[Code of Federal Regulations]
[Title 40, Volume 22]
[Revised as of July 1, 2007]
From the U.S. Government Printing Office via GPO Access
[CITE: 40CFR136.3]
[Page 5-60]
TITLE 40--PROTECTION OF ENVIRONMENT
CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)
PART 136_GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF
Sec. 136.3 Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are
listed together with test procedure descriptions and references in
Tables IA, IB, IC, ID, IE, IF, IG, and IH. In the event
[[Page 6]]
of a conflict between the reporting requirements of 40 CFR Parts 122 and
125 and any reporting requirements associated with the methods listed in
these tables, the provisions of 40 CFR Parts 122 and 125 are controlling
and will determine a permittee's reporting requirements. The full text
of the referenced test procedures are incorporated by reference into
Tables IA, IB, IC, ID, IE, IF, IG, and IH. 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. Documents may be inspected at EPA's Water Docket, EPA
West, 1301 Constitution Avenue, NW., Room B102, Washington, DC
(Telephone: 202-566-2426); or at the National Archives and Records
Administration (NARA). For information on the availability of this
material at NARA, call 202-741-6030, or go to: http://www.archives.gov/
federal--register/ code--of--federal--regulations/ ibr--locations.html.
These test procedures are incorporated as they exist on the day of
approval and a notice of any change in these test procedures will be
published in the Federal Register. The discharge parameter values for
which reports are required must be determined by one of the standard
analytical test procedures incorporated by reference and described in
Tables IA, IB, IC, ID, IE, IF, IG, and IH or by any alternate test
procedure which has been approved by the Administrator under the
provisions of paragraph (d) of this section and Sec. Sec. 136.4 and
136.5. Under certain circumstances paragraph (c) of this section, Sec.
136.5(a) through (d) or 40 CFR 401.13, other additional or alternate
test procedures may be used.
[[Page 7]]
Table IA--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter and units Method \1\ EPA 18th, 19th, 20th Standard methods AOAC, ASTM, USGS Other
ed. online
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number Most Probable p. 132 \3\........ 9221 C E.......... 9221 C E-99.......
per 100 mL or number per Number (MPN),\5\ 1680 \12,14\......
gram dry weight. tube 3 dilution, 1681 \12,19\......
or
Membrane filter p. 124 \3\........ 9222 D............ 9222 D-97......... B-0050-85 \5\.....
(MF) \2\, single
step.
2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 \3\........ 9221 C E.......... 9221 C E-99.......
presence of chlorine, dilution, or
number per 100 mL.
MF \2\, single p. 124 \3\........ 9222 D............ 9222 D-97.........
step.
3. Coliform (total), number MPN, 5 tube, 3 p. 114 \3\........ 9221 B............ 9221 B-99.........
per 100 mL. dilution, or
MF \2\, single p. 108 \3\........ 9222 B............ 9222 B-97......... B-0025-8 \5\......
step or two step.
4. Coliform (total), in MPN, 5 tube, 3 p. 114 \3\........ 9221 B............ 9221 B-99.........
presence of chlorine, dilution, or
number per 100 mL.
MF \2\ with p. 111 \3\........ 9222 (B+B.5c)..... 9222 (B+B.5c)-97..
enrichment.
5. E. coli, number per 100 MPN \7,9,15\ .................. 9223 B \13\....... 9223 B-97 \13\.... 991.15 \11\....... Colilert[supreg]\1
mL \20\. multiple tube/ 3,17\
multiple well. Colilert-
18[supreg]\13,16,
17\
MF \2,6,7,8,9\ 1603 \21\......... .................. .................. .................. mColiBlue-
single step. 24[supreg]\18\
6. Fecal streptococci, MPN, 5 tube 3 p. 139 \3\........ 9230 B............ 9230 B-93.........
number per 100 mL. dilution,.
MF \2\, or........ p. 136 \3\........ 9230 C............ 9230 C-93......... B-0055-85 \5\.....
Plate count....... p. 143 \3\........
7. Enterococci, number per MPN \7,9\, .................. .................. .................. D6503-99 \10\..... Enterolert[supreg]
100 mL \20\. multiple tube/ \13,23\
multiple well.
MF \2,6,7,8,9\ 1600 \24\.........
single step.
8. Salmonella, number per MPN multiple tube. 1682 \22\.........
gram dry weight \12\.
Aquatic Toxicity:
9. Toxicity, acute, fresh Ceriodaphnia dubia 2002.0 \25\.......
water organisms, LC 50, acute.
percent effluent.
Daphnia puplex and 2021.0 \25\.......
Daphnia magna
acute.
[[Page 8]]
Fathead Minnow, 2000.0 \25\.......
Pimephales
promelas, and
Bannerfin shiner,
Cyprinella
leedsi, acute.
Rainbow Trout, 2019.0 \25\.......
Oncorhynchus
mykiss, and brook
trout, Salvelinus
fontinalis, acute.
10. Toxicity, acute, Mysid, Mysidopsis 2007.0 \25\.......
estuarine and marine bahia, acute.
organisms of the Atlantic
Ocean and Gulf of Mexico,
LC50, percent effluent.
Sheepshead Minnow, 2004.0 \25\.......
Cyprinodon
variegatus, acute.
Silverside, 2006.0 \25\.......
Menidia
beryllina,
Menidia menidia,
and Menidia
peninsulae, acute.
11. Toxicity, chronic, fresh Fathead minnow, 1000.0 \26\.......
water organisms, NOEC or Pimephales
IC25, percent effluent. promelas, larval
survival and
growth.
Fathead minnow, 1001.0 \26\.......
Pimephales
promelas, embryo-
larval survival
and
teratogenicity.
Daphnia, 1002.0 \26\.......
Ceriodaphnia
dubia, survival
and reproduction.
Green alga, 1003.0 \26\.......
Selenastrum
capricornutum,
growth.
[[Page 9]]
12. Toxicity, chronic, Sheepshead minnow, 1004.0 \27\.......
estuarine and marine Cyprinodon
organisms of the Atlantic variegatus,
Ocean and Gulf of Mexico, larval survival
NOEC or IC25, percent and growth.
effluent.
Sheepshed minnow, 1005.0 \27\.......
Cyprinodon
variegatus,
embryo-larval
survival and
teratogenicity.
Inland silverside, 1006.0 \27\.......
Menidia
beryllina, larval
survival and
growth.
Mysid, Mysidopsis 1007.0 \27\.......
bahia, survival,
growth, and
fecundity.
Sea urchin, 1008.0 \27\.......
Arbacia
punctulata,
fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.
\4\ [Reserved]
\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 the Interior, Reston, VA.
\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 been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
results.
\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. ASTM International. 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, MD 20877-2417.
\12\ Recommended for enumeration of target organism in sewage sludge.
\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\ USEPA. July 2006. Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC
Medium. US Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-012.
[[Page 10]]
\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[supreg] may be enumerated with
the multiple-well procedures, Quanti-Tray[supreg] Quanti-Tray[supreg] 2000, and the MPN calculated from the table provided by the manufacturer.
\16\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\17\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\18\ A description of the mColiBlue24[supreg] test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\19\ USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. U.S. Environmental
Protection Agency, Office of Water, Washington, DC EPA-821-R-06-013.
\20\ Recommended for enumeration of target organism in wastewater effluent.
\21\ USEPA. July 2006. 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, DC EPA-821-R-06-011.
\22\ USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-014.
\23\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\24\ USEPA. July 2006. 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-06-009.
\25\ 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.
\26\ 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.
\27\ 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 Methodology \58\ Standard methods Standard methods Standard methods
EPA 35, 52 (18th, 19th) (20th) online ASTM USGS/AOAC/other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L....... Electrometric ..................... 2310 B(4a)........... 2310 B(4a)........... 2310 B(4a)-97......... D1067-92, 02........ I-1020-85 \2\
endpoint or
phenolphthalein
endpoint.
2. Alkalinity, as CaCO3, mg/L.... Electrometric or ..................... 2320 B............... 2320 B............... 2320 B-97............. D1067-92, 02........ 973.43 \3\, I-1030-
Colorimetric 85 \2\
titration to pH
4.5, manual, or
automatic........... 310.2 (Rev. 1974) \1\ ..................... ..................... ...................... .................... I-2030-85 \2\
3. Aluminum--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99............. .................... I-3051-85 \2\
\36\.
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99.............
[[Page 11]]
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-9750
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14\3\
(1994).
Direct Current ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Plasma (DCP) \36\.
Colorimetric ..................... 3500-Al D............ 3500-Al B............ 3500-Al B-01..........
(Eriochrome cyanine
R).
4. Ammonia (as N), mg/L.......... Manual, distillation 350.1, Rev. 2.0 4500-NH B3........... 4500-NH3 B........... 4500-NH3 B-97......... .................... 973.49 \3\
(at pH 9.5) \6\ (1993).
followed by:
Nesslerization...... ..................... 4500-NH3 C (18th ..................... ...................... D1426-98, 03 (A).... 973.49 \3\, I-3520-
only). 85 \2\
Titration........... ..................... 4500-NH3 C (19th) and 4500-NH3 C........... 4500-NH3 C-97.........
4500-NH3 E (18th).
Electrode........... ..................... 4500-NH3 D or E 4500-NH3 D or E...... 4500-NH3 D or E-97.... D1426-98, 03 (B)....
(19th) and 4500-NH3
F or G (18th).
Automated phenate, 350.1 \60\, Rev. 2.0 4500-NH3 G (19th) and 4500-NH3 G........... 4500-NH3 G-97......... .................... I-4523-85 \2\
or. (1993). 4500-NH3 H (18th).
Automated electrode. ..................... ..................... ..................... ...................... .................... See footnote 7
Ion Chromatography.. ..................... ..................... ..................... ...................... D6919-03............
5. Antimony--Total, \4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99.............
\36\.
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99.............
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
6. Arsenic--Total, \4\ mg/L...... Digestion \4\ 206.5 (Issued 1978)
followed by. \1\.
[[Page 12]]
AA gaseous hydride.. ..................... 3114 B 4.d........... ..................... 3114 B 4.d-97......... D2972-97, 03 (B).... I-3062-85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D2972-97, 03 (C).... I-4063-98 \49\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
Colorimetric (SDDC). ..................... 3500-As C............ 3500-As B............ 3500-As B-97.......... D2972-97, 03 (A).... I-3060-85
7. Barium--Total,\4\ mg/L........ Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99............. .................... I-3084-85 \2\
\36\.
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D4382-95, 02........
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP \36\............ ..................... ..................... ..................... ...................... .................... See footnote \34\
8. Beryllium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99............. D3645-93 (88), 03 I-3095-85 \2\
(A).
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D3645-93 (88), 03
(B).
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP, or............. ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
[[Page 13]]
Colorimetric ..................... 3500-Be D............
(aluminon).
9. Biochemical oxygen demand Dissolved Oxygen ..................... 5210 B............... 5210 B............... 5210 B-01............. .................... 973.44,\3\ p.
(BOD5), mg/L. Depletion. 17.\9\, I-1578-78
\8\
10. Boron--Total,\37\ mg/L....... Colorimetric ..................... 4500-B B............. 4500-B B............. 4500-B B-00........... .................... I-3112-85 \2\
(curcumin).
ICP/AES, or......... 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B 99............. .................... I-4471-97 \50\
(1994).
DCP................. ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote 34
11. Bromide, mg/L................ Titrimetric......... ..................... ..................... ..................... ...................... D1246-95, 99 (C).... p. S44.\10\
.................... ..................... ..................... ..................... ...................... .................... I-1125-85 \2\
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
12. Cadmium--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D3557-95, 02 (A or 974.27,\3\ p.
\36\. B). 37.\9\, I-3135-85
\2\ or I-3136-85
\2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D3557-95, 02 (D).... I-4138-89 \51\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-1472-85\2\ or I-
(1994). 4471-97 \50\
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP \36\............ ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Voltametry \11\, or. ..................... ..................... ..................... ...................... D3557-95, 02 (C)....
Colorimetric ..................... 3500-Cd D............
(Dithizone).
13. Calcium--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. D511-93, 03(B)...... I-3152-85 \2\
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
DCP, or............. ..................... ..................... ..................... ...................... .................... See footnote \34\
[[Page 14]]
Titrimetric (EDTA).. ..................... 3500-Ca D............ 3500-Ca B............ 3500-Ca B-97.......... D511-93, 03(A)......
Ion Chromatography.. ..................... ..................... ..................... ...................... D6919-03............
14. Carbonaceous biochemical Dissolved Oxygen ..................... 5210 B............... 5210 B............... 5210 B-01.............
oxygen demand (CBOD5), mg/L \12\. Depletion with
nitrification
inhibitor.
15. Chemical oxygen demand (COD), Titrimetric......... 410.3 (Rev. 1978) \1\ 5220 C............... 5220 C............... 5220 C-97............. D1252-95, 00 (A).... 973.46 \3\, p. 17
mg/L. \9\ I-3560-85 \2\
Spectrophotometric, 410.4, Rev. 2.0 5220 D............... 5220 D............... 5220 D-97............. D1252-95, 00 (B).... See footnotes \13,\
manual or automatic. (1993). \14\. I-3561-85 \2\
16. Chloride, mg/L............... Titrimetric: (silver ..................... 4500-Cl-B............ 4500-Cl-B............ 4500-Cl-B-97.......... D512-89(99) (B)..... I-1183-85 \2\
nitrate) or.
(Mercuric nitrate).. ..................... 4500-Cl-C............ 4500-Cl-C............ 4500-Cl-C-97.......... D512-89 (99) (A).... 973.51 \3\, I-1184-
85 \2\
Colorimetric: manual ..................... ..................... ..................... ...................... .................... I-1187-85 \2\
or.
Automated ..................... 4500-Cl-E............ 4500-Cl-E............ 4500-Cl-E-97.......... .................... I-2187-85 \2\
(Ferricyanide).
Potentiometric ..................... 4500-Cl-D............ 4500-Cl-D............ 4500-Cl-D-97..........
Titration.
Ion Selective ..................... ..................... ..................... ...................... D512-89(99)(C)......
Electrode.
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
17. Chlorine--Total residual, mg/ Amperometric direct, ..................... 4500-Cl D............ 4500-Cl D............ 4500-Cl D-00.......... D1253-86 (96), 03...
L; Titrimetric. or.
Amperometric direct ..................... 4500-Cl E............ 4500-Cl E............ 4500-Cl E-00..........
(low level).
Iodometric direct... ..................... 4500-Cl B............ 4500-Cl B............ 4500-Cl B-00..........
Back titration ether ..................... 4500-Cl C............ 4500-Cl C............ 4500-Cl C-00..........
end-point \15\ or.
DPD-FAS............. ..................... 4500-Cl F............ 4500-Cl F............ 4500-Cl F-00..........
[[Page 15]]
Spectrophotometric, ..................... 4500-Cl G............ 4500-Cl G............ 4500-Cl G-00..........
DPD or.
Electrode........... ..................... ..................... ..................... ...................... .................... See footnote \16\
18. Chromium VI dissolved, mg/L.. 0.45-micron
Filtration followed
by:
AA chelation- ..................... 3111 C............... ..................... 3111 C-99............. .................... I-1232-85
extraction or.
Ion Chromatography.. 218.6, Rev. 3.3 3500-Cr E............ 3500-Cr C............ 3500-Cr C-01.......... D5257-97............ 993.23
(1994).
Colorimetric ..................... 3500-Cr D............ 3500-Cr B............ 3500-Cr B-01.......... D1687-92, 02 (A).... I-1230-85
(Diphenyl-carbazide
).
19. Chromium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. D1687-92, 02 (B).... 974.27 \3\, I-3236-
\36\. 85 \2\
AA chelation- ..................... 3111 C............... ..................... 3111 C-99.............
extraction.
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D1687-92, 02 (C).... I-3233-93 \46\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP,\36\ or......... ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500-Cr D............ 3500-Cr B............ 3500-Cr B-01..........
(Diphenyl-carbazide
).
20. Cobalt--Total,\4\ mg/L....... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D3558-94, 03 (A or p. 37 \9\, I-3239-85
B). \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D3558-94, 03 (C).... I-4243-89 \51\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP................. ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
[[Page 16]]
21. Color, platinum cobalt units Colorimetric (ADMI), ..................... 2120 E............... 2120 E............... ...................... .................... See footnote \18\
or dominant wavelength, hue, or.
luminance purity.
(Platinum cobalt), ..................... 2120 B............... 2120 B............... 2120 B-01............. .................... I-1250-85 \2\
or.
Spectrophotometric.. ..................... 2120 C............... 2120 C...............
22. Copper--Total,\4\ mg/L....... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D1688-95, 02 (A or 974.27 \3\ p. 37 \9\
\36\. B). I-3270-85 \2\ or I-
3271-85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D1688-95, 02 (C).... I-4274-89 \51\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP \36\ or......... ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500-Cu D............ 3500-Cu B............ 3500-Cu B-99..........
(Neocuproine) or.
(Bicinchoninate).... ..................... 3500-Cu E............ 3500-Cu C............ 3500-Cu C-99.......... .................... See footnote \19\
23. Cyanide--Total, mg/L......... Automated ..................... ..................... ..................... ...................... .................... Kelada-01 \55\
Distillation and
Colorimetry, or.
Manual distillation 335.4, Rev. 1.0 4500-CN-C............ 4500-CN-C............ ...................... D2036-98(A)......... 10-204-00-1-X \56\
with MgCl2 followed (1993) \57\.
by:
Titrimetric or...... ..................... 4500-CN-D............ 4500-CN-D............ 4500-CN-D-99.......... .................... p. 22 \9\
Spectrophotometric, ..................... 4500-CN-E............ 4500-CN-E............ 4500-CN-E-99.......... D2036-98(A)......... I-3300-85
manual or.
Automated \20\ or... 335.4, Rev. 1.0 ..................... ..................... ...................... .................... 10-204-00-1-X \56\,
(1993) \57\. I-4302-85 \2\
[[Page 17]]
Ion Selective ..................... 4500-CN-F............ 4500-CN-F............ 4500-CN-F-99.......... D2036-98(A).........
Electrode.
24. Available Cyanide, mg/L...... Cyanide Amenable to ..................... 4500-CN-G............ 4500-CN-G............ 4500-CN-G-99.......... D2036-98(B).........
Chlorination
(CATC); Manual
distillation with
MgCl2 followed by
Titrimetric or
Spectrophotometric.
Flow injection and ..................... ..................... ..................... ...................... D6888-04............ OIA-1677 \44\
ligand exchange,
followed by
amperometry \61\.
Automated ..................... ..................... ..................... ...................... .................... Kelada-01 \55\
Distillation and
Colorimetry.
25. Fluoride--Total, mg/L........ Manual ..................... 4500-F-B............. 4500-F-B............. 4500-F-B-97...........
distillation\6\
followed by:
Electrode, manual or ..................... 4500-F-B............. 4500-F-B............. 4500-F-C-97........... D1179-93, 99 (B)....
Automated........... ..................... ..................... ..................... ...................... .................... I-4327-85 \2\
Colorimetric, ..................... 4500-F-D............. 4500-F-D............. 4500-F-D-97........... D1179-93, 99 (A)....
(SPADNS) or.
Automated complexone ..................... 4500-F-E............. 4500-F-E............. 4500-F-E-97...........
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97,03......... 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
26. Gold--Total,\4\ mg/L......... Digestion \4\
followed by:
AA direct ..................... 3111 B............... ..................... 3111 B-99.............
aspiration, or.
AA furnace, or...... 231.2 (Rev. 1978) \1\
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
27. Hardness--Total, as CaCO3, mg/ Automated 130.1 (Issued 1971)
L. colorimetric,. \1\.
Titrimetric (EDTA) ..................... 2340 B or C.......... 2340 B or C.......... 2340 B or C-97........ D1126-86(92), 02.... 973.5 2B \3\, I-1338-
or. 85\2\
[[Page 18]]
Ca 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 ..................... 4500-H+ B............ 4500-H+ B............ 4500-H+ B-00.......... D1293-84 (90), 99 (A 973.41.\3\, I-1586-
measurement or. or B). 85 \2\
Automated electrode. 150.2 (Dec. 1982) \1\ ..................... ..................... ...................... .................... See footnote\21\, I-
2587-85\2\
29. Iridium--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99.............
or.
AA furnace.......... 235.2 (Issued 1978)
\1\.
30. Iron--Total,\4\ mg/L......... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D1068-96, 03 (A or 974.27 \3\, I-3381-
\36\. B). 85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D1068-96, 03 (C)....
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
DCP \36\ or......... ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500-Fe D............ 3500-Fe B............ 3500-Fe B-97.......... D1068-96, 03 (D).... See footnote \22\
(Phenanthroline).
31. Kjeldahl Nitrogen \5\--Total, Digestion and ..................... 4500-Norg B or C and 4500-Norg B or C and 4500-Norg B or C-97 D3590-89, 02 (A)....
(as N), mg/L. distillation 4500-NH3 B. 4500-NH3 B. and 4500-NH3 B-97.
followed by: \20\
[[Page 19]]
Titration or........ ..................... 4500-NH3 C (19th) and 4500-NH3 C........... 4500-NH3 C-97......... D3590-89, 02 (A).... 973.48 \3\
4500-NH 3 E (18th).
Nesslerization or... ..................... 4500-NH3 C (18th ..................... ...................... D3590-89, 02 (A)....
Only).
Electrode........... ..................... 4500-NH3 F or G 4500-NH3 D or E...... 4500-NH3 D or E-97....
(18th) and 4500-NH3
D or E (19th).
Automated phenate 351.1 (Rev. 1978) \1\ ..................... ..................... ...................... .................... I-4551-78 \8\
colorimetric.
Semi-automated block 351.2, Rev. 2.0 ..................... ..................... ...................... D3590-89, 02 (B).... I-4515-91 \45\
digestor (1993).
colorimetric.
Manual or block ..................... ..................... ..................... ...................... D3590-89, 02 (A)....
digestor
potentiometric.
Block digester, ..................... ..................... ..................... ...................... .................... See footnote \39\
followed by Auto
distillation and
Titration, or.
Nesslerization, or.. ..................... ..................... ..................... ...................... .................... See footnote \40\
Flow injection gas ..................... ..................... ..................... ...................... .................... See footnote \41\
diffusion.
32. Lead--Total,\4\ mg/L......... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D3559-96, 03 (A or 974.27 \3\, I-3399-
\36\. B). 85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D3559-96, 03 (D).... I-4403-89 \51\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP \36\............ ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Voltametry \11\ or.. ..................... ..................... ..................... ...................... D3559-96, 03 (C)....
Colorimetric ..................... 3500-Pb D............ 3500-Pb B............ 3500-Pb B-97..........
(Dithizone).
33. Magnesium--Total,\4\ mg/L.... Digestion \4\
followed by:
[[Page 20]]
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. D511-93, 03(B)...... 974.27 \3\, I-3447-
85 \2\
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
DCP or.............. ..................... ..................... ..................... ...................... .................... See footnote \34\
Gravimetric......... ..................... 3500-Mg D............
Ion Chromatography.. ..................... ..................... ..................... ...................... D6919-03............
34. Manganese--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. D858-95, 02 (A or B) 974.27 \3\, I-3454-
\36\. 85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D858-95, 02 (C).....
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP36, or........... ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500--Mn D........... 3500-Mn B............ 3500-Mn B-99.......... .................... 920.203 \3\
(Persulfate), or.
(Periodate)......... ..................... ..................... ..................... ...................... .................... See footnote \23\
35. Mercury--Total \4\, mg/L..... Cold vapor, manual 245.1, Rev. 3.0 3112 B............... ..................... 3112 B-99............. D3223-97, 02........ 977.22 \3\, I-3462-
or. (1994). 85\2\
Automated........... 245.2 (Issued 1974)..
Cold vapor atomic 245.7 Rev. 2.0 (2005)
fluorescence \59\.
spectrometry
(CVAFS).
Purge and Trap CVAFS 1631E \43\...........
36. Molybdenum--Total \4\, mg/L.. Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99............. .................... I-3490-85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. .................... I-3492-96 \47\
[[Page 21]]
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
37. Nickel--Total,\4\ mg/L....... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D1886-90, 94 (98) (A I-3499-85 \2\
\36\. or B).
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D1886-90, 94 (98) I-4503-89 \51\
(C).
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP \36\, or........ ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500-Ni D (17th
(heptoxime). Edition).
38. Nitrate (as N), mg/L......... Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
Ion Selective ..................... 4500-NO3 -D.......... 4500-NO3 -D.......... 4500-NO3 -D-00........
Electrode.
Colorimetric 352.1 \1\............ ..................... ..................... ...................... .................... 973.50 \3\, 419D
(Brucine sulfate), \1,\ \7\, p. 28 \9\
or.
Nitrate-nitrite N
minus Nitrite N
(See parameters 39
and 40)..
39. Nitrate-nitrite (as N), mg/L. Cadmium reduction, ..................... 4500-NO3-E........... 4500-NO3-E........... 4500-NO3-E-00......... D3867-99(B).........
manual or.
Automated, or....... 353.2, Rev. 2.0 4500-NO3-F........... 4500-NO3-F........... 4500-NO3-F-00......... D3867-99(A)......... I-4545-85 \2\
(1993).
Automated hydrazine. ..................... 4500-NO3-H........... 4500-NO3-H........... 4500-NO3-H-00.........
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97............ 993.30 \3\
and 300.1, Rev 1.0
(1997).
[[Page 22]]
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
40. Nitrite (as N), mg/L......... Spectrophotometric: ..................... 4500-NO2-B........... 4500-NO2-B........... 4500-NO2-B-00......... .................... See footnote \25\
Manual or.
Automated ..................... ..................... ..................... ...................... .................... I-4540-85 \2\
(Diazotization).
Automated (*bypass 353.2, Rev. 2.0 4500-NO3-F........... 4500-NO3-F........... 4500-NO3-F-00......... D3867-99(A)......... I-4545-85 \2\
cadmium reduction). (1993).
Manual (*bypass ..................... 4500-NO3-E........... 4500-NO3-E........... 4500-NO3-E-00......... D3867-99(B).........
cadmium reduction).
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev.2 \54\
41. Oil and grease--Total Hexane extractable 1664A \42\........... ..................... 5520 B \38\.......... 5520 B-01 \38\........
recoverable, mg/L. material (HEM): n-
Hexane extraction
and gravimetry.
Silica gel treated 1664A \42\...........
HEM (SGT-HEM):
Silica gel
treatment and
gravimetry..
42. Organic carbon--Total (TOC), Combustion or ..................... 5310 B, C, or D...... 5310 B, C, or D...... 5310 B, C, or D-00.... D2579-93 (A or B)... 973.47,\3\ p. 14
mg/L. oxidation. \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, Rev. 2.0 4500-P F............. 4500-P F............. ...................... .................... 973.56 \3\, I-4601-
(1993). 85 \2\
[[Page 23]]
Manual single ..................... 4500-P E............. 4500-P E............. ...................... D515-88(A).......... 973.55 \3\
reagent.
Manual two reagent.. 365.3 (Issued
1978)\1\.
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
45. Osmium--Total \4\, mg/L...... Digestion \4\
followed by:
AA direct ..................... 3111 D............... ..................... 3111 D-99.............
aspiration, or.
AA furnace.......... 252.2 (Issued 1978)
\1\.
46. Oxygen, dissolved, mg/L...... Winkler (Azide ..................... 4500-O C............. 4500-O C............. 4500-O C-01........... D888-92, 03 (A)..... 973.4 5B \3\, I-1575-
modification), or. 78 \8\
Electrode........... ..................... 4500-O G............. 4500-O G............. 4500-O G-01........... D888-92, 03 (B)..... I-1576-78 \8\
47. Palladium--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ..................... 3111 B............... ..................... 3111 B-99............. .................... p. S27 \10\
aspiration, or.
AA furnace.......... 253.2 \1\ (Issued ..................... ..................... ...................... .................... p. S28 \10\
1978).
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
48. Phenols, mg/L................ Manual distillation 420.1 \1\ (Rev. 1978) ..................... ..................... ...................... .................... See footnote \27\
\26\ Followed by:
Colorimetric (4AAP) 420.1 \1\ (Rev. 1978) ..................... ..................... ...................... .................... See footnote \27\
manual, or.
Automated........... 420.4 Rev. 1.0 (1993)
49. Phosphorus (elemental), mg/L. Gas-liquid ..................... ..................... ..................... ...................... .................... See footnote \28\
chromatography.
50. Phosphorus--Total, mg/L...... Persulfate digestion ..................... 4500-P B.5........... 4500-P B.5........... ...................... .................... 973.55 \3\
followed by: \20\
Manual or........... 365.3 \1\ (Issued 4500-P E............. 4500-P E............. ...................... D515-88(A)..........
1978).
Automated ascorbic 365.1 Rev. 2.0 (1993) 4500-P F............. 4500-P F............. ...................... .................... 973.56 \3\, I-4600-
acid reduction. 85 \2\
Semi-automated block 365.4 \1\ (Issued ..................... ..................... ...................... D515-88(B).......... I-4610-91 \48\
digestor. 1974).
[[Page 24]]
51. Platinum--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99.............
AA furnace.......... 255.2 \1\............
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
52. Potassium--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. .................... 973.53 \3\, I-3630-
85 \2\
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
Flame photometric, ..................... 3500-K D............. 3500-K B............. 3500-K B-97...........
or.
Colorimetric........ ..................... ..................... ..................... ...................... .................... 317 B \17\
Ion Chromatography.. ..................... ..................... ..................... ...................... D6919-03............
53. Residue--Total, mg/L......... Gravimetric, 103- ..................... 2540 B............... 2540 B............... 2540 B-97............. .................... I-3750-85 \2\
105[deg].
54. Residue--filterable, mg/L.... Gravimetric, ..................... 2540 C............... 2540 C............... 2540 C-97............. .................... I-1750-85 \2\
180[deg].
55. Residue--non-filterable Gravimetric, 103-105 ..................... 2540 D............... 2540 D............... 2540 D-97............. .................... I-3765-85 \2\
(TSS), mg/L. [deg]C post washing
of residue.
56. Residue--settleable, mg/L.... Volumetric, (Imhoff ..................... 2540 F............... 2540 F............... 2540 F-97.............
cone), or
gravimetric.
57. Residue--Volatile, mg/L...... Gravimetric, 550 160.4 \1\............ ..................... ..................... ...................... .................... I-3753-85 \2\
[deg]C.
58. Rhodium--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct ..................... 3111 B............... ..................... 3111 B-99.............
aspiration, or.
AA furnace.......... 265.2 \1\............
59. Ruthenium--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ..................... 3111 B............... ..................... 3111 B-99.............
aspiration, or.
[[Page 25]]
AA furnace.......... 267.2 \1\............
60. Selenium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. D3859-98, 03 (B).... I-4668-98 \49\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
AA gaseous hydride.. ..................... 3114 B............... ..................... 3114 B-97............. D3859-98, 03 (A).... I-3667-85 \2\
61. Silica--Dissolved,\37\ mg/L.. 0.45 micron
filtration followed
by:
Colorimetric, Manual ..................... 4500-Si D............ 4500-SiO2 C.......... 4500-SiO2C-97......... D859-94, 00......... I-1700-85 \2\
or.
Automated ..................... ..................... ..................... ...................... .................... I-2700-85 \2\
(Molybdosilicate),
or.
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
62. Silver--Total,4, 31 mg/L..... Digestion 4, 29
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ .................... 974.27 \3\, p. 37
\9\, I-3720-85 \2\
AA furnace.......... ..................... 3113 B............... ..................... 3113 B-99............. .................... I-4724-89 \51\
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
63. Sodium--Total,\4\ mg/L....... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. .................... 973.54 \3\, I-3735-
85 \2\
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
DCP, or............. ..................... ..................... ..................... ...................... .................... See footnote \34\
Flame photometric... ..................... 3500-Na D............ 3500-Na B............ 3500-Na B-97..........
Ion Chromatography.. ..................... ..................... ..................... ...................... D 6919-03...........
[[Page 26]]
64. Specific conductance, Wheatstone bridge... 120.1 \1\ (Rev. 1982) 2510 B............... 2510 B............... 2510 B-97............. D1125-95 (99) (A)... 973.40 \3\, I-2781-
micromhos/cm at 25 [deg]C. 85 \2\
65. Sulfate (as SO4), mg/L....... Automated 375.2, Rev. 2.0
colorimetric. (1993).
Gravimetric......... ..................... 4500-SO4 \2\-C or D.. 4500-SO4 \2\-C or D.. ...................... .................... 925.54 \3\
Turbidimetric....... ..................... ..................... ..................... ...................... D516-90, 02......... 426C \3\0
Ion Chromatography.. 300.0, Rev 2.1 (1993) 4110 B............... 4110 B............... 4110 B-00............. D4327-97, 03........ 993.30 \3\
and 300.1, Rev 1.0
(1997).
CIE/UV.............. ..................... ..................... ..................... ...................... .................... D6508, Rev. 2 \54\
66. Sulfide (as S), mg/L......... Titrimetric ..................... 4500-S \2\-F (19th) 4500-S \2\-F......... 4500-S \2\-F-00....... .................... I-3840-85 \2\
(iodine), or. 4500-S \2\-E (18th).
Colorimetric ..................... 4500-S \2\-D......... 4500-S \2\-D......... 4500-S \2\-D-00.......
(methylene blue).
Ion Selective ..................... 4500-S \2\-G......... 4500-S \2\-G......... 4500-S \2\-G-00....... D4658-03............
Electrode.
67. Sulfite (as SO3), mg/L....... Titrimetric (iodine- ..................... 4500-SO3 \2\-B....... 4500-SO3 \2\-B....... 4500-SO3 \2\-B-00.....
iodate).
68. Surfactants, mg/L............ Colorimetric ..................... 5540 C............... 5540 C............... 5540 C-00............. D2330-88, 02........
(methylene blue).
69. Temperature, [deg]C.......... Thermometric........ ..................... 2550 B............... 2550 B............... 2550 B-00............. .................... See footnote \32\
70. Thallium--Total, \4\ mg/L.... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99.............
AA furnace.......... 279.2 \1\ (Issued
1978).
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99.............
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
[[Page 27]]
71. Tin--Total,\4\ mg/L.......... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B............... ..................... 3111 B-99............. .................... I-3850-78 \8\
AA furnace, or...... ..................... 3113 B............... ..................... 3113 B-99.............
STGFAA.............. 200.9, Rev. 2.2
(1994).
ICP/AES............. 200.7, Rev. 4.4
(1994).
72. Titanium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99.............
AA furnace.......... 283.2 \1\ (Issued
1978).
DCP................. ..................... ..................... ..................... ...................... .................... See footnote \34\
73. Turbidity, NTU \53\.......... Nephelometric....... 180.1, Rev. 2.0 2130 B............... 2130 B............... 2130 B-01............. D1889-94, 00........ I-3860-85 \2\
(1993).
74. Vanadium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct aspiration ..................... 3111 D............... ..................... 3111 D-99.............
AA furnace.......... ..................... ..................... ..................... ...................... D3373-93, 03........
ICP/AES............. 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99............. .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP, or............. ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric (Gallic ..................... 3500-V D............. 3500-V B............. 3500-V B-97...........
Acid).
75. Zinc -Total \4\, mg/L........ Digestion \4\
followed by:
AA direct aspiration ..................... 3111 B or C.......... ..................... 3111 B or C-99........ D1691-95, 02 (A or 974.27 \3\, p. 37
\36\. B). \9\, I-3900-85 \2\
AA furnace.......... 289.2 \1\ (Issued
1978).
ICP/AES \36\........ 200.7, Rev. 4.4 3120 B............... 3120 B............... 3120 B-99 \59\........ .................... I-4471-97 \50\
(1994).
ICP/MS.............. 200.8, Rev. 5.4 ..................... ..................... ...................... D5673-03............ 993.14 \3\
(1994).
DCP,\36\ or......... ..................... ..................... ..................... ...................... D4190-94, 99........ See footnote \34\
Colorimetric ..................... 3500-Zn E............
(Dithizone) or.
(Zincon)............ ..................... 3500-Zn F............ 3500-Zn B............ 3500-Zn B-97.......... .................... See footnote \33\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
[[Page 28]]
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI), EPA-600/4-79-020 (NTIS PB 84-
128677), 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, Sixteenth Edition, 4th Revision, 1998.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize
analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic
absorption determinations a digestion using nitric acid (as specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure
used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a
combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of ``Methods
for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using
the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury
by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up
should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique
or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used
with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the
digestion procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate may be used in place of mercuric sulfate.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual
distillation will be required to resolve any controversies.
\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, April 2, 1975. Available from ANSI, 25 West 43rd st., 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 (CBOD5) must not be confused with the traditional BOD5 test method 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 a 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\ When using a method with block digestion, this treatment is not required.
\21\ Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\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.
[[Page 29]]
\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
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 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\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen
iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After
digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and
adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well.
Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour.
Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ 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\ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. ``Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals'',
CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use n-hexane extraction solvent when determining Oil and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664A). Use of other
extraction solvents (e.g., those in the 18th and 19th editions) is prohibited.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. 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, P.O. 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, P.O. 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, VA 22161.
\43\ USEPA. 2001. 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-02-024). 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, P.O. 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.
[[Page 30]]
\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.
\52\ All EPA methods, excluding EPA Method 300.1, are published in ``Methods for the Determination of Metals in Environmental Samples,'' Supplement I, National Exposure Risk Laboratory-
Cincinnati (NERL-CI), EPA/600/R-94/111, May 1994; and ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' NERL-CI, EPA/600/R-93/100, August, 1993. EPA Method
300.1 is available from http://www.epa.gov/ safewater/methods/ pdfs/met300.pdf.
\53\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.
\54\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,'' available from
Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
\55\ Kelada-01, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,'' EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information
Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. The toll free telephone number is: 800-553-6847. Note: A 450-W UV lamp may be used in this method
instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell
configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.
\56\ QuikChem Method 10-204-00-1-X, ``Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis'' is
available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414-358-4200.
\57\ When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method, approved digestion and/or distillation are
required prior to analysis.
\59\ Method 245.7, Rev. 2.0, ``Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,'' February 2005, EPA-821-R-05-001, available from the U.S. EPA Sample Control Center (operated
by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100, Fax: 703-461-8056.
\60\ The use of EDTA may decrease method sensitivity in some samples. Analysts may omit EDTA provided that all method specified quality control acceptance criteria are met.
\61\ Samples analyzed for available cyanide using Methods OIA-1677 or D6888-04 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the
samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the
time between the addition of the ligand exchange reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples.
Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA method number \2,\ \7\ Other approved methods
--------------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter \1\ Standard Methods
GC GC/MS HPLC [Edition(s)] Standard Methods Online ASTM Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................. 610 625, 1625B........... 610 6440 B [18th, 19th, 20th] ......................... D4657-92 (99)............ See footnote \9\, p. 27
[[Page 31]]
2. Acenaphthylene................ 610 625, 1625B........... 610 6410 B, 6440 B, [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
3. Acrolein...................... 603 624 \4\, 1624B.......
4. Acrylonitrile................. 603 624 \4\, 1624B.......
5. Anthracene.................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
6. Benzene....................... 602 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th,19th], 6200 C
[20th] and 6220 B
[18th,19th].
7. Benzidine..................... ............ 625 \5\, 1625B....... 605 ......................... ......................... ......................... See footnote \3\, p.1
8. Benzo(a)anthracene............ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
9. Benzo(a)pyrene................ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
10. Benzo(b)fluoranthene......... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
11. Benzo(g,h,i) perylene........ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
12. Benzo(k) fluoranthene........ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
13. Benzyl chloride.............. ............ ..................... ............ ......................... ......................... ......................... See footnote \3\, p. 130:
See footnote \6\, p.
S102
14. Benzyl butyl phthalate....... 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
15. Bis(2-chloroethoxy) methane.. 611 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
16. Bis(2-chloroethyl) ether..... 611 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
17. Bis(2-ethylhexyl) phthalate.. 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
18. Bromodichloro-methane........ 601 624, 1624B........... ............ 6200 C [20th] and 6230 B 6200 B and C-97..........
[18th, 19th], 6200 B
[20th] and 6210 B [18th,
19th].
19. Bromoform.................... 601 624, 1624B........... ............ 6200 C [20th] and 6230 B 6200 B and C-97..........
[18th, 19th], 6200 B
[20th] and 6210 B [18th,
19th].
[[Page 32]]
20. Bromomethane................. 601 624, 1624B........... ............ 6200 C [20th] and 6230 B 6200 B and C-97..........
[18th, 19th], 6200 B
[20th] and 6210 B [18th,
19th].
21. 4-Bromophenyl phenyl ether... 611 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
22. Carbon tetrachloride......... 601 624, 1624B........... ............ 6200 C [20th] and 6230 B 6200 C-97................ ......................... See footnote \3\, p. 130
[18th, 19th].
23. 4-Chloro-3-methyl phenol..... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
24. Chlorobenzene................ 601, 602 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97.......... ......................... See footnote \3\, p. 130
[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 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
26. 2-Chloroethylvinyl ether..... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
27. Chloroform................... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97.......... ......................... See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
[[Page 33]]
28. Chloromethane................ 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th] 6200 C
[20th] and 6230 B [18th,
19th].
29. 2-Chloronaph-thalene......... 612 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
30. 2-Chlorophenol............... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B(00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
31. 4-Chlorophenyl phenyl ether.. 611 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
32. Chrysene..................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
33. Dibenzo(a,h)an-thracene...... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
34. Dibromochloro-methane........ 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th] 6200 C
[20th] and 6230 B [18th,
19th].
35. 1,2-Dichloro-benzene......... 601, 602 624, 1625B........... ............ 6200 C [20th] and 6220 B 6200 C-97................ ......................... See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
36. 1,3-Dichloro-benzene......... 601, 602 624, 1625B........... ............ 6200 C [20th] and 6220 B 6200 C-97................ ......................... See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
37. 1,4-Dichloro-benzene......... 601, 602 624, 1625B........... ............ 6200 C [20th] and 6220 B 6200 C-97................ ......................... See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
38. 3,3-Dichloro-benzidine....... ............ 625, 1625B........... 605 6410 B [18th, 19th, 20th] 6410 B-00................
39. Dichlorodifluoro-methane..... 601 ..................... ............ 6200 C [20th] and 6230 B 6200 C-97................
[18th, 19th].
[[Page 34]]
40. 1,1-Dichloroethane........... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
41. 1,2-Dichloroethane........... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
42. 1,1-Dichloroethene........... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
43. trans-1,2-Dichloro-ethene.... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
44. 2,4-Dichlorophenol........... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
45. 1,2-Dichloro-propane......... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
46. cis-1,3-Dichloro-propene..... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
47. trans-1,3-Dichloro-propene... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
[[Page 35]]
48. Diethyl phthalate............ 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
49. 2,4-Dimethylphenol........... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
50. Dimethyl phthalate........... 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
51. Di-n-butyl phthalate......... 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
52. Di-n-octyl phthalate......... 606 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
53. 2,3-Dinitrophenol............ 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... .........................
19th, 20th].
54. 2,4-Dinitrotoluene........... 609 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
55. 2,6-Dinitrotoluene........... 609 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
56. Epichlorohydrin.............. ............ ..................... ............ ......................... ......................... ......................... See footnote \3\, p. 130;
See footnote \6\, p.
S102
57. Ethylbenzene................. 602 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97.......... ......................... .........................
[18th, 19th], 6200 C
[20th] and 6220 B [18th,
19th].
58. Fluoranthene................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
59. Fluorene..................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
60. 1,2,3,4,6,7,8-Heptachloro- ............ 1613B \10\...........
dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro- ............ 1613B \10\...........
dibenzofuran.
62. 1,2,3,4,6,7,8- ............ 1613B \10\...........
Heptachlorodibenzo-p-dioxin.
63. Hexachlorobenzene............ 612 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
64. Hexachloro-butadiene......... 612 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
65. Hexachlorocyclo-pentadiene... 612 625 \5\, 1625B....... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
[[Page 36]]
66. 1,2,3,4,7,8- ............ 1613B \10\...........
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8- ............ 1613B \10\...........
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9- ............ 1613B \10\...........
Hexachlorodibenzofuran.
69. 2,3,4,6,7,8- ............ 1613B \10\...........
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-Hexachlorodibenzo- ............ 1613B \10\...........
p-dioxin.
71. 1,2,3,6,7,8-Hexachlorodibenzo- ............ 1613B \10\...........
p-dioxin.
72. 1,2,3,7,8,9-Hexachlorodibenzo- ............ 1613B \10\...........
p-dioxin 1613B \10\.
73. Hexachloroethane............. 612 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
74. Ideno(1,2,3-cd) pyrene....... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
75. Isophorone................... 609 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
76. Methylene chloride........... 601 624, 1624B........... ............ 6200 C [20th] and 6230 B 6200 C-97................ ......................... See footnote \3\, p. 130
[18th, 19th].
77. 2-Methyl-4,6-dinitrophenol... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
78. Naphthalene.................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ ......................... See footnote \9\, p. 27
19th, 20th].
79. Nitrobenzene................. 609 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
[[Page 37]]
80. 2-Nitrophenol................ 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
81. 4-Nitrophenol................ 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
82. N-Nitrosodimethylamine....... 607 6255, 1625B.......... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
83. N-Nitrosodi-n-propylamine.... 607 6255, 1625B.......... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
84. N-Nitrosodiphenylamine....... 607 6255, 1625B.......... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \9\, p. 27
85. Octachlorodibenzofuran....... ............ 1613B \10\*..........
86. Octachlorodibenzo-p-dioxin... ............ 1613B \10\...........
87. 2,2'-Oxybis(2-chloropropane) 611 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................
[also known as bis(2-
chloroisopropyl) ether].
88. PCB-1016..................... 608 625.................. ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 43;
See footnote \8\
89. PCB-1221..................... 608 625.................. ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 43;
See footnote \8\
90. PCB-1232..................... 608 625.................. ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 43;
See footnote \8\
91. PCB-1242..................... 608 625.................. ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 43;
See footnote \8\
92. PCB-1248..................... 608 625..................
93. PCB-1254..................... 608 625.................. ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 43;
See footnote \8\
94. PCB-1260..................... 608 625.................. ............ 6410 B, 6630 B [18th, 6410 B-00................ ......................... See footnote 3, p. 43;
19th, 20th]. See footnote 8
95. 1,2,3,7,8-Pentachloro- ............ 1613B\10\............
dibenzofuran.
96. 2,3,4,7,8-Pentachloro- ............ 1613B\10\............
dibenzofuran.
97. 1,2,3,7,8,-Pentachlorodibenzo- ............ 1613B\10\............
p-dioxin.
[[Page 38]]
98. Pentachlorophenol............ 604 625, 1625B........... ............ 6410 B, 6630 B [18th, 6410 B-00................ ......................... See footnote \3\, p. 140;
19th, 20th]. See footnote \9\, p. 27
99. Phenanthrene................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
100. Phenol...................... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
101. Pyrene...................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00................ D4657-92 (99)............ See footnote \9\, p. 27
19th, 20th].
102. 2,3,7,8-Tetra- ............ 1613B10..............
chlorodibenzofuran.
103. 2,3,7,8-Tetra-chlorodibenzo- ............ 613, 625 \5a\, 1613B
p-dioxin. \10\.
104. 1,1,2,2-Tetra-chloro ethane. 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97.......... ......................... See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
105. Tetrachloroethene........... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97.......... ......................... See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
106. Toluene..................... 602 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6220 B [18th,
19th].
107. 1,2,4-Trichloro-benzene..... 612 625, 1625B........... ............ 6410 B [18th, 19th, 20th] 6410 B-00................ ......................... See footnote \3\, p. 130;
See footnote \9\, p. 27
108. 1,1,1-Trichloro-ethane...... 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
[[Page 39]]
109. 1,1,2-Trichloro-ethane...... 601 624, 1624B........... 6200 B 6200 B and C-97.......... ......................... See footnote \3\, p. 130.
[20th] and
6210 B
[18th,
19th], 6200
C [20th] and
6230 B
[18th, 19th]
110. Trichloroethene............. 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
111. Trichlorofluoro-methane..... 601 624.................. ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C
[20th] and 6230 B [18th,
19th].
112. 2,4,6-Trichlorophenol....... 604 625, 1625B........... ............ 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00..... ......................... See footnote \9\, p. 27
19th, 20th].
113. Vinyl chloride.............. 601 624, 1624B........... ............ 6200 B [20th] and 6210 B 6200 B and C-97..........
[18th, 19th], 6200 C [20th] and
6230 B [18th, 19th].
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ All parameters are expressed in micrograms per liter ([mu]g/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/L).
\2\ The full text of Methods 601-613, 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, or Method 1625B, are preferred methods for these compounds.
\5a\ 625, screening only.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,'' Supplement to the Fifteenth Edition of Standard Methods for the Examination of
Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 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. The results should be reported, but cannot be used to
demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM 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.
[[Page 40]]
\10\ Analysts may use Fluid Management Systems, Inc. PowerPrep system in place of manual cleanup provided that the analysis meet the requirements of Method 1613B (as specified in Section 9 of
the method) and permitting authorities.
Table ID--List of Approved Test Procedures for Pesticides \1\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA \2,\ Standard Methods 18th,
Parameter Method \7\ 19th, 20th Ed. Standard Methods Online ASTM Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin........................ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96 (2002)......... 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
2. Ametryn....................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\, p
S68
3. Aminocarb..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S16
4. Atraton....................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
5. Atrazine...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
6. Azinphos methyl............... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
7. Barban........................ TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
8. [alpha]-BHC................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
9. [beta]-BHC.................... GC.................. 608 6630 C.................. ........................ D3086-90,............... See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
10. [delta]-BHC.................. GC.................. 608 6630 C.................. ........................ D3086-90,............... See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
11. [gamma]-BHC (Lindane)........ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
....................
12. Captan....................... GC.................. ........... 6630 B.................. ........................ D3086-90,............... See footnote \3\, p. 7
D5812-96(02)............
13. Carbaryl..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94, See footnote \6\,
p. S60
14. Carbo-phenothion............. GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
15. Chlordane.................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
[[Page 41]]
GC/MS............... 625 6410 B.................. 6410 B-00...............
16. Chloro-propham............... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64.
17. 2,4-D........................ GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
18. 4,4[min]-DDD................. GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
19. 4,4[min]-DDE................. GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
20. 4,4[min]-DDT................. GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
21. Demeton-O.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
22. Demeton-S.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
23. Diazinon..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27; See footnote \6\, p. S51
24. Dicamba...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 115
25. Dichlofen-thion.............. GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
26. Dichloran.................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
27. Dicofol...................... GC.................. ........... ........................ ........................ D3086-90,...............
D5812-96(02)............
28. Dieldrin..................... GC.................. 608 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
29. Dioxathion................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
30. Disulfoton................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
31. Diuron....................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
32. Endosulfan I................. GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
33. Endosulfan II................ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
34. Endosulfan Sulfate........... GC.................. 608 6630 C.................. ........................ ........................ See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
[[Page 42]]
35. Endrin....................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
36. Endrin aldehyde.............. GC.................. 608 ........................ ........................ ........................ See footnote \8\
GC/MS............... 625
37. Ethion....................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
38. Fenuron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
39. Fenuron-TCA.................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
40. Heptachlor................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
GC/MS............... 625 6410 B.................. 6410 B-00............... D5812-96(02)............ 27; See footnote \8\
41. Heptachlor epoxide........... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
GC/MS............... 625 6410 B.................. 6410 B-00............... D5812- 96(02)........... 27; See footnote \6\, p. S73; See footnote
\8\
42. Isodrin...................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
43. Linuron...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
44. Malathion.................... GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27; See footnote \6\, p. S51
45. Methiocarb................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S60
46. Methoxy-chlor................ GC.................. ........... 6630 B & C.............. ........................ D3086-90, D5812-96(02).. See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
47. Mexacar-bate................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S60
48. Mirex........................ GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7; See footnote \4\, p.
27
49. Monuron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
50. Monuron-TCA.................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
51. Nuburon...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
52. Parathion methyl............. GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27
[[Page 43]]
53. Parathion ethyl.............. GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27
54. PCNB......................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
55. Perthane..................... GC.................. ........... ........................ ........................ D3086-90, D5812-96(02).. See footnote \4\, p. 27
56. Prometon..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
57. Prometryn.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
58. Propazine.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
59. Propham...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
60. Propoxur..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S60
61. Secbumeton................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
62. Siduron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
63. Simazine..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
64. Strobane..................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
65. Swep......................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
66. 2,4,5-T...................... GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
67. 2,4,5-TP (Silvex)............ GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
68. Terbuthylazine............... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
69. Toxaphene.................... GC.................. 608 6630 B & C.............. ........................ D3086-90, D5812-96(02).. See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
70. Trifluralin.................. GC.................. ........... 6630 B.................. ........................ ........................ See footnote \3\, p. 7; See footnote \9\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, 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 [alpha]-BHC, [gamma]-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).
[[Page 44]]
\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 on-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. The results should be reported, but cannot be used to demonstrate regulatory
compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'', 3M Corporation, Revised 10/28/94.
\9\ USGS Method 0-3106-93 from ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Triazine and Other Nitrogen-containing Compounds by Gas
Chromatography with Nitrogen Phosphorus Detectors'' U.S. Geological Survey Open File Report 94-37.
Table IE--List of Approved Radiologic Test Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
--------------------------------------------------------------------------------------------------------------------------------------
Parameter and units Method Standard Methods 18th,
EPA \1\ 19th, 20th Ed. Standard Methods Online ASTM USGS \2\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter..... Proportional or 900.0................ 7110 B.................... 7110 B-00................. D1943-90, 96.............. pp. 75 and 78 \3\
scintillation
counter.
2. Alpha-Counting error, pCi per Proportional or Appendix B........... 7110 B.................... 7110 B-00................. D1943-90, 96.............. p. 79
liter. scintillation
counter.
3. Beta-Total, pCi per liter...... Proportional counter. 900.0................ 7110 B.................... 7110 B-00................. D1890-90, 96.............. pp. 75 and 78 \3\
4. Beta-Counting error, pCi....... Proportional counter. Appendix B........... 7110 B.................... 7110 B-00................. D1890-90, 96.............. p. 79
5. (a) Radium Total pCi per liter. Proportional counter. 903.0................ 7500-Ra B................. 7500-Ra B-01.............. D2460-90, 97.............. ..........................
(b) Ra, pCi per liter.............
Scintillation counter 903.1................ 7500-Ra C................. 7500-Ra C-01.............. D3454-91, 97.............. p. 81
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.
\2\ Fishman, M. J. and Brown, Eugene, ``Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters,'' U.S. Geological Survey, Open-File Report 76-177 (1976).
\3\ The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, the two results must be added to obtain the
``total.''
[[Page 45]]
Table IF--List of Approved Methods for Pharmaceutical Pollutants
----------------------------------------------------------------------------------------------------------------
Pharmaceuticals pollutants CAS registry No. Analytical method number
----------------------------------------------------------------------------------------------------------------
acetonitrile................... 75-05-8............................ 1666/1671/D3371/D3695.
n-amyl acetate................. 628-63-7........................... 1666/D3695.
n-amyl alcohol................. 71-41-0............................ 1666/D3695
benzene........................ 71-43-2............................ D4763/D3695/502.2/524.2.
n-butyl-acetate................ 123-86-4........................... 1666/D3695.
tert-butyl alcohol............. 75-65-0............................ 1666.
chlorobenzene.................. 108-90-7........................... 502.2/524.2.
chloroform..................... 67-66-3............................ 502.2/524.2/551.
o-dichlorobenzene.............. 95-50-1............................ 1625C/502.2/524.2.
1,2-dichloroethane............. 107-06-2........................... D3695/502.2/524.2.
diethylamine................... 109-89-7........................... 1666/1671.
dimethyl sulfoxide............. 67-68-5............................ 1666/1671.
ethanol........................ 64-17-5............................ 1666/1671/D3695.
ethyl acetate.................. 141-78-6........................... 1666/D3695.
n-heptane...................... 142-82-5........................... 1666/D3695.
n-hexane....................... 110-54-3........................... 1666/D3695.
isobutyraldehyde............... 78-84-2............................ 1666/1667.
isopropanol.................... 67-63-0............................ 1666/D3695.
isopropyl acetate.............. 108-21-4........................... 1666/D3695.
isopropyl ether................ 108-20-3........................... 1666/D3695.
methanol....................... 67-56-1............................ 1666/1671/D3695.
Methyl Cellosolve [Delta]...... 109-86-4........................... 1666/1671
methylene chloride............. 75-09-2............................ 502.2/524.2
methyl formate................. 107-31-3........................... 1666.
4-methyl-2-pentanone (MIBK).... 108-10-1........................... 1624C/1666/D3695/D4763/524.2.
phenol......................... 108-95-2........................... D4763.
n-propanol..................... 71-23-8............................ 1666/1671/D3695.
2-propanone (acetone).......... 67-64-1............................ D3695/D4763/524.2.
tetrahydrofuran................ 109-99-9........................... 1666/524.2.
toluene........................ 108-88-3........................... D3695/D4763/502.2/524.2.
triethlyamine.................. 121-44-8........................... 1666/1671.
xylenes........................ (Note 1)........................... 1624C/1666.
----------------------------------------------------------------------------------------------------------------
Table 1F note:
1. 1624C: m-xylene 108-38-3, o,p-xylene E-14095 (Not a CAS number; this is the number provided in the
Environmental Monitoring Methods Index (EMMI) database.); 1666: m,p-xylene 136777-61-2, o-xylene 95-47-6.
Table IG--Test Methods for Pesticide Active Ingredients
----------------------------------------------------------------------------------------------------------------
EPA Survey Code Pesticide name CAS No. EPA Analytical Method No.(s)
----------------------------------------------------------------------------------------------------------------
8.................. Triadimefon.............. 43121-43-3 507/633/525.1/1656
12................. Dichlorvos............... 62-73-7 1657/507/622/525.1
16................. 2,4-D; 2,4-D Salts and 94-75-7 1658/515.1/615/515.2/555
Esters [2,4-Dichloro-
phenoxyacetic acid].
17................. 2,4-DB; 2,4-DB Salts and 94-82-6 1658/515.1/615/515.2/555
Esters [2,4-
Dichlorophenoxybutyric
acid].
22................. Mevinphos................ 7786-34-7 1657/507/622/525.1
25................. Cyanazine................ 21725-46-2 629/507
26................. Propachlor............... 1918-16-7 1656/508/608.1/525.1
27................. MCPA; MCPA Salts and 94-74-6 1658/615/555
Esters [2-Methyl-4-
chlorophenoxyacetic
acid].
30................. Dichlorprop; Dichlorprop 120-36-5 1658/515.1/615/515.2/555
Salts and Esters [2-(2,4-
Dichlorophenoxy)
propionic acid].
31................. MCPP; MCPP Salts and 93-65-2 1658/615/555
Esters [2-(2-Methyl-4-
chlorophenoxy) propionic
acid].
35................. TCMTB [2- 21564-17-0 637
(Thiocyanomethylthio)
benzo-thiazole].
39................. Pronamide................ 23950-58-5 525.1/507/633.1
41................. Propanil................. 709-98-8 632.1/1656
45................. Metribuzin............... 21087-64-9 507/633/525.1/1656
52................. Acephate................. 30560-19-1 1656/1657
[[Page 46]]
53................. Acifluorfen.............. 50594-66-6 515.1/515.2/555
54................. Alachlor................. 15972-60-8 505/507/645/525.1/1656
55................. Aldicarb................. 116-06-3 531.1
58................. Ametryn.................. 834-12-8 507/619/525.1
60................. Atrazine................. 1912-24-9 505/507/619/525.1/1656
62................. Benomyl.................. 17804-35-2 631
68................. Bromacil; Bromacil Salts 314-40-9 507/633/525.1/1656
and Esters.
69................. Bromoxynil............... 1689-84-5 1625/1661
69................. Bromoxynil octanoate..... 1689-99-2 1656
70................. Butachlor................ 23184-66-9 507/645/525.1/1656
73................. Captafol................. 2425-06-1 1656
75................. Carbaryl [Sevin]......... 63-25-2 531.1/632/553
76................. Carbofuran............... 1563-66-2 531.1/632
80................. Chloroneb................ 2675-77-6 1656/508/608.1/525.1
82................. Chlorothalonil........... 1897-45-6 508/608.2/525.1/1656
84................. Stirofos................. 961-11-5 1657/507/622/525.1
86................. Chlorpyrifos............. 2921-88-2 1657/508/622
90................. Fenvalerate.............. 51630-58-1 1660
103................ Diazinon................. 333-41-5 1657/507/614/622/525.1
107................ Parathion methyl......... 298-00-0 1657/614/622
110................ DCPA [Dimethyl 2,3,5,6- 1861-32-1 508/608.2/525.1/515.1/515.2/1656
tetrachloro-
terephthalate].
112................ Dinoseb.................. 88-85-7 1658/515.1/615/515.2/555
113................ Dioxathion............... 78-34-2 1657/614.1
118................ Nabonate [Disodium 138-93-2 630.1
cyanodithio-
imidocarbonate].
119................ Diuron................... 330-54-1 632/553
123................ Endothall................ 145-73-3 548/548.1
124................ Endrin................... 72-20-8 1656/505/508/608/617/525.1
125................ Ethalfluralin............ 55283-68-6 1656/627 See footnote 1
126................ Ethion................... 563-12-2 1657/614/614.1
127................ Ethoprop................. 13194-48-4 1657/507/622/525.1
132................ Fenarimol................ 60168-88-9 507/633.1/525.1/1656
133................ Fenthion................. 55-38-9 1657/622
138................ Glyphosate 1071-83-6 547
[N(Phosphonomethyl)
glycine].
140................ Heptachlor............... 76-44-8 1656/505/508/608/617/525.1
144................ Isopropalin.............. 33820-53-0 1656/627
148................ Linuron.................. 330-55-2 553/632
150................ Malathion................ 121-75-5 1657/614
154................ Methamidophos............ 10265-92-6 1657
156................ Methomyl................. 16752-77-5 531.1/632
158................ Methoxychlor............. 72-43-5 1656/505/508/608.2/617/525.1
172................ Nabam.................... 142-59-6 630/630.1
173................ Naled.................... 300-76-5 1657/622
175................ Norflurazon.............. 27314-13-2 507/645/525.1/1656
178................ Benfluralin.............. 1861-40-1 11656/1627
182................ Fensulfothion............ 115-90-2 1657/622
183................ Disulfoton............... 298-04-4 1657/507/614/622/525.1
185................ Phosmet.................. 732-11-6 1657/622.1
186................ Azinphos Methyl.......... 86-50-0 1657/614/622
192................ Organo-tin pesticides.... 12379-54-3 Ind-01/200.7/200.9
197................ Bolstar.................. 35400-43-2 1657/622
203................ Parathion................ 56-38-2 1657/614
204................ Pendimethalin............ 40487-42-1 1656
205................ Pentachloronitrobenzene.. 82-68-8 1656/608.1/617
206................ Pentachlorophenol........ 87-86-5 625/1625/515.2/555/515.1/ 525.1
208................ Permethrin............... 52645-53-1 608.2/508/525.1/1656/1660
212................ Phorate.................. 298-02-2 1657/622
218................ Busan 85 [Potassium 128-03-0 630/630.1
dimethyldithiocarbamate].
[[Page 47]]
219................ Busan 40 [Potassium N- 51026-28-9 630/630.1
hydroxymethyl-N-
methyldithiocarbamate].
220................ KN Methyl [Potassium N- 137-41-7 630/630.1
methyl-dithiocarbamate].
223................ Prometon................. 1610-18-0 507/619/525.1
224................ Prometryn................ 7287-19-6 507/619/525.1
226................ Propazine................ 139-40-2 507/619/525.1/1656
230................ Pyrethrin I.............. 121-21-1 1660
232................ Pyrethrin II............. 121-29-9 1660
236................ DEF [S,S,S-Tributyl 78-48-8 1657
phosphorotrithioate].
239................ Simazine................. 122-34-9 505/507/619/525.1/1656
241................ Carbam-S [Sodium 128-04-1 630/630.1
dimethyldithiocarbanate].
243................ Vapam [Sodium 137-42-8 630/630.1
methyldithiocarbamate].
252................ Tebuthiuron.............. 34014-18-1 507/525.1
254................ Terbacil................. 5902-51-2 507/633/525.1/1656
255................ Terbufos................. 13071-79-9 1657/507/614.1/525.1
256................ Terbuthylazine........... 5915-41-3 619/1656
257................ Terbutryn................ 886-50-0 507/619/525.1
259................ Dazomet.................. 533-74-4 630/630.1/1659
262................ Toxaphene................ 8001-35-2 1656/505/508/608/617/525.1
263................ Merphos [Tributyl 150-50-5 1657/507/525.1/622
phosphorotrithioate].
264................ Trifluralin.............. 1582-09-8 1656/508/617/627/525.1
268................ Ziram [Zinc 137-30-4 630/630.1
dimethyldithiocarbamate].
----------------------------------------------------------------------------------------------------------------
\1\ Monitor and report as total Trifluralin.
[[Page 48]]
Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter and units Method \1\ EPA 18th, 19th, 20th Standard methods AOAC, ASTM, USGS Other
Ed. online
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. E. coli, number per 100 MPN \6,8,14\ .................. 9221 B.1/9221 F 9221 B.1-99/9221 F
mL. multiple tube, \11,13\. \11,13\.
Multiple tube/ .................. 9223 B \12\....... 9223 B-97 \12\.... 991.15 \10\....... Colilert[supreg]
multiple well, \12,16\ Colilert-
18[supreg]
\12,15,16\.
MF \2,5,6,7,8\ two 1103.1 \19\....... 9222 B/9222 G 9222 B-97/9222 G D5392-93 \9\......
step, or \18\, 9213 D. \18\.
Single step....... 1603 \20\, 1604 .................. .................. .................. mColiBlue-
\21\. 24[supreg] \17\.
2. Enterococci, number per MPN \6,8\ multiple .................. 9230 B............ 9230 B-93.........
100 mL. tube,
Multiple tube/ .................. .................. .................. D6503-99 \9\...... Enterolert[supreg]
multiple well. \12,22\.
MF \2,5,6,7,8\ two 1106.1 \23\....... 9230 C............ 9230 C-93......... D5259-92 \9\......
step.
Single step, or... 1600 \24\.........
Plate count....... p. 143 \3\........
Protozoa:
3. Cryptosporidium.......... Filtration/IMS/FA. 1622 \25,\1623
\26\.
4. Giardia.................. Filtration/IMS/FA. 1623 \26\.........
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, OH. EPA/600/8-78/017.
\4\ [Reserved]
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has not been used previously to test waters with high turbidity, large 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.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
alternate test procedure (ATP) guidelines.
\9\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. ASTM International. 100 Barr Harbor Drive,
West Conshohocken, PA 19428.
\10\ 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, MD 20877-2417.
\11\ 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.
\12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\13\ After prior enrichment in a presumptive medium for total coliform using 9221B.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 [mu]g/mL of MUG may be used.
\14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg] 2000, and the MPN calculated from the table provided by the manufacturer.
\15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\17\ A description of the mColiBlue24[supreg] test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\18\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
[[Page 49]]
\19\ USEPA. July 2006. 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, DC EPA-821-R-06-010.
\20\ USEPA. July 2006. 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, DC EPA-821-R-06-011.
\21\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. September 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.
\22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\23\ USEPA. July 2006. 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-06-008.
\24\ USEPA. July 2006. 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-06-009.
\25\ 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.
\26\ 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.
[[Page 50]]
(b) The full texts of the methods from the following references
which are cited in Tables IA, IB, IC, ID, IE, IF, IG and IH are
incorporated by reference into this regulation and may be obtained from
the source identified. All costs cited are subject to change and must be
verified from the indicated source. The full texts of all the test
procedures cited are available for inspection at the National Archives
and Records Administration (NARA). For information on the availability
of this material at NARA, call 202-741-6030, or go to: http://
www.archives.gov/ federal--register/code--of--federal--regulations/
ibr--locations.html.
References, Sources, Costs, and Table Citations:
(1) The full texts of Methods 601-613, 624, 625, 1613, 1624, and
1625 are printed in appendix A of this part 136. The full text for
determining the method detection limit when using the test procedures is
given in appendix B of this part 136. The full text of Method 200.7 is
printed in appendix C of this part 136. Cited in: Table IB, Note 5;
Table IC, Note 2; and Table ID, Note 2.
(2) USEPA. 1978. Microbiological Methods for Monitoring the
Environment, Water, and Wastes. Environmental Monitoring and Support
Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. EPA/
600/8-78/017. Available at http://www.epa.gov/clariton/srch.htm or from:
National Technical Information Service, 5285 Port Royal Road,
Springfield, Virginia 22161, Pub. No. PB-290329/A.S. Table IA, Note 3;
Table IH, Note 3.
(3) ``Methods for Chemical Analysis of Water and Wastes,'' U.S.
Environmental Protection Agency, EPA-600/4-79-020, March 1979, or
``Methods for Chemical Analysis of Water and Wastes,'' U.S.
Environmental Protection Agency, EPA-600/4-79-020, Revised March 1983.
Available from: ORD Publications, CERI, U.S. Environmental Protection
Agency, Cincinnati, Ohio 45268, Table IB, Note 1.
(4) ``Methods for Benzidine, Chlorinated Organic Compounds,
Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S.
Environmental Protection Agency, 1978. Available from: ORD Publications,
CERI, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268,
Table IC, Note 3; Table D, Note 3.
(5) ``Prescribed Procedures for Measurement of Radioactivity in
Drinking Water,'' U.S. Environmental Protection Agency, EPA-600/4-80-
032, 1980. Available from: ORD Publications, CERI, U.S. Environmental
Protection Agency, Cincinnati, Ohio 45268, Table IE, Note 1.
(6) American Public Health Association. 1992, 1995, and 1998.
Standard Methods for the Examination of Water and Wastewater. 18th,
19th, and 20th Edition (respectively). Available from: American Public
Health Association, 1015 15th Street, NW., Washington, DC 20005.
Standard Methods Online is available through the Standard Methods Web
site (http://www.standardmethods.org). Tables IA, IB, IC, ID, IE, and
IH.
(7) Ibid, 15th Edition, 1980. Table IB, Note 30; Table ID.
(8) Ibid, 14th Edition, 1975. Table IB, Notes 17 and 27.
(9) ``Selected Analytical Methods Approved and Cited by the United
States Environmental Protection Agency,'' Supplement to the 15th Edition
of Standard Methods for the Examination of Water and Wastewater, 1981.
Available from: American Public Health Association, 1015 Fifteenth
Street NW., Washington, DC 20036. Cost available from publisher. Table
IB, Note 10; Table IC, Note 6; Table ID, Note 6.
(10) ASTM International. Annual Book of ASTM Standards, Water, and
Environmental Technology, Section 11, Volumes 11.01 and 11.02, 1994,
1996, 1999, Volume 11.02, 2000, and individual standards published after
2000. Available from: ASTM International, 100 Barr Harbor Drive, P.O.
Box C700, West Conshohocken, PA 19428-2959, or http://www.astm.org.
Tables IA, IB, IC, ID, IE, and IH.
(11) USGS. 1989. U.S. Geological Survey Techniques of Water-
Resources Investigations, Book 5, Laboratory Analysis, Chapter A4,
Methods for Collection and Analysis of Aquatic Biological and
Microbiological Samples, U.S. Geological Survey, U.S. Department of the
Interior, Reston, Virginia. Available
[[Page 51]]
from USGS Books and Open-File Reports Section, Federal Center, Box
25425, Denver, Colorado 80225. Table IA, Note 5; Table IH.
(12) ``Methods for Determination of Inorganic Substances in Water
and Fluvial Sediments,'' by M.J. Fishman and Linda C. Friedman,
Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5 Chapter A1 (1989). Available from: U.S. Geological
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost:
$108.75 (subject to change). Table IB, Note 2.
(13) ``Methods for Determination of Inorganic Substances in Water
and Fluvial Sediments,'' N.W. Skougstad and others, editors. Techniques
of Water-Resources Investigations of the U.S. Geological Survey, Book 5,
Chapter A1 (1979). Available from: U.S. Geological Survey, Denver
Federal Center, Box 25425, Denver, CO 80225. Cost: $10.00 (subject to
change), Table IB, Note 8.
(14) ``Methods for the Determination of Organic Substances in Water
and Fluvial Sediments,'' Wershaw, R.L., et al, Techniques of Water-
Resources Investigations of the U.S. Geological Survey, Book 5, Chapter
A3 (1987). Available from: U.S. Geological Survey, Denver Federal
Center, Box 25425, Denver, CO 80225. Cost: $0.90 (subject to change).
Table IB, Note 24; Table ID, Note 4.
(15) ``Water Temperature--Influential Factors, Field Measurement and
Data Presentation,'' by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot,
Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 1, Chapter D1, 1975. Available from: U.S. Geological
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $1.60
(subject to change). Table IB, Note 32.
(16) ``Selected Methods of the U.S. Geological Survey of Analysis of
Wastewaters,'' by M.J. Fishman and Eugene Brown; U.S. Geological Survey
Open File Report 76-77 (1976). Available from: U.S. Geological Survey,
Branch of Distribution, 1200 South Eads Street, Arlington, VA 22202.
Cost: $13.50 (subject to change). Table IE, Note 2.
(17) AOAC-International. Official Methods of Analysis of AOAC-
International, 16th Edition, (1995). Available from: AOAC-International,
481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877. Table IB,
See footnote 3.
(18) ``American National Standard on Photographic Processing
Effluents,'' April 2, 1975. Available from: American National Standards
Institute, 1430 Broadway, New York, New York 10018. Table IB, Note 9.
(19) ``An Investigation of Improved Procedures for Measurement of
Mill Effluent and Receiving Water Color,'' NCASI Technical Bulletin No.
253, December 1971. Available from: National Council of the Paper
Industry for Air and Stream Improvements, Inc., 260 Madison Avenue, New
York, NY 10016. Cost available from publisher. Table IB, Note 18.
(20) Ammonia, Automated Electrode Method, Industrial Method Number
379-75WE, dated February 19, 1976. Technicon Auto Analyzer II. Method
and price available from Technicon Industrial Systems, Tarrytown, New
York 10591. Table IB, Note 7.
(21) Chemical Oxygen Demand, Method 8000, Hach Handbook of Water
Analysis, 1979. Method price available from Hach Chemical Company, P.O.
Box 389, Loveland, Colorado 80537. Table IB, Note 14.
(22) OIC Chemical Oxygen Demand Method, 1978. Method and price
available from Oceanography International Corporation, 512 West Loop,
P.O. Box 2980, College Station, Texas 77840. Table IB, Note 13.
(23) ORION Research Instruction Manual, Residual Chlorine Electrode
Model 97-70, 1977. Method and price available from ORION Research
Incorporation, 840 Memorial Drive, Cambridge, Massachusetts 02138. Table
IB, Note 16.
(24) Bicinchoninate Method for Copper. Method 8506, Hach Handbook of
Water Analysis, 1979, Method and price available from Hach Chemical
Company, P.O. Box 300, Loveland, Colorado 80537. Table IB, Note 19.
(25) Hydrogen Ion (pH) Automated Electrode Method, Industrial Method
Number 378-75WA. October 1976. Bran & Luebbe (Technicon) Auto Analyzer
II. Method and price available from Bran & Luebbe Analyzing
Technologies, Inc. Elmsford, N.Y. 10523. Table IB, Note 21.
(26) 1,10-Phenanthroline Method using FerroVer Iron Reagent for
Water,
[[Page 52]]
Hach Method 8008, 1980. Method and price available from Hach Chemical
Company, P.O. Box 389 Loveland, Colorado 80537. Table IB, Note 22.
(27) Periodate Oxidation Method for Manganese, Method 8034, Hach
Handbook for Water Analysis, 1979. Method and price available from Hach
Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note
23.
(28) Nitrogen, Nitrite--Low Range, Diazotization Method for Water
and Wastewater, Hach Method 8507, 1979. Method and price available from
Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB,
Note 25.
(29) Zincon Method for Zinc, Method 8009. Hach Handbook for Water
Analysis, 1979. Method and price available from Hach Chemical Company,
P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 33.
(30) ``Direct Determination of Elemental Phosphorus by Gas-Liquid
Chromatography,'' by R.F. Addison and R.G. Ackman, Journal of
Chromatography, Volume 47, No. 3, pp. 421-426, 1970. Available in most
public libraries. Back volumes of the Journal of Chromatography are
available from Elsevier/North-Holland, Inc., Journal Information Centre,
52 Vanderbilt Avenue, New York, NY 10164. Cost available from publisher.
Table IB, Note 28.
(31) ``Direct Current Plasma (DCP) Optical Emission Spectrometric
Method for Trace Elemental Analysis of Water and Wastes'', Method AES
0029, 1986-Revised 1991, Fison Instruments, Inc., 32 Commerce Center,
Cherry Hill Drive, Danvers, MA 01923. Table B, Note 34.
(32) ``Closed Vessel Microwave Digestion of Wastewater Samples for
Determination of Metals, CEM Corporation, P.O. Box 200, Matthews, North
Carolina 28106-0200, April 16, 1992. Available from the CEM Corporation.
Table IB, Note 36.
(33) ``Organochlorine Pesticides and PCBs in Wastewater Using Empore
\TM\ Disk'' Test Method 3M 0222, Revised 10/28/94. 3M Corporation, 3M
Center Building 220-9E-10, St. Paul, MN 55144-1000. Method available
from 3M Corporation. Table IC, Note 8 and Table ID, Note 8.
(34) USEPA. 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. Available at http://www.epa.gov/
epahome/index/ sources.htm or from National Technical Information
Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No.
PB2002-108488. Table IA, Note 25.
(35) ``Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion,
Steam Distillation, Titrimetric Detection)'', revised 12/22/94.
Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd.,
Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 39.
(36) ``Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion,
Steam Distillation, Colorimetric Detection)'', revised 12/22/94.
Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd.,
Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 40.
(37) ``Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion,
Automated FIA Gas Diffusion)'', revised 12/22/94. Available from
Perstorp Analytical Corporation, 9445 SW Ridder Rd., Suite 310, P.O. Box
648, Wilsonville, OK 97070. Table IB, Note 41.
(38) USEPA. October 2002. Short-Term Methods for Measuring 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. Available at http://
www.epa.gov/ epahome/ index/ sources.htm or from National Technical
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161,
Pub. No. PB2002-108489. Table IA, Note 26.
(39) USEPA. October 2002. Short-Term Methods for Measuring 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. Available at
http://www.epa.gov/ epahome/ index/ sources.htm or from National
Technical Information Service, 5285 Port Royal Road, Springfield,
Virginia 22161, Pub. No. PB2002-108490. Table IA, Note 27.
[[Page 53]]
(40) EPA Methods 1666, 1667, and 1671 listed in the table above are
published in the compendium titled Analytical Methods for the
Determination of Pollutants in Pharmaceutical Manufacturing Industry
Wastewaters (EPA 821-B-98-016). EPA Methods 502.2 and 524.2 have been
incorporated by reference into 40 CFR 141.24 and are in Methods for the
Determination of Organic Compounds in Drinking Water, EPA-600/4-88-039,
December 1988, Revised, July 1991, and Methods for the Determination of
Organic Compounds in Drinking Water-Supplement II, EPA-600/R-92-129,
August 1992, respectively. These EPA test method compendia are available
from the National Technical Information Service, NTIS PB91-231480 and
PB92-207703, U.S. Department of Commerce, 5285 Port Royal Road,
Springfield, Virginia 22161. The toll-free number is 800-553-6847. ASTM
test methods D3371, D3695, and D4763 are available from the American
Society for Testing and Materials, 100 Barr Harbor Drive, West
Conshohocken, PA 19428-2959.
(41) 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). Available from: National Technical
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.
Publication No. PB2002-108220. Cost: $25.50 (subject to change).
(42) [Reserved]
(43) Method OIA-1677, Available Cyanide by Flow Injection, Ligand
Exchange, and Amperometry. August 1999. ALPKEM, OI Analytical, Box 648,
Wilsonville, Oregon 97070 (EPA-821-R-99-013). Available from: National
Technical Information Service, 5285 Port Royal Road, Springfield,
Virginia 22161. Publication No. PB99-132011. Cost: $22.50. Table IB,
Note 44.
(44) ``Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory Determination of Ammonium Plus Organic Nitrogen
by a Kjeldahl Digestion Method and an Automated Photometric Finish that
Includes Digest Cleanup by Gas Diffusion'', Open File Report (OFR) 00-
170. Available from: U.S. Geological Survey, Denver Federal Center, Box
25425, Denver, CO 80225. Table IB, Note 45.
(45) ``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. Available from: U.S. Geological Survey, Denver Federal Center,
Box 25425, Denver, CO 80225. Table IB, Note 46.
(46) ``Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory--Determination of Molybdenum in Water by
Graphite Furnace Atomic Absorption Spectrophotometry'', Open File Report
(OFR) 97-198. Available from: U.S. Geological Survey, Denver Federal
Center, Box 25425, Denver, CO 80225. Table IB, Note 47.
(47) ``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. Available from: U.S.
Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225.
Table IB, Note 48.
(48) ``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. Table IB, Note 49.
(49) ``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. Available from: U.S. Geological Survey, Denver Federal
Center, Box 25425, Denver, CO 80225. Table IB, Note 50.
(50) ``Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory--Determination of Triazine and Other Nitrogen-
containing Compounds by Gas Chromatography with Nitrogen Phosphorus
Detectors'' U.S.Geological Survey Open File Report 94-37. Available
from: U.S.
[[Page 54]]
Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225.
Table ID, Note 9.
(51) ``Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory--Determination of Inorganic and Organic
Constituents in Water and Fluvial Sediments'', Open File Report (OFR)
93-125. Available from: U.S. Geological Survey, Denver Federal Center,
Box 25425, Denver, CO 80225. Table IB, Note 51; Table IC, Note 9.
(52) IDEXX Laboratories, Inc. 2002. Description of Colilert[reg],
Colilert-18[reg], Quanti-Tray[reg], Quanti-Tray[reg]/2000,
Enterolert[reg] methods are available from IDEXX Laboratories, Inc., One
Idexx Drive, Westbrook, Maine 04092. Table IA, Notes 17 and 23; Table
IH, Notes 16 and 22.
(53) Hach Company, Inc. Revision 2, 1999. Description of m-
ColiBlue24[reg] Method, Total Coliforms and E. coli, is available from
Hach Company, 100 Dayton Ave, Ames IA 50010. Table IA, Note 18; Table
IH, Note 17.
(54) USEPA. July 2006. 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 DC EPA-621-R-06-010. Available at http://www.epa.gov/
waterscience/methods/. Table IH, Note 19.
(55) USEPA. July 2006. 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-621-R-06-008. Available at http://www.epa.gov/waterscience/
methods/. Table IH, Note 23
(56) USEPA. July 2006. 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 DC EPA-821-R-06-011. Available at
http://www.epa.gov/waterscience/methods/. Table IH, Note 19; Table IH,
Note 20.
(57) Brenner et al. 1993. New Medium for the Simultaneous Detection
of Total Coliforms and Escherichia coli in Water. Appl. Environ.
Microbiol. 59:3534-3544. Available from the American Society for
Microbiology, 1752 N Street NW., Washington DC 20036. Table IH, Note 21.
(58) USEPA. September 2002. Method 1604: Total Coliforms and
Escherichia coli (E. coli) in Water by Membrane Filtration Using a
Simultaneous Detection Technique (MI Medium). U.S. Environmental
Protection Agency, Office of Water, Washington DC EPA-821-R-02-024.
Available at http://www.epa.gov/waterscience/methods/. Table IH, Note
20.
(59) USEPA. July 2006. 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-06-009. Available at http://www.epa.gov/waterscience/
methods/. Table IA, Note 24; Table IH, Note 24.
(60) USEPA. April 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. Available at http://www.epa.gov/
waterscience/methods/. Table IH, Note 25.
(61) USEPA. April 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. Available at http://
www.epa.gov/waterscience/methods/. Table IH, Note 26.
(62) AOAC. 1995. Official Methods of Analysis of AOAC International,
16th Edition, Volume I, Chapter 17. AOAC International, 481 North
Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-2417. Table
IA, Note 11; Table IH.
(63) Waters Corporation. Method D6508, Rev. 2, ``Test Method for
Determination of Dissolved Inorganic Anions in Aqueous Matrices Using
Capillary Ion Electrophoresis and Chromate Electrolyte,'' available from
Waters Corp, 34 Maple Street, Milford, MA 01757, Telephone: 508/482-
2131, Fax: 508/482-3625, Table IB, See footnote 54.
(64) Kelada-01, ``Kelada Automated Test Methods for Total Cyanide,
Acid Dissociable Cyanide, and Thiocyanate,'' EPA 821-B-01-009 Revision
1.2, August 2001 is available from
[[Page 55]]
National Technical Information Service (NTIS), 5285 Port Royal Road,
Springfield, VA 22161 [Order Number PB 2001-108275]. Telephone: 800-553-
6847. Table IB, See footnote 55.
(65) QuikChem Method 10-204-00-1-X, ``Digestion and Distillation of
Total Cyanide in Drinking and Wastewaters using MICRO DIST and
Determination of Cyanide by Flow Injection Analysis'' Revision 2.2,
March 2005 is available from Lachat Instruments 6645 W. Mill Road,
Milwaukee, WI 53218, Telephone: 414-358-4200. Table IB, See footnote 56.
(66) ``Methods for the Determination of Metals in Environmental
Samples,'' Supplement I, National Exposure Risk Laboratory-Cincinnati
(NERL-CI), EPA/600/R-94/111, May 1994; and ``Methods for the
Determination of Inorganic Substances in Environmental Samples,'' NERL-
CI, EPA/600/R-93/100, August, 1993 are available from National Technical
Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161.
Telephone: 800-553-6847. Table IB.
(67) ``Determination of Inorganic Ions in Drinking Water by Ion
Chromatography,'' Rev. 1.0, 1997 is available from from http://
www.epa.gov/safetwater/methods/met300.pdf. Table IB.
(68) Table IG Methods are available in ``Methods For The
Determination of Nonconventional Pesticides In Municipal and Industrial
Wastewater, Volume I,'' EPA 821-R-93-010A, August 1993 Revision I, and
``Methods For The Determination of Nonconventional Pesticides In
Municipal and Industrial Wastewater, Volume II,'' EPA 821-R-93-010B
(August 1993) are available from National Technical Information Service
(NTIS), 5285 Port Royal Road, Springfield, VA 22161. Telephone: 800-553-
6847.
(69) Method 245.7, Rev. 2.0, ``Mercury in Water by Cold Vapor Atomic
Fluorescence Spectrometry,'' February 2005, EPA-821-R-05-001, available
from the U.S. EPA Sample Control Center (operated by CSC), 6101
Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-8056. Table
IB, See footnote 59.
(70) USEPA. July 2006. Method 1680: Fecal Coliforms in Sewage Sludge
(Biosolids) by Multiple-Tube Fermentation using Lauryl Tryptose Broth
(LTB) and EC Medium. U.S. Environmental Protection Agency, Office of
Water, Washington DC. EPA 821-R-06-012. Available at http://www.epa.gov/
waterscience/methods/.
(71) USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage Sludge
(Biosolids) by Multiple-Tube Fermentation using A-1 Medium. U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA
821-R-06-013. Available at http://www.epa.gov/waterscience/methods/.
(72) USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge
(Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium.
U.S. Environmental Protection Agency, Office of Water, Washington DC.
EPA 821-R-06-014. Available at http://www.epa.gov/waterscience/methods/.
(c) Under certain circumstances, the Regional Administrator or the
Director in the Region or State where the discharge will occur may
determine for a particular discharge that additional parameters or
pollutants must be reported. Under such circumstances, additional test
procedures for analysis of pollutants may be specified by the Regional
Administrator, or the Director upon recommendation of the Alternate Test
Procedure Program Coordinator, Washington, DC.
(d) Under certain circumstances, the Administrator may approve
additional alternate test procedures for nationwide use, upon
recommendation by the Alternate Test Procedure Program Coordinator,
Washington, DC.
(e) Sample preservation procedures, container materials, and maximum
allowable holding times for parameters are cited in Tables IA, IB, IC,
ID, IE, IF, IG and IH are prescribed in Table II. Information in the
table takes precedence over information in specific methods or
elsewhere. Any person may apply for a variance from the prescribed
preservation techniques, container materials, and maximum holding times
applicable to samples taken from a specific discharge. Applications for
variances may be made by letters to the Regional Administrator in the
Region in which the discharge will occur. Sufficient data should be
provided to assure such variance does not adversely affect the integrity
of the sample. Such data will be forwarded by
[[Page 56]]
the Regional Administrator, to the Alternate Test Procedure Program
Coordinator, Washington, DC, for technical review and recommendations
for action on the variance application. Upon receipt of the
recommendations from the Alternate Test Procedure Program Coordinator,
the Regional Administrator may grant a variance applicable to the
specific discharge to the applicant. A decision to approve or deny a
variance will be made within 90 days of receipt of the application by
the Regional Administrator.
Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
Maximum holding time
Parameter No./name Container \1\ Preservation \2,3\ \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacterial Tests:
1-5. Coliform, total, fecal, and PA, G.................. Cool, <10 [deg]C, 6 hours.\22,23\
E. coli. 0.0008% Na2S2O3 \5\.
6. Fecal streptococci............ PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
7. Enterococci................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
8. Salmonella.................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
Table IA--Aquatic Toxicity Tests:
9-11. Toxicity, acute and chronic P, FP, G............... Cool, <=6 [deg]C \16\.. 36 hours.
Table lB--Inorganic Tests:
1. Acidity....................... P, FP, G............... Cool, <=6 [deg]C \18\.. 14 days.
2. Alkalinity.................... P, FP, G............... Cool, <=6 [deg]C \18\.. 14 days.
4. Ammonia....................... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
9. Biochemical oxygen demand..... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
10. Boron........................ P, FP, or Quartz....... HNO3 to pH<2........... 6 months.
11. Bromide...................... P, FP, G............... None required.......... 28 days.
14. Biochemical oxygen demand, P, FP G................ Cool, <=6 [deg]C \18\.. 48 hours.
carbonaceous.
15. Chemical oxygen demand....... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
16. Chloride..................... P, FP, G............... None required.......... 28 days.
17. Chlorine, total residual..... P, G................... None required.......... Analyze within 15
minutes.
21. Color........................ P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
23-24. Cyanide, total or P, FP, G............... Cool, <=6 [deg]C \18\, 14 days.
available (or CATC). NaOH to pH12 \6\, reducing
agent \5\.
25. Fluoride..................... P...................... None required.......... 28 days.
27. Hardness..................... P, FP, G............... HNO3 or H2SO4 to pH<2.. 6 months.
28. Hydrogen ion (pH)............ P, FP, G............... None required.......... Analyze within 15
minutes.
31, 43. Kjeldahl and organic N... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
Table IB--Metals: \7\
18. Chromium VI.................. P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
pH = 9.3-9.7 \20\.
35. Mercury (CVAA)............... P, FP, G............... HNO3 to pH<2........... 28 days.
35. Mercury (CVAFS).............. FP, G; and FP-lined cap 5 mL/L 12N HCl or 5 mL/ 90 days.\17\
\17\. L BrCl \17\.
3, 5-8, 12, 13, 19, 20, 22, 26, P, FP, G............... HNO3 to pH<2, or at 6 months.
29, 30, 32-34, 36, 37, 45, 47, least 24 hours prior
51, 52, 58-60, 62, 63, 70-72, to analysis \19\.
74, 75.
Metals, except boron, chromium
VI, and mercury.
38. Nitrate...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
39. Nitrate-nitrite.............. P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
40. Nitrite...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
41. Oil and grease............... G...................... Cool to <=6 [deg]C 28 days.
\18\, HCl or H2SO4 to
pH<2.
42. Organic Carbon............... P, FP, G............... Cool to <=6 [deg]C 28 days.
\18\, HCl, H2SO4, or
H3PO4 to pH<2.
44. Orthophosphate............... P, FP, G............... Cool, <=6 [deg]C \18\.. Filter within 15
minutes; Analyze
within 48 hours.
46. Oxygen, Dissolved Probe...... G, Bottle and top...... None required.......... Analyze within 15
minutes.
47. Winkler...................... G, Bottle and top...... Fix on site and store 8 hours.
in dark.
48. Phenols...................... G...................... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
49. Phosphorous (elemental)...... G...................... Cool, <=6 [deg]C \18\.. 48 hours.
50. Phosphorous, total........... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
53. Residue, total............... P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
54. Residue, Filterable.......... P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
55. Residue, Nonfilterable (TSS). P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
56. Residue, Settleable.......... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
[[Page 57]]
57. Residue, Volatile............ P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
61. Silica....................... P or Quartz............ Cool, <=6 [deg]C \18\.. 28 days.
64. Specific conductance......... P, FP, G............... Cool, <=6 [deg]C \18\.. 28 days.
65. Sulfate...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 28 days.
66. Sulfide...................... P, FP, G............... Cool, <=6 [deg]C \18\, 7 days.
add zinc acetate plus
sodium hydroxide to
pH9.
67. Sulfite...................... P, FP, G............... None required.......... Analyze within 15
minutes.
68. Surfactants.................. P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
69. Temperature.................. P, FP, G............... None required.......... Analyze.
73. Turbidity.................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
Table lC--Organic Tests \8\
13, 18-20, 22, 24-28, 34-37, 39- G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.
43, 45-47, 56, 76, 104, 105, 108- 0.008% Na2S2O3 \5\.
111, 113. Purgeable Halocarbons.
6, 57, 106. Purgeable aromatic G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.\9\
hydrocarbons. 0.008% Na2S2O3 \5\,
HCl to pH 2 \9\.
3, 4. Acrolein and acrylonitrile. G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.\10\
0.008% Na2S2O3 \5\, pH
to 4-5 \10\.
23, 30, 44, 49, 53, 77, 80, 81, G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
98, 100, 112. Phenols \11\. 0.008% Na2S2O3 \5\. extraction, 40 days
after extraction.
7, 38. Benzidines \11,\ \12\..... G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
0.008% Na2S2O3 \5\. extraction.\13\
14, 17, 48, 50-52. Phthalate G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 7 days until
esters \11\. extraction, 40 days
after extraction.
82-84. Nitrosamines \11,\ \14\... G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
store in dark, 0.008% extraction, 40 days
Na2S2O3 \5\. after extraction.
88-94. PCBs \11\................. G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 1 year until
extraction, 1 year
after extraction.
54, 55, 75, 79. Nitroaromatics G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
and isophorone \11\. store in dark, 0.008% extraction, 40 days
Na2S2O3 \5\. after extraction.
1, 2, 5, 8-12, 32, 33, 58, 59, G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
74, 78, 99, 101. Polynuclear store in dark, 0.008% extraction, 40 days
aromatic hydrocarbons \11\. Na2S2O3 \5\. after extraction.
15, 16, 21, 31, 87. Haloethers G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
\11\. 0.008% Na2S2O3 \5\. extraction, 40 days
after extraction.
29, 35-37, 63-65, 107. G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 7 days until
Chlorinated hydrocarbons \11\. extraction, 40 days
after extraction.
60-62, 66-72, 85, 86, 95-97, 102,
103. CDDs/CDFs \11\.
Aqueous Samples: Field and Lab G...................... Cool, <=6 [deg]C \18\, 1 year.
Preservation. 0.008% Na2S2O3 \5\,
pH<9.
Solids and Mixed-Phase Samples: G...................... Cool, <=6 [deg]C \18\.. 7 days.
Field Preservation.
Tissue Samples: Field G...................... Cool, <=6 [deg]C \18\.. 24 hours.
Preservation.
Solids, Mixed-Phase, and Tissue G...................... Freeze, <=-10 [deg]C... 1 year.
Samples: Lab Preservation.
Table lD--Pesticides Tests:
1-70. Pesticides \11\............ G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
pH 5-9 \15\. extraction, 40 days
after extraction.
Table IE--Radiological Tests:
1-5. Alpha, beta, and radium..... P, FP, G............... HNO3 to pH<2........... 6 months.
Table IH--Bacterial Tests:
1. E. coli....................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
2. Enterococci................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
Table IH--Protozoan Tests:
8. Cryptosporidium............... LDPE; field filtration. 0-8 [deg]C............. 96 hours.\21\
[[Page 58]]
9. Giardia....................... LDPE; field filtration. 0-8 [deg]C............. 96 hours.\21\
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE; Teflon[supreg]), or other
fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is made of
a sterlizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density polyethylene.
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
minutes of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour
composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at <=6
[deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <=6 [deg]C,
unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
is completed. Add the preservative to the sample container prior to sample collection when the preservative
will not compromise the integrity of a grab sample, a composite sample, or an aliquot split from a composite
sample; otherwise, preserve the grab sample, composite sample, or aliquot split from a composite sample within
15 minutes of collection. If a composite measurement is required but a composite sample would compromise
sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over
the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations
averaged. Alternatively, grab samples may be collected in the field and composited in the laboratory if the
compositing procedure produces results equivalent to results produced by arithmetic averaging of the results
of analysis of individual grab samples. For examples of laboratory compositing procedures, see EPA Method
1664A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and (v) (volatile organics).
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such
material for transportation is responsible for ensuring such compliance. For the preservation 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 the start of analysis and still be considered valid (e.g., samples analyzed for
fecal coliforms may be held up to 6 hours prior to commencing analysis). 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). For a grab sample, the holding time begins at the time of
collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), the holding time begins at the time of
the end of collection of the composite sample. For a set of grab samples composited in the field or
laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
sample stability. See Sec. 136.3(e) for details. The date and time of collection of an individual grab
sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and
that are all collected on the same calendar date, the date of collection is the date on which the samples are
collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
automatically on a given date, the date of collection is the date on which the sample is collected. For a
composite sample collected automatically, and that is collected across two calendar dates, the date of
collection is the dates of the two days; e.g., November 14-15.
\5\ Add a reducing agent only if an oxidant (e.g., chlorine) is present. Reducing agents shown to be effective
are sodium thiosulfate (Na2S2O3), ascorbic acid, sodium arsenite (NaAsO2), or sodium borohydride (NaBH4).
However, some of these agents have been shown to produce a positive or negative cyanide bias, depending on
other substances in the sample and the analytical method used. Therefore, do not add an excess of reducing
agent. Methods recommending ascorbic acid (e.g., EPA Method 335.4) specify adding ascorbic acid crystals, 0.1-
0.6 g, until a drop of sample produces no color on potassium iodide (KI) starch paper, then adding 0.06 g (60
mg) for each liter of sample volume. If NaBH4 or NaAsO2 is used, 25 mg/L NaBH4 or 100 mg/L NaAsO2 will reduce
more than 50 mg/L of chlorine (see method ``Kelada-01'' and/or Standard Method 4500-CN- for more information).
After adding reducing agent, test the sample using KI paper, a test strip (e.g. for chlorine, SenSafeTM Total
Chlorine Water Check 480010) moistened with acetate buffer solution (see Standard Method 4500-Cl.C.3e), or a
chlorine/oxidant test method (e.g., EPA Method 330.4 or 330.5), to make sure all oxidant is removed. If
oxidant remains, add more reducing agent. Whatever agent is used, it should be tested to assure that cyanide
results are not affected adversely.
\6\ Sample collection and preservation: Collect a volume of sample appropriate to the analytical method in a
bottle of the material specified. If the sample can be analyzed within 48 hours and sulfide is not present,
adjust the pH to 12 with sodium hydroxide solution (e.g., 5% w/v), refrigerate as specified, and
analyze within 48 hours. Otherwise, to extend the holding time to 14 days and mitigate interferences, treat
the sample immediately using any or all of the following techniques, as necessary, followed by adjustment of
the sample pH to 12 and refrigeration as specified. There may be interferences that are not
mitigated by approved procedures. Any procedure for removal or suppression of an interference may be employed,
provided the laboratory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g.,
ferric ferrocyanide) or a strong cyanide complex (e.g., cobalt cyanide) are more accurately measured if the
laboratory holds the sample at room temperature and pH 12 for a minimum of 4 hours prior to
analysis, and performs UV digestion or dissolution under alkaline (pH=12) conditions, if necessary.
(1) Sulfur: To remove elemental sulfur (S8), filter the sample immediately. If the filtration time will exceed
15 minutes, use a larger filter or a method that requires a smaller sample volume (e.g., EPA Method 335.4 or
Lachat Method 01). Adjust the pH of the filtrate to > 12 with NaOH, refrigerate the filter and filtrate, and
ship or transport to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for
a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with
the initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and
analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g or mg), and divide by the original sample volume to obtain the cyanide concentration.
[[Page 59]]
(2) Sulfide: If the sample contains sulfide as determined by lead acetate paper, or if sulfide is known or
suspected to be present, immediately conduct one of the volatilization treatments or the precipitation
treatment as follows: Volatilization--Headspace expelling. In a fume hood or well-ventilated area, transfer
0.75 liter of sample to a 4.4 L collapsible container (e.g., CubitainerTM). Acidify with concentrated
hydrochloric acid to pH < 2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel
the headspace into the fume hood or open area by collapsing the container without expelling the sample. Refill
the headspace by expanding the container. Repeat expelling a total of five headspace volumes. Adjust the pH to
> 12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must
maintain the air to sample volume ratio. A larger volume of air will result in too great a loss of cyanide (>
10%). Dynamic stripping: In a fume hood or well-ventilated area, transfer 0.75 liter of sample to a container
of the material specified and acidify with concentrated hydrochloric acid to pH < 2. Using a calibrated air
sampling pump or flowmeter, purge the acidified sample into the fume hood or open area through a fritted glass
aerator at a flow rate of 2.25 L/min for 4 minutes. Adjust the pH to > 12, refrigerate, and ship or transport
to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio.
A larger volume of air will result in too great a loss of cyanide (> 10%). Precipitation: If the sample
contains particulate matter that would be removed by filtration, filter the sample prior to treatment to
assure that cyanide associated with the particulate matter is included in the measurement. Ship or transport
the filter to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a
minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the
initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and
analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g or mg), and divide by the original sample volume to obtain the cyanide concentration. For removal of
sulfide by precipitation, raise the pH of the sample to > 12 with NaOH solution, then add approximately 1 mg
of powdered cadmium chloride for each mL of sample. For example, add approximately 500 mg to a 500-mL sample.
Cap and shake the container to mix. Allow the precipitate to settle and test the sample with lead acetate
paper. If necessary, add cadmium chloride but avoid adding an excess. Finally, filter through 0.45 micron
filter. Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the
laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract
and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to
approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because
the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the sample
with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids
procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from
the sample and the solids separately, add the amounts determined (in [mu]g or mg), and divide by the original
sample volume to obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM D6888), it
may be necessary to increase the ligand-exchange reagent to offset any excess of cadmium chloride.
(3) Sulfite, thiosulfate, or thiocyanate: If sulfite, thiosulfate, or thiocyanate is known or suspected to be
present, use UV digestion with a glass coil (Method Kelada-01) or ligand exchange (Method OIA-1677) to
preclude cyanide loss or positive interference.
(4) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be
present, treat the sample with 20 mL of 3.5% ethylenediamine solution per liter of sample.
(5) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the
distillation flask, a reduction in the pH of the absorber solution, and incomplete cyanide spike recovery.
When significant carbonate is present, adjust the pH to =12 using calcium hydroxide instead of
sodium hydroxide. Allow the precipitate to settle and decant or filter the sample prior to analysis (also see
Standard Method 4500-CN.B.3.d).
(6) Chlorine, hypochlorite, or other oxidant: Treat a sample known or suspected to contain chlorine,
hypochlorite, or other oxidant as directed in footnote 5.
\7\ For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives.
For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40
CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of
collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will
be compromised during collection of a composite sample collected automatically over time (e.g., by interchange
of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote
2) in place of a composite sample collected automatically.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
\10\ The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
adjustment must be analyzed within 3 days of sampling.
\11\ When the extractable analytes of concern fall within a single chemical category, the specified preservative
and maximum holding times should be observed for optimum safeguard of sample integrity (i.e., use all
necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two
or more chemical categories, the sample may be preserved by cooling to <=6 [deg]C, reducing residual chlorine
with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this
manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this
optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
\12\ If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0
0.2 to prevent rearrangement to benzidine.
\13\ Extracts may be stored up to 30 days at < 0 [deg]C.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
of sampling.
\15\ The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still
present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, it
is necessary to immediately measure the temperature of the samples and confirm that the preservation
temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding
temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance.
The request for a variance should include supportive data which show that the toxicity of the effluent samples
is not reduced because of the increased holding temperature.
\17\ Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be
collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48
hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory
within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample
should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669.
If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be
filtered in a designated clean area in the field within the time period necessary to maintain sample
integrity. A sample that has been collected for determination of total or dissolved trace level mercury must
be analyzed within 90 days of sample collection.
\18\ Aqueous samples must be preserved at <=6 [deg]C, and should not be frozen unless data demonstrating that
sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
regulatory authority. Also, for purposes of NPDES monitoring, the specification of ``<= [deg]C'' is used in
place of the ``4 [deg]C'' and ``< 4 [deg]C'' sample temperature requirements listed in some methods. It is not
necessary to measure the sample temperature to three significant figures (\1/100\th of 1 degree); rather,
three significant figures are specified so that rounding down to 6 [deg]C may not be used to meet the <=6
[deg]C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less
than 15 minutes).
[[Page 60]]
\19\ An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at
least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must
be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment
samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and
holding time requirements in the approved metals methods.
\20\ To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6.
The allowance in this footnote supersedes preservation and holding time requirements in the approved
hexavalent chromium methods, unless this supersession would compromise the measurement, in which case
requirements in the method must be followed.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
\22\ Samples analysis should begin immediately, preferably within 2 hours of collection. The maximum transport
time to the laboratory is 6 hours, and samples should be processed within 2 hours of receipt at the
laboratory.
\23\ For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for
the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B
aerobically digested, and Class B anaerobically digested.
[38 FR 28758, Oct. 16, 1973]
Editorial Note: For Federal Register citations affecting Sec.
136.3, see the List of CFR Sections Affected, which appears in the
Finding Aids section of the printed volume and on GPO Access.