b) redesignated as (d); new (b) and new (c) 
        added......................................................63896
144.24  Revised....................................................63896
144.25  (a) introductory text, (b) and (c) amended.................63896
144.26  Introductory text revised; (d) introductory text added.....63896
    (e) added; interim.............................................63896
144.27  Amended; (d) added.........................................63896
144.28  Introductory text, (d)(1), (2) and (l) revised; (f)(2) and 
        (3) redesignated as (f)(5) and (6); (d)(5), (6), new 
        (f)(2), (3) and (4) added..................................63897
144.31  (a) and (c)(2) revised; (e)(10) added......................63897
144.51  (p) removed; (o) redesignated as (p); new (o) and (q) 
        added......................................................63898
144.52  (a)(7) revised.............................................63898
146  OMB number....................................................34370
146.2  Revised.....................................................63898
146.8  (b)(1) revised; (f) added...................................63898
146.15  Removed....................................................63898
146.25  Removed....................................................63898
146.35  Removed....................................................63899
146.52  (a) removed; (b) redesignated as new (a)...................63899

                                  1994

40 CFR
                                                                   59 FR
                                                                    Page
Chapter I
136.3  (a) tables, (b) and (e) table amended........................4505
141.2  Amended.....................................................34322
141.6  (a) revised; (h) amended....................................34322
141.21  (f)(3) revised; (f)(4) removed; (f)(5), (6)(i), (ii) and 
        (8) amended; (f)(6)(iv) added..............................62466
141.22  (a) amended................................................62466
141.23  (a)(1), (2) and (5), and (f)(1) revised; (a)(4)(i) table, 
        (c)(1), (2) and (5)(iii) amended...........................34322
    (i)(1) and (2) amended; (k)(1) removed; (k)(4), (5) and (6) 
redesignated as (k)(1), (4) and (5); new (k)(1) table, (q)(3) and 
(4) amended........................................................34323
    (k)(1) revised; (k)(2), (3) and (q) removed; (k)(4) and (5) 
redesignated as (k)(2) and (3).....................................62466
    (e) added; (f)(16) and (h)(12) removed; (h)(13) introductory 
text and (i) revised...............................................62468
141.24  (a) through (e) removed; (f)(4), (7), (10), (16) 
        introductory text and (20) amended; (f)(14)(i) and (iii), 
        (h)(4)(i) and (12) introductory text revised; (q) removed; 
        (h)(10)(i), (ii) and (iii) and (12)(xv) added..............34323
141.28  Heading and (a) amended....................................34323
141.30  (e) revised; Appendixes A, B and C removed.................62469
    (g), (n)(11) and (12) revised..................................62469
141.32  (e)(30), (33), (35), (41) and (62) amended.................34323
141.40  Heading amended; (e)(5) and (g) revised....................34323
    (h) amended; (j)(2) removed; (j)(3) through (15) redesignated 
ad (j)(2) through (14); (n)(11) revised............................34324
    (g), (n) (11) and (12) revised.................................62469
141.41  (d) revised................................................62470
141.42  (a), (b) and (c) removed...................................62470
141.60  (a)(3) revised.............................................34324

[[Page 830]]

141.61  (b) introductory text amended; (b) table revised...........34324
    (c) table amended..............................................34325
141.62  (c) table amended..........................................34325
141.74  (a)(1) and (2) revised; (a)(3) through (7) removed.........62470
141.81  (c) amended................................................33862
141.87  Introductory text revised..................................33862
141.89  (a) introductory text, table, (1)(ii) and (3) revised; 
        (a)(4) removed.............................................33863
141.89  (a) introductory text revised; (a) table and (b) removed 
                                                                   62470
141.90  (g) revised................................................33864
142.2  Amended.....................................................64344
142.3  (c) amended.................................................64344
142.16  (d) added..................................................33864
142.62  (g)(2) amended.............................................33864
    (a) table amended..............................................34325
142.72--142.78 (Subpart H)  Heading revised........................64344
142.72  Heading, introductory text and (d) revised.................64344
142.76  Heading, introductory text, (b) introductory text, (c), 
        (d) introductory text (1) and (e) amended; (f) revised.....64344
142.78  Heading and (a) amended; (b), (c) and (d) removed; (e) 
        redesignated as (b)........................................64345
143.4  (b) revised.................................................62470
144.3  Amended.....................................................64345
144.70  (d) amended; eff. 8-9-94...................................29959
145.1  (h) amended.................................................64345
145.52--145.58 (Subpart E)  Heading amended........................64345
145.52  Heading, introductory text and (d) revised.................64345
145.56  Heading, (b) introductory text, (c), (d) introductory 
        text, (1), and (e) amended; (f) revised....................64345
145.58  (b), (c) and (d) removed; (e) redesignated as (b); 
        heading, (a) and new (b) amended...........................64345
148.17  (b) and (c) redesignated as (d) and (e); new (b) and new 
        (c) added..................................................48041

                                  1995

40 CFR
                                                                   60 FR
                                                                    Page
Chapter I
136.3  (a), (b) and (e) table amended..............................17160
136.3  (a) Tables IC and ID amended................................39588
    (b) amended....................................................39590
    (a) table and (b) amended......................................44672
    (a) Table IA revised; (b) amended..............................53542
    (e) Table II amended...........................................53543
140.3  (h) removed.................................................33932
140.4  (b)(1) introductory text redesignated as (b)(1)(i); 
        (b)(1)(ii) added...........................................63945
141.11  (a) and (b) revised; (c) removed...........................33932
141.21  (f)(3) table amended.......................................34085
141.23  (a)(4)(i) table and (k)(3)(ii) table amended...............33932
    (k)(1) table and (2) table amended.............................34085
141.24  (h)(18) table amended......................................34085
141.30  (c)(1) amended; (e) revised; (g) added.....................34085
141.32  (e)(56) removed............................................33932
141.34  Removed....................................................33932
141.51  (b) table amended..........................................33932
141.62  (b) table amended..........................................33932
141.74  (a)(1) revised.............................................34086
142.11  (b)(2) revised; eff. 7-28-95...............................33661
142.13  (a) amended; eff. 7-28-95..................................33661
142.17  (a)(1) amended; (a)(2) and (4) revised; eff. 7-28-95.......33661
144.15  Removed....................................................33932
144.23  (b)(2) removed.............................................33932
146.52  Removed....................................................33932
148.1  (c)(4) removed..............................................33932

                                  1996

40 CFR
                                                                   61 FR
                                                                    Page
141.2  Amended; eff. 6-18-96 through 12-31-00......................24368
141.6  (a) amended; (i) added; eff. 6-18-96 through 12-31-00.......24368
141.140--141.144 (Subpart M)  Added; eff. 6-18-96 through 12-31-00
                                                                   24368
147.1350  Revised..................................................58933
147.1351  (a) amended..............................................58933
147.1350--147.1355  Appendix A added...............................58934

[[Page 831]]

148.1  (a), (b) and (d) revised; eff. 4-8-98.......................15596
    Regulation at 61 FR 15596 withdrawn in part....................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117
    (d) revised....................................................33682
148.3  Revised; eff. 4-8-98........................................15597
    Regulation at 61 FR 15597 withdrawn............................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117
148.4  Revised; eff. 4-8-98........................................15597
    Regulation at 61 FR 15597 withdrawn............................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117
148.17  (c) removed................................................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117
148.18  Added; eff. in part 1-8-97 and in part 4-8-98..............15597
    Regulation at 61 FR 15597 withdrawn; added.....................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117
148.20  (a) introductory text revised; eff. 4-8-96.................15597
    Regulation at 61 FR 15997 withdrawn............................15662
    Regulation at 61 FR 15662 eff. date corrected to 4-8-96........19117

                                  1997

40 CFR
                                                                   62 FR
                                                                    Page
Chapter I
136.3  (e) Table II corrected; CFR correction......................13833
    (a) Table 1C amended...........................................48403
    (b)(1) and (e) Table II amended................................48404
136  Appendix A amended............................................48405
136.4  (d) introductory text revised...............................30763
136.5  (b), (c), (d), (e)(1) and (2) revised.......................30763
141.25  (a) revised.........................................10172, 10173
147.750  (a) introductory text amended..............................1834
147.2500  (a) introductory text amended.............................1834
148  Notice........................................................43109
148.18  Heading revised; (a), (b) and (c) redesignated as (c), (d) 
        and (e); new (a) added; eff. 8-11-97; new (b) added; eff. 
        5-12-99....................................................26018

                                  1998

40 CFR
                                                                   63 FR
                                                                    Page
Chapter I
136.3  (e) corrected...............................................38756
    Table 1C corrected; CFR correction.............................44146
    (a) introductory text and (b) introductory text revised; Table 
1F and (b)(40) added...............................................50423
140  Authority citation revised.....................................1320
140.4  (a) introductory text, (b) introductory text and (1) 
        amended; (c)(1), (2), (3), and (4) introductory text 
        added; (b)(1)(ii) redesignated as (c)(4)(i).................1320
141  Authority citation revised.............................43846, 44526
141.2  Amended.......................................23366, 69463, 69515
141.4  (a) revised.................................................43846
141.12  Revised....................................................69463
141.21  (f)(3) revised; (f)(5), (6)(i), (ii) and (8) amended.......47107
    Regulation at 63 FR 47107 withdrawn............................72200
141.23  (a)(4)(iii), (k)(1) table, (2), (3)(i), (ii) introductory 
        text revised...............................................47107
    Regulation at 63 FR 47107 withdrawn............................72200
141.24  (e), (f)(14)(ii), (17)(i)(A), (B), (ii)(A), (h)(10)(ii), 
        (13) introductory text, (i), (19)(i)(A) and (B) 
        introductory text revised..................................47110
    Regulation at 63 FR 47110 withdrawn............................72200
141.30  (d) and (f) amended; (h) added.............................69464
141.32  (a) heading, (1)(iii) introductory text and (c) amended; 
        (a)(1)(iii)(E) and (e)(76) through (81) added..............69464
    (e)(10) revised................................................69515
141.40  (g) and (n)(11) introductory text revised; (n)(11) table 
        amended....................................................47112
    Regulation at 63 FR 47112 withdrawn............................72200
141.50--141.54 (Subpart F)  Heading revised........................69465
141.52  Table amended..............................................69515

[[Page 832]]

141.53  Added......................................................69465
141.54  Added......................................................69465
141.60--141.65 (Subpart G)  Heading revised........................69465
141.64  Added......................................................69465
141.65  Added......................................................69465
141.70  (d) added..................................................69516
141.71  (b)(6) revised.............................................69516
141.73  (a)(3) added; (d) revised..................................69516
141.74  (a) introductory text and (2) amended; (a)(1) table 
        revised....................................................47113
    Regulation at 63 FR 47113 withdrawn............................72200
141.89  (a)(1)(i) and (ii)(B) amended..............................47113
    Regulation at 63 FR 47113 withdrawn............................72200
141.101  Revised...................................................31934
141.130--141.135 (Subpart L)  Added................................69466
141.151--141.155 (Subpart O)  Added (OMB numbers pending)..........44526
141.153  (d)(4)(v)(C) amended......................................69516
141.154  (e) added.................................................69475
141.170--141.175 (Subpart P)  Added................................69516
142  Authority citation revised....................................44535
142.2  Amended.....................................................23367
142.10  (e) revised; (f) redesignated as (g); new (f) added........23367
    (d) revised....................................................43846
    (b)(6)(vii) added..............................................44535
142.11  (a)(6) redesignated as (a)(7); new (a)(6) added (effective 
        date pending)..............................................23367
142.12  (b)(1) revised; (e) added..................................23367
142.14  (d)(12) through (16) added.................................69475
    (a)(3), (4)(i) and (ii) introductory text revised; (a)(7) 
added..............................................................69519
142.15  (c)(5) added...............................................69520
142.16  (f) added..................................................44535
    (h) added......................................................69475
    (b)(1) redesignated as (b)(1)(i); (b)(1)(ii), (3) and (g) 
added..............................................................69520
142.20  Revised....................................................43847
142.40--142.46 (Subpart E)  Heading revised........................43847
142.42  (c) revised................................................43847
142.50  Revised....................................................43847
142.53  (c)(1) revised.............................................43848
142.55  (b) revised; (c) removed...................................43848
142.56  Revised....................................................43848
142.72  Introductory text revised..................................44535
142.78  (b) revised.........................................44536, 71376
142.201--142.208 (Subpart J)  Removed..............................48077
142.301--142.313 (Subpart K)   Added...............................43848
143.4  (b) table revised...........................................47113
    Regulation at 63 FR 47113 withdrawn............................72200
148.18  (f) added; eff. 11-4-98....................................24624
    (a) through (f) redesignated as (c) through (h); new (a) and 
(b) added; eff. 8-24-98............................................28636
    (f) revised....................................................35149
    (i) added......................................................42184
    Regulation at 63 FR 35149 eff. date corrected to 11-4-98.......42581

                                  1999

   (Regulations published from January 1, 1999, through July 1, 1999)

40 CFR
                                                                   64 FR
                                                                    Page
Chapter I
136  Technical correction..........................................13053
136.3  (b)(41) added; (e) Table II amended..........................4978
    (a) introductory text corrected................................10392
    (a) table amended..............................................26327
    (a) table amended; eff. 7-8-99.................................30433
    (b)(40) added; eff. 7-8-99.....................................30434
141.40  (l) amended.................................................1498
141.153  (f) corrected.............................................34733
141.154  (d) corrected.............................................34733
141.151--141.155 (Subpart O)  Appendixes A and B corrected.........34733
142.16  (f)(2) and (3) corrected...................................34733
147.2555  Added....................................................14803