Wisconsin Administrative Code
Department of Natural Resources
NR 200-299 - Environmental Protection - Wisconsin Pollutant Discharge Elimination System
Chapter NR 219 - Analytical Test Methods And Procedures
Section NR 219.04 - Identification of test procedures

Universal Citation: WI Admin Code § NR 219.04

Current through August 26, 2024

(1) ANALYTICAL TEST PROCEDURES. Parameters or pollutants, for which wastewater analytical methods are approved, are listed together with test procedure descriptions and references in tables A to H. Parameters or pollutants, for which sludge analytical methods are approved, are listed together with test procedure descriptions and references in table EM. The discharge values for the listed parameters shall be determined by one of the standard analytical test procedures identified in a table under this subsection or by an alternate test procedure established under ss. NR 219.033 and 149.42.

Note: The laboratory performing the analyses on any samples will be certified for the applicable PFAS compounds in aqueous, sludge (biosolids), and tissue matrices in accordance with s. NR 149.41 by the Wisconsin Laboratory Certification Program established under s. 299.11, Stats. If the EPA Office of Water publishes a final approved 1600 series isotope dilution method for the analysis of PFAS in aqueous, sludge (biosolids), and tissue matrices, the department recommends use of the final approved EPA method.

(2) SAMPLE PRESERVATION PROCEDURES. Sample preservation techniques, container materials, and maximum allowable holding times for parameters identified in tables A to H are prescribed in table F. Sludge samples shall be preserved at the time of collection by cooling to less than or equal to 6°C where required. All samples requiring thermal preservation at less than or equal to 6°C shall be cooled immediately after collection, and the required temperature maintained during shipping. Any person may apply for a variance from the prescribed preservation procedures applicable to samples taken from a specific discharge. Applications for variances may be made by letters to the regional administrator and shall provide sufficient data to assure that the variance does not adversely affect the integrity of the sample. The regional administrator will make a decision on whether to approve or deny a variance within 90 days of receipt of the application.

(3) TEMPERATURE REPORTING PROCEDURES. Samples cooled with ice packs or not in direct contact with ice during shipping shall be cooled to less than or equal to 6° C prior to shipping, and a temperature blank shall be submitted with the samples. Samples cooled during shipping with ice packs may not be recorded as received on ice. Samples may be recorded as received on ice only if solid ice is present in the cooler at the time the samples are received. If the samples are not received on ice, the laboratory shall record one of the following at the time of receipt:

(a) The temperature of an actual sample.

(b) The temperature of a temperature blank shipped with the samples.

(4) INCORPORATION BY REFERENCE. The materials in this section are incorporated by reference for the purposes of the permit program under ch. 283, Stats.

Table A

List of Approved Biological Methods for Wastewater and Sewage Sludge

Parameter and units	Analytical Technology 1	EPA	Standard Methods 25,26	AOAC, ASTM, USGS	Other
Bacteria
1. Coliform (fecal), number per 100 mL or number per gram dry weight	Most Probable Number (MPN), 5 tube, 3 dilution, or	p. 1323 168011,15 168111,20	9221 E-2014
Membrane filter (MF),2,5 single step	p. 1243	9222 D-201529	B-0050-854
2. Coliform (fecal), number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1323	9221 E-2014; 9221 F.2-201433
Multiple tube/multiple well, or	Colilert-18®13,18,28
MF,2,5 single step5	p. 1243	9222 D-201529
3. Coliform (total), number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1143	9221 B-2014
MF,2,5 single step or two step	p. 1083	9222 B-201530	B-0025-854
MF2,5 with enrichment	p. 1113	9222 (B+B.4e) -201530
4. E. coli, number per 100 mL	MPN6,8,16 multiple tube, or	9221 B.3-2014/9221 F-201412,14,33
Multiple tube/multiple well, or	9223 B-201613	991.1510	Colilert®13,18 Colilert-18®13,17,18
MF,2,5,6,7,8 two step, or	9222 B-2015/ 9222 I-201531
Single step	160321	m-ColiBlue24®19
5. Fecal streptococci, number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1393	9230 B-2013
MF2, or	p. 1363	9230 C-201332	B-0055-854
Plate count	p. 1433
6. Enterococci, number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1393	9230 B-2013
MPN,6,8 multiple tube/multiple well, or	9230 D-2013	D6503-999	Enterolert®13,23
MF2,5,6,7,8 single step or	160024	9230 C-201332
Plate count	p. 1433
7. Salmonella number per gram dry weight11	MPN multiple tube	168222
Aquatic Toxicity
8. Toxicity, acute, fresh water organisms, percent effluent	Daphnia, Ceriodaphnia dubia, 48-h static-renewal mortality	Note 27
Fathead Minnow, Pimephales promelas, 96-h static-renewal mortality, or 96-h flow-through mortality	Note 27
9. Toxicity, chronic, fresh water organisms, percent effluent	Daphnia, Ceriodaphnia dubia, survival and reproduction	Note 27
Fathead Minnow, Pimephales promelas, larval survival and growth	Note 27

1 The method must be specified when results are reported.

2 A 0.45-µm 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 Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. U.S. EPA.

4 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. 1989. USGS.

5 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.

6 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.

7 When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.

8 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.

9 Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.

10 Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.

11 Recommended for enumeration of target organism in sewage sludge.

12 The multiple-tube fermentation test is used in 9221B.2-2014. 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.

14 After prior enrichment in a presumptive medium for total coliform using 9221B.2-2014, 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-2014. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 µg/mL of MUG may be used.

15 Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-14-009. September 2014. U.S. EPA.

16 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®, Quanti-Tray®/2000 and the MPN calculated from the table provided by the manufacturer.

17 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.

18 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc.

19 A description of the mColiBlue24® test, is available from Hach Company.

20 Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.

21 Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.

22 Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014. U.S. EPA.

23 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc.

24 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-ÃŽ²-D-Glucoside Agar (mEI), EPA-821-R-14-011. September 2014. U.S. EPA.

25 Standard Methods for the Examination of Water and Wastewater, Joint Editorial Board, American Public Health Association, American Water Works Association, and Water Pollution Control Federation, 23rd Edition (2017), 22nd Edition (2012), 21st Edition (2005), 20th Edition (1998), 19th Edition (1995), and 18th Edition (1992).

26 Standard Methods for the Analysis of Water and Wastewater. With the promulgation of Federal Register /Vol. 77, No. 97 / Friday, May 18, 2012, the EPA lists only the most recently EPA-approved version of a Standard Method (regardless of the printed or online edition) in 40 CFR Part 136, with few exceptions, to identify the method with the year of Standard Methods approval or adoption designated by the last four digits in the method number (e.g., Standard Method 3113B-2004). This approach clearly identifies the version of the standard method approved under Part 136 and no longer ties it to a particular compendium printing or edition of Standard Methods. Methods can be purchased at www.standardmethods.org.

27 Compliance monitoring must be performed in accordance with the specifications in the "State of Wisconsin Aquatic Life Toxicity Testing Methods Manual, 2nd Edition," Wisconsin Department of Natural Resources, 2004. This publication is available for inspection at the offices of the Department of Natural Resources and the Legislative Reference Bureau. Copies are available from the Department of Natural Resources, Bureau of Science Services, P.O. Box 7921, Madison, WI 53707.

28 To use Colilert-18® to assay for fecal coliforms, the incubation temperature is 44.5 ± 0.2 °C, and a water bath incubator is used.

29 On a monthly basis, at least ten blue colonies from positive samples must be verified using lauryl tryptose broth and EC broth, followed by count adjustment based on these results; and representative non-blue colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources.

30 On a monthly basis, at least ten sheen colonies from positive samples must be verified using lauryl tryptose broth and brilliant green lactose bile broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources.

31 Subject coliform positive samples determined by 9222 B-2015 or other membrane filter procedure to 9222 I-2015 using NA-MUG media.

32 Verification of colonies by incubation of BHI agar at 10 ± 0.5 °C for 48 ± 3 h is optional. As per the Errata to the 23rd Edition of Standard Methods for the Examination of Water and Wastewater, "Growth on a BHI agar plate incubated at 10 ± 0.5 °C for 48 ± 3 h is further verification that the colony belongs to the genus Enterococcus."

33 9221 F. 2-2014: This procedure allows for simultaneous detection of E. coli and thermotolerant coliforms by adding inverted vials to EC-MUG; the inverted vials collect gas produced by thermotolerant coliforms.

Table B

List of Approved Inorganic Test Procedures For Wastewater

Parameter, Units	Analytical Technology 58	EPA 52	Standard methods	ASTM	USGS AOAC Other
1. Acidity, as CaCO3, mg/L	Electrometric endpoint or phenolphthalein endpoint	2310 B-1997	D1067-06	I-1020-85 2
2. Alkalinity, as CaCO3, mg/L	Electrometric or Colorimetric titration to pH 4.5, Manual	2320 B-1997	D1067-06	I-1030-85 2 973.43 3
Automatic	310.2 (Rev. 1974)1	I-2030-85 2
3. Aluminum-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 D-1999 or 3111 E-1999	I-3051-85 2
Graphite furnace AA (GFAA)	3113 B-2004
Stabilized temperature graphite furnace AA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP-AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Colorimetric (Eriochrome cyanine R)	3500-Al B-2001
4. Ammonia (as N), mg/L	Manual distillation 6or gas diffusion (pH > 11), followed by any of the following:	350.1, Rev. 2.0 (1993)	4500-NH3B-1997	973.49 3
Titration	4500-NH3C-1997
Electrode	4500-NH3D-1997 or E-1997	D1426-08 (B)
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods	4500-NH3F-1997	Note 60
Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods	350.1, 30 Rev. 2.0 (1993)	4500-NH3G-1997 4500-NH3H-1997.	I-4523-85 2
Automated electrode	Note 7
Ion Chromatography	D6919-09
5. Anti-mony-Total,4 mg/ L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999
Graphite furnace AA (GFAA)	3113 B-2004
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma- mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
6. Arsenic-Total,4mg/L	Digestion,4 followed by any of the following:	206.5 (Issued 1978) 1
AA gaseous hydride	3114 B-2009 or 3114 C-2009	D2972-08 (B)	I-3062-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D2972-08 (C)	I-4063-98 49
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Colorimetric (SDDC)	3500-As B-1997	D2972-08 (A)	I-3060-85 2
7. Barium-Total,4mg/L	Digestion4, followed by any of the following:
AA direct aspiration (FLAA) 36	3111 D-1999	I-3084-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D4382-02(07)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003) 68; 200.7, Rev. 4.4 (1994)	3120 B-1999	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct Current Plasma (DCP) 36	Note 34
8. Beryl-lium-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 D-1999 or 3111 E-1999	D3645-08 (A)	I-3095-85.2
Graphite furnace AA (GFAA)	3113 B-2004	D3645-08 (B)
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasmamass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct current plasma (DCP)	D4190-08	Note 34
Colorimetric (Aluminon)	Note 61
9. Biochemical oxygen demand (BOD5), mg/L	Dissolved Oxygen Depletion	5210 B-2001	973.44, 3 p. 17, 9 I-1578-78 8 Notes 10,63
10. Boron-Total,37mg/L	Colorimetric (Curcumin)	4500-B B-2000	I-3112-85 2
Inductively coupled plasmaatomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasmamass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct current plasma (DCP)	D4190-08	Note 34
11. Bromide, mg/L	Titrimetric	I-1125-85 2
Ion selective electrode (ISE)	D1246-05
Ion Chromatography	300.0, Rev 2.1 (1993) 300.1-1, Rev 1.0 (1997)	4110 B-2000, C-2000, D-2000	D4327-03	993.30 3
CIE/UV	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
12. Cadmium-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999	D3557-02(07) (A or B)	974.27, 3 p. 37, 9 I-3135-85 2 or I-3136-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D3557-02(07) (D)	I-4138-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-1472-85 2 or I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Voltametry 11	D3557-02(07) (C)
Colorimetric (Dithizone)	3500-Cd-D-1990
13. Calcium-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999	D511-08(B)	I-3152-85 2
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Direct current plasma (DCP)	Note 34
Titrimetric (EDTA)	3500-Ca B-1997	D511-08 (A)
Ion Chromatography	D6919-09
14. Carbonaceous biochemical oxygen demand (CBOD5), mg/L12	Dissolved Oxygen Depletion with nitrification inhibitor	5210 B-2001	Note 35,63
15. Chemical oxygen demand (COD), mg/L	Titrimetric	410.3 (Rev. 1978)1	5220 B-1997 or C-1997	D1252-06 (A)	I-3560-85, 2 973.46, 3 p. 17 9
Spectrophotometric, manual or automatic	410.4, Rev. 2.0 (1993)	5220 D-1997	D1252-06 (B)	Note 13,14 I-3561-85.2
16. Chloride, mg/L	Titrimetric: (silver nitrate)	4500-Cl-B-1997	D512-04 (B)	I-1183-85 2
Colorimetric: manual	I-1187-85 2
Colorimetric, Automated (Ferricyanide)	4500-Cl-E-1997	I-2187-85 2
Potentiometric Titration	4500-Cl-D-1997
Ion Selective Electrode	D512-04 (C)
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or 4110 C-2000	D4327-03	993.30, 3 I-2057-90 51
Capillary ion electrophoresis (CIE/UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
17. Chlorine-Total residual, mg/L	Amperometric direct	4500-Cl D-2000	D1253-08
Amperometric direct (low level)	4500-Cl E-2000
Iodometric direct	4500-Cl B-2000
Back titration ether end-point15	4500-Cl C-2000
Colorimetric, DPD-FAS	4500-Cl F-2000
Spectrophotometric, DPD	4500-Cl G-2000
Ion selective electrode (ISE)	Note 16
17A. Chlorine-Free Available, mg/L	Amperometric direct	4500-Cl D-2000	D1253-08
Amperometric direct (low level)	4500-Cl E-2000
DPD-FAS	4500-Cl F-2000
Spectrophotometric, DPD	4500-Cl G-2000
18. Chromium VI dissolved, mg/L	0.45-micron Filtration followed by any of the following:
AA chelation-extraction	3111 C-1999	I-1232-85 2
Ion Chromatography	218.6, Rev. 3.3 (1994)	3500-Cr C-2009	D5257-03	993.23
Colorimetric (Diphenyl-carbazide)	3500-Cr B-2009	D1687-02(07) (A)	I-1230-85 2
19. Chromium-Total, 4mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999	D1687-02(07) (B)	974.27,3 I-3236-85 2
AA chelation-extraction	3111 C-1999
Graphite furnace AA (GFAA)	3113 B-2004	D1687-02(07) (C)	I-3233-93 46
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003),68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Colorimetric (Diphenyl-carbazide)	3500-Cr B-2009
20. Cobalt-Total,4mg /L	Digestion,4followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999 or 3111 C-1999	D3558-08 (A or B)	p. 37,9 I-3239-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D3558-08 (C)	I-4243-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Direct current plasma (DCP)	D4190-08	Note 34
21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity	Colorimetric (ADMI)	Note 18
Colorimetric (Platinum cobalt)	2120 B-2001	I-1250-85 2
22. Copper-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999	D1688-07 (A or B)	974.27,3 p. 37,9 I-3270-85 2 or I-3271-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D1688-07 (C)	I-4274-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Colorimetric (Neocuproine)	3500-Cu B-1999
Colorimetric (Bathocuproine)	3500-Cu C-1999	Note 19
23. Cyanide-Total, mg/L	Automated UV digestion/distillation and Colorimetry	Kelada-01.55
Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometry	D7511-09
Manual distillation with MgCl2, followed by any of the following:	335.4, Rev. 1.0 (1993) 57	4500-CN-B-1999 or C-1999	D2036-09(A), D7284-08	10-204-00-1-X 56
Flow Injection, gas diffusion amperometry	D2036-09(A) D7284-08
Titrimetric	4500-CN-D-1999	D2036-09(A)	p. 22 9
Colorimetry; Spectrophotometric, manual	4500-CN-E-1999	D2036-09(A)	I-3300-85 2
Colorimetry; Semi-Automated 20	335.4, Rev. 1.0 (1993) 57	10-204-00-1-X,56 I-4302-85 2
Ion Chromatography	D2036-09(A)
Ion Selective Electrode	4500-CN-F-1999	D2036-09(A)
24. Cyanide-Available, mg/L	Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl2, followed by Titrimetric or Spectrophotometric	4500-CN-G-1999	D2036-09(B)
Flow injection and ligand exchange, followed by gas diffusion amperometry 59	D6888-09	OIA-1677-09 44
Automated Distillation and Colorimetry (no UV digestion)	Kelada-01 55
24. A Cyanide-Free, mg/L	Flow Injection, followed by gas diffusion amperometry	D7237-10	OIA-1677-09 44
Manual micro-diffusion and colorimetry	D4282-02
25. Fluoride-Total, mg/L	Manual distillation,6 followed by any of the following:	4500-F-B-1997
Electrode, manual (ISE)	4500-F-C-1997	D1179-04 (B)
Electrode, automated (ISE)	I-4327-85 2
Colorimetric, (SPADNS)	4500-F-D-1997	D1179-04 (A)
Automated complexone	4500-F-E-1997
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30 3
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
26. Gold-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999
Graphite furnace AA (GFAA)	231.2 (Issued 1978)1	3113 B-2004
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Direct current plasma (DCP)	Note 34
27. Hardness-Total, as CaCO3, mg/L	Automated colorimetric	130.1 (Issued 1971)1
Titrimetric (EDTA)	2340 C-1997	D1126-02(07)	973.52B,3 I-1338-85 2
Ca plus Mg as their carbonates, by inductively coupled plasma or AA direct aspiration. (See Parameters 13 and 33).	2340 B-1997
28. Hydrogen ion (pH), pH units	Electrometric measurement	4500-norg-B-20 00	D1293-99 (A or B)	973.41,3 I-1586-85 2
Automated electrode	150.2 (Dec. 1982)1	See footnote,21 I-2587-85 2
29. Iridium-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999
Graphite furnace AA (GFAA)	235.2 (Issued 1978)1
Inductively coupled plasma-mass spectrometry (ICP/MS)	3125 B-2009
30. Iron-Total,4 mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999	D1068-05 (A or B)	974.27,3 I-3381-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D1068-05 (C)
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003) 68; 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14.3
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Colorimetric (Phenanthroline)	3500-Fe B-1997	D1068-05 (D)	Note 22
31. Kjeldahl Nitrogen 5-Total, (as N), mg/L	Manual digestion 20 and distillation or gas diffusion, followed by any of the following:	4500-Norg-B-1997 or C-1997 and 4500-NH3B-1997	D3590-02(06) (A)	I-4515-91 45
Titration	4500-NH3C-1997	973.48 3
Electrode	4500-NH3D-1997 or E-1997	D1426-08 (B)
Semi-automated phenate	350.1 Rev 2.0 1993	4500-NH3G-1997, 4500-NH3 H-1997
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods	4500-NH3F-1 997	Note 60
Automated Methods for TKN that do not require manual distillation
Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation)	351.1 (Rev. 1978)1	I-4551-78.8
Semi-automated block digestor colorimetric (distillation not required)	351.2, Rev. 2.0 (1993)	4500-Norg-D-1997	D3590-02(06) (B)	I-4515-91 45
Block digester, followed by Auto distillation and Titration	Note 39
Block Digester, followed by Flow injection gas diffusion (distillation not required)	Note 41
32. Lead-Total,4mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999.	D3559-08 (A or B)	974.27,3 I-3399-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D3559-08 (D)	I-4403-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Voltametry11	D3559-08 (C)
Colorimetric (Dithizone)	3500-Pb B-1997
33. Magnesium-Total,4 mg/ L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999	D511-08 (B)	974.27,3 I-3447-85 2
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Direct current plasma (DCP)	Note 34
Ion Chromatography	D6919-09
34. Manganese-Total 4, mg/L	Digestion 4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999	D858-07 (A or B)	974.27,3 I-3454-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D858-07 (C)
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct Current Plasma (DCP) 36	D4190-08	Note 34
Colorimetric (Persulfate)	3500-Mn B-1999	920.203 3
Colorimetric (Periodate)	Note 23
35. Mercury-Total,4 mg/L	Cold vapor, Manual	245.1, Rev. 3.0 (1994)	3112 B-2009	D3223-02(07)	977.22,3 I-3462-85 2
Cold vapor, Automated	245.2 (Issued 1974)1
Cold vapor atomic fluorescence spectrometry (CVAFS)	245.7 Rev. 2.0 (2005)17	I-4464-01 71
Purge and Trap CVAFS	1631E43
36. Molybdenum-Total,4mg/L	Digestion,4 followed by any of the following:
AA direct aspiration (FLAA)	3111 D-1999	I-3490-85 2
Graphite furnace AA (GFAA)	3113 B-2004	I-3492-96 47
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4471-97 50
Direct current plasma (DCP)	Note 34
37. Nickel-Total,4mg /L	Digestion 4 followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999	D1886-08 (A or B)	I-3499-85 2
Graphite furnace AA (GFAA)	3113 B-2004	D1886-08 (C)	I-4503-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES) 36	200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Direct Current Plasma (DCP) 36	D4190-08	Note 34
38. Nitrate (as N), mg/L	Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30 3
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
Ion Selective Electrode	4500-NO3-D-2000
Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40)	Note 62
39. Nitrate + nitrite (as N), mg/L	Cadmium reduction, Manual	4500-NO3-E-2000	D3867-04 (B)
Cadmium reduction, Automated	353.2, Rev. 2.0 (1993)	4500-NO3-F-2000	D3867-04 (A)	I-2545-90 51
Automated hydrazine	4500-NO3-H-2000
Reduction/Colorimetric	Note 62
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30 3
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
40. Nitrite (as N), mg/L	Spectrophotometric: Manual	4500-NO2-B-2000	Note 25
Automated (Diazotization)	I-4540-85,2 Note 62
Automated (*bypass cadmium reduction)	353.2, Rev. 2.0 (1993)	4500-NO3-F-2000	D3867-04 (A)	I-4545-85 2
Manual (*bypass cadmium reduction)	4500-NO3-E-2000	D3867-04 (B)
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30 3
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
41. Oil and grease-Total recoverable, mg/L	Hexane extractable material (HEM): n-Hexane extraction and gravimetry	1664 Rev. A; 1664 Rev. B 42	5520 B-200138
Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry	1664 Rev. A; 1664 Rev. B42	5520 B-200138and 5520 F-200138
42. Organic carbon-Total (TOC), mg/L	Combustion	5310 B-2000	D7573-09	973.47,3 p. 14 24
Heated persulfate or UV persulfate oxidation	5310 C- 2000 5310 D-2000	D4839-03	973.47,3 p. 14 24
43. Organic nitrogen (as N), mg/L	Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4)
44. Ortho-phosphate (as P), mg/L	Colorimetry, Ascorbic acid, Automated	365.1, Rev. 2.0 (1993)	4500-P F-1999 or G-1999	973.56,3 I-4601-85 2
Colorimetry, Ascorbic Acid, Manual single reagent	4500-P E-1999	D515-88(A)	973.55 3
Colorimetry, Ascorbic Acid, Manual two reagent	365.3 (Issued 1978)1
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30 3
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
45. Osmium-Total4, mg/L	Digestion4, followed by any of the following:
AA direct aspiration (FLAA)	3111 D-1999
Graphite furnace AA (GFAA)	252.2 (Issued 1978)1
46. Oxygen, dissolved, mg/L	Winkler (Azide modification)	4500-O B-2001, C-2001, D-2001, E-2001, F-2001	D888-09 (A)	973.45B, 3 I-1575-78 8
Electrode	4500-O G-2001	D888-09 (B)	I-1576-78 8
Luminescence Based Sensor	D888-09 (C)	Note 63 Note 64
47. Palladium-Total,4 mg/ L	Digestion 4, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999
Graphite furnace AA (GFAA)	253.21(Issued 1978)
Inductively coupled plasma-mass spectrometry (ICP/MS)	3125 B-2009
Direct current plasma (DCP)	Note 34
48. Phenols, mg/L	Manual distillation26, followed by any of the following:	420.11(Rev. 1978)	5530 B-2005	D1783-01
Colorimetric (4AAP) manual	420.11(Rev. 1978)	5530 D-200527	D1783-01 (A or B)
Colorimetric (4AAP), Automated	420.4 Rev. 1.0 (1993)
49. Phosphorus (elemental), mg/L	Gas-liquid chromatography	Note 28
50. Phosphorus-Total, mg/L	Digestion20, followed by any of the following:	4500-P B(5)-1999	973.55 3
Colorimetric, Manual ascorbic acid	365.31(Issued 1978)	4500-P E-1999	D515-88 (A)
Colorimetric, Automated ascorbic acid reduction	365.1 Rev. 2.0 (1993)	4500-P F-1999, G-1999, H-1999	973.56, 3 I-4600-85 2
Colorimetric, Semi-automated block digestor (TKP digestion)	365.41(Issued 1974)	D515-88 (B)	I-4610-91 48
51. Platinum-Total,4mg/ L	Digestion 4 followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999
Graphite furnace AA (GFAA)	255.2 (Issued 1978)1
Inductively coupled plasma-mass spectrometry (ICP/MS)	3125 B-2009
Direct current plasma (DCP)	Note 34
52. Potassium-Total,4mg/L	Digestion 4, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999	973.53, 3 I-3630-85 2
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.7, Rev. 4.4 (1994)	3120 B-1999
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Flame photometric	3500-K B-1997
Electrode	3500-K C-1997
Ion Chromatography	D6919-09
53. Residue-Total, mg/L	Gravimetric, 103-105°C	2540 B-1997	I-3750-85 2
54. Residue-filterable (TDS), mg/ L	Gravimetric, 180°C	2540 C-1997	D5907-03	I-1750-85 2
55. Residue-non-filterable (TSS), mg/L	Gravimetric, 103-105°C post washing of residue	2540 D-1997	D5907-03	I-3765-85 2
56. Residue-settleable, mg/L	Volumetric, (Imhoff cone), or gravimetric	2540 F-1997
57. Residue-Volatile, mg/L	Gravimetric, 550°C	160.4 (Issued 1971)1	2540-E-1997	I-3753-85 2
58. Rhodium-Total,4 mg/L	Digestion 4 followed by any of the following:
AA direct aspiration (FLAA), or	3111 B-1999
Graphite furnace AA (GFAA)	265.2 (Issued 1978)1
Inductively coupled plasma-mass spectrometry (ICP/MS)	3125 B-2009
59. Ruthenium-Total,4mg/ L	Digestion4 followed by any of the following:
AA direct aspiration (FLAA), or	3111 B-1999
Graphite furnace AA (GFAA)	267.21
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8	3125 B-2009
60. Selenium-Total,4mg/ L	Digestion4, followed by any of the following:
Graphite furnace AA (GFAA)	3113 B-2004	D3859-08 (B)	I-4668-98 49
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)36	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14, 3 I-4020-05 70
AA gaseous hydride	3114 B-2009, or 3111 C-2009	D3859-08 (A)	I-3667-85 2
61. Silica-Dissolved,37mg/L	0.45-micron Filtration followed by any of the following:
Colorimetric, Manual	4500-SiO2C-1997	D859-05	I-1700-85 2
Colorimetric, Automated (Molybdosilicate)	4500-SiO2E-1997 or F-1997	I-2700-85 2
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)	3120 B-1999	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
62. Silver-Total,4, 31 mg/L	Digestion4, 29, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999 or 3111 C-1999	974.27, 3 p. 37, 9 I-3720-85 2
Graphite furnace AA (GFAA)	3113 B-2004	I-4724-89 51
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14, 3 I-4471-97 50
Direct current plasma (DCP)	Note 34
63. Sodium-Total,4mg/L	Digestion 4, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999	973.54 3, I-3735-85 2
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003)68; 200.7, Rev. 4.4 (1994)	3120 B-1999	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Direct current plasma (DCP)	Note 34
Flame photometric	3500-Na B-1997
Ion Chromatography	D6919-09
64. Specific conductance, microm-hos/cm at 25 °C	Wheatstone bridge	120.11(Rev. 1982)	2510 B-1997	D1125-95( 99) (A)	973.40, 3 I-2781-85 2
65. Sulfate (as SO4), mg/L	Colorimetric, Automated	375.2, Rev. 2.0 (1993)	4500-SO42-F -1997 or G-1997
Gravimetric	4500-SO42-C -1997 or D-1997	925.54 3
Turbidimetric	4500-SO42-E -1997	D516-07
Ion Chromatography	300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)	4110 B-2000 or C-2000	D4327-03	993.30, 3 I-4020-05 70
Capillary ion electrophoresis (CIE/ UV)	4140 B-1997	D6508-00(05)	D6508, Rev. 2 54
66. Sulfide (as S), mg/L	Sample Pretreatment	4500-S2-B, C-2000
Titrimetric (iodine)	4500-S2-F-2000	I-3840-85 2
Colorimetric (methylene blue)	4500-S2-D-2000
Ion Selective Electrode	4500-S2-G-2000	D4658-08
67. Sulfite (as SO3), mg/L	Titrimetric (iodine-iodate)	4500-SO32-B -2000
68. Surfactants, mg/L	Colorimetric (methylene blue)	5540 C-2000	D2330-02
69. Temperature, °C	Thermometric	2550 B-2000	Note 32
70. Thallium-Total,4 mg/L	Digestion4, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999
Graphite furnace AA (GFAA)	279.21(Issued 1978)	3113 B-2004
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.7, Rev. 4.4 (1994); 200.5 Rev. 4.2 (2003)68	3120 B-1999	D1976-07
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14, 3 I-4471-97 50
71. Tin-Total,4mg/ L	Digestion4, followed by any of the following:
AA direct aspiration (FLAA)	3111 B-1999	I-3850-78 8
Graphite furnace AA (GFAA)	3113 B-2004
Stabilized temperature GFAA (STGFAA)	200.9, Rev. 2.2 (1994)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
72. Titanium-Total,4mg/L	Digestion4followed by any of the following:
AA direct aspiration (FLAA)	3111 D-1999
Graphite furnace AA (GFAA)	283.21(Issued 1978)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.7, Rev. 4.4 (1994)
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3
Direct current plasma (DCP)	Note 34
73. Turbidity, NTU53	Nephelometric	180.1, Rev. 2.0 (1993)	2130 B-2001	D1889-00	I-3860-85 2 Note 65 Note 66 Note 67
74. Vanadium-Total,4mg/L	Digestion4, followed by any of the following:
AA direct aspiration (FLAA)	3111 D-1999
Graphite furnace AA (GFAA)	3113 B-2004	D3373-03(07)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14,3 I-4020-05 70
Direct current plasma (DCP)	D4190-08	Note 34
Colorimetric (Gallic Acid)	3500-V B-1997
75. Zinc-Total4, mg/L	Digestion 4, followed by any of the following:
AA direct aspiration (FLAA) 36	3111 B-1999 or 3111 C-1999	D1691-02(07) (A or B)	974.27, 3 p. 37, 9 I-3900-85 2
Graphite furnace AA (GFAA)	289.21(Issued 1978)
Inductively coupled plasma-atomic emission spectrometry (ICP/AES)36	200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994)	3120 B-1999	D1976-07	I-4471-97 50
Inductively coupled plasma-mass spectrometry (ICP/MS)	200.8, Rev. 5.4 (1994)	3125 B-2009	D5673-05	993.14 3 I-4020-05 70
Direct current plasma (DCP)36	D4190-08	Note 34
Colorimetric (Zincon)	3500 Zn B-1997	Note 33
76. Acid Mine Drainage	1627 69

1 Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.

2 Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.

3 Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC International.

4 For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis).

For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness.

For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of "Methods for the Determination of Metals in Environmental Samples" EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up should be consulted for specific instruction and/or cautions.

For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as "total" metals.

5 Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.

6 Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to resolve any controversies. In general, the analytical method should be consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is defined as < 20% RPD for all tested matrices). Alternatively the two populations of spike recovery percentages may be compared using a recognized statistical test.

7 Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Bran & Luebbe Analyzing Technologies Inc.

8 The approved method is that cited in Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. USGS.

9 American National Standard on Photographic Processing Effluents. April 2, 1975. American National Standards Institute (ANSI), 25 West 43rd St., New York, NY 10036.

10 In-Situ Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

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 CBOD5parameter. 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 CBOD5is required can the permittee report data using a nitrification inhibitor.

13 OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation. 512 West Loop, P.O. Box 2980, College Station, TX 77840.

14 Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company. P.O. Box 389, Loveland, CO 80537. Available on-line at http://www.hach.com.

15 The back titration method will be used to resolve controversy.

16 Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. Thermo Scientific, 81 Wyman Street, Waltham, MA 02454. 1977. Orion Research Incorporated. The calibration for the Orion residual chlorine method must be derived using at least three standard solutions, prepared from a 0.00281 N potassium iodate solution.

17 Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA., available from the U.S. EPA Sample Control Center (operated by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304.

18 National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253, December 1971.

19 Method 8506, Biocinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company. P.O. Box 389, Loveland, CO 80537. Available on-line at http://www.hach.com.

20 When using a method with block digestion, this treatment is not required.

21 Industrial Method Number 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Autoanalyzer II. October 1976. Bran & Luebbe Analyzing Technologies. Elmsford, NY 10523.

22 Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company P.O. Box 389, Loveland, CO 80537. Available on-line at http://www.hach.com.

23 Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company Loveland, CO 80537. Available on-line at http://www.hach.com.

24 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, (1972 Revised 1987) p. 14. 1987. USGS. Available from: U.S. Geological Survey, 604 S. Pickett Street, Alexandria, VA 22304.

25 Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company P.O. Box 389, Loveland, CO 80537. Available on-line at http://www.hach.com.

26 Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.

27 The colorimetric reaction must be conducted at a pH of 10.0 ± 0.2.

28 Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography, Journal of Chromatography, 47(3):421-426. 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.

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 use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method specified quality control acceptance criteria are met.

31 For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.

32 "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. USGS. Available from: U.S. Geological Survey, 604 S. Pickett Street, Alexandria, VA 22304.

33 Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company. Loveland, CO 80537. Available on-line at http://www.hach.com.

34 Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised 1991. Thermo Jarrell Ash Corporation. Available from: Thermo Scientific, 81 Wyman Street, Waltham, MA 02454.

35 In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

36 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200.

37 When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.

38 Only use n-hexane (n-Hexane-85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil and Grease parameters-Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of other extraction solvents is prohibited.39 Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical/ALP- KEM, P.O. Box 9010, College Station, TX 77842.

40 Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.

41 Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical/ALP-KEM, P.O. Box 9010, College Station, TX 77842.

42 Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, 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. U.S. EPA. February 2010, Revision B. Method 1664, 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-10-001. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161.

43 Method 1631, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August 2002, U.S. EPA. The application of clean techniques described in EPA's 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. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, Virginia 22161.

44 Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.

45 Open File Report 00-170, 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. 2000. USGS.

46 Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.

47 Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS.

48 Open File Report 92-146, 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. 1992. USGS.

49 Open File Report 98-639, 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. 1999. USGS.

50 Open File Report 98-165, 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. 1998. USGS.

51 Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

52 Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1-1, are published in U.S. EPA. May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography.

53 Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.

54 Method D6508, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. December 2000. Waters Corp., 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.

55 Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001. US EPA. National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. The toll free telephone number is: 800-553-6847.

Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.

56 QuikChem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Lachat Instruments. Available from Hach Company, P.O. Box 389, Loveland, CO 80537.

57 When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to distillation.

58 Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation "followed by" analysis with a method, approved digestion and/or distillation are required prior to analysis.

59 Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-09 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.

60Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color reagent in Berthelot Reaction ("phenol-hypochlorite reaction") colorimetric ammonium determination methods. For example when phenol is used as the color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively-see, Patton, C.J. and S.R. Crouch. March 1977. Anal. Chem. 49:464-469. These reaction parameters increase to pH > 12.6 and 665 nm when salicylate is used as the color reagent-see, Krom, M.D. April 1980. The Analyst 105:305-316.

61 If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may be used. This method has poorer precision and bias than the methods of choice.

62 Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.

63 Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5. Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).

64 In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.

65 Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

66 Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

67 Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.

68 EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/600/R-06/115. Revision 4.2, October 2003. US EPA.

69 Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. US EPA.

70 Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis, 2006. USGS.

71 Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water With Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.

72 Quality control requirements for low level mercury are found in s. NR 106.145(9) and (10), Wis. Adm. Code. Low-level mercury methods are performance based so some method modifications are allowable, provided quality control requirements are met. If an atomic absorption detector is substituted for atomic fluorescence detector, the appropriate method citation is 245.1 (manual) or 245.2 (automated). If method 1631E is modified to eliminate the purge and trap step, the appropriate method citation is 245.7.

Table C

List of Approved Test Procedures for Non-Pesticide Organic Compounds in Wastewater

Parameter 1	Analytical Technology	EPA 2,7	Standard methods	ASTM	Other
1. Acenaphthene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
2. Acenaphthylene	GC	610
GC/MS	625,1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
3. Acrolein	GC	603
GC/MS	624 4, 1624B
4. Acrylonitrile	GC	603
GC/MS	624 4, 1624B
5. Anthracene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.27
HPLC	610	6440B-2000	D4657-92 (98)
6. Benzene	GC	602	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
7. Benzidine	Spectrophotometric	Note, 3 p.1
GC/MS	625, 5 1625B	6410 B-2000
HPLC	605
8. Benzo(a)anthracene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	610	6440 B-2000	D4657-92 (98)
9. Benzo(a)pyrene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	610	6440 B-2000	D4657-92 (98)
10. Benzo(b)fluoranthene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	610	6440 B-2000	D4657-92 (98)
11. Benzo(g,h,i)perylene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	610	6440 B-2000	D4657-92 (98)
12. Benzo(k)fluoranthene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	610	6440 B-2000	D4657-92 (98)
13. Benzyl chloride	GC	Note, 3 p.
130
GC/MS	Note, 6 p.
S102
14. Butyl benzyl phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
15. bis(2-Chloroethoxy) methane	GC	611
GC/MS	625, 1625B	6410 B-2000	Note 9, p.
27
16. bis(2-Chloroethyl) ether	GC	611
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
17. bis(2-Ethylhexyl) phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
18. Bromodichloromethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
19. Bromoform	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
20. Bromomethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
21. 4-Bromophenyl phenyl ether	GC	611
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
22. Carbon tetrachloride	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
23. 4-Chloro-3-methyl phenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
24. Chlorobenzene	GC	601, 602	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
25. Chloroethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
26. 2-Chloroethylvinyl ether	GC	601
GC/MS	624, 1624B
27. Chloroform	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
28. Chloromethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
29. 2-Chloronaphthalene	GC	612
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
30. 2-Chlorophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
31. 4-Chlorophenyl phenyl ether	GC	611
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
32. Chrysene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
33. Dibenzo(a,h)anthracene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
34. Dibromochloromethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
35. 1,2-Dichlorobenzene	GC	601, 602	6200 C-1997
GC/MS	624, 1625B	6200 B-1997	Note, 9 p. 27
36. 1,3-Dichlorobenzene	GC	601, 602	6200 C-1997
GC/MS	624, 1625B	6200 B-1997	Note, 9 p. 27
37. 1,4-Dichlorobenzene	GC	601, 602	6200 C-1997.
GC/MS	624, 1625B	6200 B-1997	Note, 9 p. 27
38. 3,3'-Dichlorobenzidine	GC/MS	625, 1625B	6410 B-2000
HPLC	605
39. Dichlorodifluoromethane	GC	601
GC/MS	6200 C-1997
40. 1,1-Dichloroethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
41. 1,2-Dichloroethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
42. 1,1-Dichloroethene	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
43. trans-1,2-Dichloroethene	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
44. 2,4-Dichlorophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
45. 1,2-Dichloropropane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
46. cis-1,3-Dichloropropene	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
47. trans-1,3-Dichloropropene	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
48. Diethyl phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
49. 2,4-Dimethylphenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
50. Dimethyl phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
51. Di-n-butyl phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
52. Di-n-octyl phthalate	GC	606
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
53. 2, 3-Dinitrophenol	GC	604	6420 B-2000	Note, 9 p. 27
GC/MS	625, 1625B	6410 B-2000
54. 2, 4-Dinitrophenol	GC	604	6420 B-2000	Note, 9 p. 27
GC/MS	625, 1625B	6410 B-2000
55. 2, 6-Dinitrophenol	GC	604	6420 B-2000	Note, 9 p. 27
GC/MS	625, 1625B	6410 B-2000
56. 2,3-Dinitrotoluene	GC	609
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
57. 2,4-Dinitrotoluene	GC	609
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
58. 2,6-Dinitrotoluene	GC	609
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
59. Epichlorohydrin	GC	Note, 3 p. 130
GC/MS	Note, 6 p. S102
60. Ethylbenzene	GC	602	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
61. Fluoranthene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
62. Fluorene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
63. 1,2,3,4,6,7,8-Heptachloro-dibenzofuran	HRGC/MS	1613B
64. 1,2,3,4,7,8,9-Heptachloro-dibenzofuran	HRGC/MS	1613B
65. 1,2,3,4,6,7,8- Heptachloro-dibenzo-p-dioxin	HRGC/MS	1613B
66. Hexachlorobenzene	GC	612
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
67. Hexachlorobutadiene	GC	612
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
68. Hexachlorocyclopentadiene	GC	612
GC/MS	625, 5 1625B	6410 B-2000	Note, 9 p. 27
69. 1,2,3,4,7,8-Hexachloro-dibenzofuran	HR GC/MS	1613B
70. 1,2,3,6,7,8-Hexachloro-dibenzofuran	HR GC/MS	1613B
71. 1,2,3,7,8,9-Hexachloro-dibenzofuran	HR GC/MS	1613B
72. 2,3,4,6,7,8-Hexachloro-dibenzofuran	HR GC/MS	1613B
73. 1,2,3,4,7,8-Hexachloro-dibenzo-p-dioxin	HR GC/MS	1613B
74. 1,2,3,6,7,8-Hexachloro-dibenzo-p-dioxin	HR GC/MS	1613B
75. 1,2,3,7,8,9-Hexachloro-dibenzo-p-dioxin	HR GC/MS	1613B
76. Hexachloroethane	GC	612
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
77. Indeno(1,2,3-c,d) pyrene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
78. Isophorone	GC	609
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
79. Methylene chloride	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
80. 2-Methyl-4,6-dinitrophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
81. Naphthalene	GC	610
GC/MS	625, 1625B	6410 B-2000.	Note, 9 p.
27
HPLC	610	6440 B-2000.
82. Nitrobenzene	GC	609
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
HPLC	D4657-92 (98)
83. 2-Nitrophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
84. 4-Nitrophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
85. N-Nitrosodimethylamine	GC	607
GC/MS	625, 5 1625B	6410 B-2000	Note, 9 p.
27
86. N-Nitrosodi-n-propylamine	GC	607
GC/MS	625, 5 1625B	6410 B-2000	Note, 9 p.
27
87. N-Nitrosodiphenylamine	GC	607
GC/MS	625, 5 1625B	6410 B-2000	Note, 9 p.
27
88. Octachlorodibenzofuran	HR GC/MS	1613B 10
89. Octachlorodibenzo-p-dioxin	HR GC/MS	1613B 10
90. 2,2'-Oxybis(2-chloro-propane)	GC	611
[prev.: bis(2-Chloroisopropyl) ether]
GC/MS	625, 1625B	6410 B-2000	Note, 9 p.
27
91. PCB-1016, (Aroclor or congeners)12,13	GC	608	Note, 3 p.43;
Note 8
GC/MS	625	6410 B-2000
HR GC/MS	1668A 14
92. PCB-1221, (Aroclor or congeners)12,13	GC	608	Note, 3 p.43;
Note 8
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
93. PCB-1232, (Aroclor or congeners)12,13	GC	608	Note, 3 p.43;
Note 8
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
94. PCB-1242, (Aroclor or congeners)12,13	GC	608	Note, 3 p. 43; Note 8
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
95. PCB-1248, (Aroclor or congeners)12,13	GC	608
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
96. PCB-1254, (Aroclor or congeners)12,13	GC	608	Note, 3 p. 43; Note 8
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
97. PCB-1260, (Aroclor or congeners)12,13	GC	608	Note, 3 p. 43; Note 8
GC/MS	625	6410 B-2000
HRGC/ MS	1668A 14
98. 1,2,3,7,8-Pentachloro-dibenzofuran	GC/MS	1613B
99. 2,3,4,7,8-Pentachloro-dibenzofuran	GC/MS	1613B
100. 1,2,3,7,8,-Pentachloro-dibenzo-p-dioxin	GC/MS	1613B
101. Pentachlorophenol	GC	604	6420 B-2000	Note, 3 p. 140
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
102. Phenanthrene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
103. Phenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
104. Pyrene	GC	610
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
HPLC	610	6440 B-2000	D4657-92 (98)
105. 2,3,7,8-Tetrachloro-dibenzofuran	HR GC/MS	1613B 10
106. 2,3,7,8-Tetrachloro-dibenzo-p-dioxin	GC/MS	613, 625, 5a
107. 1,1,2,2-Tetrachloroethane	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
108 Tetrachlorocatechol	GC	6420 B-2000
GC/MS	1653 11	6410 B-2000
109. Tetrachloroethene	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
110. Tetrachloroguaicol	GC	6420 B-2000
GC/MS	1653 11	6410 B-2000
111. 2,3,4,6- Tetrachlorophenol	GC	6420 B-2000
GC/MS	6410 B-2000
112. Toluene	GC	602	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
113. 1,2,4-Trichlorobenzene	GC	612	Note, 3 p. 130
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
114. 3,4,5-Trichlorocatechol	GC	6420 B-2000
GC/MS	1653 11	6410 B-2000
115. 3,4,6-Trichlorocatechol	GC	6420 B-2000
GC/MS	1653 11	6410 B-2000
116. 1,1,1-Trichloroethane	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
117. 1,1,2-Trichloroethane	GC	601	6200 C-1997	Note, 3 p. 130
GC/MS	624, 1624B	6200 B-1997
118. Trichloroethene	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
119. Trichlorofluoromethane	GC	601	6200 C-1997
GC/MS	624	6200 B-1997
120. 3,4,5-Trichloroguaicol	GC	6420 B-2000
GC/MS	165311	6410 B-2000
121. 3,4,6-Trichloroguaicol	GC	6420 B-2000
GC/MS	165311	6410 B-2000
122. 4,5,6-Trichloroguaicol	GC	6420 B-2000
GC/MS	165311	6410 B-2000
123. 2,4,5-Trichlorophenol	GC	6420 B-2000
GC/MS	165311	6410 B-2000
124. 2,4,6-Trichlorophenol	GC	604	6420 B-2000
GC/MS	625, 1625B	6410 B-2000	Note, 9 p. 27
125. Trichlorosyringol	GC	6420 B-2000
GC/MS	165311	6410 B-2000
126. Vinyl chloride	GC	601	6200 C-1997
GC/MS	624, 1624B	6200 B-1997
127. Nonylphenol	GC/MS	D7065-06
128. Bisphenol A (BPA)	GC/MS	D7065-06
129. p-tert-Octylphenol (OP)	GC/MS	D7065-06
130. Nonylphenol Monoethoxylate (NP1EO)	GC/MS	D7065-06
131. Nonylphenol Diethoxylate (NP2EO)	GC/MS	D7065-06
132. Adsorbable Organic Halides (AOX)	Adsorption and Coulometric Titration	165011
133. Chlorinated Phenolics	In Situ Acetylation and GC/MS	165311

1 All parameters are expressed in micrograms per liter (µg/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, 1613B, 1624B, and 1625B are provided at Appendix A, Test Procedures for Analysis of Organic Pollutants, of 40 CFR Part 136 . The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at 40 CFR Part 136, Appendix B, Definition and Procedure for the Determination of the Method Detection Limit.

3 Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA.

4 Method 624 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate the ability to detect and quantify these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample introduction techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 should be used when analyzing samples for acrolein and acrylonitrile in the absence of such criteria in Method 624.

5 Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi-n-propylamine, and N-ni-trosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.

5a Method 625, screening only.

6 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. American Public Health Association (APHA).

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 in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

8 Organochlorine Pesticides and PCBs in Wastewater Using EmporeTMDisk. Revised October 28, 1994. 3M Corporation.

9 Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

10Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in Appendix A to 40 CFR Part 136 and at http://water.epa.gov/scitech/methods/cwa/index.cfm.

11 Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997. U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS. Revision A, 1997. U.S. EPA. The full text for both of these methods is provided at Appendix A, "Methods 1650 and 1653", in Part 430, The Pulp, Paper, and Paperboard Point Source Category. Also available on-line at http://www.gpo.gov/.

12 EPA Method 1668A may be used to test for all PCB congeners. If this method is employed, all PCB congeners shall be delineated. Non-detects shall be treated as zero. The values that are between the limit of detection and the limit of quantitation shall be used when calculating the total value of all congeners. All results shall be added together and the total PCB concentration reported. It is recognized a number of congeners will co-elute with others, so there will not be 209 results to sum.

13 If congener specific analysis is performed, the list of congeners tested shall include at least congener numbers 5, 18, 31, 44, 52, 66, 87, 101, 110, 138, 141, 151, 153, 170, 180, 183, 187, and 206 plus any other additional congeners which might be reasonably expected to occur in the particular sample. If Aroclor analysis is performed, clean up steps of the extract shall be performed as necessary to remove interference. If congener specific analysis is done, clean up steps of the extract shall be performed as necessary to remove interference. If desired limits of detection cannot be achieved after using the appropriate clean up techniques, a reporting limit that is achievable for the Aroclors or each congener for sample shall be determined. This report limit should be reported and qualified indicating the presence of an interference. The laboratory conducting the analysis shall perform as many the following methods as necessary to remove interference:

Florisil, Gel Permeation, Silica Gel, Alumina, Sulfur Clean Up, Sulfuric Acid Clean Up.

14 "Method 1668A, Revision A: Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by HRGC/HRMS", EPA-821-R-00-002, Environmental Protection Agency, Office of Water, Washington, D.C., December 1999. Available from: the National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.

Table D

List of Approved Test Procedures for Pesticides 1

Parameter	Analytical Technology	EPA2,7,10	Standard methods	ASTM	Other
1. Aldrin	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96 (02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	625	6410 B-2000
2. Ametryn	GC	507, 619	Note, 3 p. 83; Note, 9 O-3106-93; Note, 6 p. S68
GC/MS	525.2	Note, 14 O-1121-91
3. Aminocarb	TLC	Note, 3 p. 94; Note, 6 p. S60
HPLC	632
4. Atraton	GC	619	Note, 3 p. 83; Note, 6 p. S68
5. Atrazine	GC	507, 619	Note, 3 p. 83; Note, 6 p. S68; Note, 9 O-3106-93
HPLC/MS	Note, 12 O-2060-01
GC/MS	525.1, 525.2	Note, 11 O-1126-95
6. Azinphos methyl	GC	614, 622, 1657	Note, 3 p. 25; Note, 6 p. S51
GC-MS	Note, 11 O-1126-95
7. Barban	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
8. [ALPHA]-BHC	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 8 3M0222
GC/MS	6255	6410 B-2000	Note, 11O-1126-95
9. [BETA]-BHC	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 8 3M0222
GC/MS	625	6410 B-2000
10. [DELTA]-BHC	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 83M0222
GC/MS	625	6410 B-2000
11. [GAMMA]-BHC (Lindane)	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	6255	6410 B-2000	Note, 11 O-1126-95
12. Captan	GC	617	6630 B-2000	D3086-90, D5812-96(02)	Note, 3 p. 7
13. Carbaryl	TLC	Note, 3 p. 94, Note, 6 p. S60
HPLC	531.1, 632
HPLC/MS	553	Note, 12 O-2060-01
GC/MS	Note, 11 O-1126-95
14. Carbophenothion	GC	617	6630 B-2000	Note, 4 page 27; Note, 6 p. S73
15. Chlordane	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	625	6410 B-2000
16. Chloropropham	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
17. 2,4-D	GC	615	6640 B-2001	Note, 3 p. 115; Note, 4 O-3105-83
HPLC/MS	Note, 12 O-2060-01
18. 4,4'-DDD	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3105-83; Note, 8 3M0222
GC/MS	625	6410 B-2000.
19. 4,4'-DDE	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	625	6410 B-2000	Note, 11 O-1126-95
20. 4,4'-DDT	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	625	6410 B-2000
21. Demeton-O	GC	614, 622	Note, 3 p. 25; Note, 6 p. S51
22. Demeton-S	GC	614, 622	Note, 3 p. 25; Note, 6 p. S51
23. Diazinon	GC	507, 614, 622, 1657	Note 3, p. 25; Note 4, O-3104-83; Note 6, p. S51
GC/MS	525.2	Note 11, O-1126-95
24. Dicamba	GC	615	Note 3, p. 115
HPLC/MS	Note 12, O-2060-01
25. Dichlofenthion	GC	622.1	Note 4, page 27; Note 6, p. S73
26. Dichloran	GC	608.2, 617	6630 B-2000	Note 3, p. 7
27. Dicofol	GC	617	Note 4, O-3104-83
28. Dieldrin	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note 3, p. 7; Note 4, O-3104-83; Note 8, 3M0222
GC/MS	625	6410 B-2000	Note 11, O-1126-95
29. Dioxathion	GC	614.1, 1657	Note 4, page 27; Note 6, p. S73
30. Disulfoton	GC	507, 614, 622, 1657	Note 3, p. 25; Note, 6 p. S51
GC/MS	525.2	Note, 11 O-1126-95
31. Diuron	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	553	Note, 12 O-2060-01
32. Endosulfan I	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	6255	6410 B-2000	Note, 13 O-2002-01
33. Endosulfan II	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 8 3M0222
GC/MS	6255	6410 B-2000	Note, 13 O-2002-01
34. Endosulfan Sulfate	GC	608, 617	6630 C-2000	Note, 8 3M0222
GC/MS	625	6410 B-2000
35. Endrin	GC	505, 508, 608, 617, 1656	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	525.1, 525.2, 6255	6410 B-2000
36. Endrin aldehyde	GC	608, 617	6630 C-2000	Note, 8 3M0222
GC/MS	625
37. Ethion	GC	614, 614.1,1657	Note, 4 page 27; Note, 6 p. S73
GC/MS	Note, 13 O-2002-01
38. Fenuron	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	Note, 12 O-2060-01
39. Fenuron-TCA	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
40. Heptachlor	GC	505, 508, 608, 617, 1656	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	525.1, 525.2, 625	6410 B-2000
41. Heptachlor epoxide	GC	608, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 6 p. S73; Note, 8 3M0222
GC/MS	625	6410 B-2000.
42. Isodrin	GC	617	6630 B-2000 6630 C-2000	Note, 4 O-3104-83; Note, 6 p. S73
43. Linuron	GC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	553	Note, 12 O-2060-01
GC/MS	Note, 11 O-1126-95
44. Malathion	GC	614, 1657	6630 B-2000	Note, 3 p. 25; Note, 6 p. S51
GC/MS	Note, 11 O-1126-95
45. Methiocarb	TLC	Note, 3 p. 94; Note, 6 p. S60
HPLC	632
HPLC/MS	Note, 12 O-2060-01
46. Methoxychlor	GC	505, 508, 608.2, 617, 1656	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83; Note, 8 3M0222
GC/MS	525.1, 525.2	Note, 11 O-1126-95
47. Mexacarbate	TLC	Note, 3 p. 94; Note, 6 p.S60
HPLC	632
48. Mirex	GC	617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7; Note, 4 O-3104-83
49. Monuron	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
50. Monuron-TCA	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
51. Neburon	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	Note, 12 O-2060-01
52. Parathion methyl	GC	614, 622, 1657	6630 B-2000	Note, 3 p. 25; Note, 4 page 27
GC/MS	Note, 11 O-1126-95
53. Parathion ethyl	GC	614	6630 B-2000	Note, 3 p. 25; Note, 4 page 27
GC/MS	Note, 11 O-1126-95
54. PCNB	GC	608.1, 617	6630 B-2000 6630 C-2000	D3086-90, D5812-96(02)	Note, 3 p. 7.
55. Perthane	GC	617	D3086-90, D5812-96(02)	Note, 4 O-3104-83
56. Prometon	GC	507, 619	Note, 3 p. 83; Note, 6 p. S68; Note, 9 O-3106-93
GC/MS	525.2	Note, 11 O-1126-95
57. Prometryn	GC	507, 619	Note, 3 p. 83; Note, 6 p. S68; Note, 9 O-3106-93
GC/MS	525.1, 525.2	Note, 13 O-2002-01
58. Propazine	GC	507, 619, 1656	Note, 3 p. 83; Note, 6 p. S68; Note, 9 O-3106-93
GC/MS	525.1, 525.2.
59. Propham	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	Note, 12 O-2060-01
60. Propoxur	TLC	Note, 3 p. 94; Note, 6 p. S60
HPLC	632
61. Secbumeton	TLC	Note, 3 p. 83; Note, 6 p. S68
GC	619
62. Siduron	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
HPLC/MS	Note, 12 O-2060-01
63. Simazine	GC	505, 507, 619, 1656	Note, 3 p. 83; Note, 6 p. S68; Note, 9 O-3106-93
GC/MS	525.1, 525.2	Note, 11 O-1126-95
64. Strobane	GC	617	6630 B-2000 6630 C-2000	Note, 3 p. 7
65. Swep	TLC	Note, 3 p. 104; Note, 6 p. S64
HPLC	632
66. 2,4,5-T	GC	615	6640 B-2001	Note, 3 p. 115; Note, 4 O-3105-83
67. 2,4,5-TP (Silvex)	GC	615	6640 B-2001	Note, 3 p. 115; Note, 4 O-3105-83
68. Terbuthylazine	GC	619, 1656	Note, 3 p. 83;
Note, 6 p. S68
GC/MS	Note, 13 O-2002-01
69. Toxaphene	GC	505, 508, 608, 617,	6630 B-2000	D3086-90,	Note, 3 p. 7;
1656	6630 C-2000	D5812-96(02)	Note, 4 O-3105-83
Note, 8 3M0222
GC/MS	525.1, 525.2, 625	6410 B-2000
70. Trifluralin	GC	508, 617, 627,	6630 B-2000	Note, 3 p. 7;
1656	Note, 9 O-3106-93
GC/MS	525.2	Note, 11 O-1126-95

1 Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table C, where entries are listed by chemical name.

2 The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at 40 CFR Part 136, Appendix B, Definition and Procedure for the Determination of the Method Detection Limit.

3 Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA publication includes thin-layer chromatography (TLC) methods.

4 Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3. 1987. USGS.

5 The method may be extended to include Ã¡-BHC, Ã£-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.

7 Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

8 Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk. Revised October 28, 1994. 3M Corporation.

9 Method O-3106-93 is in Open File Report 94-37, 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. 1994. USGS.

10 EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA.

The full text of Methods 608 and 625 are provided at 40 CFR Part 136, Appendix A, Test Procedures for Analysis of Organic Pollutants.

EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA.

EPA Method 525.2 is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry, Revision 2.0, 1995, U.S. EPA.

EPA methods 1656 and 1657 are in Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA.

11 Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995. USGS.

12 Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry. 2001. USGS.

13 Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry. 2001. USGS.

14 Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1992. USGS.

Table E

List of Approved Radiological Analytical Methods for Wastewater

Parameter and units	Method	Reference (method number or page)
Parameter and units	Method	EPA 1	Standard Methods 18th, 19th, 20th Ed.	Standard Methods Online	ASTM	USGS 2
1. Alpha-Total, pCi per liter	Proportional or scintillation counter	900.0	7110 B	7110 B-00	D1943-90, 96	pp. 75 and 78 3
2. Alpha-Counting error, pCi per liter	Proportional or scintillation counter	Appendix B	7110 B	7110 B-00	D1943-90, 96	p. 79
3. Beta-Total, pCi per liter	Proportional counter	900.0	7110 B	7110 B-00	D1890-90, 96	pp. 75 and 78 3
4. Beta-Counting error, pCi	Proportional counter	Appendix B	7110 B	7110 B-00	D1890-90, 96	p. 79
5. (a) Radium Total pCi per liter	Proportional counter	903.0	7500-Ra B	7500-Ra B-01	D2460-90, 97
(b) Radium, pCi per liter	Scintillation counter	903.1	7500-Ra C	7500-Ra C-01	D3454-91, 97	p. 81

1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.

2 Fishman, M. J. and Brown, Eugene, "Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters," U.S. Geological Survey, Open-File Report 76-177 (1976).

3 The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, the two results must be added to obtain the "total."

Table EM

List of Approved Analytical Methods for Sludge

Sample ---- Preparation----				Determinative ------------------------- Method-------------------------------
Parameter	Analytical Technology	SW-846 1	EPA4	SW-8461	EPA 2,3	Standard Methods [ed.] 8,9	Other
Metals Arsenic	Gaseous Hydride5	7061A	7061A
	Graphite Furnace Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
	Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
	Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Beryllium	Flame Atomic Absorption	3050B, 3051A	200.2	7000B	3111 D [18,19,21], 3111 D-99
	Graphite Furnace Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
	Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
	Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Cadmium	Flame Atomic Absorption	3050B, 3051A	200.2	7000B
Graphite Furnace Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Chromium	Flame Atomic Absorption	3050B, 3051A	200.2	7000B	3111 B [18,19,21], 3111 B-99
Graphite Furnace Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Copper	Flame Atomic Absorption	3050B, 3051A	200.2	7000B	3111 B or C [18,19,21], 3111 B-99 or C-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Lead	Flame Atomic Absorption	3050B, 3051A	200.2	7000B
Graphite Furnace6 Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Mercury	Cold Vapor Atomic Absorption	7471A, 7471B	7471A, 7471B
Cold vapor atomic Fluorescence Spectrometry	7474
Molybdenum	Graphite Furnace6 Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Nickel	Flame Atomic Absorption	3050B, 3051A	200.2	7000B	3111 B or C [18,19,21], 3111 B-99 or C-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Selenium	Gaseous Hydride5	7741A	7741A
Graphite Furnace Atomic Absorption	3050B, 3051A	200.2	7010	200.9	3113 B [18,19,21], 3113 B-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Zinc	Flame Atomic Absorption	3050B, 3051A	200.2	7000B	3111 B or C [18,19,21], 3111 B-99 or C-99
Inductively Coupled Plasma Emission	3050B, 3051A	200.2	6010B, 6010C	200.7	3120 B [20,21], 3120 B-99
Inductively Coupled Plasma/ Mass Spectrometry	3050B, 3051A	6020A	200.8
Organics
Dioxins and Furans	Gas Chromatography/ Mass Spectrometry	8290A	1613B	8290A	1613B
PCBs (Aroclor or Congeners)	Gas Chromatography	3540B, 3540C, 3545A	8082, 8082A12
PCB (Congeners)	Gas Chromatography/ Mass Spectrometry	1668A13,14,15	1668A 13, 14, 15
Biological
Enteric Viruses	Centrifuge Concentration	D 4994-89 (02),7 Appendix H10
Coliform (fecal), number per gram dry weight	Most Probable Number (MPN), 5 tube, 3 dilution, or	p. 132,16 1680,11,17 168111,18	p. 132,16 1680,11,17168111,18	9221 E-2014	Appendix F10
Membrane filter (MF)21,22 single step	p. 12416	p. 12416	9222 D-201519
Helminth ova	Density Gradient Flotation	Note 9 or Appendix I9
Specific Oxygen Uptake Rate	Respirometer	2710 B [18,19, 20,21], 2710 B-04	Appendix D.2.10
Salmonella number per gram dry weight11	MPN multiple tube	168220	168220
Physical
Solids	Gravimetric	2540 G [18,19,20,21], 2540 G-97
Percent Volatiles Solids Reduction	Calculation	Appendix D.1. and 310

1 "Test Methods for Evaluating Solid Waste, Physical/Chemical Methods," SW-846, Environmental Protection Agency, Office of Solid Waste and Emergency Response, 401 M Street, S.W., Washington D.C. 20460, September 1986 (Third edition), including July 1992 (Update I), September 1994 (Update II), August 1993 (Update IIA), January 1995 (Update IIB), December 1996 (Update III), April 1998 (Update IIIA), November 2004 (Update IIIB), February 2007 (Update IV) updates. Available from: The Superintendent of Documents, U.S. Government Printing Office, Room 190, Federal Building, P.O. Box 371954, Pittsburgh, PA 15250-7954. Available online at https://www.epa.gov/hw-sw846/sw-846-compendium.

2 If an alternative digestion procedure is specified in the analytical method, the digestion in this table shall be used. In all cases, consult the analytical method for special requirements and cautions. SW-846 method 3051A is an acceptable alternate digestion procedure to SW-846 method 3050B.

3 "Methods for the Determination of Metals in Environmental Samples", EPA-600/4-91-010, Environmental Protection Agency, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268, June 1991. Available from: the National Technical Information Service (NTIS), 5258 Port Royal Road, Springfield, Virginia 22161.

4 "Sample Preparation Procedure for Spectrochemical Determination of Total Recoverable Elements", Method 200.2, Revision 2.8, Environmental Protection Agency, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268, 1994. Available from: the National Technical Information Service (NTIS), 5258 Port Royal Road, Springfield, Virginia 22161.

5 High levels of chromium, copper, mercury, silver, cobalt, or molybdenum may interfere with the analysis. Consult Method 3114, of "Standard Methods for the Examination of Water and Wastewater", 18th, 19th, 20th, or 21st edition, for more information.

6 Concentrations of lead in municipal sludge may exceed the working range of graphite furnace.

7 1993 Annual Book of ASTM Standards, Section 11.02, Water and Environmental Technology", American Society for Testing and Materials, 1993, 1916 Race Street, Philadelphia, PA 19103. Available from: the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.

8 Standard Methods for the Examination of Water and Wastewater, Joint Editorial Board, American Public Health Association, American Water Works Association, and Water Pollution Control Federation, 23rd Edition (2017), 22nd Edition (2012), 21st Edition (2005), 20th Edition (1998), 19th Edition (1995), and 18th Edition (1992).

9 "Standard Methods for the Examination of Water and Wastewater", Joint Editorial Board, American Public Health Association, American Water Works Association, and Water Pollution Control Federation, 2006. On-line subscription service available at http://www.standardmethods.org.

10 "Occurrence of Pathogens in Distribution and Marketing Municipal Sludges", EPA 600/1-87-014, Environmental Protection Agency, 1987. Available from: the National Technical Information Service, order # PB 88-154273/AS, 5285 Port Royal Road, Springfield, Virginia 22161.

11 Recommended for enumeration of target organism in sewage sludge.

12 Analysts may use Fluid Management Systems, Inc. PowerPrep system in place of manual cleanup provided that the analysis meet the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities.

13 EPA Method 1668A may be used to test for all PCB congeners. If this method is employed, all PCB congeners shall be delineated. Non-detects shall be treated as zero. The values that are between the limit of detection and the limit of quantitation shall be used when calculating the total value of all congeners. All results shall be added together and the total PCB concentration by dry weight reported. It is recognized that a number of the congeners will co-elute with others, so there will not be 209 results to sum.

14 EPA Method 8082A shall be used for PCB-Aroclor analysis and may be used for congener specific analysis as well. If congener specific analysis is performed using Method 8082A, the list of congeners tested shall include at least congener numbers 5, 18, 31, 44, 52, 66, 87, 101, 110, 138, 141, 151, 153, 170, 180, 183, 187, and 206 plus any other additional congeners which might be reasonably expected to occur in the particular sample. For either type of analysis, the sample shall be extracted using Soxhlet extraction Method 3540C or Pressurized Fluid Extraction Method 3545A. If Aroclor analysis is performed using Method 8082A, clean up steps of the extract shall be performed as necessary to remove interference and achieve as close to a limit of detection of 0.11 mg/kg as possible. If congener specific analysis is done using Method 8082A, clean up steps of the extract shall be performed as necessary to remove interference and to achieve as close to a limit of detection of 0.003 mg/kg as possible for each congener. If the aforementioned limits of detection cannot be achieved after using the appropriate clean up techniques, a reporting limit that is achievable for the Aroclors or each congener for sample shall be determined. This report limit should be reported and qualified indicating the presence of an interference. The laboratory conducting the analysis shall perform as many the following methods as necessary to remove interference:

3620C- Florisil

3640A- Gel Permeation

3630C- Silica Gel

3611B- Alumina

3660B- Sulfur Clean Up

3665A- Sulfuric Acid Clean Up.

15 "Method 1668A, Revision A: Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by HRGC/HRMS", EPA-821-R-00-002, Environmental Protection Agency, Office of Water, Washington, D.C., December 1999. Available from: the National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.

16 Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. U.S. EPA.

17 Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-14-009. September 2014. U.S. EPA.

18 Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.

19 On a monthly basis, at least ten blue colonies from positive samples must be verified using lauryl tryptose broth and EC broth, followed by count adjustment based on these results; and representative non-blue colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources.

20 Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014. U.S. EPA.

21 A 0.45-µm 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.

22 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.

Table ES

List of Approved Methods for Pharmaceutical Pollutants

Pharmaceuticals pollutants	CAS registry No.	Analytical method number 1,2
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 [DAGGER]	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	(see Note 3)	1624C / 1666

1 For compounds that also appear in Table C, test methods listed in Table C may also be used.

2 EPA Methods 1666, 1667, and 1671 listed in the table above are published in the compendium titled Analytical Methods for the Determination of Pollutants in Pharmaceutical Manufacturing Industry Wastewaters (EPA 821-B-98-016).

EPA Methods 502.2 and 524.2 have been incorporated by reference into 40 CFR 141.24 and are in Methods for the Determination of Organic Compounds in Drinking Water, EPA-600/4-88-039, December 1988, Revised, July 1991, and Methods for the Determination of Organic Compounds in Drinking Water-Supplement II, EPA-600/R-92-129, August 1992, respectively. These EPA test method compendia are available from the National Technical Information Service, NTIS PB91-231480 and PB92-207703, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll-free number is 800-553-6847. ASTM test methods D3371, D3695, and D4763 are available from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959.

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

Table F

Required Containers, Preservation Techniques, and Holding Times for wastewater

Parameter Number/Name	Container1	Preservation2,3	Maximum Holding Time4
Table A - Bacterial Tests
1-5. Coliform, total, fecal and E. coli	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22,23
6. Fecal streptococci	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22
7. Enterococci	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22
8. Salmonella	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22
Table A - Aquatic Toxicity Tests
9-12. Toxicity, acute and chronic	P, FP, G	Cool, <=6°C16	36 hours
Table B - Inorganic Tests
1. Acidity	P, FP, G	Cool, <=6°C18	14 days
2. Alkalinity	P, FP, G	Cool, <=6°C18	14 days
4. Ammonia	P, FP, G	Cool, <=6°C,18 H2SO4 to pH<2	28 days
9. Biochemical oxygen demand	P, FP, G	Cool, <=6°C18	48 hours
11. Bromide	P, FP, G	None required	28 days
14. Biochemical oxygen demand, carbonaceous	P, FP, G	Cool, <=6°C18	48 hours
15. Chemical oxygen demand	P, FP, G	Cool, <=6°C,18 H2SO4 to pH<2	28 days
16. Chloride	P, FP, G	None required	28 days
17. Chlorine, total residual	P, G	None required	Analyze within 15 minutes
21. Color	P, FP, G	Cool, <=6°C18	48 hours
23-24. Cyanide, total or available (or CATC) free	P, FP, G	Cool, <=6°C, 18 NaOH to pH<10,6 reducing agent if oxidizer present	14 days
25. Fluoride	P	None required	28 days
27. Hardness	P, FP, G	HNO3 or H2SO4 to pH<2	6 months
28. Hydrogen ion (pH)	P, FP, G	None required	Analyze within 15 minutes
31, 43. Kjeldahl and organic N	P, FP, G	Cool, <=6°C, 18 H2SO4 to pH<2	28 days
38. Nitrate	P, FP, G	Cool, <=6°C18	48 hours
39. Nitrate- nitrite	P, FP, G	Cool, <=6°C, 18 H2SO4 to pH<2	28 days
40. Nitrite	P, FP, G	Cool, <=6°C18	48 hours
41. Oil and grease	G	Cool, <=6°C, 18 HCl or H2SO4 to pH<2	28 days
42. Organic carbon	P, FP, G	Cool, <=6°C, 18 HCl, H2SO4 or H3PO4 to pH<2	28 days
44. Orthophosphate	P, FP, G	Cool, to <=6°C 18,24	Filter within 15 minutes; Analyze within 48 hours.
46. Oxygen, dissolved (Probe or Luminescence)	G, Bottle and top	None required	Analyze within 15 minutes
47. Oxygen, Dissolved Winkler	G, Bottle and top	Fix on site and store in dark	8 hours
48. Phenols	G	Cool, <=6°C, 18 H2SO4 to pH<2	28 days
49. Phosphorus (elemental)	G	Cool, <=6°C18	48 hours
50. Phosphorus, total	P, FP, G	Cool, <=6°C, 18 H2SO4 to pH<2	28 days
53. Residue, total	P, FP, G	Cool, <=6°C18	7 days
54. Residue, Filterable (TDS)	P, FP, G	Cool, <=6°C18	7 days
55. Residue, Nonfilterable (TSS)	P, FP, G	Cool, <=6°C18	7 days
56. Residue, Settleable	P, FP, G	Cool, <=6°C18	48 hours
57. Residue, Volatile	P, FP, G	Cool, <=6°C18	7 days
61. Silica	P or Quartz	Cool, <=6°C18	28 days
64. Specific conductance	P, FP, G	Cool, <=6°C18	28 days
65. Sulfate	P, FP, G	Cool, <=6°C18	28 days
66. Sulfide	P, FP, G	Cool, <=6°C,18 add zinc acetate plus sodium hydroxide to pH<9	7 days
67. Sulfite	P, FP, G	None required	Analyze within 15 minutes
68. Surfactants	P, FP, G	Cool, <=6°C18	48 hours
69. Temperature	P, FP, G	None required	Analyze
73. Turbidity	P, FP, G	Cool, <=6°C18	48 hours
Table B - Metals7
10. Boron	P, FP, or Quartz	HNO3 to pH<2	6 months
18. Chromium VI	P, FP, G	Cool, <=6°C, 18 pH = 9.3- 9.720	28 days
35. Mercury (CVAA)	P, FP, G	HNO3 to pH<2	28 days
35. Mercury (CVAFS)	FP, G; and FP-lined cap17	5 mL/L 12N HCl or 5 mL/L BrCl17	90 days17
3, 5-8, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51, 52, 58-60, 62, 63, 70-72, 74, 75. Metals, except boron, chromium VI, and mercury.	P, FP, G	HNO3 to pH<2, or at least 24 hours prior to analysis19	6 months
Table C - Organic Tests8
3, 4. Acrolein and acrylonitrile	G, FP-lined septum	Cool, <=6°C, 18 0.008% Na2S2O3, pH to 4-510	14 days10
119. Adsorbable Organic Halides (AOX)	G	Cool, <6°C, 0.008% Na2S2O3HNO3 to pH <2	Hold at least 3 days, but not more than 6 months
114-118. Alkylated phenols	G	Cool, <6°C, H2SO4 to pH <2	28 days until extraction, 40 days after extraction
7, 38. Benzidines11, 12	G, FP-lined cap	Cool, <=6°C,18 0.008% Na2S2O35	7 days until extraction13
29, 35-37, 63-65, 107. Chlorinated hydrocarbons11	G, FP-lined cap	Cool, <=6°C18	7 days until extraction, 40 days after extraction
120. Chlorinated Phenolics	Cool, <6°C, 0.008% Na2S2O3, H2SO4 to pH <2	30 days until acetylation, 30 days after acetylation.
15, 16, 21, 31, 87. Haloethers 11	G, FP-lined cap	Cool, <=6°C,18 0.008% Na2S2O35	7 days until extraction, 40 days after extraction
54, 55, 75, 79. Nitroaromatics and Isophorone11	G, FP-lined cap	Cool, <=6°C,18 store in dark, 0.008% Na2S2O35	7 days until extraction, 40 days after extraction
82-84. Nitrosamines11, 14	G, FP-lined cap	Cool, <=6°C,18 store in dark, 0.008% Na2S2O35	7 days until extraction, 40 days after extraction
88-94. PCBs 11	G, FP-lined cap	Cool, <=6°C18	1 year until extraction, 1 year after extraction
60-62, 66-72, 85, 86, 95-97, 102, 103. PCDDs/PCDFs 11
Aqueous Samples: Field and Lab Preservation	G	Cool, <=6°C18, 0.008% Na2S2O35, pH<9	1 year
Solids and Mixed-Phase Samples: Field Preservation	G	Cool, <=6°C18	7 days
Tissue Samples: Field Preservation	G	Cool, <=6°C18	24 hours
Solids, Mixed-Phase, and Tissue Samples: Lab Preservation	G	Freeze, <=-10°C	1 year
Per- and polyfluoroalkyl substances (PFAS)
Aqueous samples	HDPE or PP	Cool, <=6°C	28 days until extraction, 30 days after extraction
Sludge (biosolids) samples	HDPE or PP	Cool, <=6°C	28 days until extraction, 30 days after extraction
Tissue samples	PE freezer bags or Al foil	Frozen	1 year until extraction, 30 days after extraction
23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112. Phenols 11	G, FP-lined cap	Cool, <=6°C,18 0.008% Na2S2O3	7 days until extraction, 40 days after extraction
14, 17, 48, 50-52. Phthalate esters11	G, FP-lined cap	Cool, <=6°C18	7 days until extraction, 40 days after extraction
1, 2, 5, 8-12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons 11	G, FP-lined cap	Cool, <=6°C,18 store in dark, 0.008% Na2S2O35	7 days until extraction, 40 days after extraction
6, 57, 106. Purgeable aromatic hydrocarbons	G, FP-lined septum	Cool, <=6°C,18 0.008% Na2S2O35, HCl to pH 29	14 days9
13, 18-20, 22, 24-28, 34-37, 39-43, 45-47, 56, 76, 104, 105, 108-111, 113. Purgeable halocarbons.	G, FP-lined septum	Cool, <=6°C,18 0.008% Na2S2O35	14 days
Table D - Pesticides Tests:
1-70. Pesticides11	G, FP-lined cap	Cool, <= 6°C,18 pH 5-915	7 days until extraction, 40 days after extraction
Table E - Radiological Tests:
1-5. Alpha, beta and radium	P, FP, G	HNO3 to pH<2	6 months
Table H - Bacterial Tests:
1. E. coli	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22
2. Enterococci	PA, G	Cool, <10°C, 0.0008% Na2S2O35	8 hours.22
Table H - Protozoan Tests:
8.Cryptosporidium	LDPE; field filtration	1-10 °C	96 hours.21
9.Giardia	LDPE; field filtration	1-10 °C	96 hours.21

1 "P" is for polyethylene; "FP" is fluoropolymer (polytetrafluoroethylene (PTFE); Teflon®), or other fluoropolymer, unless stated otherwise in this Table F; "G" is glass; "PA" is any plastic that is made of a sterilizable material (polypropylene or other autoclavable plastic); "LDPE" is low density polyethylene.

2 Except where noted in this table and the method for the parameter, preserve each grab sample within 15 minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour composite sampler, refrigerate the sample at <= 6 °C during collection unless specified otherwise in this table or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <= 6 °C, unless specified otherwise in this table or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite sample within 15 minutes of collection.

The temperature of the samples shall be documented upon receipt at the laboratory. If the samples are shipped in crushed or cube ice (not "blue ice" packs) and solid ice is still present in the cooler, the lab may simply report the samples as "received on ice". If the ice has melted, the lab must report the either the temperature of the melt- water or of a temperature blank. A temperature blank is defined as an aliquot of deionized water, in an appropriate sample container, which is transported along with the samples. Since shipping simply with "blue ice" packs does not insure that samples are maintained at the appropriate temperatures, the sample collector must submit a temperature blank when using these ice packs for shipping.

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

4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before the start of analysis and still be considered valid. 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 EPA Regional Administrator under s. NR219.05). For a grab sample, the holding time begins at the time of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler); the holding time begins at the time of the end of collection of the composite sample. For a set of grab samples composited in the field or laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain sample stability. See 40 CFR 136.3(e) for details.

5 ASTM D7365-09a specifies treatment options for samples containing oxidants (e.g.,chlorine). Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses dechlorination procedures.

6 Sample collection and preservation: Collect a volume of sample appropriate to the analytical method in a bottle of the material specified. If the sample can be analyzed within 48 hours and sulfide is not present, adjust the pH to >12 with sodium hydroxide solution (e.g., 5% w/v), refrigerate as specified, and analyze within 48 hours. Otherwise, to extend the holding time to 14 days and mitigate interferences, treat the sample immediately using any or all of the following techniques, as necessary, followed by adjustment of the sample pH to >12 and refrigeration as specified.

There may be interferences that are not mitigated by approved procedures. Any procedure for removal or suppression of an interference may be employed, provided the laboratory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g., ferric ferrocyanide) or a strong cyanide complex (e.g., cobalt cyanide) are more accurately measured if the laboratory holds the sample at room temperature and pH >12 for a minimum of 4 hours prior to analysis, and performs UV digestion or dissolution under alkaline (pH=12) conditions, if necessary.

Sulfur: To remove elemental sulfur (S8), filter the sample immediately. If the filtration time will exceed 15 minutes, use a larger filter or a method that requires a smaller sample volume (e.g., EPA Method 335.4 or Lachat Method 01). Adjust the pH of the filtrate to >12 with NaOH, refrigerate the filter and filtrate, and ship or transport to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in ?g or mg), and divide by the original sample volume to obtain the cyanide concentration.

(1) Sulfide: If the sample contains sulfide as determined by lead acetate paper, or if sulfide is known or suspected to be present, immediately con- duct one of the volatilization treatments or the precipitation treatment as follows: Volatilization-Headspace expelling. In a fume hood or well- ventilated area, transfer 0.75 liter of sample to a 4.4-L collapsible container (e.g., CubitainerTM). Acidify with concentrated hydrochloric acid to pH <2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel the headspace into the fume hood or open area by collapsing the container without expelling the sample. Refill the headspace by expanding the container. Repeat expelling a total of five headspace volumes. Adjust the pH to >12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio. A larger volume of air will result in too great a loss of cyanide (> 10%). Dynamic stripping: In a fume hood or well ventilated area, transfer 0.75 liter of sample to a container of the material specified and acidify with concentrated hydrochloric acid to pH <2. Using a calibrated air sampling pump or flowmeter, purge the acidified sample into the fume hood or open area through a fritted glass aerator at a flow rate of 2.25 L/min for 4 minutes. Adjust the pH to >12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio. A larger volume of air will result in too great a loss of cyanide (>10%). Precipitation: If the sample contains particulate matter that would be removed by filtration, filter the sample prior to treatment to assure that cyanide associated with the particulate matter is included in the measurement. Ship or transport the filter to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in µg or mg), and divide by the original sample volume to obtain the cyanide concentration. For removal of sulfide by precipitation, raise the pH of the sample to >12 with NaOH solution, then add approximately 1 mg of powdered cadmium chloride for each mL of sample. For example, add approximately 500 mg to a 500-mL sample. Cap and shake the container to mix. Allow the precipitate to settle and test the sample with lead acetate paper. If necessary, add cadmium chloride but avoid adding an excess. Finally, filter through 0.45 micron filter.

Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate form the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in g or mg), and divide by the original sample volume to obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM D6888), it may be necessary to increase the ligand exchange reagent to offset any excess of cadmium chloride.

(2) Sulfite, thiosulfate, or thiocyanate: If sulfite, thiosulfate, or thiocyanate is known or suspected to be present, use UV digestion with a glass coil (Method Kelada-01) or ligand exchange (Method OIA-1677) to preclude cyanide loss or positive interference.

(3) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be present, treat the sample with 20 mL of 3.5% ethylenediamine solution per liter of sample.

(4) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the distillation flask, a reduction in the pH of the absorber solution, and incomplete cyanide spike recovery. When significant carbonate is present, adjust the pH to >= 12 using calcium hydroxide instead of sodium hydroxide. Allow the precipitate to settle and decant or filter the sample prior to analysis (also see Standard Method 4500-CN.B.3.d).

(5) Chlorine, hypochlorite, or other oxidant: Treat a sample known or suspected to contain chlorine, hypochlorite, or other oxidant as directed in footnote 57 For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives. For a composite sample collected with an automated sampler, filter the sample within 15 minutes after completion of collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will be compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically.

7 For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives. For a composite sample collected with an automated sampler, filter the sample within 15 minutes after completion of collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will be compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically.

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

9 If the sample is not adjusted to pH < 2, then the sample must be analyzed within seven days of sampling.

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

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

12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine.

13 Extracts may be stored up to 30 days at < 0 °C.

14 For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours of sampling.

15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.

16 Place sufficient ice 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, immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 °C prior to test initiation.

17 Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48 hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669. If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be filtered in a designated clean area in the field within the time period necessary to maintain sample integrity. A sample that has been collected for determination of total or dissolved trace level mercury must be analyzed within 90 days of sample collection.

18 Aqueous samples must be preserved at <=6 °C, and should not be frozen unless data demonstrating that sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the regulatory authority. Also, for purposes of NPDES monitoring, the specification of "<=6 °C" is used in place of the "4 °C" and "< 4 °C" sample temperature requirements listed in some methods. It is not necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three significant figures are specified so that rounding down to 6 °C may not be used to meet the <=6 °C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than 15 minutes).

19 An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and holding time requirements in the approved metals methods.

20 To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6. The allowance in this footnote supersedes preservation and holding time requirements in the approved hexavalent chromium methods, unless this supersession would compromise the measurement, in which case requirements in the method must be followed.

21 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.

22 Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection.

23 For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B aerobically digested, and Class B anaerobically digested.

24 The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-available form of orthophosphorus (i.e., that which passes through a 0.45-micron filter), hence the requirement to filter the sample immediately upon collection (i.e., within 15 minutes of collection).

Note: If the EPA Office of Water publishes a final approved 1600 series isotope dilution method for the analysis of PFAS in aqueous, sludge, biosolids, and tissue matrices, the department recommends use of the final approved EPA method.

Table G

Test Methods for Pesticide Active Ingredients

EPA survey code	Pesticide name	CAS No.	EPA analytical method No.(s) 3
8	Triadimefon	43121-43-3	1656, 507, 633, 525.1, 525.2
12	Dichlorvos	62-73-7	1657, 507, 525.1, 525.2, 622
16	2,4-D; 2,4-D Salts and Esters [2,4-Dichloro-phenoxyacetic acid]	94-75-7	1658, 515.1, 515.2, 555, 615
17	2,4-DB; 2,4-DB Salts and Esters [2,4-Dichlorophenoxybutyric acid]	94-82-6	1658, 515.1, 515.2, 555, 615
22	Mevinphos	7786-34-7	1657, 507, 525.1, 525.2, 622
25	Cyanazine	21725-46-2	507, 629
26	Propachlor	1918-16-7	1656, 508, 608.1, 525.1, 525.2
27	MCPA; MCPA Salts and Esters [2-Methyl-4-chlorophenoxyacetic acid]	94-74-6	1658, 555, 615
30	Dichlorprop; Dichlorprop Salts and Esters [2-(2,4-Dichlorophenoxy) propionic acid]	120-36-5	1658, 515.1, 515.2, 555, 615
31	MCPP; MCPP Salts and Esters [2-(2-Methyl-4-chlorophenoxy) propionic acid]	93-65-2	1658, 555, 615
35	TCMTB [2-(Thiocyanomethylthio) benzo-thiazole]	21564-17-0	637
39	Pronamide	23950-58-5	507, 525.1, 525.2, 633.1
41	Propanil	709-98-8	1656, 632.1
45	Metribuzin	21087-64-9	1656, 507, 525.1, 525.2, 633
52	Acephate	30560-19-1	1656, 1657
53	Acifluorfen	50594-66-6	515.1, 515.2, 555
54	Alachlor	15972-60-8	1656, 505, 507, 525.1, 525.2, 645
55	Aldicarb	116-06-3	531.1
58	Ametryn	834-12-8	507, 525.2, 619
60	Atrazine	1912-24-9	1656, 505, 507, 525.1, 525.2, 619
62	Benomyl	17804-35-2	631
68	Bromacil; Bromacil Salts and Esters	314-40-9	1656, 507, 525.1, 525.2, 633
69	Bromoxynil	1689-84-5	1625, 1661
69	Bromoxynil octanoate	1689-99-2	1656
70	Butachlor	23184-66-9	1656, 507, 525.1, 525.2, 645
73	Captafol	2425-06-1	1656
75	Carbaryl [Sevin]	63-25-2	531.1, 553, 632
76	Carbofuran	1563-66-2	531.1, 632
80	Chloroneb	2675-77-6	1656, 508, 525.1, 525.2, 608.1
82	Chlorothalonil	1897-45-6	1656, 508, 525.1, 525.2, 608.2
84	Stirofos	961-11-5	1657, 507, 525.1, 525.2, 622
86	Chlorpyrifos	2921-88-2	1657, 508, 622
90	Fenvalerate	51630-58-1	1660
103	Diazinon	333-41-5	1657, 507, 525.2, 614, 622
107	Parathion methyl	298-00-0	1657, 614, 622
110	DCPA [Dimethyl 2,3,5,6-tetrachloro-terephthalate]	1861-32-1	1656, 508, 525.1, 525.2, 515.1 2, 515.2 2, 608.2
112	Dinoseb	88-85-7	1658, 515.1, 515.2, 555, 615
113	Dioxathion	78-34-2	1657, 614.1
118	Nabonate [Disodium cyanodithioimidocarbonate]	138-93-2	630.1
119	Diuron	330-54-1	553, 632
123	Endothall	145-73-3	548, 548.1
124	Endrin	72-20-8	1656, 505, 508, 525.1, 525.2, 608, 617
125	Ethalfluralin	55283-68-6	1656, 627 See footnote 1
126	Ethion	563-12-2	1657, 614, 614.1
127	Ethoprop	13194-48-4	1657, 507, 525.1, 525.2, 622
132	Fenarimol	60168-88-9	1656, 507, 525.1, 525.2, 633.1
133	Fenthion	55-38-9	1657, 622
138	Glyphosate [N-(Phosphonomethyl) glycine]	1071-83-6	547
140	Heptachlor	76-44-8	1656, 505, 508, 525.1, 525.2, 608, 617
144	Isopropalin	33820-53-0	1656, 627
148	Linuron	330-55-2	553, 632
150	Malathion	121-75-5	1657, 614
154	Methamidophos	10265-92-6	1657
156	Methomyl	16752-77-5	531.1, 632
158	Methoxychlor	72-43-5	1656, 505, 508, 525.1, 525.2, 608.2, 617
172	Nabam	142-59-6	630, 630.1
173	Naled	300-76-5	1657, 622
175	Norflurazon	27314-13-2	1656, 507, 525.1, 525.2, 645
178	Benfluralin	1861-40-1	1656, 627 See footnote 1
182	Fensulfothion	115-90-2	1657, 622
183	Disulfoton	298-04-4	1657, 507, 525,2, 614, 622
185	Phosmet	732-11-6	1657, 622.1
186	Azinphos Methyl	86-50-0	1657, 614, 622
192	Organo-tin pesticides	12379-54-3	200.7, 200.9, Ind-01
197	Bolstar	35400-43-2	1657, 622
203	Parathion	56-38-2	1657, 614
204	Pendimethalin	40487-42-1	1656
205	Pentachloronitrobenzene	82-68-8	1656, 608.1, 617
206	Pentachlorophenol	87-86-5	1625, 515.2, 555, 515.1, 525.1, 525.2, 625
208	Permethrin	52645-53-1	1656, 1660, 508, 525.1, 525.2, 608.2
212	Phorate	298-02-2	1657, 622
218	Busan 85 [Potassium dimethyldithiocarbamate]	128-03-0	630, 630.1
219	Busan 40 [Potassium N-hydroxymethyl-N-methyldithiocarbamate]	51026-28-9	630, 630.1
220	KN Methyl [Potassium N-methyl-dithiocarbamate]	137-41-7	630, 630.1
223	Prometon	1610-18-0	507, 525.2, 619
224	Prometryn	7287-19-6	507, 525.1, 525.2, 619
226	Propazine	139-40-2	1656, 507, 525.1, 525.2, 619
230	Pyrethrin I	121-21-1	1660
232	Pyrethrin II	121-29-9	1660
236	DEF [S,S,S-Tributyl phosphorotrithioate]	78-48-8	1657
239	Simazine	122-34-9	1656, 505, 507, 525.1, 525.2, 619
241	Carbam-S [Sodium dimethyldithio-carbamate]	128-04-1	630, 630.1
243	Vapam [Sodium methyldithiocarbamate]	137-42-8	630, 630.1
252	Tebuthiuron	34014-18-1	507, 525.1, 525.2
254	Terbacil	5902-51-2	1656, 507, 525.1, 525.2, 633
255	Terbufos	13071-79-9	1657, 507, 614.1, 525.1, 525.2
256	Terbuthylazine	5915-41-3	1656, 619
257	Terbutryn	886-50-0	507, 525.1, 525.2, 619
259	Dazomet	533-74-4	1659, 630, 630.1
262	Toxaphene	8001-35-2	1656, 505, 508, 525.1, 525.2, 608, 617
263	Merphos [Tributyl phosphorotrithioate]	150-50-5	1657, 507, 525.1, 525.2, 622
264	Trifluralin 1	1582-09-8	1656, 508, 525.2, 617, 627
268	Ziram [Zinc dimethyldithiocarbamate]	137-30-4	630, 630.1

1 Monitor and report as total Trifluralin.

2 Applicable to the analysis of DCPA degradates.

3 EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are available in Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, Revision I, August 1993, U.S. EPA. EPA Methods 200.9 and 505 through 555 are available in Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, August 1993, U.S. EPA. The full text of Methods 608, 625 and 1625 are provided at Appendix A of this Part 136. The full text of Method 200.7 is provided at appendix C of this part 136.

Table H

List of Approved Microbiological Methods for Ambient Water

Parameter and units	Method 1	EPA	Standard Methods33	AOAC, ASTM, USGS	Other
Bacteria:

1. Coliform (fecal), number per 100 mL	Most Probable Number (MPN), 5 tube, 3 dilution, or	p. 1323	9221 E-2014, 9221 F.2-2014 32
Membrane filter (MF),2 single step	p. 1243	9222 D-201526	B-0050-854
2. Coliform (total), number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1143	9221 B-2014
MF,2 single step or two step	p. 1083	9222 B-201527	B-0025-854
MF2 with enrichment	p. 1113	9222 (B + B.4e)-201527
3. E. coli, number per 100 mL	MPN,5,7,13 multiple tube, or	9221 B.3-2014/ 9221 F-201410,12,32
Multiple tube/multiple well, or	9223 B-201611	991.15 9	Colilert® 11,15Colilert-18®11,14,15
MF,2, 5, 6, 7 two step, or	1103.118	9222 B-2015/ 9222 I-2015,17 9213 D-2007	D5392-938
Single step	1603,19 160420	m-ColiBlue24,®16 KwikCountTM EC28,29
4. Fecal streptococci, number per 100 mL	MPN, 5 tube, 3 dilution, or	p. 1393	9230 B-2013
MF,2 or	p. 1363	9230 C-201330	B-0055-854
Plate count	p. 1433
5. Enterococci, number per 100 mL	MPN5,7, multiple tube/ multiple well, or	9230 D-2013	D6503-998	Enterolert®11,21
MF, 2, 5, 6,7 two step, or	1106.122	9230 C-201330	D5259-928
Single step, or	160023	9230 C-201330
Plate count	p. 1433
Protozoa:
6. Cryptosporidium	Filtration/IMS/FA	1622,24 1623,25 1623.125,31
7. Giardia	Filtration/IMS/FA	1623,25 1623.125,31

1 The method must be specified when results are reported.

2 A 0.45-µm 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 Microbiological Methods for Monitoring the Environment, Water and Wastes. EPA/600/8-78/017. 1978. U.S. EPA.

5 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.

6 When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.

7 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.

8 Annual Book of ASTM Standards-Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.

9 Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.

10 The multiple-tube fermentation test is used in 9221B.3-2014. 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.

11 These tests are collectively known as defined enzyme substrate tests.

12 After prior enrichment in a presumptive medium for total coliform using 9221B.3-2014, 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-2014. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 µg/mL of MUG may be used.

13 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.

14 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.

15 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories Inc.

16 A description of the mColiBlue24® test may be obtained from Hach Company.

17 Subject coliform positive samples determined by 9222B-2015 or other membrane filter procedure to 9222I-2015 using NA-MUG media.

18 Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-10-002. March 2010. U.S. EPA.

19 Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.

20 Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium), EPA 821-R-02-024. September 2002. U.S. EPA.

21 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc.

22 Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), EPA-821-R-09-015. December 2009. U.S. EPA.

23 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-ÃŽ²-D-Glucoside Agar (mEI), EPA-821-R-14-011. September 2014. U.S. EPA.

24 Method 1622 uses a 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. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. U.S. EPA.

25 Methods 1623 and 1623.1 use a 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. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002. December 2005. US EPA. Method 1623.1: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA 816-R-12-001. January 2012. U.S. EPA.

26 On a monthly basis, at least ten blue colonies from positive samples must be verified using lauryl tryptose broth and EC broth, followed by count adjustment based on these results; and representative non-blue colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources.

27 On a monthly basis, at least ten sheen colonies from positive samples must be verified using lauryl tryptose broth and brilliant green lactose bile broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources.

28 A description of KwikCount® EC may be obtained from Micrology Laboratories LLC.

29 Approved for the analyses of E. coli in freshwater only.

30 Verification of colonies by incubation of BHI agar at 10 ± 0.5 ®C for 48 ± 3 h is optional. As per the Errata to the 23rd Edition of Standard Methods for the Examination of Water and Wastewater, "Growth on a BHI agar plate incubated at 10 ± 0.5 ®C for 48 ± 3 h is further verification that the colony belongs to the genus Enterococcus."

31 Method 1623.1 includes updated acceptance criteria for IPR, OPR, and MS/MSD and clarifications and revisions based on the use of Method 1623 for years and technical support questions.

32 9221 F.2-2014: This procedure allows for simultaneous detection of E. coli and thermotolerant coliforms by adding inverted vials to EC-MUG; the inverted vials collect gas produced by thermotolerant coliforms.

33 Standard Methods for the Examination of Water and Wastewater, Joint Editorial Board, American Public Health Association, American Water Works Association, and Water Pollution Control Federation, 23rd Edition (2017), 22nd Edition (2012), 21st Edition (2005), 20th Edition (1998), 19th Edition (1995), and 18th Edition (1992).

Copies of the publications referenced in Tables A-H are available for inspection at the offices of the department of natural resources and the legislative reference bureau. Many of these materials are also available through inter-library loan.

Disclaimer: These regulations may not be the most recent version. Wisconsin may have more current or accurate information. We make no warranties or guarantees about the accuracy, completeness, or adequacy of the information contained on this site or the information linked to on the state site. Please check official sources.

This site is protected by reCAPTCHA and the Google Privacy Policy and Terms of Service apply.

Wisconsin Administrative CodeDepartment of Natural ResourcesNR 200-299 - Environmental Protection - Wisconsin Pollutant Discharge Elimination SystemChapter NR 219 - Analytical Test Methods And ProceduresSection NR 219.04 - Identification of test procedures

Wisconsin Administrative Code
Department of Natural Resources
NR 200-299 - Environmental Protection - Wisconsin Pollutant Discharge Elimination System
Chapter NR 219 - Analytical Test Methods And Procedures
Section NR 219.04 - Identification of test procedures