CR 13-112 Rule Text

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12. Place where comments are to be submitted and deadline for submission.

Public hearings were held on January 27, 2014, The deadline for written comments was also January 27, 2014.

101 S Webster St (use this for overnight deliveries)

PO Box 7921

Madison WI 53707-7921

Program fax: [phone]

Program email: [e-mail]  

Written comments could also be submitted to the Department using the Wisonsin Administrative Rules Internet Web site at http://adminrules.wisconsin.gov.

A summary of comments received on the rule is provided as an attachment.

(See PDF for image)

SECTION 1. NR 157.21 is amended to read:

NR 157.21 Approval of alternate test procedures. Applications for approval of alternate test procedures for wastewater analysis must be made as directed in s. NR 219.05 219.033.

SECTION 2. NR 219.02 (1)(intro.) and (2) are amended to read:

NR 219.02 Applicability. (1)(intro.) The procedures prescribed herein shall, except as provided in s. NR 219.06 219.037, be used in the determination of concentrations and quantities of pollutant parameters as required for:

NR 219.02 (2) Section NR 219.06 219.037 requires that laboratories conducting tests under this chapter be certified, registered, or approved under ch. NR 149.

SECTION 3. NR 219.04 (1), (2) and (4)(Note) are amended to read:

NR 219.04 Identification of test procedures. (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 E H. Parameters or pollutants, for which sludge analytical methods are approved, are listed together with test procedure descriptions and references in table EM. Metals samples digestion procedures and references are listed in table BM. 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 219.05 219.033 and 149.12.

NR 219.04 (2) Sample preservation procedures. Sample preservation techniques, container materials, and maximum allowable holding times for parameters identified in tables A to EH 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.

NR 219.04 (4) Note: Copies of the publications referenced in Tables A−F 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.

SECTION 4. NR 219.04 Table A is repealed and recreated to read:

Table A—List of Approved Biological Methods for Wastewater and Sewage Sludge

Parameter and units

Analytical Technology 1

EPA

Standard methods 27

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. 132 3 1680 11,15 1681 11,20

9221 C-2006 9221 E-2006

Membrane filter (MF) 2, single step

p. 124 3

9222 D-1997

B-0050-85 4

2. Coliform (fecal) in presence of chlorine, number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 132 3

9221 C-2006 9221 E-2006

MF 2, single step 5

p. 124 3

9222 D-1997

3. Coliform (total), number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 114 3

9221 B-2006

MF 2, single step or two step

p. 108 3

9222 B-1997

B-0025-85 4

4. Coliform (total), in presence of chlorine, number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 114 3

9221 B-2006

MF 2 with enrichment 5

p. 111 3

9222 (B + B.5c)−1997

5.E. coli,number per 100 mL 21

MPN 6,8,16 multiple tube, or

9221B.1-2006/ 9221F-2006 12,14

multiple tube/multiple well, or

9223 B-200 413

991.15 10

Colilert® 13, 18 Colilert-18® 13,17,18

MF 2,6,7,8 single step

1603 22

mColiBlue ®19

6. Fecal streptococci, number per 100 mL

MPN, 5 tube 3 dilution, or

p. 139 3

9230 B-2007

MF 2, or

p. 136 3

9230 C-2007

B-0055-85 4

Plate count

p. 143 3

7. Enterococci, number per 100 mL 22

MPN 6, 8, multiple tube/multiple well, or

D6503-99 9

Enterolert®13, 24

MF 2, 6, 7, 8 single step or

1600 25

9230 C-2007

Plate count

p. 143 3

8.Salmonella,number per gram dry weight 11

MPN multiple tube

1682 23

Aquatic Toxicity:

9. 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

10. 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. US 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.1-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.

13 These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme β-glucuronidase produced byE. coli.

14 After prior enrichment in a presumptive medium for total coliform using 9221B.1-2006, 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-2006. 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-10-003. April 2010. 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 andE. colithat 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. 1 IDEXX Drive, Westbrook, ME 04092.

19 A description of the mColiBlue24® test, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.

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

21 Recommended for enumeration of target organism in wastewater effluent.

22 Method 1603:Escherichia coli(E. coli) in Water by Membrane Filtration Using Modified membrane-ThermotolerantEscherichia coliAgar (modified mTEC), EPA-821-R-09-007. December 2009. U.S. EPA. U.S. Environmental Protection Agency, Office of Water, Washington, DC

23 Method 1682:Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-06-014. July 2006. U.S. EPA.

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

25 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-β-D-Glucoside Agar (mEI), EPA-821-R-09-016. December 2009. U.S. EPA.

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.SECTION 5. NR 219.04 Table B is repealed and recreated to read:

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

350.130, Rev. 2.0 (1993)

4500-NH3G-1997 4500-NH3H-1997.

I-4523-85 2

Automated electrode

Note 7

Ion Chromatography

D6919-09

5. Antimony—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,4 mg/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,4 mg/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. Beryllium—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 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)

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 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)

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,4followed 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,6followed 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-H+B-2000

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-NorgB-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-NH3 G-1997, 4500-NH3 H-1997

Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods

4500-NH3F-1997

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-NorgD-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,4 mg/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-4540-852, 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-2001 38

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

973.473, p. 14 24

Heated persulfate or UV persulfate oxidation

5310 C- 2000 5310 D-2000

D4839-03

973.473,, 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

973.563, 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, micromhos/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

993.143, 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.