Identification of test procedures.

§ 136.3 Identification of test procedures.

(a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, IF, IG, and IH of this section. The methods listed in Tables IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see paragraph (b) of this section, with the exception of EPA Methods 200.7, 601–613, 624.1, 625.1, 1613, 1624, and 1625. The full texts of Methods 601–613, 624.1, 625.1, 1613, 1624, and 1625 are printed in appendix A of this part, and the full text of Method 200.7 is printed in appendix C of this part. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part. In the event of a conflict between the reporting requirements of 40 CFR parts 122 and 125 and any reporting requirements associated with the methods listed in these tables, the provisions of 40 CFR parts 122 and 125 are controlling and will determine a permittee's reporting requirements. The full texts of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and IH. The date after the method number indicates the latest editorial change of the method. The discharge parameter values for which reports are required must be determined by one of the standard analytical test procedures incorporated by reference and described in Tables IA, IB, IC, ID, IE, IF, IG, and IH or by any alternate test procedure which has been approved by the Administrator under the provisions of paragraph (d) of this section and §§ 136.4 and 136.5. Under certain circumstances (paragraph (c) of this section, § 136.5(a) through (d) or 40 CFR 401.13,) other additional or alternate test procedures may be used.

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

Parameter and units Method 1EPA Standard methods AOAC, ASTM, USGS Other
Bacteria
1. Coliform (fecal), number per 100 mL or number per gram dry weightMost Probable Number (MPN), 5 tube, 3 dilution, orp. 132,3 1680,11 15 1681 11 209221 E–2014
Membrane filter (MF) 2 5, single stepp. 124 39222 D–2015 29B–0050–85 4
2. Coliform (fecal), number per 100 mLMPN, 5 tube, 3 dilution, orp. 132 39221 E–2014; 9221 F–2014 33
Multiple tube/multiple well, orColilert-18®.13 18 28
MF 2 5, single step 5p. 124 39222 D–2015 29
3. Coliform (total), number per 100 mLMPN, 5 tube, 3 dilution, orp. 114 39221 B–2014
MF 2 5, single step or two stepp. 108 39222 B–2015 30B–0025–85 4
MF 2 5, with enrichmentp. 111 39222 B–2015 30
4. E. coli, number per 100 mLMPN 6 8 16 multiple tube, or9221 B2014/9221 F–2014 12 14 33
multiple tube/multiple well, or9223 B–2016 13991.15 10Colilert® 13 18
Colilert-18® 13 17 18
MF 2 5 6 7 8, two step, or9222 B–2015/9222 I–2015 31
Single step1603 21m-ColiBlue24®.19
5. Fecal streptococci, number per 100 mLMPN, 5 tube, 3 dilution, orp. 139 39230 B–2013
MF 2, orp. 136 39230 C–2013 32B–0055–85 4
Plate countp. 143 3
6. Enterococci, number per 100 mLMPN, 5 tube, 3 dilution, orp. 139 39230 B–2013
MPN 6 8, multiple tube/multiple well, or9230 D–2013D6503–99 9Enterolert®.13 23
MF 2 5 6 7 8 single step or1600 249230 C–2013 32
Plate countp. 143 3
7. Salmonella, number per gram dry weight 11MPN multiple tube1682 22
Aquatic Toxicity
8. Toxicity, acute, fresh water organisms, LC50, percent effluentWater flea, Cladoceran, Ceriodaphnia dubia acute2002.0 25
Water fleas, Cladocerans, Daphnia pulex and Daphnia magna acute2021.0 25
Fish, Fathead minnow, Pimephales promelas, and Bannerfin shiner, Cyprinella leedsi, acute2000.0 25
Fish, Rainbow trout, Oncorhynchus mykiss, and brook trout, Salvelinus fontinalis, acute2019.0 25
9. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC50, percent effluentMysid, Mysidopsis bahia, acute2007.0 25.
Fish, Sheepshead minnow, Cyprinodon variegatus, acute2004.0 25
Fish, Silverside, Menidia beryllina, Menidia menidia, and Menidia peninsulae, acute.2006.0 25.
10. Toxicity, chronic, fresh water organisms, NOEC or IC25, percent effluentFish, Fathead minnow, Pimephales promelas, larval survival and growth1000.0 26
Fish, Fathead minnow, Pimephales promelas, embryo-larval survival and teratogenicity1001.0 26
Water flea, Cladoceran, Ceriodaphnia dubia, survival and reproduction1002.0 26
Green alga, Selenastrum capricornutum, growth1003.0 26
11. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC25, percent effluentFish, Sheepshead minnow, Cyprinodon variegatus, larval survival and growth1004.0 27.
Fish, Sheepshead minnow, Cyprinodon variegatus, embryo-larval survival and teratogenicity1005.0 27
Fish, Inland silverside, Menidia beryllina, larval survival and growth1006.0 27
Mysid, Mysidopsis bahia, survival, growth, and fecundity1007.0 27
Sea urchin, Arbacia punctulata, fertilization1008.0 27

Table IA notes:

1 The method must be specified when results are reported.

2 A 0.45-µm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.

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

4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS.

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

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

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

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

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

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

11 Recommended for enumeration of target organism in sewage sludge.

12 The multiple-tube fermentation test is used in 9221B.2–2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.

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

14 After prior enrichment in a presumptive medium for total coliform using 9221B.2–2014, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F–2014. Commercially available EC–MUG media or EC media supplemented in the laboratory with 50 µg/mL of MUG may be used.

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

16 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000 and the MPN calculated from the table provided by the manufacturer.

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

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

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

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

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

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

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

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

25 Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA–821–R–02–012. Fifth Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016.

26 Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA–821–R–02–013. Fourth Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016.

27 Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA–821–R–02–014. Third Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016.

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

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

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

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

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

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

Table IB—List of Approved Inorganic Test Procedures

Parameter Methodology 58EPA 52Standard methods 84ASTM USGS/AOAC/Other
1. Acidity, as CaCO3, mg/LElectrometric endpoint or phenolphthalein endpoint2310 B–2011D1067–16I–1020–85. 2
2. Alkalinity, as CaCO3, mg/LElectrometric or Colorimetric titration to pH 4.5, Manual2320 B–2011D1067–16973.43, 3 I–1030–85. 2
Automatic310.2 (Rev. 1974) 1I–2030–85. 2
3. Aluminum—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 D–2011 or 3111 E–2011I–3051–85. 2
AA furnace3113 B–2010.
STGFAA200.9, Rev. 2.2 (1994)/
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
Direct Current Plasma (DCP) 36D4190–15See footnote. 34
Colorimetric (Eriochrome cyanine R)3500–Al B–2011.
4. Ammonia (as N), mg/LManual distillation 6 or gas diffusion (pH > 11), followed by any of the following:350.1, Rev. 2.0 (1993)4500–NH3 B–2011973.49. 3
NesslerizationD1426–15 (A)973.49, 3 I–3520–85. 2
Titration4500–NH3 C–2011.
Electrode4500–NH3 D–2011 or E–2011D1426–15 (B).
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods4500–NH3 F–2011See footnote. 60
Automated phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods350.1, 30 Rev. 2.0 (1993)4500–NH3 G–2011 4500–NH3 H–2011I–4523–85, 2 I–2522–90. 80
Automated electrodeSee footnote. 7
Ion ChromatographyD6919–17.
Automated gas diffusion, followed by conductivity cell analysisTimberline Ammonia-001. 74
Automated gas diffusion followed by fluorescence detector analysisFIAlab100. 82
5. Antimony—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011.
AA furnace3113 B–2010.
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
6. Arsenic-Total, 4 mg/LDigestion, 4 followed by any of the following:206.5 (Issued 1978) 1.
AA gaseous hydride3114 B–2011 or 3114 C–2011D2972–15 (B)I–3062–85. 2
AA furnace3113 B–2010D2972–15 (C)I–4063–98. 49
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05. 70
Colorimetric (SDDC)3500–As B–2011D2972–15 (A)I–3060–85. 2
7. Barium-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 D–2011I–3084–85. 2
AA furnace3113 B–2010D4382–18.
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCP 36See footnote. 34
8. Beryllium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 D–2011 or 3111 E–2011D3645–15 (A)I–3095–85. 2
AA furnace3113 B–2010D3645–15 (B).
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCPD4190–15See footnote. 34
Colorimetric (aluminon)See footnote. 61.
9. Biochemical oxygen demand (BOD5), mg/LDissolved Oxygen Depletion5210 B–2016 85973.44, 3 p. 17, 9 I–1578–78, 8 See footnote. 10, 63
10. Boron—Total, 37 mg/LColorimetric (curcumin)4500–B B–2011I–3112–85. 2
ICP/AES200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPD4190–15S7ee footnote. 34
11. Bromide, mg/LElectrodeD1246–16I–1125–85. 2
Ion Chromatography300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)4110 B–2011, C–2011, D–2011D4327–17993.30, 3 I–2057–85. 79
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
12. Cadmium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D3557–17 (A or B)974.27, 3 p. 37, 9 I–3135–85 2 or I–3136–85. 2
AA furnace3113 B–2010D3557–17 (D)I–4138–89. 51
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–1472–85 2 or I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCP 36D4190–15See footnote. 34
Voltammetry 11D3557–17 (C).
Colorimetric (Dithizone)3500–Cd–D–1990.
13. Calcium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011D511–14 (B)I–3152–85. 2
ICP/AES200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPSee footnote. 34
Titrimetric (EDTA)3500-Ca B–2011D511–14 (A).
Ion ChromatographyD6919–17.
14. Carbonaceous biochemical oxygen demand (CBOD5), mg/L 12Dissolved Oxygen Depletion with nitrification inhibitor5210 B–2016 85See footnote.35 63
15. Chemical oxygen demand (COD), mg/LTitrimetric410.3 (Rev. 1978) 15220 B–2011 or C–2011D1252–06(12) (A)973.46, 3 p. 17, 9 I–3560–85. 2
Spectrophotometric, manual or automatic410.4, Rev. 2.0 (1993)5220 D–2011D1252–06(12) (B)See footnotes.13 14 83, I–3561–85. 2
16. Chloride, mg/LTitrimetric: (silver nitrate)4500–Cl- B–2011D512–12 (B)I–1183–85. 2
(Mercuric nitrate)4500–Cl- C–2011D512–12 (A)973.51, 3 I–1184–85. 2
Colorimetric: manualI–1187–85. 2
Automated (ferricyanide)4500–Cl- E–2011I–2187–85. 2
Potentiometric Titration4500–Cl- D–2011.
Ion Selective ElectrodeD512–12 (C).
Ion Chromatography300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)4110 B–2011 or 4110 C–2011D4327–17993.30, 3 I–2057–90. 51
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
17. Chlorine-Total residual, mg/LAmperometric direct4500–Cl D–2011D1253–14.
Amperometric direct (low level)4500-Cl E–2011.
Iodometric direct4500-Cl B–2011.
Back titration ether end-point 154500-Cl C–2011.
DPD–FAS4500–Cl F–2011.
Spectrophotometric, DPD4500–Cl G–2011.
ElectrodeSee footnote. 16
17A. Chlorine-Free Available, mg/LAmperometric direct4500–Cl D–2011D1253–14.
Amperometric direct (low level)4500–Cl E–2011.
DPD–FAS4500-Cl F–2011.
Spectrophotometric, DPD4500-Cl G–2011.
18. Chromium VI dissolved, mg/L0.45-micron filtration followed by any of the following:
AA chelation-extraction3111 C–2011I–1232–85. 2
Ion Chromatography218.6, Rev. 3.3 (1994)3500-Cr C–2011D5257–17993.23. 3
Colorimetric (diphenyl-carbazide)3500–Cr B–2011D1687–17 (A)I–1230–85. 2
19. Chromium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011D1687–17 (B)974.27, 3 I–3236–85. 2
AA chelation-extraction3111 C–2011.
AA furnace3113 B–2010D1687–17 (C)I–3233–93. 46
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003), 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05 70 I–4472–97. 81
DCP 36D4190–15See footnote. 34
Colorimetric (diphenyl-carbazide)3500–Cr B–2011.
20. Cobalt—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011 or 3111 C–2011D3558–15 (A or B)p. 37, 9 I–3239–85. 2
AA furnace3113 B–2010D3558–15 (C)I–4243–89. 51
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05 70 I–4472–97. 81
DCPD4190–15See footnote. 34
21. Color, platinum cobalt units or dominant wavelength, hue, luminance purityColorimetric (ADMI)2120 F–2011 78.
Platinum cobalt visual comparison2120 B–2011I–1250–85. 2
SpectrophotometricSee footnote 18
22. Copper—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D1688–17 (A or B)974.27, 3 p. 37, 9 I–3270–85 2 or I–3271–85. 2
AA furnace3113 B–2010D1688–17 (C)I–4274–89. 51
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05, 70, I–4472–97. 81
DCP 36D4190–15See footnote. 34
Colorimetric (Neocuproine)3500-Cu B–2011.
Colorimetric (Bathocuproine)3500-Cu C–2011See footnote. 19
23. Cyanide—Total, mg/LAutomated UV digestion/distillation and ColorimetryKelada-01. 55
Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometryD7511–12(17).
Manual distillation with MgCl2, followed by any of the following:335.4, Rev. 1.0 (1993) 574500–CN- B–2016 and C–2016D2036–09(15)(A), D7284–13(17)10–204–00–1–X. 56
Flow Injection, gas diffusion amperometryD2036–09(15)(A) D7284–13(17).
Titrimetric4500–CN- D–2016D2036–09(15)(A)p. 22. 9
Spectrophotometric, manual4500–CN- E–2016D2036–09(15)(A)I–3300–85. 2
Semi-Automated 20335.4, Rev. 1.0 (1993) 574500–CN- N–201610–204–00–1–X, 56 I–4302–85. 2
Ion ChromatographyD2036–09(15)(A).
Ion Selective Electrode4500–CN- F–2016D2036–09(15)(A).
24. Cyanide-Available, mg/LCyanide Amenable to Chlorination (CATC); Manual distillation with MgCl2, followed by Titrimetric or Spectrophotometric4500–CN- G–2016D2036–09(15)(B).
Flow injection and ligand exchange, followed by gas diffusion amperometry 59D6888–16OIA–1677–09. 44
Automated Distillation and Colorimetry (no UV digestion)Kelada-01. 55
24.A Cyanide-Free, mg/LFlow Injection, followed by gas diffusion amperometryD7237–15 (A)OIA–1677–09. 44
Manual micro-diffusion and colorimetryD4282–15.
25. Fluoride—Total, mg/LManual distillation, 6 followed by any of the following:4500–F- B–2011D1179–16 (A).
Electrode, manual4500–F- C–2011D1179–16 (B).
Electrode, automatedI–4327–85. 2
Colorimetric, (SPADNS)4500–F- D–2011.
Automated complexone4500–F- E–2011.
Ion Chromatography300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)4110 B–2011 or C–2011D4327–17993.30. 3
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
26. Gold—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011.
AA furnace231.2 (Issued 1978) 13113 B–2010.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPSee footnote. 34
27. Hardness—Total, as CaCO3, mg/LAutomated colorimetric130.1 (Issued 1971) 1.
Titrimetric (EDTA)2340 C–2011D1126–17973.52B 3, I–1338–85. 2
Ca plus Mg as their carbonates, by any approved method for Ca and Mg (See Parameters 13 and 33), provided that the sum of the lowest point of quantitation for Ca and Mg is below the NPDES permit requirement for Hardness2340 B–2011.
28. Hydrogen ion (pH), pH unitsElectrometric measurement4500–H + B–2011D1293–99 (A or B)973.41, 3 I–1586–85. 2
Automated electrode150.2 (Dec. 1982) 1See footnote, 21 I–2587–85. 2
29. Iridium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011.
AA furnace235.2 (Issued 1978) 1.
ICP/MS3125 B–2011.
30. Iron—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D1068–15 (A)974.27, 3 I–3381–85. 2
AA furnace3113 B–2010D1068–15 (B).
STGFAA200.9, Rev. 2.2 (1994)
ICP/AES 36200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCP 36D4190–15See footnote. 34
Colorimetric (Phenanthroline)3500–Fe B–2011D1068–15 (C)See footnote. 22
31. Kjeldahl Nitrogen 5—Total, (as N), mg/LManual digestion 20 and distillation or gas diffusion, followed by any of the following:4500–Norg B–2011 or C–2011 and 4500–NH3 B–2011D3590–17 (A)I–4515–91. 45
Titration4500–NH3 C–2011973.48. 3
NesslerizationD1426–15 (A).
Electrode4500–NH3 D–2011 or E–2011D1426–15 (B).
Semi-automated phenate350.1, Rev. 2.0 (1993)4500–NH3 G–2011 4500–NH3 H–2011
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods4500–NH3 F–2011See footnote. 60
Automated gas diffusion, followed by conductivity cell analysisTimberline Ammonia-001. 74
Automated gas diffusion followed by fluorescence detector analysisFIAlab 100. 82
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) 1I–4551–78. 8
Semi-automated block digestor colorimetric (distillation not required)351.2, Rev. 2.0 (1993)4500–Norg D–2011D3590–17 (B)I–4515–91 45
Block digester, followed by Auto distillation and TitrationSee footnote. 39
Block digester, followed by Auto distillation and NesslerizationSee footnote. 40
Block Digester, followed by Flow injection gas diffusion (distillation not required)See footnote. 41
Digestion with peroxdisulfate, followed by Spectrophotometric (2,6-dimethyl phenol)Hach 10242. 76
Digestion with persulfate, followed by ColorimetricNCASI TNTP W10900. 77
32. Lead—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D3559–15 (A or B)974.27, 3 I–3399–85. 2
AA furnace3113 B–2010D3559–15 (D)I–4403–89. 51
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCP 36D4190–15See footnote. 34
Voltammetry 11D3559–15 (C).
Colorimetric (Dithizone)3500–Pb B–2011.
33. Magnesium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011D511–14 (B)974.27, 3 I–3447–85. 2
ICP/AES200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPSee footnote. 34
Ion ChromatographyD6919–17.
34. Manganese—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011D858–17 (A or B)974.27, 3 I–3454–85. 2
AA furnace3113 B–2010D858–17 (C).
STGFAA200.9, Rev. 2.2 (1994)
ICP/AES 36200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCP 36D4190–15See footnote. 34
Colorimetric (Persulfate)3500–Mn B–2011920.203. 3
Colorimetric (Periodate)See footnote. 23
35. Mercury—Total, mg/LCold vapor, Manual245.1, Rev. 3.0 (1994)3112 B–2011D3223–17977.22, 3 I–3462–85. 2
Cold vapor, Automated245.2 (Issued 1974) 1.
Cold vapor atomic fluorescence spectrometry (CVAFS)245.7 Rev. 2.0 (2005) 17I–4464–01. 71
Purge and Trap CVAFS1631E 43.
36. Molybdenum—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 D–2011I–3490–85. 2
AA furnace3113 –2010I–3492–96. 47
ICP/AES200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCPSee footnote. 34
37. Nickel—Total, 4
mg/L
Digestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D1886–14 (A or B)I–3499–85 2
AA furnace3113 B–2010D1886–14 (C)I–4503–89. 51
STGFAA200.9, Rev. 2.2 (1994)
ICP/AES 36200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05 70 I–4472–97. 81
DCP 36D4190–15See footnote. 34
38. Nitrate (as N), mg/LIon Chromatography300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)4110 B–2011 or C–2011D4327–17993.30. 3
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
Ion Selective Electrode4500–NO3- D–2016.
Colorimetric (Brucine sulfate)352.1 (Issued 1971) 1973.50, 3 419D 17, p. 28. 9
Spectrophotometric (2,6-dimethylphenol)Hach 10206 75
Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40)
39. Nitrate-nitrite (as N), mg/LCadmium reduction, Manual4500–NO3- E–2016D3867–16 (B).
Cadmium reduction, Automated353.2, Rev. 2.0 (1993)4500–NO3- F–2016 4500–NO3- I–2016D3867–16 (A)I–2545–90. 51
Automated hydrazine4500–NO3- H–2016.
Reduction/ColorimetricSee footnote. 62
Ion Chromatography300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)4110 B–2011 or C–2011D4327–17993.30. 3
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
Enzymatic reduction, followed by automated colorimetric determinationD7781–14I–2547–11. 72
I–2548–11. 72
N07–0003. 73
Enzymatic reduction, followed by manual colorimetric determination4500–NO3- J–2018.
Spectrophotometric (2,6-dimethylphenol)Hach 10206. 75
40. Nitrite (as N), mg/LSpectrophotometric: Manual4500–NO2- B–2011See footnote. 25
Automated (Diazotization)I–4540–85, 2 See footnote. 62 I–2540–90. 80
Automated (*bypass cadmium reduction)353.2, Rev. 2.0 (1993)4500–NO3- F–2016 4500–NO3- I–2016D3867–16 (A)I–4545–85. 2
Manual (*bypass cadmium or enzymatic reduction)4500–NO3- E–2016, 4500–NO3- J–2018D3867–16 (B).
Ion Chromatography300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)4110 B–2011 or C–2011D4327–17993.30. 3
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
Automated (*bypass Enzymatic reduction)D7781–14I–2547–11 72 I–2548–11 72 N07–0003. 73
41. Oil and grease—Total recoverable, mg/LHexane extractable material (HEM): n-Hexane extraction and gravimetry1664 Rev. A; 1664 Rev. B 425520 B–2011 38.
Silica gel treated HEM (SGT–HEM): Silica gel treatment and gravimetry1664 Rev. A; 1664 Rev. B 425520 B–2011 38 and 5520 F–2011 38.
42. Organic carbon—Total (TOC), mg/LCombustion5310 B–2014D7573–09(17)973.47, 3 p. 14. 24
Heated persulfate or UV persulfate oxidation5310 C–2014 5310 D–2011D4839–03(17)973.47, 3, p. 14. 24
43. Organic nitrogen (as N), mg/LTotal Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4)
44. Ortho-phosphate (as P), mg/LAscorbic acid method:
Automated365.1, Rev. 2.0 (1993)4500–P F–2011 or G–2011973.56, 3 I–4601–85, 2 I–2601–90. 80
Manual, single-reagent4500–P E–2011D515–88 (A)973.55. 3
Manual, two-reagent365.3 (Issued 1978) 1.
Ion Chromatography300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)4110 B–2011 or C–2011D4327–17993.30. 3
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
45. Osmium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 D–2011.
AA furnace252.2 (Issued 1978) 1.
46. Oxygen, dissolved, mg/LWinkler (Azide modification)4500–O (B–F)–2016D888–12 (A)973.45B, 3 I–1575–78. 8
Electrode4500–O G–2016D888–12 (B)I–1576–78. 8
Luminescence-Based Sensor4500–O H–2016D888–12 (C)See footnote. 63 See footnote. 64
47. Palladium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011.
AA furnace253.2 (Issued 1978) 1.
ICP/MS3125 B–2011.
DCPSee footnote. 34
48. Phenols, mg/LManual distillation, 26 followed by any of the following:420.1 (Rev. 1978) 15530 B–2010D1783–01(12).
Colorimetric (4AAP) manual420.1 (Rev. 1978) 15530 D–2010 27D1783–01(12) (A or B).
Automated colorimetric (4AAP)420.4 Rev. 1.0 (1993)
49. Phosphorus (elemental), mg/LGas-liquid chromatographySee footnote. 28
50. Phosphorus—Total, mg/LDigestion, 20 followed by any of the following:4500–P B (5)–2011973.55. 3
Manual365.3 (Issued 1978) 14500–P E–2011D515–88 (A).
Automated ascorbic acid reduction365.1 Rev. 2.0 (1993)4500–P (F–H)–2011973.56, 3 I–4600–85. 2
ICP/AES 4 36200.7, Rev. 4.4 (1994)3120 B–2011I–4471–97. 50
Semi-automated block digestor (TKP digestion)365.4 (Issued 1974) 1D515–88 (B)I–4610–91. 48
Digestion with persulfate, followed by ColorimetricNCASI TNTP W10900. 77
51. Platinum—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011.
AA furnace255.2 (Issued 1978) 1.
ICP/MS3125 B–2011.
DCPSee footnote. 34
52. Potassium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011973.53, 3 I–3630–85. 2
ICP/AES200.7, Rev. 4.4 (1994)3120 B–2011.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
Flame photometric3500–K B–2011.
Electrode3500–K C–2011.
Ion ChromatographyD6919–17.
53. Residue—Total, mg/LGravimetric, 103–105°2540 B–2015I–3750–85. 2
54. Residue—filterable, mg/LGravimetric, 180°2540 C–2015D5907–13I–1750–85. 2
55. Residue—non-filterable (TSS), mg/LGravimetric, 103–105° post-washing of residue2540 D–2015D5907–13I–3765–85. 2
56. Residue—settleable, ml/LVolumetric (Imhoff cone), or gravimetric2540 F–2015.
57. Residue—Volatile, mg/LGravimetric, 550°160.4 (Issued 1971) 12540 E–2015I–3753–85. 2
58. Rhodium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration, or3111 B–2011.
AA furnace265.2 (Issued 1978) 1.
ICP/MS3125 B–2011.
59. Ruthenium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration, or3111 B–2011.
AA furnace267.2 1.
ICP/MS3125 B–2011.
60. Selenium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA furnace3113 B–2010D3859–15 (B)I–4668–98. 49
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES 36200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05 70 I–4472–97. 81
AA gaseous hydride3114 B–2011, or 3114 C–2011D3859–15 (A)I–3667–85. 2
61. Silica—Dissolved, 37 mg/L0.45-micron filtration followed by any of the following:
Colorimetric, Manual4500-SiO2 C–2011D859–16I–1700–85. 2
Automated (Molybdosilicate)4500–SiO2 E–2011 or F–2011I–2700–85. 2
ICP/AES200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994)3120 B–2011I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
62. Silver—Total,4 31 mg/LDigestion,4 29 followed by any of the following:
AA direct aspiration3111 B–2011 or 3111 C–2011974.27, 3 p. 37, 9 I–3720–85. 2
AA furnace3113 B–2010I–4724–89. 51
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4472–97. 81
DCPSee footnote. 34
63. Sodium—Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011973.54, 3 I–3735–85. 2
ICP/AES200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPSee footnote. 34
Flame photometric3500–Na B–2011.
Ion ChromatographyD6919–17.
64. Specific conductance, micromhos/cm at 25 °CWheatstone bridge120.1 (Rev. 1982) 12510 B–2011D1125–95(99) (A)973.40, 3 I–2781–85. 2
65. Sulfate (as SO4), mg/LAutomated colorimetric375.2, Rev. 2.0 (1993)4500–SO42- F–2011 or G–2011
Gravimetric4500–SO42- C–2011 or D–2011925.54. 3
Turbidimetric4500–SO42- E–2011D516–16.
Ion Chromatography300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997)4110 B–2011 or C–2011D4327–17993.303, I–4020–05 70
CIE/UV4140 B–2011D6508–15D6508, Rev. 2. 54
66. Sulfide (as S), mg/LSample Pretreatment4500–S2- B, C–2011.
Titrimetric (iodine)4500–S2- F–2011I–3840–85. 2
Colorimetric (methylene blue)4500–S2- D–2011.
Ion Selective Electrode4500–S2- G–2011D4658–15.
67. Sulfite (as SO3), mg/LTitrimetric (iodine-iodate)4500–SO32- B–2011.
68. Surfactants, mg/LColorimetric (methylene blue)5540 C–2011D2330–02.
69. Temperature, °CThermometric2550 B–2010See footnote. 32
70. Thallium-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011.
AA furnace279.2 (Issued 1978) 13113 B–2010.
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES200.7, Rev. 4.4 (1994)3120 B–2011D1976–12.
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4471–97 50 I–4472–97. 81
71. Tin-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 B–2011I–3850–78. 8
AA furnace3113 B–2010.
STGFAA200.9, Rev. 2.2 (1994).
ICP/AES200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994).
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
72. Titanium-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 D–2011.
AA furnace283.2 (Issued 1978) 1.
ICP/AES200.7, Rev. 4.4 (1994).
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14. 3
DCPSee footnote. 34
73. Turbidity, NTU 53Nephelometric180.1, Rev. 2.0 (1993)2130 B–2011D1889–00I–3860–85 2
See footnote. 65
See footnote. 66
See footnote. 67
74. Vanadium-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration3111 D–2011.
AA furnace3113 B–2010D3373–17.
ICP/AES200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05. 70
DCPD4190–15See footnote. 34
Colorimetric (Gallic Acid)3500–V B–2011.
75. Zinc-Total, 4 mg/LDigestion, 4 followed by any of the following:
AA direct aspiration 363111 B–2011 or 3111 C–2011D1691–17 (A or B)974.27, 3 p. 37, 9 I–3900–85. 2
AA furnace289.2 (Issued 1978) 1.
ICP/AES 36200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994)3120 B–2011D1976–12I–4471–97. 50
ICP/MS200.8, Rev. 5.4 (1994)3125 B–2011D5673–16993.14, 3 I–4020–05 70 I–4472–97. 81
DCP 36D4190–15See footnote. 34
Colorimetric (Zincon)3500 Zn B–2011See footnote. 33
76. Acid Mine Drainage1627 69.
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