TITLE 40 - PROTECTION OF ENVIRONMENT

CHAPTER I - ENVIRONMENTAL PROTECTION AGENCY

SUBCHAPTER D - WATER PROGRAMS

PART 136 - GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS

136.3 - Identification of test procedures.

(a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, and IF. The full text of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, and IF.

The incorporation by reference of these documents, as specified in paragraph (b) of this section, was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51.

Copies of the documents may be obtained from the sources listed in paragraph (b) of this section. Information regarding obtaining these documents can be obtained from the EPA Office of Water Statistics and Analytical Support Branch at 2025661000. Documents may be inspected at EPA's Water Docket, EPA West, 1301 Constitution Avenue, NW., Room B135, Washington, DC (Telephone: 202-5662426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 2027416030, 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 136.4 and 136.5. Under certain circumstances (paragraph (b) or (c) of this section or 40 CFR 401.13) other test procedures may be more advantageous when such other test procedures have been previously approved by the Regional Administrator of the Region in which the discharge will occur, and providing the Director of the State in which such discharge will occur does not object to the use of such alternate test procedure.

Table IA_List of Approved Biological Methods -------------------------------------------------------------------------------------------------------------------------------------------------------- Standard methods 18th, Parameter and units Method \1\ EPA 19th, 20th Ed. ASTM AOAC USGS Other -------------------------------------------------------------------------------------------------------------------------------------------------------- Bacteria: 1. Coliform (fecal), number Most Probable Number p. 132 9221C E \4\ per 100 mL. (MPN), 5 tube 3 \3\ dilution, or Membrane filter (MF) p. 124 9222D \4\ ........... ........... B-0050-85 \2\, single step. \3\ \5\ 2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 9221C E \4\ presence of chlorine, number dilution, or \3\ per 100 mL.

MF, single step \6\. p. 124 9222D \4\ \3\ 3. Coliform (total), number MPN, 5 tube, 3 p. 114 9221B \4\ per 100 mL. dilution, or \3\ MF \2\, single step p. 108 9222B \4\ ........... ........... B-0025-85 or two step. \3\ \5\ 4. Coliform (total), in MPN, 5 tube, 3 p. 114 9221B \4\ presence of chlorine, number dilution, or \3\ per 100 mL.

MF \2\ with p. 111 9222(B+B.5c) \4\ enrichment. \3\ 5. E. coli, number per 100 mL MPN \7,9,15\, ......... 9221B.1/9221F \4,12,14\ \28\. multiple tube,.

multiple tube/ ......... 9223B \4,13\ ........... 991.15 \11\ ........... Colilert multiple well, \13,17\ Colilert-18 \13,16,17\ MF \2,6,7,8,9\ two ......... 9222B/9222G \4,19\ step, or 1103.1 9213D \4\ D5392-93 \20\ \10\ single step......... 1603 \21\ 1604 \22\ ......... ....................... ........... ........... ........... mColiBue 24 \18\ 6. Fecal streptococci, number MPN, 5 tube, 3 p. 139 9230B \4\, 9230C \4\ per 100 mL. dilution, \3\ MF \2\, or.......... p. 136 ....................... ........... B-0055-85 \3\ \5\ Plate count......... p. 143 \4\ 7. Enterococci, number per MPN \7, 9\ multiple ......... 9230B \4\ 100 mL. tube.

multiple tube/ ......... ....................... D6503-99 ........... ........... Enterolert multiple well. \10\ \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.

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.

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 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 - 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 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 may be enumerated with the multiple-well procedures, Quanti-Tray or Quanti-Tray 2000, and the MPN calculated from the table provided by the manufacturer.

\16\ Colilert-18 is an optimized formulation of the Colilert for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 C rather than the 24 h required for the Colilert test and is recommended for marine water samples.

\17\ Descriptions of the Colilert , Colilert-18 , Quanti-Tray , and Quanti-Tray /2000 may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.

\18\ A description of the mColiBlue24'' test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.

\19\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.

\20\ USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC).

U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-020.

\21\ USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar ( modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington D.C. EPA-821-R-02-023.

\22\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.

Environmental Protection Agency, Office of Water, Washington DC. EPA 821-R-02-024.

\23\ A description of the Enterolert test may be obtained from IDEXX Laboratories, Inc., One IDEXX Drive, Westbrook, Maine 04092.

\24\ USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821-R-02-021.

\25\ USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl--D-Glucoside Agar (mEI). U.S.

Environmental Protection Agency, Office of Water, Washington, DC. EPA-821-R-02-022.

\26\ Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.

USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA-821- R-01-026.

\27\ Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.

Environmental Protection Agency, Office of Water, Washington DC. EPA-821-R-01-025.

\28\ Recommended for enumeration of target organism in ambient water only.

\29\ USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition.

U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/012.

\30\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/013.

\31\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms.

Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington DC. EPA/821/R-02/014.

Table IB_List of Approved Inorganic Test Procedures ------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------ Reference (method number or page) Parameter, units and method -------------------------------------------------------------------------------------------------------------------------------------------------------------- EPA 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: 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-3562-85 410.3.........................

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\................

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 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\ 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)...................

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\.................

47. Palladium_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration, or..... 253.1......................... 3111 B [18th, 19th]........... .............................. .............................. p. S27 \10\ AA furnace................... 253.2......................... .............................. .............................. .............................. p. S28 \10\ DCP.......................... .............................. .............................. .............................. .............................. Note 34.

48. Phenols, mg/L: Manual distillation \26\..... 420.1......................... .............................. .............................. .............................. Note 27.

Followed by:.................

Colorimetric (4AAP) 420.1......................... .............................. .............................. .............................. Note 27.

manual, or.

Automated \19\........... 420.2.........................

49. Phosphorus (elemental), mg/L: Gas-liquid chromatography.... .............................. .............................. .............................. .............................. Note 28.

50. Phosphorus_Total, mg/L: Persulfate digestion followed 365.2......................... 4500-P B, 5 [18th, 19th, 20th] .............................. .............................. 973.55 \3\ by.

Manual or.................... 365.2 or 365.3................ 4500-P E [18th, 19th, 20th]... D515-88(A) Automated ascorbic acid 365.1......................... 4500-P F [18th, 19th, 20th]... .............................. I-4600-85..................... 973.56 \3\ reduction.

Semi-automated block digestor 365.4......................... .............................. D515-88(B).................... I-4610-91 \48\................

51. Platinum_Total,\4\ mg/L: Digestion \4\ followed by: AA direct aspiration......... 255.1......................... 3111 B [18th, 19th]...........

AA furnace................... 255.2.........................

DCP.......................... .............................. .............................. .............................. .............................. Note 34 52. Potassium_Total,\4\ mg/L: Digestion \4\ followed by: AA direct aspiration......... 258.1......................... 3111 B [18th, 19th]........... .............................. I-3630-85..................... 973.53 \3\ ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....

Flame photometric, or........ .............................. 3500-K B [20th] and 3500-K D [18th, 19th].

Colorimetric................. .............................. .............................. .............................. .............................. 317 B \17\ 53. Residue_Total, mg/L: Gravimetric, 103-105.... 160.3......................... 2540 B [18th, 19th, 20th]..... .............................. I-3750-85.....................

54. Residue_filterable, mg/L: Gravimetric, 180........ 160.1......................... 2540 C [18th, 19th, 20th]..... .............................. I-1750-85.....................

55. Residue_nonfilterable (TSS), mg/L: Gravimetric, 103-105 160.2......................... 2540 D [18th, 19th, 20th]..... .............................. I-3765-85.....................

post washing of residue.

56. Residue_settleable, mg/L: Volumetric, (Imhoff cone), or 160.5......................... 2540 F [18th, 19th, 20th].....

gravimetric.

57. Residue_Volatile, mg/L: Gravimetric, 550........ 160.4......................... .............................. .............................. I-3753-85.....................

58. Rhodium-Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration, or..... 265.1......................... 3111 B [18th, 19th]...........

AA furnace................... 265.2.........................

59. Ruthenium_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration, or..... 267.1......................... 3111 B [18th, 19th]...........

AA furnace................... 267.2.........................

60. Selenium_Total,\4\ mg/L; Digestion \4\ followed by: AA furnace................... 270.2......................... 3113 B [18th, 19th]........... D3859-98(B)................... I-4668-98 \49\................

ICP/AES,\36\ or.............. 200.7 \5\..................... 3120 B [18th, 19th, 20th].....

AA gaseous hydride........... .............................. 3114 B [18th, 19th]........... D3859-98(A)................... I-3667-85.....................

61. Silica \37\_Dissolved, mg/L; 0.45 micron filtration followed by: Colorimetric, Manual or...... 370.1......................... 4500-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 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].

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, C: Thermometric................. 170.1......................... 2550 B [18th, 19th, 20th]..... .............................. .............................. Note 32.

70. Thallium_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration......... 279.1......................... 3111 B [18th, 19th]...........

AA furnace................... 279.2.........................

ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th].....

71. Tin_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration......... 282.1......................... 3111 B [18th, 19th]........... .............................. I-3850-78 \8\.................

AA furnace, or............... 282.2......................... 3113 B [18th, 19th]...........

ICP/AES...................... 200.7 \5\.....................

72. Titanium_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration......... 283.1......................... 3111 D [18th, 19th]...........

AA furnace................... 283.2.........................

DCP.......................... .............................. .............................. .............................. .............................. Note 34.

73. Turbidity, NTU: Nephelometric................ 180.1......................... 2130 B [18th, 19th, 20th]..... D1889-94(A)................... I-3860-85.....................

74. Vanadium_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration......... 286.1......................... 3111 D [18th, 19th]...........

AA furnace................... 286.2......................... .............................. D3373-93......................

ICP/AES...................... 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................

DCP, or...................... .............................. .............................. D4190-94...................... .............................. Note 34.

Colorimetric (Gallic Acid)... .............................. 3500-V B [20th] and 3500-V D [18th, 19th].

75. Zinc_Total,\4\ mg/L; Digestion \4\ followed by: AA direct aspiration \36\.... 289.1......................... 3111 B or C [18th, 19th]...... D1691-95(A or B).............. I-3900-85..................... 974.27,\3\ p. 37 \9\ AA furnace................... 289.2.........................

ICP/AES \36\................. 200.7 \5\..................... 3120 B [18th, 19th, 20th]..... .............................. I-4471-97 \50\................

DCP,\36\ or.................. .............................. .............................. D4190-94...................... .............................. Note 34.

Colorimetric (Dithizone) or.. .............................. 3500-Zn E [18th, 19th]........

(Zincon)..................... .............................. 3500-Zn B [20th] and 3500-Zn F .............................. .............................. Note 33.

[18th, 19th].

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------ Table 1B Notes: \1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory_Cincinnati (EMSL-CI), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.

\2\ Fishman, M.J., et al. ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, ''U.S. Department of the Interior, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.

\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' methods manual, 15th ed. (1990).

\4\ For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended material and to destroy possible organic-metal complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes, 1979 and 1983''. One (Section 4.1.3), is a vigorous digestion using nitric acid. A less vigorous digestion using nitric and hydrochloric acids (Section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types.

Particularly, if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive state. In those situations, the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing large amounts of organic materials may also benefit by this vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as well as determinations for certain elements such as antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all cases the method write-up should be consulted for specific instructions and/or cautions.

Note to Table 1B Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the above, the EPA procedure must be used.

Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the referenced procedure for total metals must be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample solution for total metals) may be omitted for AA (direct aspiration or graphite furnace) and ICP analyses, provided the sample solution to be analyzed meets the following criteria: a. has a low COD (<20) b. is visibly transparent with a turbidity measurement of 1 NTU or less c. is colorless with no perceptible odor, and d. is of one liquid phase and free of particulate or suspended matter following acidification.

\5\ The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,'' is given at Appendix C of this Part 136.

\6\ Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to resolve any controversies.

\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.

\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5, Chapter A1 (1979).

\9\ American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 25 West 43rd Street, New York, NY 10036.

\10\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater (1981).

\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.

\12\ Carbonaceous biochemical oxygen demand (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.

\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].

6. Benzene..................... 602................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th].

7. Benzidine................... ................... 625\5\, 1625B...... 605................ .................. ................. Note 3, p.1.

8. Benzo(a)anthracene.......... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

9. Benzo(a)pyrene.............. 610,............... 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

10. Benzo(b)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

11. Benzo(g, h, i)perylene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

12. Benzo(k)fluoranthene....... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

13. Benzyl chloride............ ................... ................... ................... .................. ................. Note 3, p 130: Note 6, p. S102.

14. Benzyl butyl phthalate..... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

15. Bis(2-chloroethoxy) methane 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

16. Bis(2-chloroethyl) ether... 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

17. Bis(2-ethylhexyl) phthalate 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

18. Bromodichloromethane....... 601................ 624, 1624B......... ................... 6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th].

19. Bromoform.................. 601................ 624, 1624B......... ................... 6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th].

20. Bromomethane............... 601................ 624, 1624B......... ................... 6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th].

21. 4-Bromophenylphenyl ether.. 611................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

22. Carbon tetrachloride....... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.

6230 B [18th, 19th].

23. 4-Chloro-3-methylphenol.... 604................ 625,1625B.......... ................... 6410 B, 6420 B ................. Note 9, p. 27.

[18th, 19th, 20th].

24. Chlorobenzene.............. 601, 602........... 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130.

6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th],.

25. Chloroethane............... 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

26. 2-Chloroethylvinyl ether... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

27. Chloroform:................ 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p 130.

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

28. Chloromethane.............. 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th] 6200C [20th] and 6230 B [18th, 19th].

29. 2-Chloronaphthalene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

30. 2-Chlorophenol............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.

[18th, 19th, 20th].

31. 4-Chlorophenylphenyl ether. 611................ 625, 1625B......... ................... 6410 B, [18th, ................. Note 9, p. 27.

19th, 20th].

32. Chrysene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

33. Dibenzo(a,h)anthracene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

34. Dibromochloromethane....... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th] 6200 C [20th] and 6230 B [18th, 19th].

35. 1,2-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p 27.

6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th], 6410 B [18th, 19th, 20th].

36. 1,3-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.

6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th], 6410 B [18th, 19th, 20th].

37. 1,4-Dichlorobenzene........ 601, 602, 612...... 624, 625, 1625B.... ................... 6200 C [20th] and ................. Note 9, p. 27.

6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th], 6410 B [18th, 19th, 20th].

38. 3,3-Dichlorobenzidine...... ................... 625, 1625B......... 605................ 6410 B [18th, .................

19th, 20th].

39. Dichlorodifluoromethane.... 601................ ................... ................... 6200 C [20th] and .................

6230 B [18th, 19th].

40. 1,1-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

41. 1,2-Dichloroethane......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

42. 1,1-Dichloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

43. trans-1,2-Dichloroethene... 601................ 624, 1624B......... ................... 6200 B [20th] and .................

6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

44. 2,4-Dichlorophenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.

[18th, 19th, 20th].

45. 1,2-Dichloropropane........ 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

46. cis-1,3-Dichloropropene.... 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

47. trans-1,3-Dichloropropene.. 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

48. Diethyl phthalate.......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

49. 2,4-Dimethylphenol......... 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27.

[18th, 19th, 20th].

50. Dimethyl phthalate......... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

51. Di-n-butyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

52. Di-n-octyl phthalate....... 606................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

53. 2,3-Dinitrophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6420 B [18th, 19th, 20th].

54. 2,4-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

55. 2,6-Dinitrotoluene......... 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

56. Epichlorohydrin............ ................... ................... ................... .................. ................. Note 3, p. 130; Note 6, p. S102.

57. Ethylbenzene............... 602................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th].

58. Fluoranthene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

59. Fluorene................... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

60. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B dibenzofuran.

61. 1,2,3,4,7,8,9-Heptachloro- ................... 1613B .................

dibenzofuran.

62. 1,2,3,4,6,7,8-Heptachloro- ................... 1613B .................

dibenzo-p-dioxin.

63. Hexachlorobenzene.......... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

64. Hexachlorobutadiene........ 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

65. Hexachlorocyclopentadiene.. 612................ \5\625, 1625B..... ................... 6410 [18th, 19th, ................. Note 9, p. 27.

20th].

66. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............

dibenzofuran.

67. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............

dibenzofuran.

68. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............

dibenzofuran.

69. 2,3,4,6,7,8-Hexachloro- ................... 1613B..............

dibenzofuran.

70. 1,2,3,4,7,8-Hexachloro- ................... 1613B..............

dibenzo-p-dioxin.

71. 1,2,3,6,7,8-Hexachloro- ................... 1613B..............

dibenzo-p-dioxin.

72. 1,2,3,7,8,9-Hexachloro- ................... 1613B..............

dibenzo-p-dioxin.

73. Hexachloroethane........... 616................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

74. Ideno(1,2,3-cd) pyrene..... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27.

[18th, 19th, 20th].

75. Isophorone................. 609................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27.

19th, 20th].

76. Methylene chloride......... 601................ 624, 1624B......... ................... 6200 C [20th] and ................. Note 3, p. 130.

6230 B [18th, 19th].

77. 2-Methyl-4,6-dinitrophenol. 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.

[18th, 19th, 20th].

78. Naphthalene................ 610................ 625, 1625B......... 610................ 6440 B, 6410 B ................. Note 9, p. 27.

[18th, 19th, 20th].

79. Nitrobenzene............... 609................ 625, 1625B......... ................... 6410 B [18th, D4657-92......... Note 9, p. 27.

19th, 20th].

80. 2-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27 [18th, 19th, 20th].

81. 4-Nitrophenol.............. 604................ 625, 1625B......... ................... 6410 B, 6420 B ................. Note 9, p. 27 [18th, 19th, 20th].

82. N-Nitrosodimethylamine..... 607................ 625\5\, 1625B...... ................... 6410 B [18th, ................. Note 9, p. 27 19th, 20th].

83. N-Nitrosodi-n-propylamine.. 607................ 625, 1625B......... ................... 6410 B [18th, ................. Note 9, p. 27 19th, 20th].

84. N-Nitrosodiphenylamine..... 607................ 625\5\, 1625B...... ................... 6410 B [18th, ................. Note 9, p. 27 19th, 20th].

85. Octachlorodibenzofuran..... ................... 1613B..............

86. Octachlorodibenzo-p-dioxin. ................... 1613B..............

87. 2,2'-Oxybis(2- 611................ 625, 1625B......... ................... 6410 B [18th, chloropropane) [also known as 19th, 20th].

bis(2-chloroisopropyl) ether].

88. PCB-1016................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43 19th, 20th].

89. PCB-1221................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43 19th, 20th].

90. PCB-1232................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43 19th, 20th].

91. PCB-1242................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43 19th, 20th].

92. PCB-1248................... 608................ 625................

93. PCB-1254................... 608................ 625................ ................... 6410 B [18th, ................. Note 3, p. 43 19th, 20th].

94. PCB-1260................... 608................ 625................ ................... 6410 B, 6630 B ................. Note 3, p. 43 [18th, 19th, 20th].

95. 1,2,3,7,8-Pentachloro- ................... 1613B..............

dibenzofuran.

96. 2,3,4,7,8-Pentachloro- ................... 1613B..............

dibenzofuran.

97. 1,2,3,7,8,- ................... 1613B..............

Pentachlorodibenzo-p-dioxin.

98. Pentachlorophenol.......... 604................ 625, 1625B......... ................... 6410 B, 6630 B ................. Note 3, p. 140; [18th, 19th, Note 9, p. 27 20th].

99. Phenanthrene............... 610................ 625, 1625B......... 610................ 6410 B, 6440 B D4657-92......... Note 9, p. 27 [18th, 19th, 20th].

100. Phenol.................... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27 [18th, 19th, 20th].

101. Pyrene.................... 610................ 625, 1625B......... 610................ 6440 B, 6410 B D4675-92......... Note 9, p. 27 D4675-92 [18th, 19th, 20th].

102. 2,3,7,8-Tetrachloro- ................... 1613B..............

dibenzofuran.

103. 2,3,7,8-Tetrachlorodibenzo- ................... 613, 1613B.........

p-dioxin.

104. 1,1,2,2-Tetrachloroethane. 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

105. Tetrachloroethene......... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

106. Toluene................... 602................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th].

107. 1,2,4-Trichlorobenzene.... 612................ 625, 1625B......... ................... 6410 B [18th, ................. Note 3, p. 130; 19th, 20th]. Note 9, p. 27.

108. 1,1,1-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

109. 1,1,2-Trichloroethane..... 601................ 624, 1624B......... ................... 6200 B [20th] and ................. Note 3, p. 130 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

110. Trichloroethene........... 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

111. Trichlorofluoromethane.... 601................ 624................ ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

112. 2,4,6-Trichlorophenol..... 604................ 625, 1625B......... ................... 6420 B, 6410 B ................. Note 9, p. 27.

[18th, 19th, 20th].

113. Vinyl chloride............ 601................ 624, 1624B......... ................... 6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th].

-------------------------------------------------------------------------------------------------------------------------------------------------------- Table IC notes: \1\ All parameters are expressed in micrograms per liter (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).

\7\ Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624B, and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these Methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory compliance.

Note: These warning limits are promulgated as an ``interim final action with a request for comments.'' \8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'' 3M Corporation Revised 10/28/94.

\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory_Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments'' U.S. Geological Survey, Open File Report 93-125.

Table ID_List of Approved Test Procedures for Pesticides \1\ -------------------------------------------------------------------------------------------------------------------------------------------------------- Standard Methods 18th, Parameter Method EPA 2, 7 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. -BHC.................... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 8.

GC/MS................. 625 \5\............... 6410 B................

9. -BHC..................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.

GC/MS................. 625 \5\............... 6410 B................

10. -BHC................... GC.................... 608................... 6630 C................ D3086-90.............. Note 8.

GC/MS................. 625 \5\............... 6410 B................

11. -BHC (Lindane)......... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 4, p. 27; Note 8.

GC/MS................. 625................... 6410 B................

12. Captan........................ GC.................... ...................... 6630 B................ D3086-90.............. Note 3, p. 7.

13. Carbaryl...................... TLC................... ...................... ...................... ...................... Note 3, p. 94, Note 6, p. S60.

14. Carbophenothion............... GC.................... ...................... ...................... ...................... Note 4, p. 27; Note 6, p. S73.

15. Chlordane..................... GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 4, p. 27; Note 8.

GC/MS................. 625................... 6410 B................

16. Chloropropham................. TLC................... ...................... ...................... ...................... Note 3, p. 104; Note 6, p. S64.

17. 2,4-D......................... GC.................... ...................... 6640 B................ ...................... Note 3, p. 115; Note 4, p. 40.

18. 4,4[prime]-DDD................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 4, p. 27; Note 8.

GC/MS................. 625................... 6410 B................

19. 4,4[prime]-DDE................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 4, p. 27; Note 8.

GC/MS................. 625................... 6410 B................

20. 4,4[prime]-DDT................ GC.................... 608................... 6630 B & C........ D3086-90.............. Note 3, p. 7; Note 4, p. 27; Note 8.

GC/MS................. 625................... 6410 B................

21. Demeton-O..................... GC.................... ...................... ...................... ...................... 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.

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.

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 -BHC, -BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.

\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater (1981).

\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 (See Appendix A of this Part 136) in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an 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''.

Table IF_List of Approved Methods for Pharmaceutical Pollutants ---------------------------------------------------------------------------------------------------------------- Pharmaceuticals pollutants CAS registry No. Analytical method number ---------------------------------------------------------------------------------------------------------------- acetonitrile................... 75-05-8............................ 1666/1671/D3371/D3695.

n-amyl acetate................. 628-63-7........................... 1666/D3695.

n-amyl alcohol................. 71-41-0............................ 1666/D3695 benzene........................ 71-43-2............................ D4763/D3695/502.2/524.2.

n-butyl-acetate................ 123-86-4........................... 1666/D3695.

tert-butyl alcohol............. 75-65-0............................ 1666.

chlorobenzene.................. 108-90-7........................... 502.2/524.2.

chloroform..................... 67-66-3............................ 502.2/524.2/551.

o-dichlorobenzene.............. 95-50-1............................ 1625C/502.2/524.2.

1,2-dichloroethane............. 107-06-2........................... D3695/502.2/524.2.

diethylamine................... 109-89-7........................... 1666/1671.

dimethyl sulfoxide............. 67-68-5............................ 1666/1671.

ethanol........................ 64-17-5............................ 1666/1671/D3695.

ethyl acetate.................. 141-78-6........................... 1666/D3695.

n-heptane...................... 142-82-5........................... 1666/D3695.

n-hexane....................... 110-54-3........................... 1666/D3695.

isobutyraldehyde............... 78-84-2............................ 1666/1667.

isopropanol.................... 67-63-0............................ 1666/D3695.

isopropyl acetate.............. 108-21-4........................... 1666/D3695.

isopropyl ether................ 108-20-3........................... 1666/D3695.

methanol....................... 67-56-1............................ 1666/1671/D3695.

Methyl Cellosolve ...... 109-86-4........................... 1666/1671 methylene chloride............. 75-09-2............................ 502.2/524.2 methyl formate................. 107-31-3........................... 1666.

4-methyl-2-pentanone (MIBK).... 108-10-1........................... 1624C/1666/D3695/D4763/524.2.

phenol......................... 108-95-2........................... D4763.

n-propanol..................... 71-23-8............................ 1666/1671/D3695.

2-propanone (acetone).......... 67-64-1............................ D3695/D4763/524.2.

tetrahydrofuran................ 109-99-9........................... 1666/524.2.

toluene........................ 108-88-3........................... D3695/D4763/502.2/524.2.

triethlyamine.................. 121-44-8........................... 1666/1671.

xylenes........................ (Note 1)........................... 1624C/1666.

---------------------------------------------------------------------------------------------------------------- Table 1F note: 1. 1624C: m-xylene 108-38-3, o,p-xylene E-14095 (Not a CAS number; this is the number provided in the Environmental Monitoring Methods Index (EMMI) database.); 1666: m,p-xylene 136777-61-2, o-xylene 95-47-6.

(b) The full texts of the methods from the following references which are cited in Tables IA, IB, IC, ID, IE,and IF are incorporated by reference into this regulation and may be obtained from the sources identified. All costs cited are subject to change and must be verified from the indicated sources. The full texts of all the test procedures cited are available for inspection at the National Exposure Research Laboratory, Office of Research and Development, U.S. Environmental Protection Agency, 26 West Martin Luther King Dr., Cincinnati, OH 45268 and the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 2027416030, 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 601613, 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/600/878/017.

Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB290329/AS. Cost: $36.95.

Table IA, Note 3.

(3) Methods for Chemical Analysis of Water and Wastes, U.S.

Environmental Protection Agency, EPA600/479020, March 1979, or Methods for Chemical Analysis of Water and Wastes, U.S. Environmental Protection Agency, EPA600/479020, 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, EPA600/480032, 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 TemperatureInfluential 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 7677 (1976). Available from: U.S. Geological Survey, Branch of Distribution, 1200 South Eads Street, Arlington, VA 22202.

Cost: $13.50 (subject to change). Table IE, Note 2.

(17) Official Methods of Analysis of the Association of Official Analytical Chemicals, Methods manual, 15th Edition (1990). Price: $240.00. Available from: The Association of Official Analytical Chemists, 2200 Wilson Boulevard, Suite 400, Arlington, VA 22201. Table IB, Note 3.

(18) American National Standard on Photographic Processing Effluents, April 2, 1975. Available from: American 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 37975WE, 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 9770, 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 37875WA. 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, NitriteLow 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. 421426, 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 281060200, 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 2209E10, St. Paul, MN 551441000. 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 821R02012. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002108488. 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 EPA821R02013. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002108489. 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 EPA821R02014. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002108490. 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 821B98016). 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, EPA600/488039, December 1988, Revised, July 1991, and Methods for the Determination of Organic Compounds in Drinking Water-Supplement II, EPA600/R92129, August 1992, respectively. These EPA test method compendia are available from the National Technical Information Service, NTIS PB91231480 and PB92207703, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll-free number is 8005536847. ASTM test methods D3371, D3695, and D4763 are available from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 194282959.

(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 (EPA821R02019). Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.

Publication No. PB2002108220. Cost: $25.50 (subject to change).

(42) [Reserved] (43) Method OIA1677, Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry. August 1999. ALPKEM, OI Analytical, Box 648, Wilsonville, Oregon 97070 (EPA821R99013). Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161. Publication No. PB99132011. 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) 00170.

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 LaboratoryDetermination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry, Open File Report (OFR) 93449.

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 LaboratoryDetermination of Molybdenum in Water by Graphite Furnace Atomic Absorption Spectrophotometry, Open File Report (OFR) 97198.

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 LaboratoryDetermination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis Open File Report (OFR) 92146. 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 LaboratoryDetermination of Arsenic and Selenium in Water and Sediment by Graphite FurnaceAtomic Absorption Spectrometry Open File Report (OFR) 98639. Table IB, Note 49.

(49) Methods of Analysis by the U.S. Geological Survey National Water Quality LaboratoryDetermination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry , Open File Report (OFR) 98165.

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 LaboratoryDetermination of Triazine and Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors U.S.Geological Survey Open File Report 9437.

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 LaboratoryDetermination of Inorganic and Organic Constituents in Water and Fluvial Sediments, Open File Report (OFR) 93125. 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, Colilert-18, Quanti-Tray, Quanti-Tray/2000, Enterolert 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 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, EPA821R02020. Available at NTIS, PB2003100125.

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, EPA821R02021. Available at NTIS, PB2003100126. 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, EPA821R02023. Available at NTIS, PB2003100128. 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.

59:35343544. 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 821R02024. Available from NTIS, PB2003100129. Table IA, Note 22.

(59) USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration using membrane-Enterococcus Indoxyl--D-Glucoside Agar (mEI).

U.S. Environmental Protection Agency, Office of Water, Washington D.C.

September 2002, EPA821R02022. Available from NTIS, PB2003100127. 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, EPA821R01026.

Available from NTIS, PB2002108709. 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, EPA821R01025. Available from NTIS, PB2002108710. 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 LaboratoryCincinnati.

(d) Under certain circumstances, the Administrator may approve, upon recommendation by the Director, Environmental Monitoring Systems LaboratoryCincinnati, 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 LaboratoryCincinnati, 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 C, 0.0008% 6 hours.

and E. coli. Na2S2O35.

6 Fecal streptococci.......... PP, G........... Cool, <10 0.0008% 6 hours.

Na2S2O35.

7 Enterococci................. PP, G........... Cool, <10 0.0008% 6 hours.

Na2S2O35.

Table IA_Protozoa Tests: 8 Cryptosporidium............. LDPE............ 0-8 C...................... 96 hours. \17\ 9 Giardia..................... LDPE............ 0-8 C...................... 96 hours. \17\ Table IA_Aquatic Toxicity Tests: 6-10 Toxicity, acute and P,G............. Cool, 4 C 16............... 36 hours.

chronic.

Table IB_Inorganic Tests: 1. Acidity.................... P, G............ Cool, 4C................... 14 days.

2. Alkalinity................. P, G............ ......do........................ Do.

4. Ammonia.................... P, G............ Cool, 4C, H2SO4 to pH<2. 28 days.

9. Biochemical oxygen demand.. P, G............ Cool, 4C................... 48 hours.

10. Boron..................... P, PFTE, or HNO3 TO pH<2................. 6 months.

Quartz.

11. Bromide................... P, G............ None required................... 28 days.

14. Biochemical oxygen demand, P, G............ Cool, 4C................... 48 hours.

carbonaceous.

15. Chemical oxygen demand.... P, G............ Cool, 4C, H2SO4 to pH<2. 28 days.

16. Chloride.................. P, G............ None required................... Do.

17. Chlorine, total residual.. P, G............ ......do........................ Analyze immediately.

21. Color..................... P, G............ Cool, 4C................... 48 hours.

23-24. Cyanide, total and P, G............ Cool, 4C, NaOH to pH>12, 14 days.6 amenable to chlorination. 0.6g ascorbic acid 5.

25. Fluoride.................. P............... None required................... 28 days.

27. Hardness.................. P, G............ HNO3 to pH<2, H2SO4 to 6 months.

pH<2.

28. Hydrogen ion (pH)......... P, G............ None required................... Analyze immediately.

31, 43. Kjeldahl and organic P, G............ Cool, 4C, H2SO4 to pH<2. 28 days.

nitrogen.

Metals:7 18. Chromium VI \7\........... P, G............ Cool, 4 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, 4C................... 48 hours.

39. Nitrate-nitrite........... P, G............ Cool, 4C, H2SO4 to pH<2. 28 days.

40. Nitrite................... P, G............ Cool, 4C................... 48 hours.

41. Oil and grease............ G............... Cool to 4C, HCl or H2SO4 to 28 days.

pH<2.

42. Organic Carbon............ P, G............ Cool to 4 C HC1 or H2SO4 or 28 days.

H3PO4, to pH<2.

44. Orthophosphate............ P, G............ Filter immediately, Cool, 48 hours.

4C.

46. Oxygen, Dissolved Probe... G Bottle and top None required................... Analyze immediately.

47. Winkler................... ......do........ Fix on site and store in dark... 8 hours.

48. Phenols................... G only.......... Cool, 4C, H2SO4 to pH<2. 28 days.

49. Phosphorus (elemental).... G............... Cool, 4C................... 48 hours.

50. Phosphorus, total......... P, G............ Cool, 4C, H2SO4 to pH<2. 28 days.

53. Residue, total............ P, G............ Cool, 4C................... 7 days.

54. Residue, Filterable....... P, G............ ......do........................ 7 days.

55. Residue, Nonfilterable P, G............ ......do........................ 7 days.

(TSS).

56. Residue, Settleable....... P, G............ ......do........................ 48 hours.

57. Residue, volatile......... P, G............ ......do........................ 7 days.

61. Silica.................... P, PFTE, or Cool, 4 C.................. 28 days.

Quartz.

64. Specific conductance...... P, G............ ......do........................ Do.

65. Sulfate................... P, G............ ......do........................ Do.

66. Sulfide................... P, G............ Cool, 4C add zinc acetate 7 days.

plus sodium hydroxide to pH>9.

67. Sulfite................... P, G............ None required................... Analyze immediately.

68. Surfactants............... P ,G............ Cool, 4C................... 48 hours.

69. Temperature............... P, G............ None required................... Analyze.

73. Turbidity................. P, G............ Cool, 4C................... 48 hours.

Table IC_Organic Tests \8\ 13, 18-20, 22, 24-28, 34-37, G, Teflon-lined Cool, 4 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 C, 0.008% Do.

hydrocarbons. Na2S2O3,\5\ HCl to pH2\9\.

3, 4. Acrolein and ......do........ Cool, 4 C, 0.008% Do.

acrylonitrile. Na2S2O3,\5\ adjust pH to 4-510.

23, 30, 44, 49, 53, 77, 80, G, Teflon-lined Cool, 4 C, 0.008% Na2S2O3 7 days until extraction; 81, 98, 100, 112. Phenols 11. cap.. \5\. 40 days after extraction.

7, 38. Benzidines 11.......... ......do........ ......do........................ 7 days until extraction.13 14, 17, 48, 50-52. Phthalate ......do........ Cool, 4 C.................. 7 days until extraction; esters 11. 40 days after extraction.

82-84. Nitrosamines 11 14..... ......do........ Cool, 4 C, 0.008% Do.

Na2S2O3,\5\ store in dark.

88-94. PCBs 11................ .....do......... Cool, 4 C.................. Do.

54, 55, 75, 79. Nitroaromatics ......do........ Cool, 4 C, 0.008% Do.

and isophorone 11. Na2S2O3,\5\ store in dark.

1, 2, 5, 8-12, 32, 33, 58, 59, ......do........ ......do........................ Do.

74, 78, 99, 101. Polynuclear aromatic hydrocarbons 11.

15, 16, 21, 31, 87. Haloethers ......do........ Cool, 4 C, 0.008% Na2S2O3 Do.

11. \5\.

29, 35-37, 63-65, 73, 107. ......do........ Cool, 4 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 C, pH<9, 1 year.

preservation.. 0.008% Na2S2O3 \5\.

Solids, mixed phase, and ......do........ Cool, <4 C.............. 7 days.

tissue: field preservation..

Solids, mixed phase, and ......do........ Freeze, <-10 C.......... 1 year.

tissue: lab preservation.

Table ID_Pesticides Tests: 1-70. Pesticides \11\......... ......do........ Cool, 4C, pH 5-9 15........ Do.

Table IE_Radiological Tests: 1-5. Alpha, beta and radium... P, G............ HNO3 to pH<2................. 6 months.

---------------------------------------------------------------------------------------------------------------- Table II Notes \1\ Polyethylene (P) or glass (G). For microbiology, plastic sample containers must be made of sterilizable materials (polypropylene or other autoclavable plastic).

2 Sample preservation should be performed immediately upon sample collection. For composite chemical samples each aliquot should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4C until compositing and sample splitting is completed.

3 When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply with the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less).

\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 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 136.3(e) for details. The term ``analyze immediately'' usually means within 15 minutes or less of sample collection.

5 Should only be used in the presence of residual chlorine.

6 Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is filtered and then NaOH is added to pH 12.

7 Samples should be filtered immediately on-site before adding preservative for dissolved metals.

8 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.

9 Sample receiving no pH adjustment must be analyzed within seven days of sampling.

10 The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.

11 When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to 4C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (re the requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of benzidine).

12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 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.

[38 FR 28758, Oct. 16, 1973, as amended at 41 FR 52781, Dec. 1, 1976; 49 FR 43251, 43258, 43259, Oct. 26, 1984; 50 FR 691, 692, 695, Jan. 4, 1985; 51 FR 23693, June 30, 1986; 52 FR 33543, Sept. 3, 1987; 55 FR 24534, June 15, 1990; 55 FR 33440, Aug. 15, 1990; 56 FR 50759, Oct. 8, 1991; 57 FR 41833, Sept. 11, 1992; 58 FR 4505, Jan. 31, 1994; 60 FR 17160, Apr. 4, 1995; 60 FR 39588, 39590, Aug. 2, 1995; 60 FR 44672, Aug.

28, 1995; 60 FR 53542, 53543, Oct. 16, 1995; 62 FR 48403, 48404, Sept.

15, 1997; 63 FR 50423, Sept. 21, 1998; 64 FR 4978, Feb. 2, 1999; 64 FR 10392, Mar. 4, 1999; 64 FR 26327, May 14, 1999; 64 FR 30433, 30434, June 8, 1999; 64 FR 73423, Dec. 30, 1999; 66 FR 32776, June 18, 2001; 67 FR 65226, Oct. 23, 2002; 67 FR 65886, Oct. 29, 2002; 67 FR 69971, Nov. 19, 2002; 68 FR 43278, July 21, 2003; 68 FR 54934, Sept. 19, 2003; 69 FR 18803, Apr. 9, 2004]