[Federal Register Volume 59, Number 20 (Monday, January 31, 1994)]
[Unknown Section]
[Page 0]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 94-1625]


[[Page Unknown]]

[Federal Register: January 31, 1994]


_______________________________________________________________________

Part IV





Environmental Protection Agency





_______________________________________________________________________



40 CFR Part 136



Preparation of Guidelines Establishing Test Procedures for the analysis 
of Pollutants Under the Clean Water Act: Technical Amendments; Final 
Rule
ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 136

[FRL-4828-0]

 

Guidelines Establishing Test Procedures for the Analysis of 
Pollutants Under the Clean Water Act; Technical Amendments

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule: technical amendments.

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

SUMMARY: This action under the Clean Water Act (CWA) section 304(h) 
amends 40 CFR part 136 to add clarifying footnotes to the lists of 
approved test procedures, update method citations in Tables IA, IB, IC, 
ID, and IE, to amend the incorporation by reference section of the 
regulation accordingly, and to correct certain typographical errors and 
omissions in the Technical Amendments appearing in the Federal 
Register, of October 8, 1991.

EFFECTIVE DATE: This amendment becomes effective on January 31, 1994. 
The incorporation by reference of the publications listed in this 
notice are approved by the Director of Federal Register as of January 
31, 1994.

FOR FURTHER INFORMATION CONTACT: James J. Lichtenberg Environmental 
Monitoring Systems Laboratory, Office of Research and Development, U.S. 
Environmental Protection Agency, Cincinnati, Ohio 45268, Telephone 
Number: (513) 569-7306.

SUPPLEMENTARY INFORMATION:
    I. These technical amendments update and/or correct errors and 
inadvertant omissions in the references to analytical methods already 
approved under section 304(h) to the current editions published by EPA, 
U.S. Geological Survey, Standard Methods for the Examination of Water 
and Wastewater (Standard Methods), the American Society for Testing and 
Materials (ASTM), and the Association of Official Analytical Chemists 
(AOAC) International. No new methods are introduced. EPA has carefully 
reviewed each approved method for substantive changes between the 
current editions and the previously approved editions. Methods cited in 
this amendment that were not previously cited are substantively the 
same as the approved EPA method and/or were derived from the EPA 
method.
    II. The Standard Methods references in Tables IA, IB, IC, ID, and 
IE are generally updated to the 18th Edition by today's notice. Each 
approved method was carefully reviewed for substantive changes between 
the 17th and 18th editions. With the exception of the Turbidimetric 
Method for Sulfate, the 18th edition methods were found to be 
technically equivalent to the approved 17th edition methods. Therefore, 
we are updating the Standard Methods citations to the 18th edition for 
all but the Turbidimetric Method for Sulfate which will continue to be 
cited to the 15th edition. The list of references incorporated into 
this regulation continues to cite the 14th edition for phenols by 
manual distillation and colorimetric determination.
    III. References in Tables IA, IB, IC, ID, and IE to the American 
Society for Testing and Materials (ASTM), AOAC International and/or, 
U.S. Geological Survey (USGS), have also been updated and corrected 
where appropriate to the most recent editions. Several ASTM methods are 
no longer cited because they have been discontinued by ASTM and are not 
included in the 1993 Standards book.
    IV. Table II--Required Containers, Preservation Techniques, and 
Holding Times is amended as follows: Quartz glass is added to the list 
of sample containers for boron and silica. Borosilicate glass 
containers are not acceptable when samples are to be analyzed for these 
two parameters.
    Phosphoric acid is added as an option for preserving samples which 
are to be analyzed for organic carbon. Previously approved methods for 
organic carbon, published by Standard Methods use phosphoric acid for 
this purpose.
    V. The remaining amendments in this notice are very minor and are 
typo- graphical or editorial in nature. The parts of Tables IA, IC and 
ID, and certain notes to Tables IB and IC where reference updates, 
corrections, and clarifications have been made are reprinted in this 
notice for the information and use of the regulated community. Tables 
IB and IE have been reprinted in their entirety for the convenience of 
the user.
    Unless otherwise indicated in this notice, the methods contained in 
the Standard Methods 18th edition and the ASTM Standards are previously 
approved methods that were reballoted without technical change or were 
not reballoted. Any changes are editorial, typographical, or 
grammatical.

V. Regulatory Requirements

A. Executive Order 12866

    For Executive Order 12866, EPA must judge whether a regulation is 
``major'' and, therefore, requires a regulatory impact analysis. EPA 
has determined that these technical amendments are not major as they 
will not result in an effect on the economy of $100 million or more, a 
significant increase in cost or prices, or any of the effects described 
in the Executive Order. These amendments simply specify analytical 
techniques which may be used by laboratories in measuring 
concentrations of certain analytes and, therefore, have no adverse 
economic impacts.

B. Administrative Procedure Act

    The Administrative Procedure Act, 5 U.S.C. 553 (b)(B), authorizes 
an agency to forego notice and comment rulemaking when the agency for 
good cause finds that notice and public procedure thereon are 
impracticable, unnecessary or contrary to the public interest. EPA 
believes that public comment on the foregoing technical amendments is 
unnecessary because the updates to method references do not change the 
methods contained therein. In publishing the new editions of their test 
protocols, ASTM and Standard Methods have balloted these methods for 
reapproval without technical change or the methods were republished as 
unballoted. Additionally, the typographical errors corrected in the CFR 
do not amend substantive requirements. Therefore, notice and public 
procedure is unnecessary and does not apply to this technical amendment 
notice.

C. Regulatory Flexibility Act

    This amendment is consistent with the objectives of the Regulatory 
Flexibility Act (5 U.S.C. 602 et seq.) because it will not have a 
significant economic impact on a substantial number of small entities. 
The procedures cited in this rule give all laboratories the flexibility 
to use these procedures or already approved alternative procedures.

D. Paperwork Reduction Act

    This rule contains no request for information activities and, 
therefore, no information collection request (ICR) was submitted to the 
office of Management and Budget (OMB) for review in compliance with the 
Paperwork Reduction Act, 44 U.S.C. 3501 et seq.

Lists of Subjects in 40 CFR Part 136

    Incorporation by reference, Water pollution control.

    Dated: January 13, 1994.
Gary J. Foley,
Acting Assistant Administrator, Office Research and Development (8101).

    40 CFR part 136 is amended as follows:

PART 136--[AMENDED]

    1. The authority citation for part 136 continues to read as 
follows:

    Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 
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).

    2. In Sec. 136.3, paragraph (a) is amended as follows:
    a. In Table IA by revising the heading, by revising entries 1 and 2 
and by revising footnote 3.
    b. By revising Table IB.
    c. In Table IC by revising the heading and by revising entries 1, 
2, 5, 8, 9, 10, 11, 12, 32, 33, 37, 54, 58, 59, 64, 67, 69, 84, and 86 
and Table IC--Notes 5, 6, and 7.
    d. In Table ID by revising the heading and by revising entries 8, 
9, 10, 12, 13, 15, 36 and 41.
    e. By revising Table IE.
    3. In Sec. 136.3, paragraph (b) is amended as follows:
    a. By removing reference 9 and redesignating references 10 through 
33 as 9 through 32, and by revising reference 6 and newly designated 
reference 10.
    4. In Sec. 136.3 paragraph (e) is amended as follows:
    a. In Table II by revising the entry for, ``3, 5-8, 12, 13, 19, 20, 
22, 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.''; by revising 
entries 42 and 61; by adding entry 10 in numerical order; and by 
revising Table II--Note 4.


Sec. 136.3  Identification of test procedures.

* * * * *

                                                 Table IA.--List of Approved Biological Test Procedures                                                 
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                              Reference (method No. or page)                            
                                                                 ---------------------------------------------------------------------------------------
  Parameter, units and method               Method\1\                                     Standard methods                                              
                                                                         EPA\2\               18th Ed.                ASTM                 USGS\3\      
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:                                                                                                                                               
    1. Coliform (fecal), number  MPN, 5 tube, dilution or,        p.132                 9221C                 ....................  B-0050-85.          
     per 100 ml.                  membrane filter (MF)\4\,        p.124                 9222D                 ....................                      
                                  single step.                                                                                                          
    2. Coliform (fecal) in       MPN, 5 tube, 3 dilution; or,     p.132                 9221C                 ....................  ....................
     presence of chlorine,        MF\4\, single step\5\.          p.124                 9222D                 ....................  ....................
     number per 100 ml.                                                                                                                                 
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:                                                                                                                                         
\1\The method used must be specified when results are reported.                                                                                         
\2\Bordner, R.H., and J.A. Winter, eds. 1978. ``Mircobiological Methods for Monitoring the Environment, Water and Waste''. Environmental Monitoring     
  Systems Laboratory, U.S. Environmental Protection Agency. EPA-600/8-78-017.                                                                           
\3\Britton, L.J., and P.E. Greeson, eds., 1989. ``Methods for Collection and Analysis of Aquatic Biological and Microbological Samples,'' Techniques of 
  Water Resources Investigations of the U.S. Geological Survey, Techniques of Water Resources Investigations, Book 5, Chapter A4, Laboratory Analysis,  
  U.S. Geological Survey, U.S. Department of Interior, Reston, Virginia.                                                                                
\4\A 0.45 m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated, and to be free of
  extractables which could interfere with their growth.                                                                                                 
\5\Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to  
  resolve any controversies.                                                                                                                            


                                                  Table IB.--List of Approved Inorganic Test Procedures                                                 
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                    Reference (method number or page)                                   
                                                --------------------------------------------------------------------------------------------------------
          Parameter, units and method                           Std. methods 18th                                                                       
                                                   EPA1,35             Ed.                    ASTM                   USGS\2\                Other       
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:                                                                                                                             
    Electrometric endpoint or phenolphthalein          305.1  2310 B(4a)..........  D1067-92                  ....................                      
     endpoint.                                                                                                                                          
2. Alkalinity, as CaCO3, mg/L:                                                                                                                          
    Electrometric or Colorimetric titration to         310.1  2320 B..............  D1067-92                  I-1030-85             973.43.\3\          
     pH 4.5, manual or automated.                      310.2  ....................  ........................  I-2030-85...........                      
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/Atomic Emission      \5\200.7  3120 B                                                                                    
     Spectrometry (ICP/AES)\36\.                                                                                                                        
    Direct Current Plasma (DCP)\36\............  ...........  ....................  D4190-82(88)              ....................  Note 34.            
    Colorimetric (Eriochrome cyanine R)........  ...........  3500-A1 D                                                                                 
4. Ammonia (as N), mg/L:                                                                                                                                
    Manual distillation (at pH 9.5)\6\,                350.2  4500-NH3 B            ........................  ....................  973.49.\3\          
     followed by.                                                                                                                                       
    Nesslerization.............................        350.2  4500-NH3 C            D1426-89(A)               I-3520-85             973.49.\3\          
    Titration..................................        350.2  4500-NH3 E            ........................  ....................                      
    Electrode..................................        350.3  4500-NH3 F or G       D1426-89(B)               ....................                      
    Automated phenate, or......................        350.1  4500-NH3 H            ........................  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  314 B 4.d             D2972-88(B)               I-3062-85                                 
    AA furnace.................................        206.2  3113 B                D2972-88(C)                                                         
    ICP/AES\36\, or............................     \5\200.7  3120 B                                                                                    
    Colorimetric (SDDC)........................        206.4  3500-As C             D2972-88(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                D3645-84(88)(A)           I-3095-85                                 
    AA furnace.................................        210.2  3113 B                D3645(88)(B)                                                        
    ICP/AES....................................     \5\200.7  3120 B                                                                                    
    DCP, or....................................  ...........  ....................  D4190-82(88)              ....................  Note 34.            
    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, or............................        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-  974.27\3\, p.37\9\. 
                                                                                                               85                                       
    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                D511-92(B)                I-3152-85             ....................
    ICP/AES....................................     \5\200.7  3120 B                                                                ....................
    DCP, or....................................  ...........  ....................  ........................  ....................  Note 34.            
    Titrimetric (EDTA).........................        215.2  3500-Ca D             D511-92(A)                                      ....................
14. Carbonaceous biochemical oxygen demand                                                                                                              
 (CBOD5), mg/L\12\:                                                                                                                                     
    Dissolved Oxygen Depletion with              ...........  5210 B                                                                ....................
     nitrification inhibitor.                                                                                                                           
15. Chemical oxygen demand (COD), mg/L;                410.1  5220 C                D1252-88(A)               I-3560-85             973.46\3\, p. 17\9\.
 Titrimetric, or.                                      410.2  ....................  ........................  I-3562-85                                 
                                                       410.3                                                                                            
    Spectrophotometric, manual or automated....        410.4  5220 D                D1252-88(B)               I-3561-85             Notes 13 or 14.     
16. Chloride, mg/L:                                                                                                                                     
    Titrimetric (silver nitrate)...............  ...........  4500-C1 B             D512-89(B)                I-1183-85             ....................
    Or (Mercuric nitrate)......................        325.3  4500-C1 C             D512-89(A)                I-1184-85             973.51\3\.          
    Colorimetric, manual or....................  ...........  ....................  ........................  I-1187-85             ....................
    Automated (Ferricyanide)...................     325.1 or  4500-C1 E             ........................  I-2187-85             ....................
                                                       325.2                                                                                            
17. Chlorine--Total residual, mg/L;                                                                                                                     
 Titrimetric:                                                                                                                                           
    Amperometric direct........................        330.1  4500-C1 D             D1253-86(92)                                    ....................
    Iodometric direct..........................        330.3  4500-C1 B                                                             ....................
    Black titration ether end-point\15\ or.....        330.2  4500-C1 C                                                             ....................
    DPD-FAS....................................        330.4  4500-C1 F                                                             ....................
    Spectrophotometric, DPD....................        330.5  4500-C1 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 (Diphenylcarbazide)...........  ...........  3500-Cr D             D1687-92(A)               I-1230-85             ....................
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)                                     ....................
    ICP/AES\36\................................     \5\200.7  3120 B                                                                ....................
    DCP\36\, or................................  ...........  ....................  D4190-82(88)              ....................  Note 34.            
    Colorimetric (Diphenylcarbazide)...........  ...........  3500-Cr D                                                             ....................
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  2120C                                                                                     
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 I-3271-  974.27\3\, p.37\9\. 
                                                                                                               85                                       
    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) or..............  ...........  3500-Cu D                                                                                 
    (Bicinchoninate)...........................  ...........  or E                  ........................  ....................  Note 19.            
23. Cyanide--Total, mg/L:                                                                                                                               
    Manual distillation with MgCl2 followed by.  ...........  4500-CN C                                                                                 
    Titrimetric, or............................  ...........  4500-CN D             ........................  ....................  p. 22.\9\           
    Spectrophotometric, manual or..............    \31\335.3  4500-CN E             D2036-91(A)               I-3300-85                                 
    Automoted\20\..............................    \31\335.3                                                                                            
24. Cyanide amenable to chlorination, mg/L:                                                                                                             
    Manual distillation with MgCl2 followed by         335.1  4500-CN G             2036-91(B)                                                          
     titrimetric or Spectrophotometric.                                                                                                                 
25. Fluoride--Total, mg/L:                                                                                                                              
    Manual distillation\6\ followed by.........  ...........  4500-F- B                                                                                 
    Electrode, manual or.......................        340.2  4500-F- C             D1179-88(B)                                                         
    Automated..................................  ...........  ....................  ........................  I-4327-85                                 
    Colorimetric (SPADNS)......................        340.1  4500-F- D             D1179-88(A)                                                         
    Or Automated complexone or.................        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 plus Mg as their         130.2  2340 C                D1126-86(92)              I-1338-85             973.52B.\3\         
     carbonates, by inductively coupled plasma                                                                                                          
     or AA direct aspiration. (See Parameters                                                                                                           
     13 and 33)                                                                                                                                         
28. Hydrogen ion (pH), pH units:                                                                                                                        
    Electrometric measurement, or..............        150.1  4500-H+ B             D1293-84(90) (A or B)     I-1586-85             973.41.\3\          
    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 (Phenanthroline)..............  ...........  3500-Fe D             D1068-90(D)               ....................  Note 22.            
31. Kjeldahl Nitrogen--Total, (as N), mg/L:                                                                                                             
    Digestion and distillation followed by.....        351.3  4500-NH\3\ B or C     D3590-89(A)                                     ....................
    Titration..................................        351.3  4500-NH\3\ E          D3590-89(A)               ....................  973.48.\3\          
    Nesslerization.............................        351.3  4500-NH\3\ C          D3590-89(A)                                     ....................
    Electrode..................................        351.3  4500-NH\3\ F or G                                                     ....................
    Automated phenate colorimetric.............        351.1  ....................  ........................  I-4551-78\8\          ....................
    Semi-automated block digestor colorimetric,        351.2  ....................  3590-89(B)                                      ....................
     or.                                                                                                                                                
    Manual or block digestor Potentiometric....        351.4  ....................  D359-89(A)                                      ....................
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)                                     ....................
    Colorimtric (Dithizone)....................  ...........  3500-Pb D                                                             ....................
33. Magnesium--Total\4\, mg/L; Digestion\4\                                                                                                             
 followed by:                                                                                                                                           
    AA direct aspiration.......................        242.1  3111 B                D511-92(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), or..............  ...........  3500-Mn D             ........................  ....................  920.203.\3\         
    (Periodate)................................  ...........  ....................  ........................  ....................  Note 23.            
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                                                                        ....................
36. Molybdenum--Total\4\, mg/L; Digestion\4\                                                                                                            
 followed by:                                                                                                                                           
    AA direct aspiration.......................        246.1  3111 D                ........................  I-3490-85             ....................
    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.......................        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 sulfate), or Nitrate-        352.1  ....................  ........................  ....................  973.50\3\, 419      
     nitrite N minus Nitrite N (See parameters                                                                                       D\17\, p.28.\9\    
     39 and 40).                                                                                                                                        
39. Nitrate-nitrite (as N), mg/L:                                                                                                                       
    Cadmium reduction, Manual or...............        353.3  4500-NO\3\ E          D3867-90(B)                                     ....................
    Automated, or..............................        353.2  4500-NO\3\ F          D3867-90(A)               I-4545-85             ....................
    Automated hydrazine........................        353.1  4500-NO\3\ H                                                          ....................
40. Nitrite (as N), mg/L; Spectrophotometric:                                                                                                           
    Manual or..................................        354.1  ....................  ........................  ....................  Note 25.            
    Automated (Diazotization)..................  ...........  ....................  ........................  4500-No2              ....................
41. Oil and grease--Total recoverable, mg/L:                                                                                                            
    Gravimetric (extraction)...................        413.1  5520 B                                                                                    
42. Organic carbon--Total (TOC), mg/L:                                                                                                                  
    Combustion or oxidation....................    \17\415.1  5310 B, C, or D       D2579-85(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 modification), or...........        360.2  4500-0 C              D888-92(A)                \8\I-1575-78          973.45B.\3\         
    Electrode..................................        360.1  4500-0-G              D888-92(B)..............  \8\I-1576-78                              
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\          
    DCP........................................  ...........  ....................  ........................  ....................  Note 34.            
48. Phenols, mg/L:                                                                                                                                      
    Manual distillation\26\....................        420.1  ....................  ........................  ....................  Note 27.            
    Followed by:                                                                                                                                        
        Colorimetric (4AAP) manual, or.........        420.1  ....................  ........................  ....................  Note 27.            
        Automated\19\..........................        420.2                                                                                            
49. Phosphorus (elemental), mg/L:                                                                                                                       
    Gas-liquid chromatography..................  ...........  ....................  ........................  ....................  Note 28.            
50. Phosphorus--Total, mg/L:                                                                                                                            
    Persulfate digestion followed by...........        365.2  4500-P B,5            ........................  ....................  973.55.\3\          
    Manual or..................................     365.2 or  4500-P E              D515-88(A)                                                          
                                                       365.3                                                                                            
    Automated ascorbic acid reduction..........        365.1  -4500-P F             ........................  I4600-85              973.56.\3\          
    Semi-automated block digestor..............        365.4  ....................  D515-88(B)                                                          
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                                                                                  
    Colormetric................................  ...........  ....................  ........................  ....................  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. post washing of          160.2  2540 D                ........................  I-3765-85                                 
     residue.                                                                                                                                           
56. Residue--settleable, mg/L:                                                                                                                          
    Volumetric, (Imhoff cone), or gravimetric..        160.5  2540 F                ........................                                            
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                                                                ....................
    ICP/AES,\36\ or............................     \5\200.7  3120 B                                                                ....................
    AA gaseous hydride.........................  ...........  3114 B                D3859-88(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 (Molybdosilicate), or............  ...........  ....................  ........................  I-2700-85                                 
    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\
    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.I  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 (barium                     375.1  ....................  ........................  ....................  ....................
     chloranilate).                                                                                                                                     
    Gravimetric................................        375.3  4500-SO4-2 C or D     ........................  ....................  925.54.\3\          
    Turbidimetric, or..........................        375.4  ....................  516-90                    ....................  426C.\30\           
66. Sulfide (as S), mg/L:                                                                                                                               
    Titrimetric (iodine), or...................        376.1  4500-S-2 E            ........................  I-3840-85             ....................
    Colorimetric (methylene blue)..............        376.2  4500-S-2 D                                                            ....................
67. Sulfite (as SO3), mg/L:                                                                                                                             
    Titrimetric (iodine-iodate)................        377.1  4500-SO3-2 B                                                          ....................
68. Surfactants, mg/L:                                                                                                                                  
    Colorimetric (methylene blue)..............        425.1  5540 C                D2330-88                                        ....................
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                                                                                            
    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:                                                                                                                                                    
    AA direct aspiration\36\...................        289.1  3111 B or C           D1691-90 (A or B)         1-3900-85...........  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) or................  ...........  3500-Zn E             ........................  ....................  ....................
    (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: 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, N.Y. 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 manifold 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, N.Y. 10523.                                                                                            
\22\Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.                                       
\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 spectrophotometric 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 Trade Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--      
  Revised 1991, Applied Research Laboratories, Inc., 24911 Avenue Stanford, Valencia, CA 91355.                                                         
\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 sampling and laboratory ware must be used from time of collection until completion 
  of analysis.                                                                                                                                          


                                     Table IC.--List of Approved Test Procedures for Non-Pesticide Organic Compounds                                    
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                  EPA method number27                                                   
         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                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
5. Anthracene................                 610           625, 1625        610  6410 B, 6440 B                     D4657-92                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
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                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
32. Chrysene.................                 610           625, 1625        610  6410 B, 6440 B                     D4657-92                           
33. Dibenzo(a,h)antracene....                 610           625, 1625        610  6410 B, 6440 B                     D4657-92                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
37. 2,4-Dichlorobenzene......       601, 602, 612      624, 625, 1625  .........  6410 B, 6220 B, 6230 B                                                
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
54. 2,4-Dinitrotoluene.......                 609           625, 1625  .........  6410 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                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
64. Ideno(1,2,3-cd) pyrene...                 610           625, 1625        610  6410 B, 6440 B                     D4657-92                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
67. 2-Methyl-4,6-                             604           625, 1625  .........  6420 B, 6410 B                                                        
 dinitrophenol.                                                                                                                                         
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
69. Nitrobenezene............                 609           625, 1625  .........  6410 B                                                                
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
84. Phenanthrene.............                 610           625, 1625        610  6410 B, 6440 B                     D4657-92                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
86. Pyrene...................                 610           625, 1625        610  6410 B, 6440 B                     D4675-92                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC--Notes:                                                                                                                                        
\1\All parameters are expressed in micrograms per liter (g/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 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, Pentacshlorophenol 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.                                        
\5\6a625, 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.''                                                  


                                              Table ID.--List of Approved Test Procedures for Pesticides\1\                                             
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                           Standard methods                                                             
             Parameter                       Method          EPA\2\\7\         18th Ed.                ASTM                         Other               
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
8. =BHC....................  GC                            608  6630 B & C..........  D3086-90              Note 3, p. 7.                      
                                      GC/MS                      \5\625  6410 B..............                                                           
9. =BHC....................  GC                            608  6630................  D3086-90                                                 
                                      GC/MS                      \5\625  6410 B..............                                                           
10. =BHC...................  GC                            608  6630 B & C..........  D3086-90                                                 
                                      GC/MS                      \5\625  6410 B..............                                                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
12. Captan..........................  GC                    ...........  6630 B                D3086-90              Note 3, p. 7.                      
13. Carbaryl........................  TLC                   ...........  ....................  ....................  Note 3, p. 94: Note 6, p. S60.     
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
15. Chlordane.......................  GC                            608  6630 B & C..........  D3086-90              Note 3, p. 7.                      
                                      GC/MS                         625  6410 B..............                                                           
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
36. Endrin aldehyde.................  GC                            608                                                                                 
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
41. Heptachlor epoxide..............  GC                            608  6630 B..............  D3086-90              Note 3, p. 7; Note 4, p. 30;       
                                      GC/MS                         625  6410 B..............                        Note 6, p. S73.                    
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
--------------------------------------------------------------------------------------------------------------------------------------------------------
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.''                                                  


                                                 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 scintillation        900...............  7110 B            D1943-90          pp. 75 and 78.\3\    
                                       counter.                                                                                                         
2. Alpha-Counting error, pCi per      Proportional or scintillation        Appendix B........  7110 B            D1943-90          P. 79.               
 liter.                                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 liter...  Proportional counter...............  903.0.............  7500Ra B          D2460-90                               
  (b)\226\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''.                                                                                                        

    (b)
* * * * *
    (6) ``Standard Methods for the Examination of Water and 
Wastewater'', Joint Editorial Board, American Public Health 
Association, American Water Works Association, and Water Environment 
Federation, 18th Edition, 1992. Available from: American Public Health 
Association, 1015 Fifteenth Street, NW., Washington, DC 20005. Cost 
$160.00. Tables IA, IB, IC, ID and IE.
* * * * *
    (10) ``Annual Book of Standards--Water and Environmental 
Technology,'' Section 11, Parts 11.01 and 11.02, American Society for 
Testing and Materials, 1993. 1916 Race Street, Philadelphia, PA 19103. 
Cost available from publisher. Tables IB, IC, ID, and IE.
* * * * *
    e.
* * * * *

                                       Table II.--Required Containers, Preservation Techniques, and Holding Times                                       
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                              Maximum   
             Parameter No./name                       Container\1\                                Preservation\2\\3\                          holding   
                                                                                                                                              time\4\   
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
Metals\7\:                                                                                                                                              
    10. Boron..............................  P (PFTE), or Quartz...........  HNO3 TO pH<2................................................  6 months.    
                                                                      * * * * * * *                                                                     
    3, 5-8, 12, 13, 19, 20, 22, 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.                                                                                                                    
                                                                      * * * * * * *                                                                     
42. Organic Carbon.........................  G.............................  Cool to 4  deg.C HC1 or H2SO4 or H3PO4, to pH<2.............  28 days.     
                                                                      * * * * * * *                                                                     
61. Silica.................................  P (PFTE), or Quartz...........  Cool, 4  deg.C..............................................  28 days.     
                                                                                                                                                        
                                                                      * * * * * * *                                                                     
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table II--Notes:                                                                                                                                        
\1\Polyethylene (P) or Glass (G).                                                                                                                       
\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 4  deg.C 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).                                    
\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.                                               
* * * * * * *                                                                                                                                           
\7\Samples should be filtered immediately on-site before adding preservative for dissolved metals.                                                      
* * * * * * *                                                                                                                                           

[FR Doc. 94-1625 Filed 1-28-94; 8:45 am]
BILLING CODE 6560-50-P