[Code of Federal Regulations]
[Title 40, Volume 22]
[Revised as of July 1, 2006]
From the U.S. Government Printing Office via GPO Access
[CITE: 40CFR136.3]
[Page 5-39]
TITLE 40--PROTECTION OF ENVIRONMENT
CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)
PART 136_GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF
POLLUTANTS--Table of Contents
Sec. 136.3 Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are
listed together with test procedure descriptions and references in
Tables IA, IB, IC, ID, IE, and IF. The full text of the referenced test
procedures are incorporated by reference into Tables IA, IB, IC, ID, IE,
and IF. The 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
[[Page 6]]
this section. Information regarding obtaining these documents can be
obtained from the EPA Office of Water Statistics and Analytical Support
Branch at 202-566-1000. Documents may be inspected at EPA's Water
Docket, EPA West, 1301 Constitution Avenue, NW., Room B135, Washington,
DC (Telephone: 202-566-2426); or at the 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 anys change in these test procedures will be
published in the Federal Register. The discharge parameter values for
which reports are required must be determined by one of the standard
analytical test procedures incorporated by reference and described in
Tables IA, IB, IC, IE, and IF, or by any alternate test procedure which
has been approved by the Administrator under the provisions of paragraph
(d) of this section and Sec. Sec. 136.4 and 136.5. Under certain
circumstances (paragraph (b) or (c) of this section or 40 CFR 401.13)
other test procedures may be more advantageous when such other test
procedures have been previously approved by the Regional Administrator
of the Region in which the discharge will occur, and providing the
Director of the State in which such discharge will occur does not object
to the use of such alternate test procedure.
[[Page 7]]
Table IA--List of Approved Biological Methods
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods 18th,
Parameter and units Method \1\ EPA 19th, 20th Ed. ASTM AOAC USGS Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number Most Probable Number p. 132 9221C E \4\
per 100 mL. (MPN), 5 tube 3 \3\
dilution, or
Membrane filter (MF) p. 124 9222D \4\ ........... ........... B-0050-85
\2\, single step. \3\ \5\
2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 9221C E \4\
presence of chlorine, number dilution, or \3\
per 100 mL.
MF, single step \6\. p. 124 9222D \4\
\3\
3. Coliform (total), number MPN, 5 tube, 3 p. 114 9221B \4\
per 100 mL. dilution, or \3\
MF \2\, single step p. 108 9222B \4\ ........... ........... B-0025-85
or two step. \3\ \5\
4. Coliform (total), in MPN, 5 tube, 3 p. 114 9221B \4\
presence of chlorine, number dilution, or \3\
per 100 mL.
MF \2\ with p. 111 9222(B+B.5c) \4\
enrichment. \3\
5. E. coli, number per 100 mL MPN \7,9,15\, ......... 9221B.1/9221F \4,12,14\
\28\. multiple tube,.
multiple tube/ ......... 9223B \4,13\ ........... 991.15 \11\ ........... Colilert [reg]
multiple well, \13,17\
Colilert-18 [reg]
\13,16,17\
MF \2,6,7,8,9\ two ......... 9222B/9222G \4,19\
step, or
1103.1 9213D \4\ D5392-93
\20\ \10\
single step......... 1603 \21\
1604 \22\
......... ....................... ........... ........... ........... mColiBue 24 \18\
6. Fecal streptococci, number MPN, 5 tube, 3 p. 139 9230B \4\, 9230C \4\
per 100 mL. dilution, \3\
MF \2\, or.......... p. 136 ....................... ........... B-0055-85
\3\ \5\
Plate count......... p. 143
\4\
7. Enterococci, number per MPN \7,9\ multiple ......... 9230B \4\
100 mL. tube.
multiple tube/ ......... ....................... D6503-99 ........... ........... Enterolert
multiple well. \10\ [reg]\13,23\
MF \2,6,7,8,9\ two 1106.1 9230C \4\ D5259-92
step. \24\ \10\
single step, or..... 1600 \25\
Plate count......... p. 143
\3\
Protozoa:
8. Cryptosporidium \28\...... Filtration/IMS/FA... 1622 \26\
1623 \27\
9. Giardia \28\.............. Filtration/IMS/FA... 1623 \27\
Aquatic Toxicity:
10. Toxicity, acute, fresh Ceriodaphnia dubia 2002.0
water organisms, LC50, acute. \29\
percent effluent.
[[Page 8]]
Daphnia puplex and 2021.0
Daphnia magna acute. \29\
Fathead Minnow, 2000.0
Pimephales \29\
promelas, and
Bannerfin shiner,
Cyprinella leedsi,
acute.
Rainbow Trout, 2019.0
Oncorhynchus \29\
mykiss, and brook
trout, Salvelinus
fontinalis, acute.
11. Toxicity, acute, Mysid, Mysidopsis 2007.0
estuarine and marine bahia, acute. \29\
organisms of the Atlantic
Ocean and Gulf of Mexico,
LC50, percent effluent.
Sheepshead Minnow, 2004.0
Cyprinodon \29\
variegatus, acute.
Silverside, Menidia 2006.0
beryllina, Menidia \29\
menidia, and
Menidia peninsulae,
acute.
12. Toxicity, chronic, fresh Fathead minnow, 1000.0
water organisms, NOEC or Pimephales \30\
IC25, percent effluent. promelas, larval
survival and growth.
Fathead minnow, 1001.0
Pimephales \30\
promelas, embryo-
larval survival and
teratogenicity.
Daphnia, 1002.0
Ceriodaphnia dubia, \30\
survival and
reproduction.
Green alga, 1003.0
Selenastrum \30\
capricornutum,
growth.
13. Toxicity, chronic, Sheepshead minnow, 1004.0
estuarine and marine Cyprinodon \31\
organisms of the Atlantic variegatus, larval
Ocean and Gulf of Mexico, survival and growth.
NOEC or IC25, percent
effluent.
Sheepshead minnow, 1005.0
Cyprinodon \31\
variegatus, embryo-
larval survival and
teratogenicity.
Inland silverside, 1006.0
Menidia beryllina, \31\
larval survival and
growth.
Mysid, Mysidopsis 1007.0
bahia, survival, \31\
growth, and
fecundity.
[[Page 9]]
Sea urchin, Arbacia 1008.0
punctulata, \31\
fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Notes to Table IA:
\1\ The method must be specified when results are reported.
\2\ A 0.45 [micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, Ohio. EPA/600/8-78/017.
\4\ APHA. 1998, 1995, 1992. Standard Methods for the Examination of Water and Wastewater. American Public Health Association. 20th, 19th, and 18th
Editions. Amer. Publ. Hlth. Assoc., Washington, D.C.
\5\ USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and
Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of Interior, Reston, Virginia.
\6\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
\7\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
\8\ When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncoliform bacteria, or samples that
may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
comparability of results.
\9\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
alternate test procedure (ATP) guidelines.
\10\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. American Society for Testing and
Materials. 100 Barr Harbor Drive, West Conshohocken, PA 19428.
\11\ AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists
International. 481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-2417.
\12\ The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate
and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent
of all total coliform-positive tubes on a seasonal basis.
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth
or acidity within 48 h 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media
supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\15\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert [reg] may be enumerated with
the multiple-well procedures, Quanti-Tray [reg] or Quanti-Tray [reg] 2000, and the MPN calculated from the table provided by the manufacturer.
\16\ Colilert-18 [reg] is an optimized formulation of the Colilert [reg] 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 [reg] test and is recommended for marine water samples.
\17\ Descriptions of the Colilert [reg], Colilert-18 [reg], Quanti-Tray [reg], and Quanti-Tray [reg]/2000 may be obtained from IDEXX Laboratories, Inc.,
One IDEXX Drive, Westbrook, Maine 04092.
\18\ A description of the mColiBlue24'' test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\19\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
\20\ USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC).
U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-020.
\21\ USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (
modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-023.
\22\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604:
Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA 821-R-02-024.
\23\ A description of the Enterolert [reg] test may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.
\24\ USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental
Protection Agency, Office of Water, Washington DC. EPA-821-R-02-021.
\25\ USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). U.S.
Environmental Protection Agency, Office of Water, Washington, DC. EPA-821-R-02-022.
\26\ Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821-
R-01-026.
\27\ Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA-821-R-01-025.
\28\ Recommended for enumeration of target organism in ambient water only.
[[Page 10]]
\29\ USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition.
U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/012.
\30\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth
Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/013.
\31\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms.
Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/014.
Table IB--List of Approved Inorganic Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
Parameter, units and method --------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA \1,35\ Standard Methods [Edition(s)] ASTM USGS \2\ Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:
Electrometric endpoint or 305.1......................... 2310 B(4a) [18th, 19th, 20th]. D1067-92...................... I-1020-85
phenolphthalein endpoint.
I-2030-85
2. Alkalinity, as CaCO3, mg/L:
Electrometric of Colorimetric 310.1......................... 2320 B [18th, 19th, 20th]..... D1067-92...................... I-1030-85..................... 973.43 \3\
titration to pH 4.5, manual .............................. .............................. .............................. ..............................
or automatic. 310.2......................... .............................. I-2030-85.....................
3. Aluminium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 202.1......................... 3111 D [18th, 19th]........... .............................. I-3051-85
AA furnace................... 202.2......................... 3113 B [18th, 19th]...........
Inductively Coupled Plasma/ 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
Atomic Emission Spectrometry
(ICP/AES) \36\.
Direct Current Plasma (DCP) .............................. .............................. D4190-94...................... .............................. Note 34.
\36\.
Colorimetric (Eriochrome .............................. 3500-Al B [20th] and 3500-Al D
cyanine R). [18th, 19th].
4. Ammonia (as N), mg/L:
Manual, distillation (at pH 350.2......................... 4500-NH3 B [18th, 19th, 20th]. .............................. .............................. 973.49 \3\
9.5) \6\ followed by.
Nesslerization............... 350.2......................... 4500-NH3 C [18th]............. D1426-98(A)................... I-3520-85..................... 973.49 \3\
Titration.................... 350.2......................... 4500-NH3 C [19th, 20th] and
4500-NH3 E [18th].
Electrode.................... 350.3......................... 4500-NH3 D or E [19th, 20th] D1426-98(B)...................
and 4500-NH3 F or G [18th].
Automated phenate, or........ 350.1......................... 4500-NH3 G [19th, 20th] and .............................. I-4523-85 .............................
4500-NH3 H [18th].
Automated electrode.......... .............................. .............................. .............................. .............................. Note 7.
5. Antimony-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 204.1......................... 3111 B [18th, 19th]
AA furnace................... 204.2......................... 3113 B [18th, 19th]...........
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
6. Arsenic-Total \4\ mg/L:
[[Page 11]]
Digestion \4\ followed by.... 206.5.........................
AA gaseous hydride........... 206.3......................... 3114 B 4.d [18th, 19th]....... D2972-97(B) I-3062-85
AA furnace................... 206.2......................... 3113 B [18th, 19th]........... D2972-97(C) I-4063-98 \49\ .............................
ICP/AES \36\ or.............. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
Colorimetric (SDDC).......... 206.4......................... 3500-As B [20th] and 3500-As C D2972-97(A) I-3060-85
[18th, 19th].
7. Barium-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \14\.... 208.1......................... 3111 D [18th, 19th]........... .............................. I-3084-85
AA furnace................... 208.2......................... 3113 B [18th, 19th]........... D4382-95
ICP/AES \14\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
DCP \14\..................... .............................. .............................. .............................. .............................. Note 34.
8. Beryllium-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 210.1......................... 3111 D [18th, 19th]........... D3645-93(88)(A)............... I-3095-85
AA furnace................... 210.2......................... 3113 B [18th, 19th]........... D3645-93(88)(B)
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
DCP, or...................... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (aluminon....... .............................. 3500-Be D [18th, 19th]........
9. Biochemical oxygen demand
(BOD5), mg/L:
Dissolved Oxygen Depletion... 405.1......................... 5210 B [18th, 19th, 20th]..... .............................. I-1578-78 \8\................. 973.44, \3\ p. 17 \9\
10. Boron \37\-Total, mg/L:
Colorimetric (curcumin)...... 212.3......................... 4500-B B [18th, 19th, 20th]... .............................. I-3112-85
ICP/AES, or.................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\ .............................
DCP.......................... .............................. .............................. D4190-94...................... .............................. Note 34.
11. Bromide, mg/L:
Titrimetric.................. 320.1......................... .............................. D1246-95(C)................... I-1125-85..................... p. S44 \10\
12. Cadmium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 213.1......................... 3111 B or C [18th, 19th]...... D3557-95 (A or B)............. I-3135-85 or I-3136-85........ 974.27, \3\ p. 37 \9\
AA furnace................... 213.2......................... 3113 B [18th, 19th]........... D3557-95(D)................... I-4138-89 \51\
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-1472-85 or I-4471-97 \50\
DCP \36\..................... .............................. .............................. D4190-94...................... .............................. Note 34.
Voltametry \11\, or.......... .............................. .............................. D3557-95(C)...................
Colorimetric (Dithizone)..... .............................. 3500-Cd D [18th, 19th]........
13. Calcium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 215.1......................... 3111 B [18th, 19th]........... D511-93(B).................... I-3152-85
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP, or...................... .............................. .............................. .............................. .............................. Note 34.
Titrimetric (EDTA)........... 215.2......................... 3500-Ca B [20th] and 3500-Ca D D511-93(A)....................
[18th, 19th].
14. Carbonaceous biochemical
oxygen demand (CBOD 3), mg/L
\12\:
Dissolved Oxygen Depletion .............................. 5210 B [18th, 19th, 20th].....
with nitrification inhibitor.
15. Chemical oxygen demand (COD), 410.1......................... 5220 C [18th, 19th, 20th]..... D1252-95(A)................... I-3560-85..................... 973.46, \3\ p. 17 \9\
mg/L; Titrimetric
or........................... 410.2......................... .............................. .............................. I-3562-85
[[Page 12]]
410.3.........................
Spectrophotometric, manual or 410.4......................... 5220 D [18th, 19th, 20th]..... D1252-95(B)................... I-3561-85..................... Notes 13, 14.
automatic.
16. Chloride, mg/L:
Titrimetric (silver nitrate) .............................. 4500-Cl-B [18th, 19th, 20th].. D512-89(B).................... I-1183-85
or.
(Mercuric nitrate)........... 325.3......................... 4500-Cl-C [18th, 19th, 20th].. D512-89(A).................... I-1184-85..................... 973.51 \3\
Colorimetric, manual or...... .............................. .............................. .............................. I-1187-85
Automated (Ferricyanide)..... 325.1 or 325.2................ 4500-Cl-E [18th, 19th, 20th].. .............................. I-2187-85
17. Chlorine--Total residual, mg/
L; Titrimetric:
Amperometric direct.......... 330.1......................... 4500-Cl D [18th, 19th, 20th].. D1253-86(92)..................
Iodometric direct............ 330.3......................... 4500-Cl B [18th, 19th, 20th]..
Back titration ether end- 330.2......................... 4500-Cl C [18th, 19th, 20th]..
point \15\ or.
DPD-FAS...................... 330.4......................... 4500-Cl F [18th, 19th, 20th]..
Spectrophotometric, DPD...... 330.5......................... 4500-Cl G [18th, 19th, 20th]..
Or Electrode................. .............................. .............................. .............................. .............................. Note 16.
18. Chromium VI dissolved, mg/L;
0.45 micron filtration followed
by:
AA chelation-extraction or... 218.4......................... 3111 C [18th, 19th]........... .............................. I-1232-85
Colorimetric .............................. 3500-Cr B [20th] and 3500-Cr D D1687-92(A)................... I-1230-85
(Diphenylcarbazide). [18th, 19th].
19. Chromium-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 218.1......................... 3111 B [18th, 19th]........... D1687-92(B)................... I-3236-85..................... 974.27 \3\
AA chelation-extraction...... 218.3......................... 3111 C [18th, 19th]...........
AA furnace................... 218.2......................... 3113 B [18th, 19th]........... D1687-92(C)................... I-3233-93 \46\................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
DCP \36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric .............................. 3500-Cr B [20th] and 3500-Cr D
(Diphenylcarbazide). [18th, 19th].
20. Cobalt--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 219.1......................... 3111 B or C [18th, 19th]...... D3558-94(A or B).............. I-3239-85..................... p. 37 \9\
AA furnace................... 219.2......................... 3113 B [18th, 19th]........... D3558-94(C)................... I-4243-89 \51\................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
[[Page 13]]
DCP.......................... .............................. .............................. D4190-94...................... .............................. Note 34.
21. Color platinum cobalt units
or dominant wavelength, hue,
luminance purity:
Colorimetric (ADMI), or......
(Platinum cobalt), or........ 110.1......................... 2120 E [18th, 19th, 20th]..... .............................. .............................. Note 18.
Spectrophotometric........... 110.2......................... 2120 B [18th, 19th, 20th]..... .............................. I-1250-85
110.3......................... 2120 C [18th, 19th, 20th].....
22. Copper--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 220.1......................... 3111 B or C [18th, 19th]...... D1688-95(A or B).............. I-3270-85 or I-3271-85........ 974.27 \3\ p. 37 \9\
AA furnace................... 220.2......................... 3113 B [18th, 19th]........... D1688-95(C)................... I-4274-89 \51\
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I--4471--97 \50\
DCP \36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Neocuproine) or .............................. 3500-Cu B [20th] and 3500-Cu D
[18th, 19th].
(Bicinchoninate)............. .............................. 3500-Cu C [20th] and 3500-As B .............................. .............................. Note 19.
[18th, 19th].
23. Cyanide--Total, mg/L:
Manual distillation with .............................. 4500-CN C [18th, 19th, 20th].. D2036-98(A)
MgCl2 followed by..
Titrimetric, or.............. .............................. 4500-CN D [18th, 19th, 20th].. .............................. .............................. p. 22 \9\
Spectrophotometric, manual or 335.2 \31\.................... 4500-CN E [18th, 19th, 20th].. D2036-98(A)................... I-3300-85
Automated \20\............... 335.3 \31\.................... .............................. .............................. I-4302-85
24. Available Cyanide, mg/L:
Manual distillation with 335.1......................... 4500-CN G [18th, 19th, 20th].. D2036-98(B)
MgCl2 followed by
titrimetric or
Spectrophotometric.
Flow injection and ligand .............................. .............................. .............................. .............................. OIA-1677 \44\
exchange, followed by
amperometry.
25. Fluoride--Total, mg/L:
Manual distillation \6\ .............................. 4500-F B [18th, 19th, 20th]...
followed by.
Electrode, manual or......... 340.2......................... 4500-F C [18th, 19th, 20th]... D1179-93(B)
Automated.................... .............................. .............................. .............................. I-4327-85
Colorimetric (SPADNS)........ 340.1......................... 4500-F D [18th, 19th, 20th]... D1179-93(A)
Or Automated complexone...... 340.3......................... 4500-F E [18th, 19th, 20th]...
26. Gold--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 231.1......................... 3111 B [18th, 19th]...........
AA furnace, or............... 231.2
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
27. Hardness--Total, as CaCO3, mg/
L:
Automated colorimetric,...... 130.1
[[Page 14]]
Titrimetric (EDTA), or Ca 130.2......................... 2340 B or C [18th, 19th, 20th] D1126-86(92).................. I-1338-85..................... 973.52B \3\
plus Mg as their carbonates,
by inductively coupled
plasma or AA direct
aspiration (See Parameters
13 and 33).
28. Hydrogen ion (pH), pH units:
Electrometric measurement, or 150.1......................... 4500-H+ B [18th, 19th, 20th].. D1293-84 (90)(A or B)......... I-1586-85..................... 973.41 \3\
Automated electrode.......... .............................. .............................. .............................. I-2587-85..................... Note 21.
29. Iridium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration or...... 235.1......................... 3111 B [18th, 19th]...........
AA furnace................... 235.2
30. Iron--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 236.1......................... 3111 B or C [18th, 19th]...... D1068-96(A or B).............. I-3381-85..................... 974.27 \3\
AA furnace................... 236.2......................... 3113 B [18th, 19th]........... D1068-96(C)
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP \36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Phenanthroline) .............................. 3500-Fe B [20th] and 3500-Fe D D1068-96(D)................... .............................. Note 22.
[18th, 19th].
31. Kjeldahl Nitrogen--Total, (as
N), mg/L:
Digestion and distillation 351.3......................... 4500-Norg B or C and 4500-NH3 D3590-89(A)
followed by. B [18th, 19th, 20th].
Titration.................... 351.3......................... .............................. D3590-89(A)................... .............................. 973.48 \3\
Nesslerization............... 351.3......................... 4500-NH3 C [18th]............. D3590-89(A)...................
Electrode.................... 351.3......................... 4500-NH3 C [19th, 20th] and
4500-NH3 E [18th].
Automated phenate colorimetric... 351.1......................... .............................. .............................. I-4551-78 \8\
Semi-automated block digestor 351.2......................... .............................. D3590-89(B)................... I-4515-91 \45\................
colorimetric.
Manual or block digestor 351.4......................... .............................. D3590-89(A)
potentiometric.
Block digester, followed by Auto .............................. .............................. .............................. .............................. Note 39.
distillation and Titration, or.
Nesslerization, or............... .............................. .............................. .............................. .............................. Note 40.
Flow injection gas diffusion..... .............................. .............................. .............................. .............................. Note 41.
32. Lead--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 239.1......................... 3111 B or C [18th, 19th]...... D3559-96(A or B).............. I-3399-85..................... 974.27 \3\
[[Page 15]]
AA furnace................... 239.2......................... 3113 B [18th, 19th]........... D3559-96(D)................... I-4403-89 \51\
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP \36\..................... .............................. .............................. D4190-94...................... .............................. Note 34.
Voltametry \11\ or........... D3559-96(C)...................
Colorimetric (Dithizone)..... 3500-Pb B [ 20th] and 3500-Pb
D [18th, 19th].
33. Magnesium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 242.1......................... 3111 B [18th, 19th]........... D511-93(B).................... I-3447-85..................... 974.27 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP or....................... .............................. .............................. .............................. .............................. Note 34.
Gravimetric.................. .............................. 3500-Mg D [18th, 19th]........
34. Manganese-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 243.1......................... 3111 B [18th, 19th]........... D858-95(A or B)............... I-3454-85..................... 974.27 \3\
AA furnace................... 243.2......................... 3113 B [18th, 19th]........... D858-95(C)
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP \36\, or................. .............................. .............................. D4190-94...................... .............................. Note 34
Colorimetric (Persulfate), or .............................. 3500-Mn B [20th] and 3500-Mn D .............................. .............................. 920.203 \3\
[18th, 19th].
(Periodate).................. .............................. .............................. .............................. .............................. Note 23.
35. Mercury--Total, \4\ mg/L:
Cold vapor, manual or........ 245.1......................... 3112 B [18th, 19th]........... D3223-91...................... I-3462-85..................... 977.22 \3\
Automated.................... 245.2
Oxidation, purge and trap, 1631E \43\
and cold vapor atomic
fluorescence spectrometry
(ng/L).
36. Molybdenum--Total \4\, mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 246.1......................... 3111 D [18th, 19th]........... .............................. I-3490-85
AA furnace................... 246.2......................... 3113 B [18th, 19th]........... .............................. I-3492-96 \47\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
37. Nickel--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 249.1......................... 3111 B or C [18th, 19th]...... D1886-90(A or B).............. I-3499-85.....................
AA furnace................... 249.2......................... 3113 B [18th, 19th]........... D1886-90(C)................... I-4503-89 \51\................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP \36\, or................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (heptoxime)..... .............................. 3500-Ni D [17th]..............
38. Nitrate (as N), mg/L:
Colorimetric (Brucine 352.1......................... .............................. .............................. .............................. 973.50, \3\ 419D, \17\ p. 28
sulfate), or Nitrate-nitrite \9\
N minus Nitrite N (See
parameters 39 and 40).
39. Nitrate-nitrite (as N),
mg/L:
Cadmium reduction, Manual or. 353.3......................... 4500-NO3-E [18th, 19th, 20th]. D3867-99(B)...................
[[Page 16]]
Automated, or................ 353.2......................... 4500-NO3-F [18th, 19th, 20th]. D3867-99(A)................... I-4545-85.....................
Automated hydrazine.......... 353.1......................... 4500-NO3-H [18th, 19th, 20th].
40. Nitrite (as N), mg/L;
Spectrophotometric:
Manual or.................... 354.1......................... 4500-NO2-B [18th, 19th, 20th]. .............................. .............................. Note 25.
Automated (Diazotization).... .............................. .............................. .............................. I-4540-85.....................
41. Oil and grease--Total
recoverable, mg/L:
Gravimetric (extraction)..... 413.1......................... 5520B [18th, 19th, 20th] \38\.
Oil and grease and non-polar 1664A \42\.................... 5520B [18th, 19th, 20th] \38\.
material, mg/L: Hexane
extractable material (HEM):
n-Hexane extraction and
gravimetry.
Silica gel treated HEM (SGT- 1664A \42\....................
HEM): Silica gel treatment
and gravimetry.
42. Organic carbon--Total (TOC),
mg/L:
Combustion or oxidation...... 415.1......................... 5310 B, C, or D [18th, 19th, D2579-93 (A or B)............. .............................. 973.47, \3\ p. 14 \24\
20th].
43. Organic nitrogen (as N), mg/
L:
Total Kjeldahl N (Parameter
31) minus ammonia N
(Parameter 4).
44. Orthophosphate (as P), mg/L;
Ascorbic acid method:
Automated, or................ 365.1......................... 4500-P F [18th, 19th, 20th]... .............................. I-4601-85..................... 973.56 \3\
Manual single reagent........ 365.2......................... 4500-P E [18th, 19th, 20th]... D515-88(A).................... .............................. 973.55 \3\
Manual two reagent........... 365.3.........................
45. Osmium--Total \4\, mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 252.1......................... 3111 D [18th, 19th]...........
AA furnace................... 252.2.........................
46. Oxygen, dissolved, mg/L:
Winkler (Azide modification), 360.2......................... 4500-O C [18th, 19th, 20th]... D888-92(A).................... I-1575-78 \8\................. 973.45B \3\
or.
Electrode.................... 360.1......................... 4500-O G [18th, 19th, 20th]... D888-92(B).................... I-1576-78 \8\.................
[[Page 17]]
47. Palladium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 253.1......................... 3111 B [18th, 19th]........... .............................. .............................. p. S27 \10\
AA furnace................... 253.2......................... .............................. .............................. .............................. p. S28 \10\
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
48. Phenols, mg/L:
Manual distillation \26\..... 420.1......................... .............................. .............................. .............................. Note 27.
Followed by:.................
Colorimetric (4AAP) 420.1......................... .............................. .............................. .............................. Note 27.
manual, or.
Automated \19\........... 420.2.........................
49. Phosphorus (elemental), mg/L:
Gas-liquid chromatography.... .............................. .............................. .............................. .............................. Note 28.
50. Phosphorus--Total, mg/L:
Persulfate digestion followed 365.2......................... 4500-P B, 5 [18th, 19th, 20th] .............................. .............................. 973.55 \3\
by.
Manual or.................... 365.2 or 365.3................ 4500-P E [18th, 19th, 20th]... D515-88(A)
Automated ascorbic acid 365.1......................... 4500-P F [18th, 19th, 20th]... .............................. I-4600-85..................... 973.56 \3\
reduction.
Semi-automated block digestor 365.4......................... .............................. D515-88(B).................... I-4610-91 \48\................
51. Platinum--Total, \4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration......... 255.1......................... 3111 B [18th, 19th]...........
AA furnace................... 255.2.........................
DCP.......................... .............................. .............................. .............................. .............................. Note 34
52. Potassium--Total, \4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration......... 258.1......................... 3111 B [18th, 19th]........... .............................. I-3630-85..................... 973.53 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
Flame photometric, or........ .............................. 3500-K B [20th] and 3500-K D
[18th, 19th].
Colorimetric................. .............................. .............................. .............................. .............................. 317 B \17\
53. Residue--Total, mg/L:
Gravimetric, 103-105[deg].... 160.3......................... 2540 B [18th, 19th, 20th]..... .............................. I-3750-85.....................
54. Residue--filterable, mg/L:
Gravimetric, 180[deg]........ 160.1......................... 2540 C [18th, 19th, 20th]..... .............................. I-1750-85.....................
55. Residue--nonfilterable (TSS),
mg/L:
Gravimetric, 103-105[deg] 160.2......................... 2540 D [18th, 19th, 20th]..... .............................. I-3765-85.....................
post washing of residue.
56. Residue--settleable, mg/L:
Volumetric, (Imhoff cone), or 160.5......................... 2540 F [18th, 19th, 20th].....
gravimetric.
57. Residue--Volatile, mg/L:
Gravimetric, 550[deg]........ 160.4......................... .............................. .............................. I-3753-85.....................
58. Rhodium-Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 265.1......................... 3111 B [18th, 19th]...........
[[Page 18]]
AA furnace................... 265.2.........................
59. Ruthenium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or..... 267.1......................... 3111 B [18th, 19th]...........
AA furnace................... 267.2.........................
60. Selenium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA furnace................... 270.2......................... 3113 B [18th, 19th]........... D3859-98(B)................... I-4668-98 \49\................
ICP/AES, \36\ or............. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
AA gaseous hydride........... .............................. 3114 B [18th, 19th]........... D3859-98(A)................... I-3667-85.....................
61. Silica \37\--Dissolved, mg/L;
0.45 micron filtration followed
by:
Colorimetric, Manual or...... 370.1......................... 4500-SiO2 C [20th] and 4500-Si D859-94....................... I-1700-85.....................
D [18th, 19th].
Automated (Molybdosilicate), .............................. .............................. .............................. I-2700-85.....................
or.
ICP.......................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
62. Silver--Total, \4\ mg/L:
Digestion \4,29\ followed by:
AA direct aspiration......... 272.1......................... 3111 B or C [18th, 19th]...... .............................. I-3720-85..................... 974.27, \3\ p. 37 \9\
AA furnace................... 272.2......................... 3113 B [18th, 19th]........... .............................. I-4724-89 \51\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
63. Sodium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 273.1......................... 3111 B [18th, 19th]........... .............................. I-3735-85..................... 973.54 \3\
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\
DCP, or...................... .............................. .............................. .............................. .............................. Note 34.
Flame photometric............ .............................. 3500 Na B [20th] and 3500 Na D
[18th, 19th].
64. Specific conductance,
micromhos/cm at 25 [deg]C:
Wheatstone bridge............ 120.1......................... 2510 B [18th, 19th, 20th]..... D1125-95(A)................... I-2781-85..................... 973.40 \3\
65. Sulfate (as SO4), mg/L:
Automated colorimetric 375.1.........................
(barium chloranilate).
Gravimetric.................. 375.3......................... 4500-SO4-\2\C or D [18th, .............................. .............................. 925.54 \3\
19th, 20th].
Turbidimetric................ 375.4......................... .............................. D516-90....................... .............................. 426C \30\
66. Sulfide (as S), mg/L:
Titrimetric (iodine), or..... 376.1......................... 4500-S-\2\F [19th, 20th] or .............................. I-3840-85.....................
4500-S-\2\E [18th].
[[Page 19]]
Colorimetric (methylene blue) 376.2......................... 4500-S-\2\D [18th, 19th, 20th]
67. Sulfite (as SO3), mg/L:
Titrimetric (iodine-iodate).. 377.1......................... 4500-SO3-\2\B [18th, 19th,
20th].
68. Surfactants, mg/L:
Colorimetric (methylene blue) 425.1......................... 5540 C [18th, 19th, 20th]..... D2330-88......................
69. Temperature, [deg]C:
Thermometric................. 170.1......................... 2550 B [18th, 19th, 20th]..... .............................. .............................. Note 32.
70. Thallium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 279.1......................... 3111 B [18th, 19th]...........
AA furnace................... 279.2.........................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....
71. Tin--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 282.1......................... 3111 B [18th, 19th]........... .............................. I-3850-78 \8\.................
AA furnace, or............... 282.2......................... 3113 B [18th, 19th]...........
ICP/AES...................... 200.7 \5\.....................
72. Titanium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 283.1......................... 3111 D [18th, 19th]...........
AA furnace................... 283.2.........................
DCP.......................... .............................. .............................. .............................. .............................. Note 34.
73. Turbidity, NTU:
Nephelometric................ 180.1......................... 2130 B [18th, 19th, 20th]..... D1889-94(A)................... I-3860-85.....................
74. Vanadium--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration......... 286.1......................... 3111 D [18th, 19th]...........
AA furnace................... 286.2......................... .............................. D3373-93......................
ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP, or...................... .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Gallic Acid)... .............................. 3500-V B [20th] and 3500-V D
[18th, 19th].
75. Zinc--Total, \4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.... 289.1......................... 3111 B or C [18th, 19th]...... D1691-95(A or B).............. I-3900-85..................... 974.27, \3\ p. 37 \9\
AA furnace................... 289.2.........................
ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................
DCP, \36\ or................. .............................. .............................. D4190-94...................... .............................. Note 34.
Colorimetric (Dithizone) or.. .............................. 3500-Zn E [18th, 19th]........
(Zincon)..................... .............................. 3500-Zn B [20th] and 3500-Zn F .............................. .............................. Note 33.
[18th, 19th].
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory--Cincinnati (EMSL-CI), EPA-600/4-79-020, Revised March
1983 and 1979 where applicable.
\2\ Fishman, M.J., et al. ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, ''U.S. Department of the Interior, Techniques of Water-Resource Investigations of the
U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' methods manual, 15th ed. (1990).
[[Page 20]]
\4\ For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended material and to destroy possible organic-metal
complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes, 1979 and 1983''. One (Section 4.1.3), is a vigorous digestion using nitric acid. A less
vigorous digestion using nitric and hydrochloric acids (Section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types.
Particularly, if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive state. In those situations,
the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing large amounts of organic materials may also benefit by this
vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as
well as determinations for certain elements such as antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all
cases the method write-up should be consulted for specific instructions and/or cautions.
Note to Table 1B Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the above, the EPA procedure must be used.
Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the referenced procedure for total metals must
be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample solution for total metals) may be omitted for AA (direct aspiration or graphite
furnace) and ICP analyses, provided the sample solution to be analyzed meets the following criteria:
a. has a low COD (<20)
b. is visibly transparent with a turbidity measurement of 1 NTU or less
c. is colorless with no perceptible odor, and
d. is of one liquid phase and free of particulate or suspended matter following acidification.
\5\ The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,'' is given at Appendix C of this Part 136.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary distillation step is not necessary: however,
manual distillation will be required to resolve any controversies.
\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5, Chapter A1 (1979).
\9\ American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 25 West 43rd Street, New York, NY 10036.
\10\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of Standard Methods for the Examination of
Water and Wastewater (1981).
\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\ Carbonaceous biochemical oxygen demand (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, PO Box 2980, College Station, TX 77840.
\14\ Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, PO Box 389, Loveland, CO 80537.
\15\ The back titration method will be used to resolve controversy.
\16\ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph for the Orion
residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
\17\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
\18\ National Council of the Paper Industry for Air and Stream Improvement, Inc. Technical Bulletin 253, December 1971.
\19\ Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, PO Box 389, Loveland, CO 80537.
\20\ After the manual distillation is completed, the autoanalyzer manifolds in EPA Methods 335.3 (cyanide) or 420.2 (phenols) are simplified by connecting the re-sample line directly to the
sampler. When using the manifold setup shown in Method 335.3, the buffer 6.2 should be replaced with the buffer 7.6 found in Method 335.2.
\21\ Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, PO Box 389, Loveland, CO 80537.
\23\ Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.
\24\ Wershaw, R.L., et al, ``Methods for Analysis of Organic Substances in Water,'' Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised
1987) p. 14.
\25\ Nitrogen, Nitrite, Method 8507, Hach Chemical Company, PO Box 389, Loveland, CO 80537.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted at a pH of 10.0 0.2. The approved methods are given on pp 576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 510C for the manual
spectrometric procedure.
\28\ R.F. Addison and R.G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,'' Journal of Chromatography, Vol. 47, No. 3, pp. 421-426, 1970.
\29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such
as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12.
Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M 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.
[[Page 21]]
\31\ EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of total cyanide.
\32\ Stevens, H.H., Ficke, J.F., and Smoot, G.F., ``Water Temperature--Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.
Geological Survey, Book 1, Chapter D1, 1975.
\33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\ ``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--Revised 1991, Thermo Jarrell Ash Corporation,
27 Forge Parkway, Franklin, MA 02038.
\35\ Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC method for arsenic are provided in Appendix
D of this part titled, ``Precision and Recovery Statements for Methods for Measuring Metals''.
\36\ ``Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals'', CEM Corporation, PO Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM
Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use Trichlorotrifluorethane (1,1,2-trichloro-1,2,2-trifluoroethane; CFC-113) extraction solvent when determining Total Recoverable Oil and Grease (analogous to EPA Method 413.1).
Only use n-hexane extraction solvent when determining Hexane Extractable Material (analogous to EPA Method 1664A). Use of other extraction solvents is strictly prohibited.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\40\ Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, OI Analytical/ALPKEM, PO Box 9010, College Station, TX 77842.
\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and
Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, Virginia 22161.
\43\ USEPA. 2002. Method 1631, Revision E, ``Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry.'' September 2002. Office of Water, U.S.
Environmental Protection Agency (EPA-821-R-02-019). The application of clean techniques described in EPA's draft Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality
Criteria Levels (EPA-821-R-96-011) are recommended to preclude contamination at low-level, trace metal determinations.
\44\ Available Cyanide, Method OIA-1677 (Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry), ALPKEM, A Division of OI Analytical, PO Box 9010, College Station, TX 77842-
9010.
\45\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method'', Open File Report
(OFR) 00-170.
\46\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry'', Open
File Report (OFR) 93-449.
\47\ ''Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry'', Open File
Report (OFR) 97-198.
\48\ ''Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish
That Includes Dialysis'' Open File Report (OFR) 92-146.
\49\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption
Spectrometry'' Open File Report (OFR) 98-639.
\50\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission
Spectrometry and Inductively Coupled Plasma-Mass Spectrometry'', Open File Report (OFR) 98-165.
\51\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment'', Open File
Report (OFR) 93-125.
Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
EPA method number \2,7\ Other approved methods
------------------------------------------------------------------------------------------------------------------------
Parameter \1\ Standard Methods
GC GC/MS HPLC [Edition(s)] ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene................ 610................ 625, 1625B......... 610................ 6440 B [18th, D4657-92......... Note 9, p.27.
19th, 20th].
2. Acenaphthylene.............. 610................ 625, 1625B......... 610................ 6440 B, 6410 B D4657-92......... Note 9, p.27.
[18th, 19th,
20th].
3. Acrolein.................... 603................ 624 \4\, 1624B..... .................
4. Acrylonitrile............... 603................ 624 \4\, 1624B..... .................
5. Anthracene.................. 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
[[Page 22]]
6. Benzene..................... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
7. Benzidine................... ................... 625 \5\, 1625B..... 605................ .................. ................. Note 3, p.1.
8. Benzo(a)anthracene.......... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
9. Benzo(a)pyrene.............. 610,............... 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
10. Benzo(b)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
11. Benzo(g, h, i)perylene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
12. Benzo(k)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
13. Benzyl chloride............ ................... ................... ................... .................. ................. Note 3, p 130:
Note 6, p. S102.
14. Benzyl butyl phthalate..... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
15. Bis(2-chloroethoxy) methane 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
16. Bis(2-chloroethyl) ether... 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
17. Bis(2-ethylhexyl) phthalate 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
18. Bromodichloromethane....... 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
19. Bromoform.................. 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
20. Bromomethane............... 601................ 624, 1624B......... ................... 6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210 B
[18th, 19th].
21. 4-Bromophenylphenyl ether.. 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
22. Carbon tetrachloride....... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.
6230 B [18th,
19th].
23. 4-Chloro-3-methylphenol.... 604................ 625,1625B.......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
[[Page 23]]
24. Chlorobenzene.............. 601, 602........... 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130.
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th],
6200 C [20th] and
6230 B [18th,
19th],.
25. Chloroethane............... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
26. 2-Chloroethylvinyl ether... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
27. Chloroform:................ 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p 130.
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
28. Chloromethane.............. 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th] 6200C
[20th] and 6230 B
[18th, 19th].
29. 2-Chloronaphthalene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
30. 2-Chlorophenol............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
31. 4-Chlorophenylphenyl ether. 611................ 625, 1625B......... ................... 6410 B, [18th, ................. Note 9, p. 27.
19th, 20th].
32. Chrysene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
33. Dibenzo(a,h)anthracene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
34. Dibromochloromethane....... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th] 6200 C
[20th] and 6230 B
[18th, 19th].
35. 1,2-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
36. 1,3-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
[[Page 24]]
37. 1,4-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.
6220 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th],
6410 B [18th,
19th, 20th].
38. 3,3-Dichlorobenzidine...... ................... 625, 1625B......... 605................ 6410 B [18th, .................
19th, 20th].
39. Dichlorodifluoromethane.... 601................ ................... ................... 6200 C [20th] and .................
6230 B [18th,
19th].
40. 1,1-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
41. 1,2-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
42. 1,1-Dichloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
43. trans-1,2-Dichloroethene... 601................ 624, 1624B......... ................... 6200 B [20th] and .................
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
44. 2,4-Dichlorophenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
45. 1,2-Dichloropropane........ 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
46. cis-1,3-Dichloropropene.... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
47. trans-1,3-Dichloropropene.. 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
48. Diethyl phthalate.......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
[[Page 25]]
49. 2,4-Dimethylphenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.
[18th, 19th,
20th].
50. Dimethyl phthalate......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
51. Di-n-butyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
52. Di-n-octyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
53. 2,3-Dinitrophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6420 B
[18th, 19th,
20th].
54. 2,4-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
55. 2,6-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
56. Epichlorohydrin............ ................... ................... ................... .................. ................. Note 3, p. 130;
Note 6, p. S102.
57. Ethylbenzene............... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
58. Fluoranthene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
59. Fluorene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
60. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B
dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro- ................... 1613B .................
dibenzofuran.
62. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B .................
dibenzo-p-dioxin.
63. Hexachlorobenzene.......... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
64. Hexachlorobutadiene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
65. Hexachlorocyclopentadiene.. 612................ \5\625, 1625B...... ................... 6410 [18th, 19th, ................. Note 9, p. 27.
20th].
66. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
67. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
68. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............
dibenzofuran.
69. 2,3,4,6,7,8-Hexachloro- ................... 1613B..............
dibenzofuran.
70. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
71. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
72. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............
dibenzo-p-dioxin.
73. Hexachloroethane........... 616................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
74. Ideno(1,2,3-cd) pyrene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.
[18th, 19th,
20th].
75. Isophorone................. 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.
19th, 20th].
76. Methylene chloride......... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.
6230 B [18th,
19th].
77. 2-Methyl-4,6-dinitrophenol. 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
[[Page 26]]
78. Naphthalene................ 610................ 625, 1625B......... 610................ 6440 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
79. Nitrobenzene............... 609................ 625, 1625B......... ................... 6410 B [18th, D4657-92......... Note 9, p. 27.
19th, 20th].
80. 2-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27
[18th, 19th,
20th].
81. 4-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27
[18th, 19th,
20th].
82. N-Nitrosodimethylamine..... 607................ 625, \5\ 1625B..... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
83. N-Nitrosodi-n-propylamine.. 607................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
84. N-Nitrosodiphenylamine..... 607................ 625, \5\ 1625B..... ................... 6410 B [18th, ................. Note 9, p. 27
19th, 20th].
85. Octachlorodibenzofuran..... ................... 1613B..............
86. Octachlorodibenzo-p-dioxin. ................... 1613B..............
87. 2,2'-Oxybis(2- 611................ 625, 1625B......... ................... 6410 B [18th,
chloropropane) [also known as 19th, 20th].
bis(2-chloroisopropyl) ether].
88. PCB-1016................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
89. PCB-1221................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
90. PCB-1232................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
91. PCB-1242................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
92. PCB-1248................... 608................ 625................
93. PCB-1254................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43
19th, 20th].
94. PCB-1260................... 608................ 625................ ................... 6410 B, 6630 B ................. Note 3, p. 43
[18th, 19th,
20th].
95. 1,2,3,7,8-Pentachloro- ................... 1613B..............
dibenzofuran.
96. 2,3,4,7,8-Pentachloro- ................... 1613B..............
dibenzofuran.
97. 1,2,3,7,8,- ................... 1613B..............
Pentachlorodibenzo-p-dioxin.
98. Pentachlorophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6630 B ................. Note 3, p. 140;
[18th, 19th, Note 9, p. 27
20th].
99. Phenanthrene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27
[18th, 19th,
20th].
100. Phenol.................... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27
[18th, 19th,
20th].
101. Pyrene.................... 610................ 625, 1625B......... 610................ 6440 B, 6410 B D4675-92......... Note 9, p. 27
D4675-92 [18th,
19th, 20th].
[[Page 27]]
102. 2,3,7,8-Tetrachloro- ................... 1613B..............
dibenzofuran.
103. 2,3,7,8-Tetrachlorodibenzo- ................... 613, 1613B.........
p-dioxin.
104. 1,1,2,2-Tetrachloroethane. 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
105. Tetrachloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
106. Toluene................... 602................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220 B
[18th, 19th].
107. 1,2,4-Trichlorobenzene.... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 3, p. 130;
19th, 20th]. Note 9, p. 27.
108. 1,1,1-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
109. 1,1,2-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
110. Trichloroethene........... 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
111. Trichlorofluoromethane.... 601................ 624................ ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
112. 2,4,6-Trichlorophenol..... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.
[18th, 19th,
20th].
113. Vinyl chloride............ 601................ 624, 1624B......... ................... 6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230 B
[18th, 19th].
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([micro]g/L) except for Method 1613B in which the parameters are expressed in picograms per
liter (pg/L).
\2\ The full text of Methods 601-613, 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.
\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 28]]
\7\ Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624,
625, 1624B, and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each
laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to
monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these Methods. When the recovery of any parameter falls
outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate
regulatory compliance.
Note: These warning limits are promulgated as an ``interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'' 3M Corporation Revised 10/28/94.
\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic
Constituents in Water and Fluvial Sediments'' U.S. Geological Survey, Open File Report 93-125.
Table ID--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard Methods
Parameter Method EPA \2,7\ 18th, 19th, 20th Ed. ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin......................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B
2. Ametryn........................ GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p S68.
3. Aminocarb...................... TLC................... ...................... ...................... ...................... Note 3, p. 94; Note
6, p. S16.
4. Atraton........................ GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68.
5. Atrazine....................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
6. Azinphos methyl................ GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
6, p. S51.
7. Barban......................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
8. [alpha]-BHC.................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
8.
GC/MS................. 625 \5\............... 6410 B................
9. [beta]-BHC..................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.
GC/MS................. 625 \5\............... 6410 B................
10. [delta]-BHC................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.
GC/MS................. 625 \5\............... 6410 B................
11. [gamma]-BHC (Lindane)......... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
12. Captan........................ GC.................... ...................... 6630 B................ D3086-90.............. Note 3, p. 7.
13. Carbaryl...................... TLC................... ...................... ...................... ...................... Note 3, p. 94, Note
6, p. S60.
14. Carbophenothion............... GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
15. Chlordane..................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
16. Chloropropham................. TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
17. 2,4-D......................... GC.................... ...................... 6640 B................ ...................... Note 3, p. 115; Note
4, p. 40.
18. 4,4'-DDD...................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
19. 4,4'-DDE...................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
20. 4,4'-DDT...................... GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
21. Demeton-O..................... GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
6, p. S51.
22. Demeton-S..................... GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
6, p. S51.
23. Diazinon...................... GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
4, p. 27; Note 6,
p. S51.
24. Dicamba....................... GC.................... ...................... ...................... ...................... Note 3, p. 115.
25. Dichlofenthion................ GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
26. Dichloran..................... GC.................... ...................... 6630 B & C............ ...................... Note 3, p. 7.
[[Page 29]]
27. Dicofol....................... GC.................... ...................... ...................... D3086-90..............
28. Dieldrin...................... GC.................... 608................... 6630 B & C............ ...................... Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
29. Dioxathion.................... GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
30. Disulfoton.................... GC.................... ...................... ...................... ...................... Note 3, p. 25; Note
6 p. S51.
31. Diuron........................ TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
32. Endosulfan I.................. GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625 \5\............... 6410 B................
33. Endosulfan II................. GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
8.
GC/MS................. 625 \5\............... 6410 B................
34. Endosulfan Sulfate............ GC.................... 608................... 6630 C................ ...................... Note 8.
GC/MS................. 625................... 6410 B................
35. Endrin........................ GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
...................... ...................... ...................... 4, p. 27; Note 8.
GC/MS................. 625 \5\............... 6410 B................
36. Endrin aldehyde............... GC.................... 608................... ...................... ...................... Note 8.
GC/MS................. 625...................
37. Ethion........................ GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
38. Fenuron....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
39. Fenuron-TCA................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
40. Heptachlor.................... GC.................... 608................... 6630 B & C............ 3086-90............... Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410 B................
41. Heptachlor epoxide............ GC.................... 608................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
...................... ...................... ...................... 4, p. 27; Note 6,
GC/MS................. 625................... 6410 B................ p. S73; Note 8.
42. Isodrin....................... GC.................... ...................... ...................... ...................... Note 4, p. 27; Note
6, p. S73.
43. Linuron....................... GC.................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
44. Malathion..................... GC.................... ...................... 6630 C................ ...................... Note 3, p. 25; Note
4, p. 27; Note 6,
p. S51
45. Methiocarb.................... TLC................... ...................... ...................... ...................... Note 3, p. 94; Note
6, p. S60.
46. Methoxychlor.................. GC.................... ...................... 6630 B & C............ D3086-90.............. Note 3, p. 7; Note
4, p. 27; Note 8.
47. Mexacarbate................... TLC................... ...................... ...................... ...................... Note 3, p. 94; Note
6, p. S60.
48. Mirex......................... GC.................... ...................... 6630 B & C............ ...................... Note 3, p. 7; Note
4, p. 27.
49. Monuron....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
50. Monuron....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
51. Nuburon....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
52. Parathion methyl.............. GC.................... ...................... 6630 C................ ...................... Note 3, p. 25; Note
4, p. 27.
53. Parathion ethyl............... GC.................... ...................... 6630 C................ ...................... Note 3, p. 25; Note
4, p. 27.
54. PCNB.......................... GC.................... ...................... 6630 B & C............ ...................... Note 3, p. 7.
55. Perthane...................... GC.................... ...................... ...................... D3086-90.............. Note 4, p. 27.
56. Prometron..................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
57. Prometryn..................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
58. Propazine..................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
59. Propham....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
60. Propoxur...................... TLC................... ...................... ...................... ...................... Note 3, p. 94; Note
6, p. S60.
61. Secbumeton.................... TLC................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68.
62. Siduron....................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
63. Simazine...................... GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68; Note 9.
64. Strobane...................... GC.................... ...................... 6630 B & C............ ...................... Note 3, p. 7.
65. Swep.......................... TLC................... ...................... ...................... ...................... Note 3, p. 104; Note
6, p. S64.
66. 2,4,5-T....................... GC.................... ...................... 6640 B................ ...................... Note 3, p. 115; Note
4, p. 40.
[[Page 30]]
67. 2,4,5-TP (Silvex)............. GC.................... ...................... 6640 B................ ...................... Note 3, p. 115; Note
4, p. 40.
68. Terbuthylazine................ GC.................... ...................... ...................... ...................... Note 3, p. 83; Note
6, p. S68.
69. Toxaphene..................... GC.................... 608................... 6630 B & C............ D3086--90............. Note 3, p. 7; Note
4, p. 27; Note 8.
GC/MS................. 625................... 6410B.................
70. Trifluralin................... GC.................... ...................... 6630 B................ ...................... Note 3, p. 7; Note
9.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, where
entries are listed by chemical name.
\2\ The full text of Methods 608 and 625 are given at Appendix A. ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The
standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition
and Procedure for the Determination of the Method Detection Limit,'' of this Part 136.
\3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September 1978. This EPA publication includes thin-layer chromatography (TLC) methods.
\4\ ``Methods for Analysis of Organic Substances in Water and Fluvial Sediments,'' Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5, Chapter A3 (1987).
\5\ The method may be extended to include [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).
\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 and cannot be reported to demonstrate regulatory compliance. These
quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
Note: These warning limits are promulgated as an ``Interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore \TM\ 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 Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
---------------------------------------------------------------------------------------------------
Parameter and units Method Standard Methods 18th,
EPA \1\ 19th, 20th Ed. ASTM USGS \2\
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter... Proportional or 900 7110 B D1943-90 pp. 75 and 78 \3\
scintillation
counter.
2. Alpha-Counting error, pCi per Proportional or Appendix B 7110 B D1943-90 p. 79
liter. scintillation
counter.
3. Beta-Total, pCi per liter.... Proportional 900.0 7110 B D1890-90 pp. 75 and 78 \3\
counter.
4. Beta-Counting error, pCi..... Proportional Appendix B 7110 B D1890-90 p. 79
counter.
5. (a) Radium Total pCi per Proportional 903.0 7500Ra B D2460-90 .......................
liter. counter.
(b) Ra, pCi per liter....... Scintillation 903.1 7500Ra C D3454-91 p. 81
counter.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1E notes:
\1\ ``Prescribed Procedures for Measurement of Radioactivity in Drinking Water,'' EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August
1980.
\2\ Fishman, M.J. and Brown, Eugene, ``Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters,'' U.S. Geological Survey, Open-File
Report 76-177 (1976).
\3\ The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, the two
results must be added to obtain the ``total''.
[[Page 31]]
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.
(b) The full texts of the methods from the following references
which are cited in Tables IA, IB, IC, ID, IE,and IF are incorporated by
reference into this regulation and may be obtained from the sources
identified. All costs cited are subject to change and must be verified
from the indicated sources. The full texts of all the test procedures
cited are available for inspection at the National Exposure Research
Laboratory, Office of Research and Development, U.S. Environmental
Protection Agency, 26 West Martin Luther King Dr., Cincinnati, OH 45268
and the 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 from: National Technical Information Service,
5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB-290329/
AS. Cost: $36.95. Table IA, Note 3.
(3) ``Methods for Chemical Analysis of Water and Wastes,'' U.S.
Environmental Protection Agency, EPA-600/4-
[[Page 32]]
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: Amer. Publ. Hlth.
Assoc., 1015 15th Street, NW., Washington, DC 20005. Table IA, Note 4.
Tables IB, IC, ID, IE.
(7) Ibid, 15th Edition, 1980. Table IB, Note 30; Table ID.
(8) Ibid, 14th Edition, 1975. Table IB, Notes 17 and 27.
(9) ``Selected Analytical Methods Approved and Cited by the United
States Environmental Protection Agency,'' Supplement to the 15th Edition
of Standard Methods for the Examination of Water and Wastewater, 1981.
Available from: American Public Health Association, 1015 Fifteenth
Street NW., Washington, DC 20036. Cost available from publisher. Table
IB, Note 10; Table IC, Note 6; Table ID, Note 6.
(10) Annual Book of ASTM Standards, Water, and Environmental
Technology, Section 11, Volumes 11.01 and 11.02, 1994, 1996, 1999, and
Volume 11.02, 2000 in 40 CFR 136.3, Tables IA, IB, IC, ID, and IE.
(11) USGS. 1989. U.S. Geological Survey Techniques of Water-
Resources Investigations, Book 5, Laboratory Analysis, Chapter A4,
Methods for Collection and Analysis of Aquatic Biological and
Microbiological Samples, U.S. Geological Survey, U.S. Department of the
Interior, Reston, Virginia. Available from: USGS Books and Open-File
Reports Section, Federal Center, Box 25425, Denver, Colorado 80225.
Cost: $18.00. Table IA, Note 5.
(12) ``Methods for Determination of Inorganic Substances in Water
and Fluvial Sediments,'' by M.J. Fishman and Linda C. Friedman,
Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5 Chapter A1 (1989). Available from: U.S. Geological
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost:
$108.75 (subject to change). Table IB, Note 2.
(13) ``Methods for Determination of Inorganic Substances in Water
and Fluvial Sediments,'' N.W. Skougstad and others, editors. Techniques
of Water-Resources Investigations of the U.S. Geological Survey, Book 5,
Chapter A1 (1979). Available from: U.S. Geological Survey, Denver
Federal Center, Box 25425, Denver, CO 80225. Cost: $10.00 (subject to
change), Table IB, Note 8.
(14) ``Methods for the Determination of Organic Substances in Water
and Fluvial Sediments,'' Wershaw, R.L., et al, Techniques of Water-
Resources Investigations of the U.S. Geological Survey, Book 5, Chapter
A3 (1987). Available from: U.S. Geological Survey, Denver Federal
Center, Box 25425, Denver, CO 80225. Cost: $0.90 (subject to change).
Table IB, Note 24; Table ID, Note 4.
(15) ``Water Temperature--Influential Factors, Field Measurement and
Data Presentation,'' by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot,
Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 1, Chapter D1, 1975. Available from: U.S. Geological
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $1.60
(subject to change). Table IB, Note 32.
(16) ``Selected Methods of the U.S. Geological Survey of Analysis of
Wastewaters,'' by M.J. Fishman and Eugene Brown; U.S. Geological Survey
Open File Report 76-77 (1976). Available from: U.S. Geological Survey,
Branch of Distribution, 1200 South Eads Street, Arlington, VA 22202.
Cost: $13.50 (subject to change). Table IE, Note 2.
(17) ``Official Methods of Analysis of the Association of Official
Analytical
[[Page 33]]
Chemicals'', Methods manual, 15th Edition (1990). Price: $240.00.
Available from: The Association of Official Analytical Chemists, 2200
Wilson Boulevard, Suite 400, Arlington, VA 22201. Table IB, Note 3.
(18) ``American National Standard on Photographic Processing
Effluents,'' April 2, 1975. Available from: American National Standards
Institute, 1430 Broadway, New York, New York 10018. Table IB, Note 9.
(19) ``An Investigation of Improved Procedures for Measurement of
Mill Effluent and Receiving Water Color,'' NCASI Technical Bulletin No.
253, December 1971. Available from: National Council of the Paper
Industry for Air and Stream Improvements, Inc., 260 Madison Avenue, New
York, NY 10016. Cost available from publisher. Table IB, Note 18.
(20) Ammonia, Automated Electrode Method, Industrial Method Number
379-75WE, dated February 19, 1976. Technicon Auto Analyzer II. Method
and price available from Technicon Industrial Systems, Tarrytown, New
York 10591. Table IB, Note 7.
(21) Chemical Oxygen Demand, Method 8000, Hach Handbook of Water
Analysis, 1979. Method price available from Hach Chemical Company, P.O.
Box 389, Loveland, Colorado 80537. Table IB, Note 14.
(22) OIC Chemical Oxygen Demand Method, 1978. Method and price
available from Oceanography International Corporation, 512 West Loop,
P.O. Box 2980, College Station, Texas 77840. Table IB, Note 13.
(23) ORION Research Instruction Manual, Residual Chlorine Electrode
Model 97-70, 1977. Method and price available from ORION Research
Incorporation, 840 Memorial Drive, Cambridge, Massachusetts 02138. Table
IB, Note 16.
(24) Bicinchoninate Method for Copper. Method 8506, Hach Handbook of
Water Analysis, 1979, Method and price available from Hach Chemical
Company, P.O. Box 300, Loveland, Colorado 80537. Table IB, Note 19.
(25) Hydrogen Ion (pH) Automated Electrode Method, Industrial Method
Number 378-75WA. October 1976. Bran & Luebbe (Technicon) Auto Analyzer
II. Method and price available from Bran & Luebbe Analyzing
Technologies, Inc. Elmsford, N.Y. 10523. Table IB, Note 21.
(26) 1,10-Phenanthroline Method using FerroVer Iron Reagent for
Water, Hach Method 8008, 1980. Method and price available from Hach
Chemical Company, P.O. Box 389 Loveland, Colorado 80537. Table IB, Note
22.
(27) Periodate Oxidation Method for Manganese, Method 8034, Hach
Handbook for Water Analysis, 1979. Method and price available from Hach
Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note
23.
(28) Nitrogen, Nitrite--Low Range, Diazotization Method for Water
and Wastewater, Hach Method 8507, 1979. Method and price available from
Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB,
Note 25.
(29) Zincon Method for Zinc, Method 8009. Hach Handbook for Water
Analysis, 1979. Method and price available from Hach Chemical Company,
P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 33.
(30) ``Direct Determination of Elemental Phosphorus by Gas-Liquid
Chromatography,'' by R.F. Addison and R.G. Ackman, Journal of
Chromatography, Volume 47, No. 3, pp. 421-426, 1970. Available in most
public libraries. Back volumes of the Journal of Chromatography are
available from Elsevier/North-Holland, Inc., Journal Information Centre,
52 Vanderbilt Avenue, New York, NY 10164. Cost available from publisher.
Table IB, Note 28.
(31) ``Direct Current Plasma (DCP) Optical Emission Spectrometric
Method for Trace Elemental Analysis of Water and Wastes'', Method AES
0029, 1986-Revised 1991, Fison Instruments, Inc., 32 Commerce Center,
Cherry Hill Drive, Danvers, MA 01923. Table B, Note 34.
(32) ``Closed Vessel Microwave Digestion of Wastewater Samples for
Determination of Metals, CEM Corporation, P.O. Box 200, Matthews, North
Carolina 28106-0200, April 16, 1992. Available from the CEM Corporation.
Table IB, Note 36.
(33) ``Organochlorine Pesticides and PCBs in Wastewater Using Empore
\TM\ Disk'' Test Method 3M 0222, Revised 10/28/94. 3M Corporation, 3M
Center Building 220-9E-10, St. Paul, MN 55144-1000.
[[Page 34]]
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 from: National Technical
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161,
Pub. No. PB2002-108488. Table IA, Note 29.
(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 from: National
Technical Information Service, 5285 Port Royal Road, Springfield,
Virginia 22161, Pub. No. PB2002-108489. Table IA, Note 30.
(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
from: National Technical Information Service, 5285 Port Royal Road,
Springfield, Virginia 22161, Pub. No. PB2002-108490. Table IA, Note 31.
(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.
[[Page 35]]
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. 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.
(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.
(54) USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) in Water
by Membrane Filtration Using membrane-Thermotolerant Escherichia coli
Agar (mTEC). U.S. Environmental Protection Agency, Office of Water,
Washington D.C. September 2002, EPA-821-R-02-020. Available at NTIS,
PB2003-100125. Table IA, Note 20.
(55) USEPA. 2002. Method 1106.1: Enterococci in Water by Membrane
Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S.
Environmental Protection Agency, Office of Water, Washington D.C.
September 2002, EPA-821-R-02-021. Available at NTIS, PB2003-100126.
Table IA, Note 24.
(56) USEPA. 2002. Method 1603: Escherichia coli (E. coli) in Water
by Membrane Filtration Using Modified membrane-Thermotolerant
Escherichia coli Agar (Modified mTEC). U.S. Environmental Protection
Agency, Office of Water, Washington, DC September 2002, EPA-821-R-02-
023. Available at NTIS, PB2003-100128. Table IA, Note 21.
(57) Brenner et al. 1993. New Medium for the Simultaneous Detection
of Total Coliforms and Escherichia coli in Water. Appl. Environ.
Microbiol. 59:3534-
[[Page 36]]
3544. Available from the American Society for Microbiology, 1752 N
Street NW., Washington, DC 20036. Table IA, Note 22.
(58) USEPA. 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 D.C. September 2002, EPA 821-R-02-024. Available from
NTIS, PB2003-100129. Table IA, Note 22.
(59) USEPA. 2002. Method 1600: Enterococci in Water by Membrane
Filtration using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar
(mEI). U.S. Environmental Protection Agency, Office of Water, Washington
D.C. September 2002, EPA-821-R-02-022. Available from NTIS, PB2003-
100127. Table IA, Note 25.
(60) USEPA. 2001. Method 1622: Cryptosporidium in Water by
Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of
Water, Washington, DC April 2001, EPA-821-R-01-026.
Available from NTIS, PB2002-108709. Table IA, Note 26.
(61) USEPA. 2001. Method 1623: Cryptosporidium and Giardia in Water
by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of
Water, Washington, DC April 2001, EPA-821-R-01-025. Available from NTIS,
PB2002-108710. Table IA, Note 27.
(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.
(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 the recommendation of the Director
of the Environmental Monitoring Systems Laboratory--Cincinnati.
(d) Under certain circumstances, the Administrator may approve, upon
recommendation by the Director, Environmental Monitoring Systems
Laboratory--Cincinnati, additional alternate test procedures for
nationwide use.
(e) Sample preservation procedures, container materials, and maximum
allowable holding times for parameters cited in Tables IA, IB, IC, ID,
and IE are prescribed in Table II. Any person may apply for a variance
from the prescribed preservation techniques, container materials, and
maximum holding times applicable to samples taken from a specific
discharge. Applications for variances may be made by letters to the
Regional Administrator in the Region in which the discharge will occur.
Sufficient data should be provided to assure such variance does not
adversely affect the integrity of the sample. Such data will be
forwarded, by the Regional Administrator, to the Director of the
Environmental Monitoring Systems Laboratory--Cincinnati, Ohio for
technical review and recommendations for action on the variance
application. Upon receipt of the recommendations from the Director of
the Environmental Monitoring Systems Laboratory, the Regional
Administrator may grant a variance applicable to the specific charge to
the applicant. A decision to approve or deny a variance will be made
within 90 days of receipt of the application by the Regional
Administrator.
Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
Parameter No./name Container \1\ Preservation \2,3\ Maximum holding time \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacteria Tests:
1-5 Coliform, total, fecal, PP, G........... Cool, <10 [deg]C, 0.0008% 6 hours.
and E. coli. Na2S2O3 \5\.
6 Fecal streptococci.......... PP, G........... Cool, <10[deg] 0.0008% Na2S2O3 6 hours.
\5\.
7 Enterococci................. PP, G........... Cool, <10[deg] 0.0008% Na2S2O3 6 hours.
\5\.
Table IA--Protozoa Tests:
8 Cryptosporidium............. LDPE............ 0-8 [deg]C...................... 96 hours. \17\
9 Giardia..................... LDPE............ 0-8 [deg]C...................... 96 hours. \17\
Table IA--Aquatic Toxicity
Tests:
6-10 Toxicity, acute and P,G............. Cool, 4 [deg]C \16\............. 36 hours.
chronic.
[[Page 37]]
Table IB--Inorganic Tests:
1. Acidity.................... P, G............ Cool, 4[deg]C................... 14 days.
2. Alkalinity................. P, G............ ......do........................ Do.
4. Ammonia.................... P, G............ Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
9. Biochemical oxygen demand.. P, G............ Cool, 4[deg]C................... 48 hours.
10. Boron..................... P, PFTE, or HNO3 TO pH<2.................... 6 months.
Quartz.
11. Bromide................... P, G............ None required................... 28 days.
14. Biochemical oxygen demand, P, G............ Cool, 4[deg]C................... 48 hours.
carbonaceous.
15. Chemical oxygen demand.... P, G............ Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
16. Chloride.................. P, G............ None required................... Do.
17. Chlorine, total residual.. P, G............ ......do........................ Analyze immediately.
21. Color..................... P, G............ Cool, 4[deg]C................... 48 hours.
23-24. Cyanide, total and P, G............ Cool, 4[deg]C, NaOH to pH12, 0.6g ascorbic acid \5\.
25. Fluoride.................. P............... None required................... 28 days.
27. Hardness.................. P, G............ HNO3 to pH<2, H2SO4 to pH<2..... 6 months.
28. Hydrogen ion (pH)......... P, G............ None required................... Analyze immediately.
31, 43. Kjeldahl and organic P, G............ Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
nitrogen.
Metals: \7\
18. Chromium VI \7\........... P, G............ Cool, 4 [deg]C.................. 24 hours.
35. Mercury \17\.............. P, G............ HNO3 to pH<2.................... 28 days.
3, 5-8, 12,13, 19, 20, 22, 26, P, G............ do.............................. 6 months.
29, 30, 32-34, 36, 37, 45,
47, 51, 52, 58-60, 62, 63, 70-
72, 74, 75. Metals except
boron, chromium VI and
mercury \7\.
38. Nitrate................... P, G............ Cool, 4[deg]C................... 48 hours.
39. Nitrate-nitrite........... P, G............ Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
40. Nitrite................... P, G............ Cool, 4[deg]C................... 48 hours.
41. Oil and grease............ G............... Cool to 4[deg]C, HCl or H2SO4 to 28 days.
pH<2.
42. Organic Carbon............ P, G............ Cool to 4 [deg]C HC1 or H2SO4 or 28 days.
H3PO4, to pH<2.
44. Orthophosphate............ P, G............ Filter immediately, Cool, 48 hours.
4[deg]C.
46. Oxygen, Dissolved Probe... G Bottle and top None required................... Analyze immediately.
47. Winkler................... ......do........ Fix on site and store in dark... 8 hours.
48. Phenols................... G only.......... Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
49. Phosphorus (elemental).... G............... Cool, 4[deg]C................... 48 hours.
50. Phosphorus, total......... P, G............ Cool, 4[deg]C, H2SO4 to pH<2.... 28 days.
53. Residue, total............ P, G............ Cool, 4[deg]C................... 7 days.
54. Residue, Filterable....... P, G............ ......do........................ 7 days.
55. Residue, Nonfilterable P, G............ ......do........................ 7 days.
(TSS).
56. Residue, Settleable....... P, G............ ......do........................ 48 hours.
57. Residue, volatile......... P, G............ ......do........................ 7 days.
61. Silica.................... P, PFTE, or Cool, 4 [deg]C.................. 28 days.
Quartz.
64. Specific conductance...... P, G............ ......do........................ Do.
65. Sulfate................... P, G............ ......do........................ Do.
66. Sulfide................... P, G............ Cool, 4[deg]C add zinc acetate 7 days.
plus sodium hydroxide to pH9.
67. Sulfite................... P, G............ None required................... Analyze immediately.
68. Surfactants............... P ,G............ Cool, 4[deg]C................... 48 hours.
69. Temperature............... P, G............ None required................... Analyze.
73. Turbidity................. P, G............ Cool, 4[deg]C................... 48 hours.
Table IC--Organic Tests \8\
13, 18-20, 22, 24-28, 34-37, G, Teflon-lined Cool, 4 [deg]C, 0.008% Na2S2O3 14 days.
39-43, 45-47, 56, 76, 104, septum. \5\..
105, 108-111, 113. Purgeable
Halocarbons.
6, 57, 106. Purgeable aromatic ......do........ Cool, 4 [deg]C, 0.008% Na2S2O3, Do.
hydrocarbons. \5\ HCl to pH2 \9\.
3, 4. Acrolein and ......do........ Cool, 4 [deg]C, 0.008% Na2S2O3, Do.
acrylonitrile. \5\ adjust pH to 4-5 \10\.
23, 30, 44, 49, 53, 77, 80, G, Teflon-lined Cool, 4 [deg]C, 0.008% Na2S2O3 7 days until extraction;
81, 98, 100, 112. Phenols cap.. \5\. 40 days after extraction.
\11\.
7, 38. Benzidines \11\........ ......do........ ......do........................ 7 days until extraction.
\13\
14, 17, 48, 50-52. Phthalate ......do........ Cool, 4 [deg]C.................. 7 days until extraction;
esters \11\. 40 days after extraction.
[[Page 38]]
82-84. Nitrosamines \11,14\... ......do........ Cool, 4 [deg]C, 0.008% Na2S2O3, Do.
\5\ store in dark.
88-94. PCBs \11\.............. .....do......... Cool, 4 [deg]C.................. Do.
54, 55, 75, 79. Nitroaromatics ......do........ Cool, 4 [deg]C, 0.008% Na2S2O3, Do.
and isophorone \11\. \5\ store in dark.
1, 2, 5, 8-12, 32, 33, 58, 59, ......do........ ......do........................ Do.
74, 78, 99, 101. Polynuclear
aromatic hydrocarbons \11\.
15, 16, 21, 31, 87. Haloethers ......do........ Cool, 4 [deg]C, 0.008% Na2S2O3 Do.
\11\. \5\.
29, 35-37, 63-65, 73, 107. ......do........ Cool, 4 [deg]C.................. Do.
Chlorinated hydrocarbons \11\.
60-62, 66-72, 85, 86, 95-97,
102, 103. CDDs/CDFs \11\.
aqueous: field and lab G............... Cool, 0-4 [deg]C, pH<9, 0.008% 1 year.
preservation.. Na2S2O3 \5\.
Solids, mixed phase, and ......do........ Cool, <4 [deg]C................. 7 days.
tissue: field preservation..
Solids, mixed phase, and ......do........ Freeze, <-10 [deg]C............. 1 year.
tissue: lab preservation.
Table ID--Pesticides Tests:
1-70. Pesticides \11\......... ......do........ Cool, 4[deg]C, pH 5-9 \15\...... Do.
Table IE--Radiological Tests:
1-5. Alpha, beta and radium... P, G............ HNO3 to pH<2.................... 6 months.
----------------------------------------------------------------------------------------------------------------
Table II Notes
\1\ Polyethylene (P) or glass (G). For microbiology, plastic sample containers must be made of sterilizable
materials (polypropylene or other autoclavable plastic).
\2\ Sample preservation should be performed immediately upon sample collection. For composite chemical samples
each aliquot should be preserved at the time of collection. When use of an automated sampler makes it
impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4[deg]C until
compositing and sample splitting is completed.
\3\ When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply
with the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering
such material for transportation is responsible for ensuring such compliance. For the preservation
requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of
Transportation has determined that the Hazardous Materials Regulations do not apply to the following
materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about
1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about
1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH
about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight
or less (pH about 12.30 or less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before analysis and still be considered valid. Samples may be held for longer periods only
if the permittee, or monitoring laboratory, has data on file to show that for the specific types of samples
under study, the analytes are stable for the longer time, and has received a variance from the Regional
Administrator under Sec. 136.3(e). Some samples may not be stable for the maximum time period given in the
table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge
exists to show that this is necessary to maintain sample stability. See Sec. 136.3(e) for details. The term
``analyze immediately'' usually means within 15 minutes or less of sample collection.
\5\ Should only be used in the presence of residual chlorine.
\6\ Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead
acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can
be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is
filtered and then NaOH is added to pH 12.
\7\ Samples should be filtered immediately on-site before adding preservative for dissolved metals.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ Sample receiving no pH adjustment must be analyzed within seven days of sampling.
\10\ The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
adjustment must be analyzed within 3 days of sampling.
\11\ When the extractable analytes of concern fall within a single chemical category, the specified preservative
and maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of
concern fall within two or more chemical categories, the sample may be preserved by cooling to 4[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 (re
the requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of
benzidine).
\12\ If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 0.2 to prevent rearrangement to benzidine.
\13\ Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)
atmosphere.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
of sampling.
\15\ The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still
present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, it
is necessary to immediately measure the temperature of the samples and confirm that the 4C temperature maximum
has not been exceeded. In the isolated cases where it can be documented that this holding temperature can not
be met, the permittee can be given the option of on-site testing or can request a variance. The request for a
variance should include supportive data which show that the toxicity of the effluent samples is not reduced
because of the increased holding temperature.
\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. Samples collected for dissolved trace level mercury should be filtered in the laboratory.
However, if circumstances prevent overnight shipment, samples should be filtered in a designated clean area in
the field in accordance with procedures given in Method 1669. Samples that have been collected for
determination of total or dissolved trace level mercury must be analyzed within 90 days of sample collection.
[[Page 39]]
[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.