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§136.3 Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, and IF. The full text of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, and IF. The incorporation by reference of these documents, as specified in paragraph (b) of this section, was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources listed in paragraph (b) of this section. Information regarding obtaining these documents can be obtained from the EPA Office of Water Statistics and Analytical Support Branch at 202-566-1000. Documents may be inspected at EPA's Water Docket, EPA West, 1301 Constitution Avenue, NW., Room B135, Washington, DC (Telephone: 202-566-2426); or at the Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC. These test procedures are incorporated as they exist on the day of approval and a notice of anys change in these test procedures will be published in the FEDERAL REGISTER. The discharge parameter values for which reports are required must be determined by one of the standard analytical test procedures incorporated by reference and described in Tables IA, IB, IC, IE, and IF, or by any alternate test procedure which has been approved by the Administrator under the provisions of paragraph (d) of this section and §§136.4 and 136.5. Under certain circumstances (paragraph (b) or (c) of this section or 40 CFR 401.13) other test procedures may be more advantageous when such other test procedures have been previously approved by the Regional Administrator of the Region in which the discharge will occur, and providing the Director of the State in which such discharge will occur does not object to the use of such alternate test procedure.
Table IA_List of Approved Biological Methods
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods 18th,
Parameter and units Method \1\ EPA 19th, 20th Ed. ASTM AOAC USGS Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number Most Probable Number p. 132 9221C E \4\
per 100 mL. (MPN), 5 tube 3 \3\
dilution, or
Membrane filter (MF) p. 124 9222D \4\ ........... ........... B-0050-85
\2\, single step. \3\ \5\
2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 9221C E \4\ ........... ........... ...........
presence of chlorine, number dilution, or \3\
per 100 mL.
MF, single step \6\. p. 124 9222D \4\ ........... ........... ........... ....................
\3\
3. Coliform (total), number MPN, 5 tube, 3 p. 114 9221B \4\
per 100 mL. dilution, or \3\
MF \2\, single step p. 108 9222B \4\ ........... ........... B-0025-85 ....................
or two step. \3\ \5\
4. Coliform (total), in MPN, 5 tube, 3 p. 114 9221B \4\ ........... ........... ........... ....................
presence of chlorine, number dilution, or \3\
per 100 mL.
MF \2\ with p. 111 9222(B+B.5c) \4\
enrichment. \3\
5. E. coli, number per 100 mL MPN \7,9,15\, ......... 9221B.1/9221F \4,12,14\
\28\. multiple tube,.
multiple tube/ ......... 9223B \4,13\ ........... 991.15 \11\ ........... Colilert®
multiple well, \13,17\
Colilert-18®
\13,16,17\
MF \2,6,7,8,9\ two ......... 9222B/9222G \4,19\
step, or
1103.1 9213D \4\ D5392-93
\20\ \10\
single step......... 1603 \21\
1604 \22\
......... ....................... ........... ........... ........... mColiBue 24 \18\
6. Fecal streptococci, number MPN, 5 tube, 3 p. 139 9230B \4\, 9230C \4\
per 100 mL. dilution, \3\
MF \2\, or.......... p. 136 ....................... ........... B-0055-85 ...........
\3\ \5\
Plate count......... p. 143
\4\
7. Enterococci, number per MPN \7, 9\ multiple ......... 9230B \4\
100 mL. tube.
multiple tube/ ......... ....................... D6503-99 ........... ........... Enterolert®\13,
multiple well. \10\ 23\
MF \2,6,7,8,9\ two 1106.1 9230C \4\ D5259-92
step. \24\ \10\
single step, or..... 1600 \25\
Plate count......... p. 143
\3\
Protozoa:
8. Cryptosporidium \28\...... Filtration/IMS/FA... 1622 \26\
1623 \27\
9. Giardia \28\.............. Filtration/IMS/FA... 1623 \27\
Aquatic Toxicity:
10. Toxicity, acute, fresh Ceriodaphnia dubia 2002.0
water organisms, LC50, acute. \29\
percent effluent.
Daphnia puplex and 2021.0
Daphnia magna acute. \29\
Fathead Minnow, 2000.0
Pimephales \29\
promelas, and
Bannerfin shiner,
Cyprinella leedsi,
acute.
Rainbow Trout, 2019.0
Oncorhynchus \29\
mykiss, and brook
trout, Salvelinus
fontinalis, acute.
11. Toxicity, acute, Mysid, Mysidopsis 2007.0
estuarine and marine bahia, acute. \29\
organisms of the Atlantic
Ocean and Gulf of Mexico,
LC50, percent effluent.
Sheepshead Minnow, 2004.0
Cyprinodon \29\
variegatus, acute.
Silverside, Menidia 2006.0
beryllina, Menidia \29\
menidia, and
Menidia peninsulae,
acute.
12. Toxicity, chronic, fresh Fathead minnow, 1000.0
water organisms, NOEC or Pimephales \30\
IC25, percent effluent. promelas,
larvalsurvival and
growth.
Fathead minnow, 1001.0
Pimephales \30\
promelas, embryo-
larval survival and
teratogenicity.
Daphnia, 1002.0
Ceriodaphnia dubia, \30\
survival and
reproduction.
Green alga, 1003.0
Selenastrum \30\
capricornutum,
growth.
13. Toxicity, chronic, Sheepshead minnow, 1004.0
estuarine and marine Cyprinodon \31\
organisms of the Atlantic variegatus,larval
Ocean and Gulf of Mexico, survival and growth.
NOEC or IC25, percent
effluent.
Sheepshead minnow, 1005.0
Cyprinodon \31\
variegatus,embryo-
larval survival and
teratogenicity.
Inland silverside, 1006.0
Menidia beryllina, \31\
larval survival and
growth.
Mysid, Mysidopsis 1007.0
bahia, survival, \31\
growth,and
fecundity.
Sea urchin, Arbacia 1008.0
punctulata, \31\
fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Notes to Table IA:
\1\ The method must be specified when results are reported.
\2\ A 0.45 mm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, Ohio. EPA/600/8-78/017.
\4\ APHA. 1998, 1995, 1992. Standard Methods for the Examination of Water and Wastewater. American Public Health Association. 20th, 19th, and 18th
Editions. Amer. Publ. Hlth. Assoc., Washington, D.C.
\5\ USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and
Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of Interior, Reston, Virginia.
\6\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
\7\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
\8\ When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncoliform bacteria, or samples that
may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
comparability of results.
\9\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
alternate test procedure (ATP) guidelines.
\10\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards_Water and Environmental Technology. Section 11.02. American Society for Testing and
Materials. 100 Barr Harbor Drive, West Conshohocken, PA 19428.
\11\ AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists
International. 481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-2417.
\12\ The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate
and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent
of all total coliform-positive tubes on a seasonal basis.
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth
or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supplemented in the
laboratory with 50 mg/mL of MUG may be used.
\15\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with
the multiple-well procedures, Quanti-Tray® or Quanti-Tray® 2000, and the MPN calculated from the table provided by the manufacturer.
\16\ Colilert-18 ® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
\17\ Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc.,
One IDEXX Drive, Westbrook, Maine 04092.
\18\ A description of the mColiBlue24'' test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\19\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
\20\ USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC).
U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-020.
\21\ USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (
modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-023.
\22\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604:
Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA 821-R-02-024.
\23\ A description of the Enterolert ® test may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.
\24\ USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental
Protection Agency, Office of Water, Washington DC. EPA-821-R-02-021.
\25\ USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). U.S.
Environmental Protection Agency, Office of Water, Washington, DC. EPA-821-R-02-022.
\26\ Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821-
R-01-026.
\27\ Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA-821-R-01-025.
\28\ Recommended for enumeration of target organism in ambient water only.
\29\ USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition.
U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/012.
\30\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth
Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/013.
\31\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms.
Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/014.
Table IB_List of Approved Inorganic Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
Parameter, units and method --------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA [SU]1, 35[/SU] Standard Methods [Edition(s)] ASTM USGS \2\ Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO[INF]3[/INF],
mg/L:
Electrometric endpoint or 305.1......................... 2310 B(4a) [18th, 19th, 20th]. D1067-92...................... I-1020-85
phenolphthalein endpoint.
I-2030-85
2. Alkalinity, as CaCO[INF]3[/
INF], mg/L:
Electrometric of Colorimetric 310.1......................... 2320 B [18th, 19th, 20th]..... D1067-92...................... I-1030-85..................... 973.43 \3\
titration to pH 4.5, manual .............................. .............................. .............................. ..............................
or automatic. 310.2......................... .............................. I-2030-85.....................
3. Aluminium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 202.1......................... 3111 D [18th, 19th]........... .............................. I-3051-85
AA furnace................... 202.2......................... 3113 B [18th, 19th]...........
Inductively Coupled Plasma/ 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
Atomic Emission Spectrometry
(ICP/AES) \36\.
Direct Current Plasma (DCP) .............................. .............................. D4190-94...................... .............................. Note 34.
\36\.
Colorimetric (Eriochrome .............................. 3500-Al B [20th] and 3500-Al D
cyanine R). [18th, 19th].
4. Ammonia (as N), mg/L:
Manual, distillation (at pH 350.2......................... 4500-NH[INF]3[/INF] B [18th, .............................. .............................. 973.49 \3\
9.5) \6\ followed by. 19th, 20th].
Nesslerization............... 350.2......................... 4500-NH[INF]3[/INF] C [18th].. D1426-98(A)................... I-3520-85..................... 973.49 \3\
Titration.................... 350.2......................... 4500-NH[INF]3[/INF] C [19th,
20th] and 4500-NH[INF]3[/INF]
E [18th].
Electrode.................... 350.3......................... 4500-NH[INF]3[/INF] D or E D1426-98(B)...................
[19th, 20th] and 4500-
NH[INF]3[/INF] F or G [18th].
Automated phenate, or........ 350.1......................... 4500-NH[INF]3[/INF] G [19th, .............................. I-4523-85 .............................
20th] and 4500-NH[INF]3[/INF]
H [18th].
Automated electrode.......... .............................. .............................. .............................. .............................. Note 7.
5. Antimony-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 204.1......................... 3111 B [18th, 19th]
AA furnace................... 204.2......................... 3113 B [18th, 19th]...........
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
6. Arsenic-Total\4\ mg/L:
Digestion \4\ followed by.... 206.5.........................
AA gaseous hydride........... 206.3......................... 3114 B 4.d [18th, 19th]....... D2972-97(B) I-3062-85
AA furnace................... 206.2......................... 3113 B [18th, 19th]........... D2972-97(C) I-4063-98 \49\ .............................
ICP/AES \36\ or.............. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
Colorimetric (SDDC).......... 206.4......................... 3500-As B [20th] and 3500-As C D2972-97(A) I-3060-85 .............................
[18th, 19th].
7. Barium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \14\.... 208.1......................... 3111 D [18th, 19th]........... .............................. I-3084-85 .............................
AA furnace................... 208.2......................... 3113 B [18th, 19th]........... D4382-95
ICP/AES \14\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
DCP \14\..................... .............................. .............................. .............................. .............................. Note 34.
8. Beryllium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 210.1......................... 3111 D [18th, 19th]........... D3645-93(88)(A)............... I-3095-85 .............................
AA furnace................... 210.2......................... 3113 B [18th, 19th]........... D3645-93(88)(B) .............................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
DCP, or...................... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (aluminon....... .............................. 3500-Be D [18th, 19th]........
9. Biochemical oxygen demand
(BOD[INF]5[/INF]), mg/L:
Dissolved Oxygen Depletion... 405.1......................... 5210 B [18th, 19th, 20th]..... .............................. I-1578-78 \8\................. 973.44,\3\ p. 17 \9\
10. Boron \37\-Total, mg/L:
Colorimetric (curcumin)...... 212.3......................... 4500-B B [18th, 19th, 20th]... .............................. I-3112-85
ICP/AES, or.................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
DCP.......................... .............................. .............................. D4190-94...................... .............................. Note 34.
11. Bromide, mg/L:
Titrimetric.................. 320.1......................... .............................. D1246-95(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 [18th, 19th]...... D3557-95 (A or B)............. I-3135-85 or I-3136-85........ 974.27,\3\ p. 37 \9\
AA furnace................... 213.2......................... 3113 B [18th, 19th]........... D3557-95(D)................... I-4138-89 \51\
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-1472-85 or I-4471-97 \50\
DCP \36\..................... .............................. .............................. D4190-94...................... .............................. Note 34.
Voltametry \11\, or.......... .............................. .............................. D3557-95(C)...................
Colorimetric (Dithizone)..... .............................. 3500-Cd D [18th, 19th]........
13. Calcium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 215.1......................... 3111 B [18th, 19th]........... D511-93(B).................... I-3152-85
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP, or...................... .............................. .............................. .............................. .............................. Note 34.
Titrimetric (EDTA)........... 215.2......................... 3500-Ca B [20th] and 3500-Ca D D511-93(A)....................
[18th, 19th].
14. Carbonaceous biochemical
oxygen demand (CBOD 3), mg/
L\12\:
Dissolved Oxygen Depletion .............................. 5210 B [18th, 19th, 20th].....
with nitrification inhibitor.
15. Chemical oxygen demand (COD), 410.1......................... 5220 C [18th, 19th, 20th]..... D1252-95(A)................... I-3560-85..................... 973.46,\3\ p. 17 \9\
mg/L; Titrimetric
or........................... 410.2......................... .............................. .............................. I-3562-85
410.3.........................
Spectrophotometric, manual or 410.4......................... 5220 D [18th, 19th, 20th]..... D1252-95(B)................... I-3561-85..................... Notes 13, 14.
automatic.
16. Chloride, mg/L:
Titrimetric (silver nitrate) .............................. 4500-Cl[SU]-[/SU]B [18th, D512-89(B).................... I-1183-85
or. 19th, 20th].
(Mercuric nitrate)........... 325.3......................... 4500-Cl[SU]-[/SU]C [18th, D512-89(A).................... I-1184-85..................... 973.51 \3\
19th, 20th].
Colorimetric, manual or...... .............................. .............................. .............................. I-1187-85
Automated (Ferricyanide)..... 325.1 or 325.2................ 4500-Cl[SU]-[/SU]E [18th, .............................. I-2187-85
19th, 20th].
17. Chlorine_Total residual, mg/
L; Titrimetric:
Amperometric direct.......... 330.1......................... 4500-Cl D [18th, 19th, 20th].. D1253-86(92)..................
Iodometric direct............ 330.3......................... 4500-Cl B [18th, 19th, 20th]..
Back titration ether end- 330.2......................... 4500-Cl C [18th, 19th, 20th]..
point \15\ or.
DPD-FAS...................... 330.4......................... 4500-Cl F [18th, 19th, 20th]..
Spectrophotometric, DPD...... 330.5......................... 4500-Cl G [18th, 19th, 20th]..
Or Electrode................. .............................. .............................. .............................. .............................. Note 16.
18. Chromium VI dissolved, mg/L;
0.45 micron filtration followed
by:
AA chelation-extraction or... 218.4......................... 3111 C [18th, 19th]........... .............................. I-1232-85
Colorimetric .............................. 3500-Cr B [20th] and 3500-Cr D D1687-92(A)................... I-1230-85
(Diphenylcarbazide). [18th, 19th].
19. Chromium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 218.1......................... 3111 B [18th, 19th]........... D1687-92(B)................... I-3236-85..................... 974.27 \3\
AA chelation-extraction...... 218.3......................... 3111 C [18th, 19th]...........
AA furnace................... 218.2......................... 3113 B [18th, 19th]........... D1687-92(C)................... I-3233-93 \46\................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
DCP \36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric .............................. 3500-Cr B [20th] and 3500-Cr D
(Diphenylcarbazide). [18th, 19th].
20. Cobalt_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 219.1......................... 3111 B or C [18th, 19th]...... D3558-94(A or B).............. I-3239-85..................... p. 37 \9\
AA furnace................... 219.2......................... 3113 B [18th, 19th]........... D3558-94(C)................... I-4243-89 \51\................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP.......................... .............................. .............................. D4190-94...................... .............................. Note 34.
21. Color platinum cobalt units
or dominant wavelength, hue,
luminance purity:
Colorimetric (ADMI), or......
(Platinum cobalt), or........ 110.1......................... 2120 E [18th, 19th, 20th]..... .............................. .............................. Note 18.
Spectrophotometric........... 110.2......................... 2120 B [18th, 19th, 20th]..... .............................. I-1250-85
110.3......................... 2120 C [18th, 19th, 20th].....
22. Copper_Total,[SU]4[/SU] mg/L;
Digestion [SU]4[/SU] followed
by:
AA direct aspiration [SU]36[/ 220.1......................... 3111 B or C [18th, 19th]...... D1688-95(A or B).............. I-3270-85 or I-3271-85........ 974.27 [SU]3[/SU] p. 37
SU]. [SU]9[/SU]
AA furnace................... 220.2......................... 3113 B [18th, 19th]........... D1688-95(C)................... I-4274-89 [SU]51[/SU]
ICP/AES [SU]36[/SU].......... 200.7 [SU]5[/SU].............. 3120 B [18th, 19th, 20th]..... .............................. I_4471_97 [SU]50[/SU]
DCP [SU]36[/SU] or........... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Neocuproine) or .............................. 3500-Cu B [20th] and 3500-Cu D
[18th, 19th].
(Bicinchoninate)............. .............................. 3500-Cu C [20th] and 3500-As B .............................. .............................. Note 19.
[18th, 19th].
23. Cyanide_Total, mg/L:
Manual distillation with .............................. 4500-CN C [18th, 19th, 20th].. D2036-98(A)
MgCl[INF]2[/INF] followed
by..
Titrimetric, or.............. .............................. 4500-CN D [18th, 19th, 20th].. .............................. .............................. p. 22 [SU]9[/SU]
Spectrophotometric, manual or 335.2 [SU]31[/SU]............. 4500-CN E [18th, 19th, 20th].. D2036-98(A)................... I-3300-85
Automated [SU]20[/SU]........ 335.3 [SU]31[/SU]............. .............................. .............................. I-4302-85
24. Available Cyanide, mg/L:
Manual distillation with 335.1......................... 4500-CN G [18th, 19th, 20th].. D2036-98(B)
MgCl[INF]2[/INF] followed by
titrimetric or
Spectrophotometric.
Flow injection and ligand .............................. .............................. .............................. .............................. OIA-1677 [SU]44[/SU]
exchange, followed by
amperometry.
25. Fluoride_Total, mg/L:
Manual distillation [SU]6[/ .............................. 4500-F B [18th, 19th, 20th]...
SU] followed by.
Electrode, manual or......... 340.2......................... 4500-F C [18th, 19th, 20th]... D1179-93(B)
Automated.................... .............................. .............................. .............................. I-4327-85 .............................
Colorimetric (SPADNS)........ 340.1......................... 4500-F D [18th, 19th, 20th]... D1179-93(A)
Or Automated complexone...... 340.3......................... 4500-F E [18th, 19th, 20th]...
26. Gold_Total,[SU]4[/SU] mg/L;
Digestion [SU]4[/SU] followed
by:
AA direct aspiration......... 231.1......................... 3111 B [18th, 19th]...........
AA furnace, or............... 231.2
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
27. Hardness_Total, as
CaCO[INF]3[/INF], mg/L:
Automated colorimetric,...... 130.1
Titrimetric (EDTA), or Ca 130.2......................... 2340 B or C [18th, 19th, 20th] D1126-86(92).................. I-1338-85..................... 973.52B [SU]3[/SU]
plus Mg as their 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[SU]+[/SU] B [18th, D1293-84 (90)(A or B)......... I-1586-85..................... 973.41 [SU]3[/SU]
19th, 20th].
Automated electrode.......... .............................. .............................. .............................. I-2587-85..................... Note 21.
29. Iridium_Total,[SU]4[/SU] mg/
L; Digestion [SU]4[/SU] followed
by:
AA direct aspiration or...... 235.1......................... 3111 B [18th, 19th]...........
AA furnace................... 235.2
30. Iron_Total,[SU]4[/SU] mg/L;
Digestion [SU]4[/SU] followed
by:
AA direct aspiration [SU]36[/ 236.1......................... 3111 B or C [18th, 19th]...... D1068-96(A or B).............. I-3381-85..................... 974.27 [SU]3[/SU]
SU].
AA furnace................... 236.2......................... 3113 B [18th, 19th]........... D1068-96(C)
ICP/AES [SU]36[/SU].......... 200.7 [SU]5[/SU].............. 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 [SU]50[/SU]
DCP [SU]36[/SU] or........... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Phenanthroline) .............................. 3500-Fe B [20th] and 3500-Fe D D1068-96(D)................... .............................. Note 22.
[18th, 19th].
31. Kjeldahl Nitrogen_Total, (as
N), mg/L:
Digestion and distillation 351.3......................... 4500-N[INF]org[/INF] B or C D3590-89(A)
followed by. and 4500-NH[INF]3[/INF] B
[18th, 19th, 20th].
Titration.................... 351.3......................... .............................. D3590-89(A)................... .............................. 973.48 \3\
Nesslerization............... 351.3......................... 4500-NH[INF]3[/INF] C [18th].. D3590-89(A)...................
Electrode.................... 351.3......................... 4500-NH[INF]3[/INF] C [19th,
20th] and 4500-NH[INF]3[/INF]
E [18th].
Automated phenate colorimetric... 351.1......................... .............................. .............................. I-4551-78\8\
Semi-automated block digestor 351.2......................... .............................. D3590-89(B)................... I-4515-91 \45\................
colorimetric.
Manual or block digestor 351.4......................... .............................. D3590-89(A)
potentiometric.
Block digester, followed by Auto .............................. .............................. .............................. .............................. Note 39.
distillation and Titration, or.
Nesslerization, or............... .............................. .............................. .............................. .............................. Note 40.
Flow injection gas diffusion..... .............................. .............................. .............................. .............................. Note 41.
32. Lead_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 239.1......................... 3111 B or C [18th, 19th]...... D3559-96(A or B).............. I-3399-85..................... 974.27 \3\
AA furnace................... 239.2......................... 3113 B [18th, 19th]........... D3559-96(D)................... I-4403-89 \51\
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP [SU]36[/SU].............. .............................. .............................. D4190-94...................... .............................. Note 34.
Voltametry \11\ or........... D3559-96(C)...................
Colorimetric (Dithizone)..... 3500-Pb B [ 20th] and 3500-Pb
D [18th, 19th].
33. Magnesium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 242.1......................... 3111 B [18th, 19th]........... D511-93(B).................... I-3447-85..................... 974.27 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP or....................... .............................. .............................. .............................. .............................. Note 34.
Gravimetric.................. .............................. 3500-Mg D [18th, 19th]........
34. Manganese-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 243.1......................... 3111 B [18th, 19th]........... D858-95(A or B)............... I-3454-85..................... 974.27 \3\
AA furnace................... 243.2......................... 3113 B [18th, 19th]........... D858-95(C)
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP \36\, or................. .............................. .............................. D4190-94...................... .............................. Note 34
Colorimetric (Persulfate), or .............................. 3500-Mn B [20th] and 3500-Mn D .............................. .............................. 920.203 \3\
[18th, 19th].
(Periodate).................. .............................. .............................. .............................. .............................. Note 23.
35. Mercury_Total,\4\ mg/L:
Cold vapor, manual or........ 245.1......................... 3112 B [18th, 19th]........... D3223-91...................... I-3462-85..................... 977.22 \3\
Automated.................... 245.2
Oxidation, purge and trap, 1631E \43\
and cold vapor atomic
fluorescence spectrometry
(ng/L).
36. Molybdenum_Total \4\, mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 246.1......................... 3111 D [18th, 19th]........... .............................. I-3490-85
AA furnace................... 246.2......................... 3113 B [18th, 19th]........... .............................. I-3492-96 \47\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
37. Nickel_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 249.1......................... 3111 B or C [18th, 19th]...... D1886-90(A or B).............. I-3499-85.....................
AA furnace................... 249.2......................... 3113 B [18th, 19th]........... D1886-90(C)................... I-4503-89 \51\................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP \36\, or................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (heptoxime)..... .............................. 3500-Ni D [17th]..............
38. Nitrate (as N), mg/L:
Colorimetric (Brucine 352.1......................... .............................. .............................. .............................. 973.50,\3\ 419D,\17\ p. 28
sulfate), or Nitrate-nitrite \9\
N minus Nitrite N (See
parameters 39 and 40).
39. Nitrate-nitrite (as N),
mg/L:
Cadmium reduction, Manual or. 353.3......................... 4500-NO[INF]3[/INF][SU]-[/SU]E D3867-99(B)...................
[18th, 19th, 20th].
Automated, or................ 353.2......................... 4500-NO[INF]3[/INF][SU]-[/SU]F D3867-99(A)................... I-4545-85.....................
[18th, 19th, 20th].
Automated hydrazine.......... 353.1......................... 4500-NO[INF]3[/INF][SU]-[/SU]H
[18th, 19th, 20th].
40. Nitrite (as N), mg/L;
Spectrophotometric:
Manual or.................... 354.1......................... 4500-NO[INF]2[/INF][SU]-[/SU]B .............................. .............................. Note 25.
[18th, 19th, 20th].
Automated (Diazotization).... .............................. .............................. .............................. I-4540-85.....................
41. Oil and grease_Total
recoverable, mg/L:
Gravimetric (extraction)..... 413.1......................... 5520B [18th, 19th, 20th] \38\.
Oil and grease and non-polar 1664A \42\.................... 5520B [18th, 19th, 20th] \38\.
material, mg/L: Hexane
extractable material (HEM):
n-Hexane extraction and
gravimetry.
Silica gel treated HEM (SGT- 1664A \42\....................
HEM): Silica gel treatment
and gravimetry.
42. Organic carbon_Total (TOC),
mg/L:
Combustion or oxidation...... 415.1......................... 5310 B, C, or D [18th, 19th, D2579-93 (A or B)............. .............................. 973.47,\3\ p. 14 \24\
20th].
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 [18th, 19th, 20th]... .............................. I-4601-85..................... 973.56 \3\
Manual single reagent........ 365.2......................... 4500-P E [18th, 19th, 20th]... 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 [18th, 19th]...........
AA furnace................... 252.2.........................
46. Oxygen, dissolved, mg/L:
Winkler (Azide modification), 360.2......................... 4500-O C [18th, 19th, 20th]... D888-92(A).................... I-1575-78 \8\................. 973.45B \3\
or.
Electrode.................... 360.1......................... 4500-O G [18th, 19th, 20th]... D888-92(B).................... I-1576-78 \8\.................
47. Palladium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 253.1......................... 3111 B [18th, 19th]........... .............................. .............................. 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) 420.1......................... .............................. .............................. .............................. Note 27.
manual, or.
Automated \19\........... 420.2.........................
49. Phosphorus (elemental), mg/L:
Gas-liquid chromatography.... .............................. .............................. .............................. .............................. Note 28.
50. Phosphorus_Total, mg/L:
Persulfate digestion followed 365.2......................... 4500-P B, 5 [18th, 19th, 20th] .............................. .............................. 973.55 \3\
by.
Manual or.................... 365.2 or 365.3................ 4500-P E [18th, 19th, 20th]... D515-88(A)
Automated ascorbic acid 365.1......................... 4500-P F [18th, 19th, 20th]... .............................. I-4600-85..................... 973.56 \3\
reduction.
Semi-automated block digestor 365.4......................... .............................. D515-88(B).................... I-4610-91 \48\................
51. Platinum_Total,\4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration......... 255.1......................... 3111 B [18th, 19th]...........
AA furnace................... 255.2.........................
DCP.......................... .............................. .............................. .............................. .............................. Note 34
52. Potassium_Total,\4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration......... 258.1......................... 3111 B [18th, 19th]........... .............................. I-3630-85..................... 973.53 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
Flame photometric, or........ .............................. 3500-K B [20th] and 3500-K D
[18th, 19th].
Colorimetric................. .............................. .............................. .............................. .............................. 317 B \17\
53. Residue_Total, mg/L:
Gravimetric, 103-105°... 160.3......................... 2540 B [18th, 19th, 20th]..... .............................. I-3750-85.....................
54. Residue_filterable, mg/L:
Gravimetric, 180°....... 160.1......................... 2540 C [18th, 19th, 20th]..... .............................. I-1750-85.....................
55. Residue_nonfilterable (TSS),
mg/L:
Gravimetric, 103-105° 160.2......................... 2540 D [18th, 19th, 20th]..... .............................. I-3765-85.....................
post washing of residue.
56. Residue_settleable, mg/L:
Volumetric, (Imhoff cone), or 160.5......................... 2540 F [18th, 19th, 20th].....
gravimetric.
57. Residue_Volatile, mg/L:
Gravimetric, 550°....... 160.4......................... .............................. .............................. I-3753-85.....................
58. Rhodium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 265.1......................... 3111 B [18th, 19th]...........
AA furnace................... 265.2.........................
59. Ruthenium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 267.1......................... 3111 B [18th, 19th]...........
AA furnace................... 267.2.........................
60. Selenium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA furnace................... 270.2......................... 3113 B [18th, 19th]........... D3859-98(B)................... I-4668-98 \49\................
ICP/AES,\36\ or.............. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
AA gaseous hydride........... .............................. 3114 B [18th, 19th]........... D3859-98(A)................... I-3667-85.....................
61. Silica \37\_Dissolved, mg/L;
0.45 micron filtration followed
by:
Colorimetric, Manual or...... 370.1......................... 4500-SiO[INF]2[/INF] C [20th] D859-94....................... I-1700-85.....................
and 4500-Si D [18th, 19th].
Automated (Molybdosilicate), .............................. .............................. .............................. I-2700-85.....................
or.
ICP.......................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
62. Silver_Total,\4\ mg/L:
Digestion [SU]4 29[/SU] followed
by:
AA direct aspiration......... 272.1......................... 3111 B or C [18th, 19th]...... .............................. I-3720-85..................... 974.27,\3\ p. 37 \9\
AA furnace................... 272.2......................... 3113 B [18th, 19th]........... .............................. I-4724-89 \51\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
63. Sodium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 273.1......................... 3111 B [18th, 19th]........... .............................. I-3735-85..................... 973.54 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP, or...................... .............................. .............................. .............................. .............................. Note 34.
Flame photometric............ .............................. 3500 Na B [20th] and 3500 Na D
[18th, 19th].
64. Specific conductance,
micromhos/cm at 25 °C:
Wheatstone bridge............ 120.1......................... 2510 B [18th, 19th, 20th]..... D1125-95(A)................... I-2781-85..................... 973.40 \3\
65. Sulfate (as SO[INF]4[/INF]),
mg/L:
Automated colorimetric 375.1.........................
(barium chloranilate).
Gravimetric.................. 375.3......................... 4500-SO[INF]4[/INF][SU]-[/ .............................. .............................. 925.54 \3\
SU]\2\C or D [18th, 19th,
20th].
Turbidimetric................ 375.4......................... .............................. D516-90....................... .............................. 426C \30\
66. Sulfide (as S), mg/L:
Titrimetric (iodine), or..... 376.1......................... 4500-S[SU]-[/SU]\2\F [19th, .............................. I-3840-85.....................
20th] or 4500-S[SU]-[/SU]\2\E
[18th].
Colorimetric (methylene blue) 376.2......................... 4500-S[SU]-[/SU]\2\D [18th,
19th, 20th].
67. Sulfite (as SO[INF]3[/INF]),
mg/L:
Titrimetric (iodine-iodate).. 377.1......................... 4500-SO[INF]3[/INF][SU]-[/
SU]\2\B [18th, 19th, 20th].
68. Surfactants, mg/L:
Colorimetric (methylene blue) 425.1......................... 5540 C [18th, 19th, 20th]..... D2330-88......................
69. Temperature, °C:
Thermometric................. 170.1......................... 2550 B [18th, 19th, 20th]..... .............................. .............................. Note 32.
70. Thallium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 279.1......................... 3111 B [18th, 19th]...........
AA furnace................... 279.2.........................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
71. Tin_Total,\4\ mg/L; Digestion
\4\ followed by:
AA direct aspiration......... 282.1......................... 3111 B [18th, 19th]........... .............................. I-3850-78 \8\.................
AA furnace, or............... 282.2......................... 3113 B [18th, 19th]...........
ICP/AES...................... 200.7 \5\.....................
72. Titanium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 283.1......................... 3111 D [18th, 19th]...........
AA furnace................... 283.2.........................
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
73. Turbidity, NTU:
Nephelometric................ 180.1......................... 2130 B [18th, 19th, 20th]..... D1889-94(A)................... I-3860-85.....................
74. Vanadium_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 286.1......................... 3111 D [18th, 19th]...........
AA furnace................... 286.2......................... .............................. D3373-93......................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP, or...................... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Gallic Acid)... .............................. 3500-V B [20th] and 3500-V D
[18th, 19th].
75. Zinc_Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 289.1......................... 3111 B or C [18th, 19th]...... D1691-95(A or B).............. I-3900-85..................... 974.27,\3\ p. 37 \9\
AA furnace................... 289.2.........................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP,\36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Dithizone) or.. .............................. 3500-Zn E [18th, 19th]........
(Zincon)..................... .............................. 3500-Zn B [20th] and 3500-Zn F .............................. .............................. Note 33.
[18th, 19th].
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory_Cincinnati (EMSL-CI), EPA-600/4-79-020, Revised March
1983 and 1979 where applicable.
\2\ Fishman, M.J., et al. ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, ''U.S. Department of the Interior, Techniques of Water-Resource Investigations of the
U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' methods manual, 15th ed. (1990).
\4\ For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended material and to destroy possible organic-metal
complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes, 1979 and 1983''. One (Section 4.1.3), is a vigorous digestion using nitric acid. A less
vigorous digestion using nitric and hydrochloric acids (Section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types.
Particularly, if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive state. In those situations,
the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing large amounts of organic materials may also benefit by this
vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as
well as determinations for certain elements such as antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all
cases the method write-up should be consulted for specific instructions and/or cautions.
Note to Table 1B Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the above, the EPA procedure must be used.
Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the referenced procedure for total metals must
be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample solution for total metals) may be omitted for AA (direct aspiration or graphite
furnace) and ICP analyses, provided the sample solution to be analyzed meets the following criteria:
a. has a low COD (<20)
b. is visibly transparent with a turbidity measurement of 1 NTU or less
c. is colorless with no perceptible odor, and
d. is of one liquid phase and free of particulate or suspended matter following acidification.
\5\ The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,'' is given at Appendix C of this Part 136.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary distillation step is not necessary: however,
manual distillation will be required to resolve any controversies.
\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies,
Inc., Elmsford, NY 10523.
\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5, Chapter A1 (1979).
\9\ American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 25 West 43rd Street, New York, NY 10036.
\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 (CBOD[INF]5[/INF]) must not be confused with the traditional BOD[INF]5[/INF] test method which measures ``total BOD''. The addition of the
nitrification inhibitor is not a procedural option, but must be included to report the CBOD[INF]5[/INF] parameter. A discharger whose permit requires reporting the traditional BOD[INF]5[/
INF] may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's permit specifically states CBOD[INF]5[/INF] is required can the permittee
report data using a nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, PO Box 2980, College Station, TX 77840.
\14\ Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, PO 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, PO 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, NY 10523.
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, PO 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, PO 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 10.0±0.2. 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 spectrometric 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 Na[INF]2[/INF]S[INF]2[/INF]O[INF]3[/INF] and NaOH. Standards should be
prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.
\30\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition.
\31\ EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of total cyanide.
\32\ Stevens, H.H., Ficke, J.F., and Smoot, G.F., ``Water Temperature_Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.
Geological Survey, Book 1, Chapter D1, 1975.
\33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\ ``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986_Revised 1991, Thermo Jarrell Ash Corporation,
27 Forge Parkway, Franklin, MA 02038.
\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, PO Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM
Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use Trichlorotrifluorethane (1,1,2-trichloro-1,2,2-trifluoroethane; CFC-113) extraction solvent when determining Total Recoverable Oil and Grease (analogous to EPA Method 413.1).
Only use n-hexane extraction solvent when determining Hexane Extractable Material (analogous to EPA Method 1664A). Use of other extraction solvents is strictly prohibited.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\40\ Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and
Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, Virginia 22161.
\43\ USEPA. 2002. Method 1631, Revision E, ``Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry.'' September 2002. Office of Water, U.S.
Environmental Protection Agency (EPA-821-R-02-019). The application of clean techniques described in EPA's draft Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality
Criteria Levels (EPA-821-R-96-011) are recommended to preclude contamination at low-level, trace metal determinations.
\44\ Available Cyanide, Method OIA-1677 (Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry), ALPKEM, A Division of OI Analytical, PO Box 9010, College Station, TX 77842-
9010.
\45\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method'', Open File Report
(OFR) 00-170.
\46\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry'', Open
File Report (OFR) 93-449.
\47\ ''Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry'', Open File
Report (OFR) 97-198.
\48\ ''Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish
That Includes Dialysis'' Open File Report (OFR) 92-146.
\49\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption
Spectrometry'' Open File Report (OFR) 98-639.
\50\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission
Spectrometry and Inductively Coupled Plasma-Mass Spectrometry'', Open File Report (OFR) 98-165.
\51\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory_Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment'', Open File Report
(OFR) 93-125.
Table IC_List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
EPA method number [SU]2, 7[/SU] Other approved methods
------------------------------------------------------------------------------------------------------------------------
Parameter \1\ Standard Methods
GC GC/MS HPLC [Edition(s)] ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene................ 610................ 625, 1625B......... 610................ 6440 B [18th, D4657-92......... Note 9, p.27.
19th, 20th].
2. Acenaphthylene.............. 610................ 625, 1625B......... 610................ 6440 B, 6410 B D4657-92......... Note 9, p.27.
[18th, 19th,
20th].
3. Acrolein.................... 603................ 624\4\, 1624B...... .................
4. Acrylonitrile............... 603................ 624\4\, 1624B...... .................
5. Anthracene.................. 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
6. Benzene..................... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
7. Benzidine................... ................... 625\5\, 1625B...... 605................ .................. ................. Note 3, p.1.
8. Benzo(a)anthracene.......... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
9. Benzo(a)pyrene.............. 610,............... 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
10. Benzo(b)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
11. Benzo(g, h, i)perylene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
12. Benzo(k)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
13. Benzyl chloride............ ................... ................... ................... .................. ................. Note 3, p 130:
Note 6, p. S102.
14. Benzyl butyl phthalate..... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
15. Bis(2-chloroethoxy) methane 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
16. Bis(2-chloroethyl) ether... 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
17. Bis(2-ethylhexyl) phthalate 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
18. Bromodichloromethane....... 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
19. Bromoform.................. 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
20. Bromomethane............... 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
21. 4-Bromophenylphenyl ether.. 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
22. Carbon tetrachloride....... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.
6230 B [18th,
19th].
23. 4-Chloro-3-methylphenol.... 604................ 625,1625B.......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
24. Chlorobenzene.............. 601, 602........... 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130.
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th],
6200 C [20th] and
6230 B [18th,
19th],.
25. Chloroethane............... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
26. 2-Chloroethylvinyl ether... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
27. Chloroform:................ 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p 130.
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
28. Chloromethane.............. 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th] 6200C
[20th] and 6230 B
[18th, 19th].
29. 2-Chloronaphthalene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
30. 2-Chlorophenol............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
31. 4-Chlorophenylphenyl ether. 611................ 625, 1625B......... ................... 6410 B, [18th, ................. Note 9, p. 27.
19th, 20th].
32. Chrysene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
33. Dibenzo(a,h)anthracene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
34. Dibromochloromethane....... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th] 6200 C
[20th] and 6230 B
[18th, 19th].
35. 1,2-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
36. 1,3-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
37. 1,4-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
38. 3,3-Dichlorobenzidine...... ................... 625, 1625B......... 605................ 6410 B [18th, .................
19th, 20th].
39. Dichlorodifluoromethane.... 601................ ................... ................... 6200 C [20th] and .................
6230 B [18th,
19th].
40. 1,1-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
41. 1,2-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
42. 1,1-Dichloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
43. trans-1,2-Dichloroethene... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
44. 2,4-Dichlorophenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
45. 1,2-Dichloropropane........ 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
46. cis-1,3-Dichloropropene.... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
47. trans-1,3-Dichloropropene.. 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
48. Diethyl phthalate.......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
49. 2,4-Dimethylphenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
50. Dimethyl phthalate......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
51. Di-n-butyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
52. Di-n-octyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
53. 2,3-Dinitrophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6420 B
[18th, 19th,
20th].
54. 2,4-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
55. 2,6-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
56. Epichlorohydrin............ ................... ................... ................... .................. ................. Note 3, p. 130;
Note 6, p. S102.
57. Ethylbenzene............... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
58. Fluoranthene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
59. Fluorene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
60. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B
dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro- ................... 1613B .................
dibenzofuran.
62. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B .................
dibenzo-p-dioxin.
63. Hexachlorobenzene.......... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
64. Hexachlorobutadiene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
65. Hexachlorocyclopentadiene.. 612................ \5\625, 1625B..... ................... 6410 [18th, 19th, ................. Note 9, p. 27.
20th].
66. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
67. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
68. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............
dibenzofuran.
69. 2,3,4,6,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
70. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
71. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
72. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
73. Hexachloroethane........... 616................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
74. Ideno(1,2,3-cd) pyrene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
75. Isophorone................. 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
76. Methylene chloride......... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.
6230 B [18th,
19th].
77. 2-Methyl-4,6-dinitrophenol. 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
78. Naphthalene................ 610................ 625, 1625B......... 610................ 6440 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
79. Nitrobenzene............... 609................ 625, 1625B......... ................... 6410 B [18th, D4657-92......... Note 9, p. 27.
19th, 20th].
80. 2-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27
[18th, 19th,
20th].
81. 4-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27
[18th, 19th,
20th].
82. N-Nitrosodimethylamine..... 607................ 625\5\, 1625B...... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
83. N-Nitrosodi-n-propylamine.. 607................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
84. N-Nitrosodiphenylamine..... 607................ 625\5\, 1625B...... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
85. Octachlorodibenzofuran..... ................... 1613B..............
86. Octachlorodibenzo-p-dioxin. ................... 1613B..............
87. 2,2'-Oxybis(2- 611................ 625, 1625B......... ................... 6410 B [18th,
chloropropane) [also known as 19th, 20th].
bis(2-chloroisopropyl) ether].
88. PCB-1016................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
89. PCB-1221................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
90. PCB-1232................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
91. PCB-1242................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
92. PCB-1248................... 608................ 625................
93. PCB-1254................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
94. PCB-1260................... 608................ 625................ ................... 6410 B, 6630 B ................. Note 3, p. 43
[18th, 19th,
20th].
95. 1,2,3,7,8-Pentachloro- ................... 1613B..............
dibenzofuran.
96. 2,3,4,7,8-Pentachloro- ................... 1613B..............
dibenzofuran.
97. 1,2,3,7,8,- ................... 1613B..............
Pentachlorodibenzo-p-dioxin.
98. Pentachlorophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6630 B ................. Note 3, p. 140;
[18th, 19th, Note 9, p. 27
20th].
99. Phenanthrene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27
[18th, 19th,
20th].
100. Phenol.................... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27
[18th, 19th,
20th].
101. Pyrene.................... 610................ 625, 1625B......... 610................ 6440 B, 6410 B D4675-92......... Note 9, p. 27
D4675-92 [18th,
19th, 20th].
102. 2,3,7,8-Tetrachloro- ................... 1613B..............
dibenzofuran.
103. 2,3,7,8-Tetrachlorodibenzo- ................... 613, 1613B.........
p-dioxin.
104. 1,1,2,2-Tetrachloroethane. 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
105. Tetrachloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
106. Toluene................... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
107. 1,2,4-Trichlorobenzene.... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 3, p. 130;
19th, 20th]. Note 9, p. 27.
108. 1,1,1-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
109. 1,1,2-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
110. Trichloroethene........... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
111. Trichlorofluoromethane.... 601................ 624................ ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
112. 2,4,6-Trichlorophenol..... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
113. Vinyl chloride............ 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter (mg/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/
L).
\2\ The full text of Methods 601-613, 624, 625, 1624B, and 1625B, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of
this Part 136. The full text of Method 1613B is incorporated by reference into this Part 136 and is available from the National Technical Information
Services as stock number PB95-104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test
procedures is given at Appendix B, ``Definition and 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.
\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 1624B.
\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, orMethod 1625B, are preferred methods for these compounds.
\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, 1624B, and 1625B (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 1624B and 1625B) of all samples to
monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these Methods. When the recovery of any parameter falls
outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate
regulatory compliance.
Note: These warning limits are promulgated as an ``interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'' 3M Corporation Revised 10/28/94.
\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory_Determination of Inorganic and Organic
Constituents in Water and Fluvial Sediments'' U.S. Geological Survey, Open File Report 93-125.
Table ID_List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard Methods 18th,
Parameter Method EPA [SU]2, 7[/SU] 19th, 20th Ed. ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin......................... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B
2. Ametryn........................ GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p S68.
3. Aminocarb...................... TLC................... ...................... ...................... ...................... Note 3, p. 94; Note
6, p. S16.
4. Atraton........................ GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68.
5. Atrazine....................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
6. Azinphos methyl................ GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
6, p. S51.
7. Barban......................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
8. [agr]-BHC...................... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
8.
GC/MS................. 625 \5\............... 6410 B................
9. [beta]-BHC..................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.
GC/MS................. 625 \5\............... 6410 B................
10. [delta]-BHC................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.
GC/MS................. 625 \5\............... 6410 B................
11. [gamma]-BHC (Lindane)......... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 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.
14. Carbophenothion............... GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
15. Chlordane..................... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
16. Chloropropham................. TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
17. 2,4-D......................... GC.................... ...................... 6640 B................ ...................... Note 3, p. 115; Note
4, p. 40.
18. 4,4[prime]-DDD................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
19. 4,4[prime]-DDE................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
20. 4,4[prime]-DDT................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
21. Demeton-O..................... GC.......