CR 13-112 Rule Text

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 NR 219.04 Table B is repealed and recreated to read: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

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 BOD5test 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 BOD5may 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. Avail- able 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/ALPKEM, 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 StablCalTMor 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: [phone], Fax: [phone].

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.

60 Analysts 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 BOD5and 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.SECTION 6. NR 219.04 Table BM is repealed.

SECTION 7. NR 219.04 Table C is repealed and recreated to read:

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

Spectro-photometric

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) [prev.: bis(2-Chloroisopropyl) ether]

GC

611

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

1668A14

93. PCB-1232, (Aroclor or congeners)12,13

GC

608

Note 3, p. 43; Note 8

GC/MS

625

6410 B-2000

HRGC/ MS

1668A14

94. PCB-1242, (Aroclor or congeners)12,13

GC

608

Note 3, p. 43; Note 8

GC/MS

625

6410 B-2000

HRGC/ MS

1668A14

95. PCB-1248, (Aroclor or congeners)12,13

GC

608

GC/MS

625

6410 B-2000

HRGC/ MS

1668A14

96. PCB-1254, (Aroclor or congeners)12,13

GC

608

Note 3, p. 43; Note 8

GC/MS

625

6410 B-2000

HRGC/ MS

1668A14

97. PCB-1260, (Aroclor or congeners)12,13

GC

608

Note 3, p. 43; Note 8

GC/MS

625

6410 B-2000

HRGC/ MS

1668A14

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

1613B10

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

165311

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

165311

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

165311

6410 B-2000

115. 3,4,6−Trichlorocatechol

GC

6420 B-2000

GC/MS

165311

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

1650 11

133. Chlorinated Phenolics

In Situ Acetylation and GC/MS

1653 11

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 Part136, Appendix B, Definition and Procedure for the Determination of the Method Detection Limit.