Table IA-List of Approved Biological Methods for Wastewater and Sewage Sludge
Parameter and units | Method 1 | EPA | Standard methods | AOAC, ASTM, USGS | Other |
Bacteria | |||||
1. Coliform (fecal), number per gram dry weight | Most Probable Number (MPN), 5 tube, 3 dilution, or | p. 132,3 1680,1115 1681 1120 | 9221 E-2014. | ||
Membrane filter (MF),25 single step | p. 124 3 | 9222 D-2015.29 | |||
2. Coliform (fecal), number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 132 3 | 9221 E-2014, 9221 F-2014.33 | ||
Multiple tube/multiple well, or | Colilert-18®.131828 | ||||
MF,25 single step 5 | p. 124 3 | 9222 D-2015 29 | B-0050-85. 4 | ||
3. Coliform (total), number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 114 3 | 9221 B-2014. | ||
MF,25 single step or | p. 108 3 | 9222 B-2015 30 | B-0025-85.4 | ||
MF, 25 two step with enrichment | p. 111 3 | 9222 B-2015.30 | |||
4. E. coli, number per 100 mL | MPN 6816 multiple tube, or | 9221 B2014/9221 F-2014.121433 | |||
multiple tube/multiple well, or | 9223 B-2016 13 | 991.15 10 | Colilert®.1318 Colilert-18®.131718 | ||
MF,25678 two step, or | 9222 B-2015/9222 I-2015.31 | ||||
Single step | 1603.1 21 | m-ColiBlue24®.19 | |||
5. Fecal streptococci, number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 139 3 | 9230 B-2013. | ||
MF,2 or | p. 136 3 | 9230 C-2013 32 | B-0055-85.4 | ||
Plate count | p. 143.3 | ||||
6. Enterococci, number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 139 3 | 9230 B-2013. | ||
MPN,68 multiple tube/multiple well, or | 9230 D-2013 | D6503-99 9 | Enterolert®.1323 | ||
MF 25678 single step or | 1600.1 24 | 9230 C-2013.32 | |||
Plate count | p. 143.3 | ||||
7. Salmonella, number per gram dry weight 11 | MPN multiple tube | 1682.22 | |||
Aquatic Toxicity | |||||
8. Toxicity, acute, fresh water organisms, LC 50, percent effluent | Water flea, Cladoceran, Ceriodaphnia dubia acute | 2002.0.25 | |||
Water flea, Cladocerans, Daphnia pulex and Daphnia magna acute | 2021.0.25 | ||||
Fish, Fathead minnow, Pimephales promelas, and Bannerfin shiner, Cyprinella leedsi, acute | 2000.0.25 | ||||
Fish, Rainbow trout, Oncorhynchus mykiss, and brook trout, Salvelinus fontinalis, acute | 2019.0.25 | ||||
9. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC 50, percent effluent | Mysid, Mysidopsis bahia, acute | 2007.0.25 | |||
Fish, Sheepshead minnow, Cyprinodon variegatus, acute | 2004.0.25 | ||||
Fish, Silverside, Menidia beryllina, Menidia menidia, and Menidia peninsulae, acute | 2006.0.25 | ||||
10. Toxicity, chronic, fresh water organisms, NOEC or IC 25, percent effluent | Fish, Fathead minnow, Pimephales promelas, larval survival and growth | 1000.0.26 | |||
Fish, Fathead minnow, Pimephales promelas, embryo-larval survival and teratogenicity | 1001.0.26 | ||||
Water flea, Cladoceran, Ceriodaphnia dubia, survival and reproduction | 1002.0.26 | ||||
Green alga, Selenastrum capricornutum, growth | 1003.0.26 | ||||
11. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC 25, percent effluent | Fish, Sheepshead minnow, Cyprinodon variegatus, larval survival and growth. | 1004.0.27 | |||
Fish, Sheepshead minnow, Cyprinodon variegatus, embryo-larval survival and teratogenicity | 1005.0.27 | ||||
Fish, Inland silverside, Menidia beryllina, larval survival and growth | 1006.0.27 | ||||
Mysid, Mysidopsis bahia, survival, growth, and fecundity | 1007.0.27 | ||||
Sea urchin, Arbacia punctulata, fertilization | 1008.0.27 |
Table IA notes:
1 The method must be specified when results are reported.
2 A 0.45-[MICRO]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.
3 Microbiological Methods for Monitoring the Environment, Water and Wastes, EPA/600/8-78/017. 1978. US EPA.
4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS.
5 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.
6 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.
7 When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.
8 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.
9 Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
10 Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
11 Recommended for enumeration of target organism in sewage sludge.
12 The multiple-tube fermentation test is used in 9221B.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 [MICRO]g/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 1603.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified mTEC), EPA-821-R-23-008. September 2023. 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 1600.1: Enterococci in Water by Membrane Filtration Using Membrane-Enterococcus Indoxyl-[BETA]-D-Glucoside Agar (mEI), EPA-821-R-23-006. September 2023. 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 9221F. 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 58 | EPA 52 | Standard methods 84 | ASTM | USGS/AOAC/Other |
1. Acidity (as CaCO 3 ), mg/L | Electrometric endpoint or phenolphthalein endpoint | 2310 B-2020 | D1067-16 | I-1020-85.2 | |
2. Alkalinity (as CaCO 3 ), mg/L | Electrometric or Colorimetric titration to pH 4.5, Manual | 2320 B-2021 | D1067-16 | 973.43,3 I-1030-85.2 | |
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 36 | 3111 D-2019 or 3111 E-2019 | I-3051-85.2 | |||
AA furnace | 3113 B-2020. | ||||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97,81 | |
Direct Current Plasma (DCP) 36 | D4190-15 | See footnote.34 | |||
Colorimetric (Eriochrome cyanine R) | 3500-Al B-2020. | ||||
4. Ammonia (as N), mg/L | Manual distillation 6 or gas diffusion (pH > 11), followed by any of the following: | 350.1 Rev. 2.0 (1993) | 4500-NH 3 B-2021 | 973.49.3 | |
Nesslerization | D1426-15 (A) | 973.49,3 I-3520-85.2 | |||
Titration | 4500-NH 3 C-2021. | ||||
Electrode | 4500-NH 3 D-2021 or E-2021 | D1426-15 (B) | |||
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods | 4500-NH 3 F-2021 | See footnote.60 | |||
Automated phenate, salicylate, or other substituted phenols in Berthelot reaction-based methods | 350.1,30 Rev. 2.0 (1993) | 4500-NH 3 G-2021, 4500-NH 3 H-2021 | I-4523-85,2 I-2522-90.80 | ||
Automated electrode | See footnote.7 | ||||
Ion Chromatography | D6919-17. | ||||
Automated gas diffusion, followed by conductivity cell analysis | Timberline Ammonia-001.74 | ||||
Automated gas diffusion followed by fluorescence detector analysis | FIAlab100.82 | ||||
5. Antimony-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019. | ||||
AA furnace | 3113 B-2020. | ||||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20. | ||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
6. Arsenic-Total,4 mg/L | Digestion,4 followed by any of the following: | 206.5 (Issued 1978).1 | |||
AA gaseous hydride | 3114 B-2020 or 3114 C-2020 | D2972-15 (B) | I-3062-85.2 | ||
AA furnace | 3113 B-2020 | D2972-15 (C) | I-4063-98.49 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5, Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20. | ||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05.70 | |
Colorimetric (SDDC) | 3500-As B-2020 | D2972-15 (A) | I-3060-85.2 | ||
7. Barium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 D-2019 | I-3084-85.2 | |||
AA furnace | 3113 B-2020 | D4382-18. | |||
ICP/AES 36 | 200.5, Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | I-4471-97.50 | ||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP36 | See footnote.34 | ||||
8. Beryllium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 D-2019 or 3111 E-2019 | D3645-15 (A) | I-3095-85.2 | ||
AA furnace | 3113 B-2020 | D3645-15 (B). | |||
STGFAA | 200.9, Rev. 2.2 (1994). | ||||
ICP/AES | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP | D4190-15 | See footnote.34 | |||
Colorimetric (aluminon) | See footnote 61 | ||||
9. Biochemical oxygen demand (BOD 5 ), mg/L | Dissolved Oxygen Depletion | 5210 B-2016 85 | 973.443 p. 17,9 I-1578-78,8 see footnote.1063 | ||
10. Boron-Total,37 mg/L | Colorimetric (curcumin) | 4500-B B-2011 | I-3112-85.2 | ||
ICP/AES | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | D4190-15 | See footnote.34 | |||
11. Bromide, mg/L | Electrode | D1246-16 | I-1125-85.2 | ||
Ion Chromatography | 300.0 Rev 2.1 (1993), and 300.1 Rev 1.0 (1997) | 4110 B-2020, C-2020 or D-2020 | D4327-17 | 993.30,3 I-2057-85.79 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508 Rev. 2.54 | ||
12. Cadmium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D3557-17 (A or B) | 974.27 3 p. 37,9 I-3135-85 2 or I-3136-85.2 | ||
AA furnace | 3113 B-2020 | D3557-17 (D) | I-4138-89.51 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-1472-85 2 or I-4471-97.50 | |
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Voltammetry 11 | D3557-17 (C). | ||||
Colorimetric (Dithizone) | 3500-Cd D-1990. | ||||
13. Calcium-Total,4 mg/L | Digestion 4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 or 3111 D-2019 | D511-14 (B) | I-3152-85.2 | ||
ICP/AES | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | I-4471-97.50 | ||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | See footnote.34 | ||||
Titrimetric (EDTA) | 3500-Ca B-2020 | D511-14 (A). | |||
Ion Chromatography | D6919-17. | ||||
14. Carbonaceous biochemical oxygen demand (CBOD 5 ), mg/L12 | Dissolved Oxygen Depletion with nitrification inhibitor | 5210 B-2016 85 | See footnotes.35 63 | ||
15. Chemical oxygen demand (COD), mg/L | Titrimetric | 410.3 (Rev. 1978) 1 | 5220 B-2011 or C-2011 | D1252-06(12) (A) | 973.46 3 p. 17,9 I-3560-85.2 |
Spectrophotometric, manual or automatic | 410.4 Rev. 2.0 (1993) | 5220 D-2011 | D1252-06(12) (B) | See footnotes,131483 I-3561-85.2 | |
16. Chloride, mg/L | Titrimetric: (silver nitrate) | 4500-Cl - B-2021 | D512-12 (B) | I-1183-85.2 | |
(Mercuric nitrate) | 4500-Cl - C-2021 | D512-12 (A) | 973.51,3 I-1184-85.2 | ||
Colorimetric: manual | I-1187-85.2 | ||||
Automated (ferricyanide) | 4500-Cl - E-2021 | I-2187-85.2 | |||
Potentiometric Titration | 4500-Cl - D-2021. | ||||
Ion Selective Electrode | D512-12 (C). | ||||
Ion Chromatography | 300.0 Rev 2.1 (1993), and 300.1 Rev 1.0 (1997) | 4110 B-2020 or 4110 C-2020 | D4327-17 | 993.30,3 I-2057-90.51 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
17. Chlorine-Total residual, mg/L | Amperometric direct | 4500-Cl D-2011 | D1253-14. | ||
Amperometric direct (low level) | 4500-Cl E-2011. | ||||
Iodometric direct | 4500-Cl B-2011. | ||||
Back titration ether end-point 15 | 4500-Cl C-2011. | ||||
DPD-FAS | 4500-Cl F-2011. | ||||
Spectrophotometric, DPD | 4500-Cl G-2011. | ||||
Electrode | See footnote.16 | ||||
17A. Chlorine-Free Available, mg/L | Amperometric direct | 4500-Cl D-2011 | D1253-14. | ||
Amperometric direct (low level) | 4500-Cl E-2011. | ||||
DPD-FAS | 4500-Cl F-2011. | ||||
Spectrophotometric, DPD | 4500-Cl G-2011. | ||||
18. Chromium VI dissolved, mg/L | 0.45-micron filtration followed by any of the following: | ||||
AA chelation-extraction | 3111 C-2019 | I-1232-85.2 | |||
Ion Chromatography | 218.6 Rev. 3.3 (1994) | 3500-Cr C-2020 | D5257-17 | 993.23.3 | |
Colorimetric (diphenyl-carbazide) | 3500-Cr B-2020 | D1687-17 (A) | I-1230-85.2 | ||
19. Chromium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 | D1687-17 (B) | 974.27,3 I-3236-85.2 | ||
AA chelation-extraction | 3111 C-2019. | ||||
AA furnace | 3113 B-2020 | D1687-17 (C) | I-3233-93.46 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20. | ||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05 70 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Colorimetric (diphenyl-carbazide) | 3500-Cr B-2020. | ||||
20. Cobalt-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 or 3111 C-2019 | D3558-15 (A or B) | p. 37,9 I-323985.2 | ||
AA furnace | 3113 B-2020 | D3558-15 (C) | I-4243-89.51 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES | 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05 70 I-4472-97.81 | |
DCP | D4190-15 | See footnote.34 | |||
21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity | Colorimetric (ADMI) | 2120 F-2021.78 | |||
Platinum cobalt visual comparison | 2120 B-2021 | I-1250-85.2 | |||
Spectrophotometric | See footnote.18 | ||||
22. Copper-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D1688-17 (A or B) | 974.27,3 p. 37,9 I-3270-85 2 or I-3271-85.2 | ||
AA furnace | 3113 B-2020 | D1688-17 (C) | I-4274-89.51 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05,70 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Colorimetric (Neocuproine) | 3500-Cu B-2020. | ||||
Colorimetric (Bathocuproine) | 3500-Cu C-2020 | See footnote.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 | 4500-CN - P-2021 | D7511-12 (17). | |||
Manual distillation with MgCl 2, followed by any of the following: | 335.4 Rev. 1.0 (1993) 57 | 4500-CN - B-2021 and C-2021 | D2036-09(15)(A), D7284-20 | 10-204-00-1-X.56 | |
Flow Injection, gas diffusion amperometry | D2036-09(15)(A) D7284-20. | ||||
Titrimetric | 4500-CN - D-2021 | D2036-09(15)(A) | See footnote 9 p. 22. | ||
Spectrophotometric, manual | 4500-CN - E-2021 | D2036-09(15)(A) | I-3300-85.2 | ||
Semi-Automated 20 | 335.4 Rev. 1.0 (1993) 57 | 4500-CN - N-2021 | 10-204-00-1-X,56 I-4302-85.2 | ||
Ion Chromatography | D2036-09(15)(A). | ||||
Ion Selective Electrode | 4500-CN - F-2021 | D2036-09(15)(A). | |||
24. Cyanide-Available, mg/L | Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl 2, followed by Titrimetric or Spectrophotometric | 4500-CN - G-2021 | D2036-09(15)(B). | ||
Flow injection and ligand exchange, followed by gas diffusion amperometry 59 | 4500-CN - Q-2021 | D6888-16 | OIA-1677-09.44 | ||
Automated Distillation and Colorimetry (no UV digestion) | Kelada-01.55 | ||||
24A. Cyanide-Free, mg/L | Flow Injection, followed by gas diffusion amperometry | 4500-CN - R-2021 | D7237-18 (A) | OIA-1677-09.44 | |
Manual micro-diffusion and colorimetry | D4282-15. | ||||
25. Fluoride-Total, mg/L | Manual distillation,6 followed by any of the following: | 4500-F - B-2021 | D1179-16 (A). | ||
Electrode, manual | 4500-F - C-2021 | D1179-16 (B). | |||
Electrode, automated | 4500-F - G-2021 | I-4327-85.2 | |||
Colorimetric, (SPADNS) | 4500-F - D-2021. | ||||
Automated complexone | 4500-F - E-2021. | ||||
Ion Chromatography | 300.0 Rev 2.1 (1993) and 300.1 Rev 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30.3 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
26. Gold-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019. | ||||
AA furnace | 231.2 (Issued 1978) 1 | 3113 B-2020. | |||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | See footnote.34 | ||||
27. Hardness-Total (as CaCO (3), mg/L | Automated colorimetric | 130.1 (Issued 1971).1 | |||
Titrimetric (EDTA) | 2340 C-2021 | D1126-17 | 973.52B,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 Hardness. | 2340 B-2021. | ||||
28. Hydrogen ion (pH), pH units | Electrometric measurement | 4500-H+ B-2021 | D1293-18 (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 | 3111 B-2019. | ||||
AA furnace | 235.2 (Issued 1978).1 | ||||
ICP/MS | 3125 B-2020. | ||||
30. Iron-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D1068-15 (A) | 974.27,3 I-3381-85.2 | ||
AA furnace | 3113 B-2020 | D1068-15 (B). | |||
STGFAA | 200.9, Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Colorimetric (Phenanthroline) | 3500-Fe B-2011 | D1068-15 (C) | See footnote.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-N org B-2021 or C-2021 and 4500-NH 3 B-2021 | D3590-17 (A) | I-4515-91.45 | |
Titration | 4500-NH 3 C-2021 | 973.48.3 | |||
Nesslerization | D1426-15 (A). | ||||
Electrode | 4500-NH 3 D-2021 or E-2021 | D1426-15 (B). | |||
Semi-automated phenate | 350.1 Rev. 2.0 (1993) | 4500-NH 3 G-2021 or 4500-NH 3 H-2021. | |||
Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods | 4500-NH 3 F-2021 | See footnote.60 | |||
Automated gas diffusion, followed by conductivity cell analysis | Timberline Ammonia-001.74 | ||||
Automated gas diffusion followed by fluorescence detector analysis | FIAlab 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) 1 | I-4551-78.8 | |||
Semi-automated block digestor colorimetric (distillation not required) | 351.2 Rev. 2.0 (1993) | 4500-N org D-2021 | D3590-17 (B) | I-4515-91.45 | |
Block digester, followed by Auto distillation and Titration | See footnote.39 | ||||
Block digester, followed by Auto distillation and Nesslerization | See 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 Colorimetric | NCASI TNTP W10900.77 | ||||
32. Lead-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D3559-15 (A or B) | 974.27,3 I-3399-85.2 | ||
AA furnace | 3113 B-2020 | D3559-15 (D) | I-4403-89.51 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Voltammetry 11 | D3559-15 (C). | ||||
Colorimetric (Dithizone) | 3500-Pb B-2020. | ||||
33. Magnesium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 | D511-14 (B) | 974.27,3 I-3447-85.2 | ||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | See footnote.34 | ||||
Ion Chromatography | D6919-17. | ||||
34. Manganese-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D858-17 (A or B) | 974.27,3 I-3454-85.2 | ||
AA furnace | 3113 B-2020 | D858-17 (C). | |||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Colorimetric (Persulfate) | 3500-Mn B-2020 | 920.203.3 | |||
Colorimetric (Periodate) | See footnote.23 | ||||
35. Mercury-Total, mg/L | Cold vapor, Manual | 245.1 Rev. 3.0 (1994) | 3112 B-2020 | D3223-17 | 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 | 1631E.43 | ||||
36. Molybdenum-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 D-2019 | I-3490-85.2 | |||
AA furnace | 3113 B-2020 | I-3492-96.47 | |||
ICP/AES | 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP | See footnote.34 | ||||
37. Nickel-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D1886-14 (A or B) | I-3499-85.2 | ||
AA furnace | 3113 B-2020 | D1886-14 (C) | I-4503-89.51 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05,70 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
38. Nitrate (as N), mg/L | Ion Chromatography | 300.0 Rev. 2.1 (1993) and 300.1 Rev. 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30.3 |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
Ion Selective Electrode | 4500-NO 3- D-2019. | ||||
Colorimetric (Brucine sulfate) | 352.1 (Issued 1971) 1 | 973.50,3 419D,86 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/L | Cadmium reduction, Manual | 4500-NO 3- E-2019 | D3867-16 (B). | ||
Cadmium reduction, Automated | 353.2 Rev. 2.0 (1993) | 4500-NO 3- F-2019 or 4500-NO 3- I-2019 | D3867-16 (A) | I-2545-90.51 | |
Automated hydrazine | 4500-NO 3- H-2019. | ||||
Reduction/Colorimetric | See footnote.62 | ||||
Ion Chromatography | 300.0 Rev. 2.1 (1993) and 300.1 Rev. 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30.3 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
Enzymatic reduction, followed by automated colorimetric determination | D7781-14 | I-2547-11,72 I-2548-11,72 N07-0003.73 | |||
Enzymatic reduction, followed by manual colorimetric determination | 4500-NO 3- J-2018. | ||||
Spectrophotometric (2,6-dimethylphenol) | Hach 10206.75 | ||||
40. Nitrite (as N), mg/L | Spectrophotometric: Manual | 4500-NO 2- B-2021 | See 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-NO 3- F-2019, 4500-NO 3- I-2019 | D3867-16 (A) | I-4545-85.2 | |
Manual (*bypass cadmium or enzymatic reduction) | 4500-NO 3- E-2019, 4500-NO 3- J-2018 | D3867-16 (B). | |||
Ion Chromatography | 300.0 Rev. 2.1 (1993) and 300.1 Rev. 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30.3 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
Automated (*bypass Enzymatic reduction) | D7781-14 | I-2547-11,72 I-2548-11,72 N07-0003.73 | |||
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 or G-2021.38 | ||
Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry | 1664 Rev. A, 1664 Rev. B 42 | 5520 B or G-2021 38 and 5520 F-2021.38 | |||
42. Organic carbon-Total (TOC), mg/L | Combustion | 5310 B-2014 | D7573-18ae1 | 973.47,3 p. 14.24 | |
Heated persulfate or UV persulfate oxidation | 5310 C-2014, 5310 D-2011 | D4839-03(17) | 973.47,3, p. 14.24 | ||
43. Organic nitrogen (as N), mg/L | Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4). | ||||
44. Ortho-phosphate (as P), mg/L | Ascorbic acid method: | ||||
Automated | 365.1 Rev. 2.0 (1993) | 4500-P F-2021 or G-2021 | 973.56,3 I-4601-85,2 I-2601-90.80 | ||
Manual, single-reagent | 4500-P E-2021 | D515-88 (A) | 973.55.3 | ||
Manual, two-reagent | 365.3 (Issued 1978).1 | ||||
Ion Chromatography | 300.0 Rev. 2.1 (1993) and 300.1 Rev. 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30.3 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508, Rev. 2.54 | ||
45. Osmium-Total4, mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 D-2019. | ||||
AA furnace | 252.2 (Issued 1978).1 | ||||
46. Oxygen, dissolved, mg/L | Winkler (Azide modification) | 4500-O (B-F)-2021 | D888-18 (A) | 973.45B,3 I-1575-78.8 | |
Electrode | 4500-O G-2021 | D888-18 (B) | I-1576-78.8 | ||
Luminescence-Based Sensor | 4500-O H-2021 | D888-18 (C) | See footnotes. 63 64 | ||
47. Palladium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019. | ||||
AA furnace | 253.2 (Issued 1978).1 | ||||
ICP/MS | 3125 B-2020. | ||||
DCP | See footnote.34 | ||||
48. Phenols, mg/L | Manual distillation,26 followed by any of the following: | 420.1 (Rev. 1978) 1 | 5530 B-2021 | D1783-01(12) | |
Colorimetric (4AAP) manual | 420.1 (Rev. 1978) 1 | 5530 D-2021 27 | D1783-01(12) (A or B). | ||
Automated colorimetric (4AAP) | 420.4 Rev. 1.0 (1993). | ||||
49. Phosphorus (elemental), mg/L | Gas-liquid chromatography | See footnote.28 | |||
50. Phosphorus-Total, mg/L | Digestion,20 followed by any of the following: | 4500-P B (5)-2021 | 973.55.3 | ||
Manual | 365.3 (Issued 1978) 1 | 4500-P E-2021 | D515-88 (A). | ||
Automated ascorbic acid reduction | 365.1 Rev. 2.0 (1993) | 4500-P (F-H)-2021 | 973.56,3 I-4600-85.2 | ||
ICP/AES 436 | 200.7Rev. 4.4 (1994) | 3120 B-2020 | I-4471-97.50 | ||
Semi-automated block digestor (TKP digestion) | 365.4 (Issued 1974) 1 | D515-88 (B) | I-4610-91.48 | ||
Digestion with persulfate, followed by Colorimetric | NCASI TNTP W10900.77 | ||||
51. Platinum-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019. | ||||
AA furnace | 255.2 (Issued 1978).1 | ||||
ICP/MS | 3125 B-2020. | ||||
DCP | See footnote.34 | ||||
52. Potassium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 | 973.5,3 I-3630-85.2 | |||
ICP/AES | 200.7 Rev. 4.4 (1994) | 3120 B-2020. | |||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
Flame photometric | 3500-K B-2020. | ||||
Electrode | 3500-K C-2020. | ||||
Ion Chromatography | D6919-17. | ||||
53. Residue-Total, mg/L | Gravimetric, 103-105° | 2540 B-2020 | I-3750-85.2 | ||
54. Residue-filterable, mg/L | Gravimetric, 180° | 2540 C-2020 | D5907-18 (B) | I-1750-85.2 | |
55. Residue-non-filterable (TSS), mg/L | Gravimetric, 103-105° post-washing of residue | 2540 D-2020 | D5907-18 (A) | I-3765-85.2 | |
56. Residue-settleable, mg/L | Volumetric (Imhoff cone), or gravimetric | 2540 F-2020. | |||
57. Residue-Volatile, mg/L | Gravimetric, 550° | 160.4 (Issued 1971) 1 | 2540 E-2020 | I-3753-85.2 | |
58. Rhodium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration, or | 3111 B-2019. | ||||
AA furnace | 265.2 (Issued 1978).1 | ||||
ICP/MS | 3125 B-2020. | ||||
59. Ruthenium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration, or | 3111 B-2019. | ||||
AA furnace | 267.2.1 | ||||
ICP/MS | 3125 B-2020. | ||||
60. Selenium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA furnace | 3113 B-2020 | D3859-15 (B) | I-4668-98.49 | ||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES 36 | 200.5 Rev 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20. | ||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05 70 I-4472-97.81 | |
AA gaseous hydride | 3114 B-2020, or 3114 C-2020 | D3859-15 (A) | I-3667-85.2 | ||
61. Silica-Dissolved,37 mg/L | 0.45-micron filtration followed by any of the following: | ||||
Colorimetric, Manual | 4500-SiO 2 C-2021 | D859-16 | I-1700-85.2 | ||
Automated (Molybdosilicate) | 4500-SiO 2 E-2021 or F-2021 | I-2700-85.2 | |||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | I-4471-97.50 | ||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
62. Silver-Total,4 31 mg/L | Digestion,4 29 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 or 3111 C-2019 | 974.27,3 p. 37,9 I-3720-85.2 | |||
AA furnace | 3113 B-2020 | I-4724-89.51 | |||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4472-97.81 | |
DCP | See footnote.34 | ||||
63. Sodium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 | 973.54,3 I-3735-85.2 | |||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | I-4471-97.50 | ||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | See footnote.34 | ||||
Flame photometric | 3500-Na B-2020. | ||||
Ion Chromatography | D6919-17. | ||||
64. Specific conductance, micromhos/cm at 25 °C | Wheatstone bridge | 120.1 (Rev. 1982) 1 | 2510 B-2021 | D1125-95(99) (A) | 973.40,3 I-2781-85.2 |
65. Sulfate (as SO 4 ), mg/L | Automated colorimetric | 375.2 Rev. 2.0 (1993) | 4500-SO 42- F-2021 or G-2021. | ||
Gravimetric | 4500-SO 42- C-2021 or D-2021 | 925.54.3 | |||
Turbidimetric | 4500-SO 42- E-2021 | D516-16. | |||
Ion Chromatography | 300.0 Rev. 2.1 (1993) and 300.1 Rev. 1.0 (1997) | 4110 B-2020 or C-2020 | D4327-17 | 993.30,3 I-4020-05.70 | |
CIE/UV | 4140 B-2020 | D6508-15 | D6508 Rev. 2.54 | ||
66. Sulfide (as S), mg/L | Sample Pretreatment | 4500-S2- B, C-2021. | |||
Titrimetric (iodine) | 4500-S2- F-2021 | I-3840-85.2 | |||
Colorimetric (methylene blue) | 4500-S2- D-2021. | ||||
Ion Selective Electrode | 4500-S2- G-2021 | D4658-15. | |||
67. Sulfite (as SO 3 ), mg/L | Titrimetric (iodine-iodate) | 4500-SO 32- B-2021. | |||
68. Surfactants, mg/L | Colorimetric (methylene blue) | 5540 C-2021 | D2330-20. | ||
69. Temperature, °C | Thermometric | 2550 B-2010 | See footnote.32 | ||
70. Thallium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019. | ||||
AA furnace | 279.2 (Issued 1978) 1 | 3113 B-2020. | |||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES | 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20. | ||
ICP/MS | 200.8, Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4471-97 50 I-4472-97.81 | |
71. Tin-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 B-2019 | I-3850-78.8 | |||
AA furnace | 3113 B-2020. | ||||
STGFAA | 200.9 Rev. 2.2 (1994). | ||||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994). | ||||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
72. Titanium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 D-2019. | ||||
AA furnace | 283.2 (Issued 1978).1 | ||||
ICP/AES | 200.7 Rev. 4.4 (1994). | ||||
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14.3 | |
DCP | See footnote.34 | ||||
73. Turbidity, NTU 53 | Nephelometric | 180.1, Rev. 2.0 (1993) | 2130 B-2020 | D1889-00 | I-3860-85,2 see footnotes.656667 |
74. Vanadium-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration | 3111 D-2019. | ||||
AA furnace | 3113 B-2020 | D3373-17. | |||
ICP/AES | 200.5 Rev. 4.2 (2003),68 200.7 Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05.70 | |
DCP | D4190-15 | See footnote.34 | |||
Colorimetric (Gallic Acid) | 3500-V B-2011. | ||||
75. Zinc-Total,4 mg/L | Digestion,4 followed by any of the following: | ||||
AA direct aspiration 36 | 3111 B-2019 or 3111 C-2019 | D1691-17 (A or B) | 974.27 3 p. 37,9 I-3900-85.2 | ||
AA furnace | 289.2 (Issued 1978).1 | ||||
ICP/AES 36 | 200.5 Rev. 4.2 (2003),68 200.7, Rev. 4.4 (1994) | 3120 B-2020 | D1976-20 | I-4471-97.50 | |
ICP/MS | 200.8 Rev. 5.4 (1994) | 3125 B-2020 | D5673-16 | 993.14,3 I-4020-05,70 I-4472-97.81 | |
DCP 36 | D4190-15 | See footnote.34 | |||
Colorimetric (Zincon) | 3500 Zn B-2020 | See footnote.33 | |||
76. Acid Mine Drainage | 1627.69 |
Table IB Notes:
1 Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.
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 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 (FLAA) determinations, 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 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 this 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 (for 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.
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 (CBOD 5 ) must not be confused with the traditional BOD 5 test method which measures "total 5-day BOD." The addition of the nitrification inhibitor is not a procedural option but must be included to report the CBOD 5 parameter. A discharger whose permit requires reporting the traditional BOD 5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's permit specifically states CBOD 5 is required can the permittee report data using a nitrification inhibitor.
13 OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation.
14 Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company.
15 The back-titration method will be used to resolve controversy.
16 Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research Incorporated. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
17 Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA.
18 National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253 (1971) and Technical Bulletin 803, May 2000.
19 Method 8506, Bicinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company.
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.
22 Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company.
23 Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company.
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). 1987. USGS.
25 Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company.
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 Chromatograph y, 47(3):421-426.
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 Na 2 S 2 O 3 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 NH 4 OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I 2 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 NH 4 OH. 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.
33 Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.
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.
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.
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.
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.
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.
43 Method 1631, Revision E, 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.
44 Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.
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, 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 U.S. EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography.
53 Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.
54 Waters Corp. Now included in ASTM D6508-15, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. 2015.
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. 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.
57 When using sulfide removal test procedures described in EPA Method 335.4, 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 D6888-16 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 for the Examination of Water and Wastewater 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 BOD 5 and CBOD 5 . Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in this 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 USGS Techniques and Methods 5-B8, Chapter 8, Section B, Methods of the National Water Quality Laboratory Book 5, Laboratory Analysis, 2011 USGS.
73 NECi Method N07-0003, "Nitrate Reductase Nitrate-Nitrogen Analysis," Revision 9.0, March 2014, The Nitrate Elimination Co., Inc.
74 Timberline Instruments, LLC Method Ammonia-001, "Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis," June 2011, Timberline Instruments, LLC.
75 Hach Company Method 10206, "Spectrophotometric Measurement of Nitrate in Water and Wastewater," Revision 2.1, January 2013, Hach Company.
76 Hach Company Method 10242, "Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater," Revision 1.1, January 2013, Hach Company.
77 National Council for Air and Stream Improvement (NCASI) Method TNTP-W10900, "Total (Kjeldahl) Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion," June 2011, National Council for Air and Stream Improvement, Inc.
78 The pH adjusted sample is to be adjusted to 7.6 for NPDES reporting purposes.
79 I-2057-85 in U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. A1, Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, 1989.
80 Methods I-2522-90, I-2540-90, and I-2601-90 in U.S. Geological Survey 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.
81 Method I-4472-97 in U.S. Geological Survey Open-File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, 1998.
82 FIAlab 100, "Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis", April 4, 2018, FIAlab Instruments, Inc.
83 MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR® COD LR/HR, "Spectrophotometric Measurement of Chemical Oxygen Demand in Water and Wastewater", Revision 1.5, May 2018, MACHEREY-NAGEL GmbH and Co. KG.
84 Please refer to the following applicable Quality Control Sections: Part 2000 Methods, Physical and Aggregate Properties 2020 (2021); Part 3000 Methods, Metals, 3020 (2021); Part 4000 Methods, Inorganic Nonmetallic Constituents, 4020 (2022); Part 5000 Methods, and Aggregate Organic Constituents, 5020 (2022). These Quality Control Standards are available for download at www.standardmethods.org at no charge.
85 Each laboratory may establish its own control limits by performing at least 25 glucose-glutamic acid (GGA) checks over several weeks or months and calculating the mean and standard deviation. The laboratory may then use the mean ± 3 standard deviations as the control limit for future GGA checks. However, GGA acceptance criteria can be no wider than 198 ± 30.5 mg/L for BOD 5 . GGA acceptance criteria for CBOD must be either 198 ± 30.5 mg/L, or the lab may develop control charts under the following conditions: dissolved oxygen uptake from the seed contribution is between 0.6-1.0 mg/L; control charts are performed on at least 25 GGA checks with three standard deviations from the derived mean; the RSD must not exceed 7.5%; and any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L.
86 The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
Dissolved oxygen uptake from the seed contribution is between 0.6-1.0 mg/L. Control charts are performed on at least 25 GGA checks with three standard deviations from the derived mean. The RSD must not exceed 7.5%. Any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L.Table IC-List of Approved Test Procedures for Non-Pesticide Organic Compounds
Parameter 1 | Method | EPA 27 | Standard methods 17 | ASTM | Other |
1. Acenaphthene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
2. Acenaphthylene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
3. Acrolein | GC | 603 | |||
GC/MS | 624.1 4, 1624B. | ||||
4. Acrylonitrile | GC | 603 | |||
GC/MS | 624.1 4, 1624B | O-4127-96.13 | |||
5. Anthracene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
6. Benzene | GC | 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
7. Benzidine | Spectro-photometric | See footnote 3 p.1. | |||
GC/MS | 625.1 5, 1625B | 6410 B-2020. | |||
HPLC | 605 | ||||
8. Benzo(a)anthracene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
9. Benzo(a)pyrene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
10. Benzo(b)fluoranthene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
11. Benzo(g,h,i)perylene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
12. Benzo(k)fluoranthene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
13. Benzyl chloride | GC | See footnote 3 p. 130. | |||
GC/MS | See footnote 6 p. S102. | ||||
14. Butyl benzyl phthalate | GC | 606 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
15. bis(2-Chloroethoxy) methane | GC | 611 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
16. bis(2-Chloroethyl) ether | GC | 611 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
17. bis(2-Ethylhexyl) phthalate | GC | 606 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
18. Bromodichloromethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
19. Bromoform | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
20. Bromomethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
21. 4-Bromophenyl phenyl ether | GC | 611 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
22. Carbon tetrachloride | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
23. 4-Chloro-3-methyl phenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
24. Chlorobenzene | GC | 601, 602 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13 O-4436-16.14 | ||
25. Chloroethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96.13 | ||
26. 2-Chloroethylvinyl ether | GC | 601 | |||
GC/MS | 624.1, 1624B. | ||||
27. Chloroform | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
28. Chloromethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
29. 2-Chloronaphthalene | GC | 612 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
30. 2-Chlorophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
31. 4-Chlorophenyl phenyl ether | GC | 611 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
32. Chrysene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
33. Dibenzo(a,h)anthracene | GC | 610 | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
34. Dibromochloromethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
35. 1,2-Dichlorobenzene | GC | 601, 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1625B | 6200 B-2020 | See footnote 9 p. 27, O-4127-96 13, O-4436-16.14 | ||
36. 1,3-Dichlorobenzene | GC | 601, 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1625B | 6200 B-2020 | See footnote 9 p. 27, O-4127-96.13 | ||
37. 1,4-Dichlorobenzene | GC | 601, 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1625B | 6200 B-2020 | See footnote 9 p. 27, O-4127-96 13, O-4436-16.14 | ||
38. 3,3'-Dichlorobenzidine | GC/MS | 625.1, 1625B | 6410 B-2020. | ||
HPLC | 605. | ||||
39. Dichlorodifluoromethane | GC | 601. | |||
GC/MS | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | |||
40. 1,1-Dichloroethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
41. 1,2-Dichloroethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
42. 1,1-Dichloroethene | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
43. trans -1,2-Dichloroethene | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
44. 2,4-Dichlorophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
45. 1,2-Dichloropropane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13 O-4436-16.14 | ||
46. cis -1,3-Dichloropropene | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
47. trans -1,3-Dichloropropene | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
48. Diethyl phthalate | GC | 606. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
49. 2,4-Dimethylphenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
50. Dimethyl phthalate | GC | 606. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
51. Di- n -butyl phthalate | GC | 606. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
52. Di- n -octyl phthalate | GC | 606. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
53. 2, 4-Dinitrophenol | GC | 604 | 6420 B-2021 | See footnote 9 p. 27. | |
GC/MS | 625.1, 1625B | 6410 B-2020. | |||
54. 2,4-Dinitrotoluene | GC | 609. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
55. 2,6-Dinitrotoluene | GC | 609. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
56. Epichlorohydrin | GC | See footnote 3 p. 130. | |||
GC/MS | See footnote 6 p. S102. | ||||
57. Ethylbenzene | GC | 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
58. Fluoranthene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
59. Fluorene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
60. 1,2,3,4,6,7,8-Heptachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
61. 1,2,3,4,7,8,9-Heptachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
62. 1,2,3,4,6,7,8- Heptachloro-dibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
63. Hexachlorobenzene | GC | 612. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
64. Hexachlorobutadiene | GC | 612. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27, O-4127-96.13 | ||
65. Hexachlorocyclopentadiene | GC | 612. | |||
GC/MS | 625.1 5, 1625B | 6410 B-2020 | See footnote 9, p. 27, O-4127-96.13 | ||
66. 1,2,3,4,7,8-Hexachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
67. 1,2,3,6,7,8-Hexachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
68. 1,2,3,7,8,9-Hexachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
69. 2,3,4,6,7,8-Hexachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
70. 1,2,3,4,7,8-Hexachloro-dibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
71. 1,2,3,6,7,8-Hexachloro-dibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
72. 1,2,3,7,8,9-Hexachloro-dibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
73. Hexachloroethane | GC | 612. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27, O-4127-96.13 | ||
74. Indeno(1,2,3-c,d) pyrene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
75. Isophorone | GC | 609. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
76. Methylene chloride | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
77. 2-Methyl-4,6-dinitrophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
78. Naphthalene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021. | |||
79. Nitrobenzene | GC | 609. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | D4657-92 (98). | ||||
80. 2-Nitrophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
81. 4-Nitrophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
82. N-Nitrosodimethylamine | GC | 607. | |||
GC/MS | 625.1 5, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
83. N-Nitrosodi- n -propylamine | GC | 607. | |||
GC/MS | 625.1 5, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
84. N-Nitrosodiphenylamine | GC | 607. | |||
GC/MS | 625.1 5, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
85. Octachlorodibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
86. Octachlorodibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
87. 2,2'-oxybis(1-chloropropane) 12 [also known as bis(2-Chloro-1-methylethyl) ether] | GC | 611. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
88. PCB-1016 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
89. PCB-1221 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
90. PCB-1232 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
91. PCB-1242 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
92. PCB-1248 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
93. PCB-1254 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
94. PCB-1260 | GC | 608.3 | See footnote 3 p. 43, see footnote.8 | ||
GC/MS | 625.1 | 6410 B-2020. | |||
95. 1,2,3,7,8-Pentachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
96. 2,3,4,7,8-Pentachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
97. 1,2,3,7,8-Pentachloro-dibenzo- p -dioxin | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
98. Pentachlorophenol | GC | 604 | 6420 B-2021 | See footnote 3 p. 140. | |
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
99. Phenanthrene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
100. Phenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
101. Pyrene | GC | 610. | |||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
HPLC | 610 | 6440 B-2021 | D4657-92 (98). | ||
102. 2,3,7,8-Tetrachloro-dibenzofuran | GC/MS | 1613B 10 | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
103. 2,3,7,8-Tetrachloro-dibenzo- p -dioxin | GC/MS | 613, 625.1 5, 1613B | SGS AXYS 16130 15, PAM 16130-SSI.16 | ||
104. 1,1,2,2-Tetrachloroethane | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96.13 | ||
105. Tetrachloroethene | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
106. Toluene | GC | 602 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
107. 1,2,4-Trichlorobenzene | GC | 612 | See footnote 3 p. 130. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27, O-4127-96 13, O-4436-16.14 | ||
108. 1,1,1-Trichloroethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
109. 1,1,2-Trichloroethane | GC | 601 | 6200 C-2020 | See footnote 3 p. 130. | |
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
110. Trichloroethene | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
111. Trichlorofluoromethane | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1 | 6200 B-2020 | O-4127-96.13 | ||
112. 2,4,6-Trichlorophenol | GC | 604 | 6420 B-2021. | ||
GC/MS | 625.1, 1625B | 6410 B-2020 | See footnote 9 p. 27. | ||
113. Vinyl chloride | GC | 601 | 6200 C-2020. | ||
GC/MS | 624.1, 1624B | 6200 B-2020 | O-4127-96 13, O-4436-16.14 | ||
114. Nonylphenol | GC/MS | D7065-17. | |||
115. Bisphenol A (BPA) | GC/MS | D7065-17. | |||
116. p-tert -Octylphenol (OP) | GC/MS | D7065-17. | |||
117. Nonylphenol Monoethoxylate (NP1EO) | GC/MS | D7065-17. | |||
118. Nonylphenol Diethoxylate (NP2EO) | GC/MS | D7065-17. | |||
119. Adsorbable Organic Halides (AOX) | Adsorption and Coulometric Titration | 1650.11 | |||
120. Chlorinated Phenolics | In Situ Acetylation and GC/MS | 1653.11 |
Table IC notes:
1 All parameters are expressed in micrograms per liter ([MICRO]g/L) except for Method 1613B, in which the parameters are expressed in picograms per liter (pg/L).
2 The full text of Methods 601-613, 1613B, 1624B, and 1625B are provided at appendix A, Test Procedures for Analysis of Organic Pollutants. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at appendix B of this part, Definition and Procedure for the Determination of the Method Detection Limit. These methods are available at: https://www.epa.gov/cwa-methods as individual PDF files.
3 Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA.
4 Method 624.1 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate the ability to detect and quantify these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample introduction techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 should be used when analyzing samples for acrolein and acrylonitrile in the absence of such criteria in Method 624.1.
5 Method 625.1 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi- n -propylamine, and N-nitrosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds. Method 625.1 may be applied to 2,3,7,8-Tetrachloro-dibenzo- p -dioxin for screening purposes only.
6 Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).
7 Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 1624B, and 1625B in accordance with procedures in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624.1 and 625.1 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the quality control (QC) acceptance criteria in the pertinent method, analytical results for that parameter in the unspiked sample are suspect. The results should be reported but cannot be used to demonstrate regulatory compliance. If the method does not contain QC acceptance criteria, control limits of ±three standard deviations around the mean of a minimum of five replicate measurements must be used. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
8 Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk. Revised October 28, 1994. 3M Corporation.
9 Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.
10 Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in appendix A to this part and at https://www.epa.gov/cwa-methods/approved-cwa-test-methods-organic-compounds.
11 Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997 U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS. Revision A, 1997 U.S. EPA. The full text for both of these methods is provided at appendix A in part 430 of this chapter, The Pulp, Paper, and Paperboard Point Source Category.
12 The compound was formerly inaccurately labeled as 2,2'-oxybis(2-chloropropane) and bis(2-chloroisopropyl) ether. Some versions of Methods 611, and 1625 inaccurately list the analyte as "bis(2-chloroisopropyl) ether," but use the correct CAS number of 108-60-1.
13 Method O-4127-96, U.S. Geological Survey Open-File Report 97-829, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of 86 volatile organic compounds in water by gas chromatography/mass spectrometry, including detections less than reporting limits,1998, USGS.
14 Method O-4436-16 U.S. Geological Survey Techniques and Methods, book 5, chap. B12, Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry, 2016, USGS.
15 SGS AXYS Method 16130, "Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo- p -Dioxins and Dibenzofurans (CDDs/CDFs) Using Waters and Agilent Gas Chromatography-Tandem-Mass Spectrometry (GC/MS/MS), Revision 1.0" is available at: https://www.sgsaxys.com/wp-content/uploads/2022/09/SGS-AXYS-Method-16130-Rev-1.0.pdf.
16 Pace Analytical Method PAM-16130-SSI, "Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo- p -Dioxins and Dibenzofurans (CDDs/CDFs) Using Shimadzu Gas Chromatography Mass Spectrometry (GC-MS/MS), Revision 1.1," is available at: pacelabs.com.
17 Please refer to the following applicable Quality Control Section: Part 6000 Individual Organic Compounds, 6020 (2019). The Quality Control Standards are available for download at standardmethods.org at no charge.
Table ID-List of Approved Test Procedures for Pesticides1
Parameter | Method | EPA 2 7 10 | Standard methods 15 | ASTM | Other |
1. Aldrin | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96 (02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
2. Ametryn | GC | 507, 619 | See footnote 3 p. 83, see footnote 9 O-3106-93, see footnote 6 p. S68. | ||
GC/MS | 525.2, 625.1 | See footnote 14 O-1121-91. | |||
3. Aminocarb | TLC | See footnote 3 p. 94, see footnote 6 p. S60. | |||
HPLC | 632. | ||||
4. Atraton | GC | 619 | See footnote 3 p. 83, see footnote 6 p. S68. | ||
GC/MS | 625.1. | ||||
5. Atrazine | GC | 507, 619, 608.3 | See footnote 3 p. 83, see footnote 6 p. S68, see footnote 9 O-3106-93. | ||
HPLC/MS | See footnote 12 O-2060-01. | ||||
GC/MS | 525.1, 525.2, 625.1 | See footnote 11 O-1126-95. | |||
6. Azinphos methyl | GC | 614, 622, 1657 | See footnote 3 p. 25, see footnote 6 p. S51. | ||
GC-MS | 625.1 | See footnote 11 O-1126-95. | |||
7. Barban | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
GC/MS | 625.1. | ||||
8. [ALPHA]-BHC | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 8 3M0222. |
GC/MS | 625.1 5 | 6410 B-2020 | See footnote 11 O-1126-95. | ||
9. [BETA]-BHC | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
10. [DELTA]-BHC | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
11. [GAMMA]-BHC (Lindane) | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4, O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 5 | 6410 B-2020 | See footnote 11, O-1126-95. | ||
12. Captan | GC | 617, 608.3 | 6630 B-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7. |
13. Carbaryl | TLC | See footnote 3 p. 94, see footnote 6 p. S60. | |||
HPLC | 531.1, 632. | ||||
HPLC/MS | 553 | See footnote 12 O-2060-01. | |||
GC/MS | 625.1 | See footnote 11 O-1126-95. | |||
14. Carbophenothion | GC | 617, 608.3 | 6630 B-2021 | See footnote 4 page 27, see footnote 6 p. S73. | |
GC/MS | 625.1. | ||||
15. Chlordane | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
16. Chloropropham | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
GC/MS | 625.1. | ||||
17. 2,4-D | GC | 615 | 6640 B-2021 | See footnote 3 p. 115, see footnote 4 O-3105-83. | |
HPLC/MS | See footnote 12 O-2060-01. | ||||
18. 4,4'-DDD | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3105-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
19. 4,4'-DDE | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4, O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020 | See footnote 11 O-1126-95. | ||
20. 4,4'-DDT | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
21. Demeton-O | GC | 614, 622 | See footnote 3 p. 25, see footnote 6 p. S51. | ||
GC/MS | 625.1 | ||||
22. Demeton-S. | GC | 614, 622 | See footnote 3 p. 25, see footnote 6 p. S51. | ||
GC/MS | 625.1. | ||||
23. Diazinon | GC | 507, 614, 622, 1657 | See footnote 3 p. 25, see footnote 4 O-3104-83, see footnote 6 p. S51. | ||
GC/MS | 525.2, 625.1 | See footnote 11 O-1126-95. | |||
24. Dicamba | GC | 615 | See footnote 3 p. 115. | ||
HPLC/MS | See footnote 12 O-2060-01. | ||||
25. Dichlofenthion | GC | 622.1 | See footnote 4 page 27, see footnote 6 p. S73. | ||
26. Dichloran | GC | 608.2, 617, 608.3 | 6630 B-2021 | See footnote 3 p. 7. | |
27. Dicofol | GC | 617, 608.3 | See footnote 4 O-3104-83. | ||
28. Dieldrin | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020 | See footnote 11 O-1126-95. | ||
29. Dioxathion | GC | 614.1, 1657 | See footnote 4 page 27, see footnote 6 p. S73. | ||
30. Disulfoton | GC | 507, 614, 622, 1657 | See footnote 3 p. 25, see footnote 6 p. S51. | ||
GC/MS | 525.2, 625.1 | See footnote 11 O-1126-95. | |||
31. Diuron | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | 553 | See footnote 12 O-2060-01. | |||
32. Endosulfan I | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 625.1 5 | 6410 B-2020 | See footnote 13 O-2002-01. | ||
33. Endosulfan II | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 8 3M0222. |
GC/MS | 625.1 5 | 6410 B-2020 | See footnote 13 O-2002-01. | ||
34. Endosulfan Sulfate | GC | 617, 608.3 | 6630 C-2021 | See footnote 8 3M0222. | |
GC/MS | 625.1 | 6410 B-2020. | |||
35. Endrin | GC | 505, 508, 617, 1656, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 525.1, 525.2, 625.1 5 | 6410 B-2020. | |||
36. Endrin aldehyde | GC | 617, 608.3 | 6630 C-2021 | See footnote 8 3M0222. | |
GC/MS | 625.1 | 6410 B-2020. | |||
37. Ethion | GC | 614, 614.1, 1657 | See footnote 4 page 27, see footnote 6, p. S73. | ||
GC/MS | 625.1 | See footnote 13 O-2002-01. | |||
38. Fenuron | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | See footnote 12 O-2060-01. | ||||
39. Fenuron-TCA | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
40. Heptachlor | GC | 505, 508, 617, 1656, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 525.1, 525.2, 625.1 | 6410 B-2020. | |||
41. Heptachlor epoxide | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 6 p. S73, see footnote 8 3M0222. |
GC/MS | 625.1 | 6410 B-2020. | |||
42. Isodrin | GC | 617, 608.3 | 6630 B-2021 & C-2021 | See footnote 4 O-3104-83, see footnote 6 p. S73. | |
GC/MS | 625.1. | ||||
43. Linuron | GC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | 553 | See footnote 12 O-2060-01. | |||
GC/MS | See footnote 11 O-1126-95. | ||||
44. Malathion | GC | 614, 1657 | 6630 B-2021 | See footnote 3 p. 25, see footnote 6 p. S51. | |
GC/MS | 625.1 | See footnote 11 O-1126-95. | |||
45. Methiocarb | TLC | See footnote 3 p. 94, see footnote 6 p. S60. | |||
HPLC | 632. | ||||
HPLC/MS | See footnote 12 O-2060-01. | ||||
46. Methoxychlor | GC | 505, 508, 608.2, 617, 1656, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83, see footnote 8 3M0222. |
GC/MS | 525.1, 525.2, 625.1 | See footnote 11 O-1126-95. | |||
47. Mexacarbate | TLC | See footnote 3 p. 94, see footnote 6 p. S60. | |||
HPLC | 632. | ||||
GC/MS | 625.1. | ||||
48. Mirex | GC | 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 4 O-3104-83. |
GC/MS | 625.1. | ||||
49. Monuron | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
50. Monuron-TCA | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
51. Neburon | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | See footnote 12 O-2060-01. | ||||
52. Parathion methyl | GC | 614, 622, 1657 | 6630 B-2021 | See footnote 4 page 27, see footnote 3 p. 25. | |
GC/MS | 625.1 | See footnote 11 O-1126-95. | |||
53. Parathion ethyl | GC | 614 | 6630 B-2021 | See footnote 4 page 27, see footnote 3 p. 25. | |
GC/MS | See footnote 11 O-1126-95. | ||||
54. PCNB | GC | 608.1, 617, 608.3 | 6630 B-2021 & C-2021 | D3086-90 , D5812-96(02) | See footnote 3 p. 7. |
55. Perthane | GC | 617, 608.3 | D3086-90, D5812-96(02) | See footnote 4 O-3104-83. | |
56. Prometon | GC | 507, 619 | See footnote 3 p. 83, see footnote 6 p. S68, see footnote 9 O-3106-93. | ||
GC/MS | 525.2, 625.1 | See footnote 11 O-1126-95. | |||
57. Prometryn | GC | 507, 619 | See footnote 3 p. 83, see footnote 6 p. S68, see footnote 9 O-3106-93. | ||
GC/MS | 525.1, 525.2, 625.1 | See footnote 13 O-2002-01. | |||
58. Propazine | GC | 507, 619, 1656, 608.3 | See footnote 3 p. 83, see footnote 6 p. S68, see footnote 9 O-3106-93. | ||
GC/MS | 525.1, 525.2, 625.1 | ||||
59. Propham | TLC | See footnote 3 p. 10, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | See footnote 12 O-2060-01. | ||||
60. Propoxur | TLC | See footnote 3 p. 94, see footnote 6, p. S60. | |||
HPLC | 632. | ||||
61. Secbumeton | TLC | See footnote 3 p. 83, see footnote 6 p. S68. | |||
GC | 619. | ||||
62. Siduron | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
HPLC/MS | See footnote 12 O-2060-01. | ||||
63. Simazine | GC | 505, 507, 619, 1656, 608.3 | See footnote 3 p. 83, see footnote 6 p. S68, see footnote 9 O-3106-93. | ||
GC/MS | 525.1, 525.2, 625.1 | See footnote 11 O-1126-95. | |||
64. Strobane | GC | 617, 608.3 | 6630 B-2021 & C-2021 | See footnote 3 p. 7. | |
65. Swep | TLC | See footnote 3 p. 104, see footnote 6 p. S64. | |||
HPLC | 632. | ||||
66. 2,4,5-T | GC | 615 | 6640 B-2021 | See footnote 3 p. 115, see footnote 4 O-3105-83. | |
67. 2,4,5-TP (Silvex) | GC | 615 | 6640 B-2021 | See footnote 3 p. 115, see footnote 4 O-3105-83. | |
68. Terbuthylazine | GC | 619, 1656, 608.3 | See footnote 3 p. 83, see footnote 6 p. S68. | ||
GC/MS | See footnote 13 O-2002-01. | ||||
69. Toxaphene | GC | 505, 508, 617, 1656, 608.3 | 6630 B-2021 & C-2021 | D3086-90, D5812-96(02) | See footnote 3 p. 7, see footnote 8, see footnote 4 O-3105-83. |
GC/MS | 525.1, 525.2, 625.1 | 6410 B-2020. | |||
70. Trifluralin | GC | 508, 617, 627, 1656, 608.3 | 6630 B-2021 | See footnote 3 p. 7, see footnote 9 O-3106-93. | |
GC/MS | 525.2, 625.1 | See footnote 11 O-1126-95. |
Table ID notes:
1 Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under table IC of this section, where entries are listed by chemical name.
2 The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at appendix B to this part, Definition and Procedure for the Determination of the Method Detection Limit.
3 Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA publication includes thin-layer chromatography (TLC) methods.
4 Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3. 1987. USGS.
5 The method may be extended to include [ALPHA]-BHC, [GAMMA]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.
6 Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).
7 Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608.3 and 625.1 in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 10% of all samples analyzed with Method 608.3 or 5% of all samples analyzed with Method 625.1 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
8 Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk. Revised October 28, 1994. 3M Corporation.
9 Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors. 1994. USGS.
10 EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA Method 525.2 is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry, Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods for The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA. Methods 608.3 and 625.1 are available at: cwa-methods/approved-cwa-test-methods-organic-compounds.
11 Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995. USGS.
12 Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry. 2001. USGS.
13 Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry. 2001. USGS.
14 Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1992. USGS.
15 Please refer to the following applicable Quality Control Section: Part 6000 Methods, Individual Organic Compounds 6020 (2019). These Quality Control Standards are available for download at www.standardmethods.org at no charge.
Table IE-List of Approved Radiologic Test Test Procedures
Parameter and units | Method | Reference (method number or page) | ||||
EPA1 | Standard Methods 18th, 19th, 20th Ed. | Standard Methods Online | ASTM | USGS2 | ||
1. Alpha-Total, pCi per liter | Proportional or scintillation counter | 900.0 | 7110 B | 7110 B-00 | D1943-90, 96 | pp. 75 and 783 |
2. Alpha-Counting error, pCi per liter | Proportional or scintillation counter | Appendix B | 7110 B | 7110 B-00 | D1943-90, 96 | p. 79 |
3. Beta-Total, pCi per liter | Proportional counter | 900.0 | 7110 B | 7110 B-00 | D1890-90, 96 | pp. 75 and 783 |
4. Beta-Counting error, pCi | Proportional counter | Appendix B | 7110 B | 7110 B-00 | D1890-90, 96 | p. 79 |
5. (a) Radium Total pCi per liter (b) Ra, pCi per liter | Proportional counter | 903.0 | 7500-Ra B | 7500-Ra B-01 | D2460-90, 97 | |
Scintillation counter | 903.1 | 7500-Ra C | 7500-Ra C-01 | D3454-91, 97 | p. 81 |
1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.
2 Fishman, M. J. and Brown, Eugene, "Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters," U.S. Geological Survey, Open-File Report 76-177 (1976).
3 The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, the two results must be added to obtain the "total."
Table IF-List of Approved Methods for Pharmaceutical Pollutants
Pharmaceuticals pollutants | CAS registry No. | Analytical method number |
Acetonitrile | 75-05-8 | 1666/1671/D3371/D3695/624.1 |
n-Amyl acetate | 628-63-7 | 1666/D3695 |
n-Amyl alcohol | 71-41-0 | 1666/D3695 |
Benzene | 71-43-2 | D4763/D3695/502.2/524.2/624.1 |
n-Butyl-acetate | 123-86-4 | 1666/D3695 |
tert-Butyl alcohol | 75-65-0 | 1666/624.1 |
Chlorobenzene | 108-90-7 | 502.2/524.2/624.1 |
Chloroform | 67-66-3 | 502.2/524.2/551/624.1 |
o-Dichlorobenzene | 95-50-1 | 1625C/502.2/524.2/624.1 |
1,2-Dichloroethane | 107-06-2 | D3695/502.2/524.2/624.1 |
Diethylamine | 109-89-7 | 1666/1671 |
Dimethyl sulfoxide | 67-68-5 | 1666/1671 |
Ethanol | 64-17-5 | 1666/1671/D3695/624.1 |
Ethyl acetate | 141-78-6 | 1666/D3695/624.1 |
n-Heptane | 142-82-5 | 1666/D3695 |
n-Hexane | 110-54-3 | 1666/D3695 |
Isobutyraldehyde | 78-84-2 | 1666/1667 |
Isopropanol | 67-63-0 | 1666/D3695 |
Isopropyl acetate | 108-21-4 | 1666/D3695 |
Isopropyl ether | 108-20-3 | 1666/D3695 |
Methanol | 67-56-1 | 1666/1671/D3695/624.1 |
Methyl Cellosolve® (2-Methoxy ethanol) | 109-86-4 | 1666/1671 |
Methylene chloride | 75-09-2 | 502.2/524.2/624.1 |
Methyl formate | 107-31-3 | 1666 |
4-Methyl-2-pentanone (MIBK) | 108-10-1 | 1624C/1666/D3695/D4763/524.2/624.1 |
Phenol | 108-95-2 | D4763 |
n-Propanol | 71-23-8 | 1666/1671/D3695/624.1 |
2-Propanone (Acetone) | 67-64-1 | D3695/D4763/524.2/624.1 |
Tetrahydrofuran | 109-99-9 | 1666/524.2/624.1 |
Toluene | 108-88-3 | D3695/D4763/502.2/524.2/624.1 |
Triethlyamine | 121-44-8 | 1666/1671 |
Xylenes | (Note 1) | 1624C/1666/624.1 |
Table IF note:
1 1624C: m-xylene 108-38-3, o,p-xylene, E-14095 (Not a CAS number; this is the number provided in the Environmental Monitoring Methods Index [EMMI] database.); 1666: m,p-xylene 136777-61-2, o-xylene 95-47-6.
Table IG-Test Methods for Pesticide Active Ingredients
[ 40 CFR part 455 ]
EPA survey code | Pesticide name | CAS No. | EPA analytical method No.(s)3 |
8 | Triadimefon | 43121-43-3 | 507/633/525.1/525.2/1656/625.1. |
12 | Dichlorvos | 62-73-7 | 1657/507/622/525.1/525.2/625.1. |
16 | 2,4-D; 2,4-D Salts and Esters [2,4-Dichloro-phenoxyacetic acid] | 94-75-7 | 1658/515.1/615/515.2/555. |
17 | 2,4-DB; 2,4-DB Salts and Esters [2,4-Dichlorophenoxybutyric acid] | 94-82-6 | 1658/515.1/615/515.2/555. |
22 | Mevinphos | 7786-34-7 | 1657/507/622/525.1/525.2/625.1. |
25 | Cyanazine | 21725-46-2 | 629/507/608.3/625.1. |
26 | Propachlor | 1918-16-7 | 1656/508/608.1/525.1/525.2/608.3/625.1. |
27 | MCPA; MCPA Salts and Esters [2-Methyl-4-chlorophenoxyacetic acid] | 94-74-6 | 1658/615/555. |
30 | Dichlorprop; Dichlorprop Salts and Esters [2-(2,4-Dichlorophenoxy) propionic acid] | 120-36-5 | 1658/515.1/615/515.2/555. |
31 | MCPP; MCPP Salts and Esters [2-(2-Methyl-4-chlorophenoxy) propionic acid] | 93-65-2 | 1658/615/555. |
35 | TCMTB [2-(Thiocyanomethylthio) benzo-thiazole] | 21564-17-0 | 637. |
39 | Pronamide | 23950-58-5 | 525.1/525.2/507/633.1/625.1. |
41 | Propanil | 709-98-8 | 632.1/1656/608.3. |
45 | Metribuzin | 21087-64-9 | 507/633/525.1/525.2/1656/608.3/625.1. |
52 | Acephate | 30560-19-1 | 1656/1657/608.3. |
53 | Acifluorfen | 50594-66-6 | 515.1/515.2/555. |
54 | Alachlor | 15972-60-8 | 505/507/645/525.1/525.2/1656/608.3/625.1. |
55 | Aldicarb | 116-06-3 | 531.1. |
58 | Ametryn | 834-12-8 | 507/619/525.2/625.1. |
60 | Atrazine | 1912-24-9 | 505/507/619/525.1/525.2/1656/ 608.3/625.1. |
62 | Benomyl | 17804-35-2 | 631. |
68 | Bromacil; Bromacil Salts and Esters | 314-40-9 | 507/633/525.1/525.2/1656/608.3/625.1. |
69 | Bromoxynil | 1689-84-5 | 1625/1661/625.1. |
69 | Bromoxynil Octanoate | 1689-99-2 | 1656/608.3. |
70 | Butachlor | 23184-66-9 | 507/645/525.1/525.2/1656/608.3/625.1. |
73 | Captafol | 2425-06-1 | 1656/608.3/625.1. |
75 | Carbaryl [Sevin] | 63-25-2 | 531.1/632/553/625.1. |
76 | Carbofuran | 1563-66-2 | 531.1/632/625.1. |
80 | Chloroneb | 2675-77-6 | 1656/508/608.1/525.1/525.2/608.3/625.1. |
82 | Chlorothalonil | 1897-45-6 | 508/608.2/525.1/525.2/1656/608.3/625.1. |
84 | Stirofos | 961-11-5 | 1657/507/622/525.1/525.2/625.1. |
86 | Chlorpyrifos | 2921-88-2 | 1657/508/622/625.1. |
90 | Fenvalerate | 51630-58-1 | 1660. |
103 | Diazinon | 333-41-5 | 1657/507/614/622/525.2/625.1. |
107 | Parathion methyl | 298-00-0 | 1657/614/622/625.1. |
110 | DCPA [Dimethyl 2,3,5,6-tetrachloro-terephthalate] | 1861-32-1 | 508/608.2/525.1/525.2/515.12/515.22/1656/608.3/625.1. |
112 | Dinoseb | 88-85-7 | 1658/515.1/615/515.2/555/625.1. |
113 | Dioxathion | 78-34-2 | 1657/614.1. |
118 | Nabonate [Disodium cyanodithio-imidocarbonate] | 138-93-2 | 630.1. |
119 | Diuron | 330-54-1 | 632/553. |
123 | Endothall | 145-73-3 | 548/548.1. |
124 | Endrin | 72-20-8 | 1656/505/508/617/525.1/525.2/608.3/625.1. |
125 | Ethalfluralin | 55283-68-6 | 1656/627/608.3 See footnote 1. |
126 | Ethion | 563-12-2 | 1657/614/614.1/625.1. |
127 | Ethoprop | 13194-48-4 | 1657/507/622/525.1/525.2/625.1. |
132 | Fenarimol | 60168-88-9 | 507/633.1/525.1/525.2/1656/608.3/625.1. |
133 | Fenthion | 55-38-9 | 1657/622/625.1. |
138 | Glyphosate [N-(Phosphonomethyl) glycine] | 1071-83-6 | 547. |
140 | Heptachlor | 76-44-8 | 1656/505/508/617/525.1/525.2/608.3/625.1. |
144 | Isopropalin | 33820-53-0 | 1656/627/608.3. |
148 | Linuron | 330-55-2 | 553/632. |
150 | Malathion | 121-75-5 | 1657/614/625.1. |
154 | Methamidophos | 10265-92-6 | 1657. |
156 | Methomyl | 16752-77-5 | 531.1/632. |
158 | Methoxychlor | 72-43-5 | 1656/505/508/608.2/617/525.1/525.2/608.3/625.1. |
172 | Nabam | 142-59-6 | 630/630.1. |
173 | Naled | 300-76-5 | 1657/622/625.1. |
175 | Norflurazon | 27314-13-2 | 507/645/525.1/525.2/1656/608.3/625.1. |
178 | Benfluralin | 1861-40-1 | 1656/627/608.3 See footnote 1. |
182 | Fensulfothion | 115-90-2 | 1657/622/625.1. |
183 | Disulfoton | 298-04-4 | 1657/507/614/622/525.2/625.1. |
185 | Phosmet | 732-11-6 | 1657/622.1/625.1. |
186 | Azinphos Methyl | 86-50-0 | 1657/614/622/625.1. |
192 | Organo-tin pesticides | 12379-54-3 | Ind-01/200.7/200.9. |
197 | Bolstar | 35400-43-2 | 1657/622. |
203 | Parathion | 56-38-2 | 1657/614/625.1. |
204 | Pendimethalin | 40487-42-1 | 1656. |
205 | Pentachloronitrobenzene | 82-68-8 | 1656/608.1/617/608.3/625.1. |
206 | Pentachlorophenol | 87-86-5 | 1625/515.2/555/515.1/525.1/525.2/625.1. |
208 | Permethrin | 52645-53-1 | 608.2/508/525.1/525.2/1656/1660/608.34/625.14. |
212 | Phorate | 298-02-2 | 1657/622/625.1. |
218 | Busan 85 [Potassium dimethyldithiocarbamate] | 128-03-0 | 630/630.1. |
219 | Busan 40 [Potassium N-hydroxymethyl-N-methyldithiocarbamate] | 51026-28-9 | 630/630.1. |
220 | KN Methyl [Potassium N-methyl-dithiocarbamate] | 137-41-7 | 630/630.1. |
223 | Prometon | 1610-18-0 | 507/619/525.2/625.1. |
224 | Prometryn | 7287-19-6 | 507/619/525.1/525.2/625.1. |
226 | Propazine | 139-40-2 | 507/619/525.1/525.2/1656/608.3/625.1. |
230 | Pyrethrin I | 121-21-1 | 1660. |
232 | Pyrethrin II | 121-29-9 | 1660. |
236 | DEF [S,S,S-Tributyl phosphorotrithioate] | 78-48-8 | 1657. |
239 | Simazine | 122-34-9 | 505/507/619/525.1/525.2/1656/608.3/625.1. |
241 | Carbam-S [Sodium dimethyldithio-carbamate] | 128-04-1 | 630/630.1. |
243 | Vapam [Sodium methyldithiocarbamate] | 137-42-8 | 630/630.1. |
252 | Tebuthiuron | 34014-18-1 | 507/525.1/525.2/625.1. |
254 | Terbacil | 5902-51-2 | 507/633/525.1/525.2/1656/608.3/625.1. |
255 | Terbufos | 13071-79-9 | 1657/507/614.1/525.1/525.2/625.1. |
256 | Terbuthylazine | 5915-41-3 | 619/1656/608.3. |
257 | Terbutryn | 886-50-0 | 507/619/525.1/525.2/625.1. |
259 | Dazomet | 533-74-4 | 630/630.1/1659. |
262 | Toxaphene | 8001-35-2 | 1656/505/508/617/525.1/525.2/608.3/625.1. |
263 | Merphos [Tributyl phosphorotrithioate] | 150-50-5 | 1657/507/525.1/525.2/622/625.1. |
264 | Trifluralin1 | 1582-09-8 | 1656/508/617/627/525.2/608.3/625.1. |
268 | Ziram [Zinc dimethyldithiocarbamate] | 137-30-4 | 630/630.1. |
Table IG notes:
1 Monitor and report as total Trifluralin.
2 Applicable to the analysis of DCPA degradates.
3 EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are available in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, Revision I, August 1993, U.S. EPA. EPA Methods 200.9 and 505 through 555 are available in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, August 1993, U.S. EPA. The full text of Methods 608.3, 625.1, and 1625 are provided at appendix A of this part. The full text of Method 200.7 is provided at appendix C of this part. Methods 608.3 and 625.1 are available at https://www.epa.gov/cwa-methods/approved-cwa-test-methods-organic-compounds.
4 Permethrin is not listed within methods 608.3 and 625.1; however, cis-permethrin and trans-permethrin are listed. Permethrin can be calculated by adding the results of cis- and trans-permethrin.
Table IH-List of Approved Microbiological Methods for Ambient Water
Parameter and units | Method 1 | EPA | Standard methods | AOAC, ASTM, USGS | Other |
Bacteria | |||||
1. Coliform (fecal), number per 100 mL | Most Probable Number (MPN), 5 tube, 3 dilution, or | p. 132 3 | 9221 E-2014, 9221 F-2014.32 | ||
Membrane filter (MF) 2, single step | p. 124 3 | 9222 D-2015 26 | B-0050-85.4 | ||
2. Coliform (total), number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 114 3 | 9221 B-2014. | ||
MF 2, single step or | p. 108 3 | 9222 B-2015 27 | B-0025-85.4 | ||
MF 2, two step with enrichment | p. 111 3 | 9222 B-2015.27 | |||
3. E. coli, number per 100 mL | MPN 5713, multiple tube, or | 9221 B.3-2014/9221 F-2014.101232 | |||
Multiple tube/multiple well, or | 9223 B-2016 11 | 991.15 9 | Colilert®1115, Colilert-18®.111415 | ||
MF 2567, two step, or | 1103.2 18 | 9222 B-2015/9222 I-2015 17, 9213 D-2007 | D5392-93.8 | ||
Single step | 1603.1 19, 1604 20 | m-ColiBlue24®16, KwikCount TM EC.2829 | |||
4. Fecal streptococci, number per 100 mL | MPN, 5 tube, 3 dilution, or | p. 139 3 | 9230 B-2013. | ||
MF 2, or | p. 136 3 | 9230 C-2013 30 | B-0055-85.4 | ||
Plate count | p. 143.3 | ||||
5. Enterococci, number per 100 mL | MPN 57, multiple tube/multiple well, or | 9230 D-2013 | D6503-99 8 | Enterolert®.1121 | |
MF 2567 two step, or | 1106.2 22 | 9230 C-2013 30 | D5259-92.8 | ||
Single step, or | 1600.1 23 | 9230 C-2013.30 | |||
Plate count | p. 143.3 | ||||
Protozoa | |||||
6. Cryptosporidium | Filtration/IMS/FA | 1622 24, 1623 25, 1623.1.2531 | |||
7. Giardia | Filtration/IMS/FA | 1623 25, 1623.1.2531 |
Table 1H notes:
1 The method must be specified when results are reported.
2 A 0.45-[MICRO]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.
3 Microbiological Methods for Monitoring the Environment, Water and Wastes. EPA/600/8-78/017. 1978. US EPA.
4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS.
5 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.
6 When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.
7 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.
8 Annual Book of ASTM Standards-Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.
9 Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.
10 The multiple-tube fermentation test is used in 9221B.3-2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.
11 These tests are collectively known as defined enzyme substrate tests.
12 After prior enrichment in a presumptive medium for total coliform using 9221B.3-2014, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F-2014. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 [MICRO]g/mL of MUG may be used.
13 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000, and the MPN calculated from the table provided by the manufacturer.
14 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 °C, rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
15 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories Inc.
16 A description of the mColiBlue24® test may be obtained from Hach Company.
17 Subject coliform positive samples determined by 9222B-2015 or other membrane filter procedure to 9222I-2015 using NA-MUG media.
18 Method 1103.2: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-23-009. September 2023. US EPA.
19 Method 1603.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified mTEC), EPA-821-R-23-008. September 2023 . US EPA.
20 Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium), EPA 821-R-02-024. September 2002. US EPA.
21 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc.
22 Method 1106.2: Enterococci in Water by Membrane Filtration Using membrane- Enterococcus -Esculin Iron Agar (mE-EIA), EPA-821-R-23-007. September 2023. US EPA.
23 Method 1600.1: Enterococci in Water by Membrane Filtration Using membrane- Enterococcus Indoxyl-[BETA]-D-Glucoside Agar (mEI), EPA-821-R-21-006. September 2023. US EPA.
24 Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. US EPA.
25 Methods 1623 and 1623.1 use a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of Cryptosporidium and Giardia oocysts and cysts. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002. December 2005. US EPA. Method 1623.1: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA 816-R-12-001. January 2012. US EPA.
26 On a monthly basis, at least ten blue colonies from positive samples must be verified using Lauryl Tryptose Broth and EC broth, followed by count adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications should be done from randomized sample sources.
27 On a monthly basis, at least ten sheen colonies from positive samples must be verified using Lauryl Tryptose Broth and brilliant green lactose bile broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications should be done from randomized sample sources.
28 A description of KwikCount TM EC may be obtained from Roth Bioscience, LLC.
29 Approved for the analyses of E. coli in freshwater only.
30 Verification of colonies by incubation of BHI agar at 10 ± 0.5 °C for 48 ± 3 h is optional. As per the Errata to the 23rd Edition of Standard Methods for the Examination of Water and Wastewater "Growth on a BHI agar plate incubated at 10 ± 0.5 °C for 48 ± 3 h is further verification that the colony belongs to the genus Enterococcus."
31 Method 1623.1 includes updated acceptance criteria for IPR, OPR, and MS/MSD and clarifications and revisions based on the use of Method 1623 for years and technical support questions.
32 9221 F.2-2014 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 II-Required Containers, Preservation Techniques, and Holding Times
Parameter number/name | Container 1 | Preservation 2 3 | Maximum holding time 4 |
Table IA-Bacterial Tests | |||
1-4. Coliform, total, fecal, and E. coli | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 23 |
5. Fecal streptococci | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
6. Enterococci | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
7. Salmonella | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
Table IA-Aquatic Toxicity Tests | |||
8-11. Toxicity, acute and chronic | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 16 | 36 hours. |
Table IB-Inorganic Tests | |||
1. Acidity | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 14 days. |
2. Alkalinity | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 14 days. |
4. Ammonia | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
9. Biochemical oxygen demand | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
10. Boron | P, FP, or Quartz | HNO3 to pH [LESS THAN]2 | 6 months. |
11. Bromide | P, FP, G | None required | 28 days. |
14. Biochemical oxygen demand, carbonaceous | P, FP G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
15. Chemical oxygen demand | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
16. Chloride | P, FP, G | None required | 28 days. |
17. Chlorine, total residual | P, G | None required | Analyze within 15 minutes. |
21. Color | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
23-24. Cyanide, total or available (or CATC) and free | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, NaOH to pH [GREATER THAN]10 5 6, reducing agent if oxidizer present | 14 days. |
25. Fluoride | P | None required | 28 days. |
27. Hardness | P, FP, G | HNO3 or H2SO4 to pH [LESS THAN]2 | 6 months. |
28. Hydrogen ion (pH) | P, FP, G | None required | Analyze within 15 minutes. |
31, 43. Kjeldahl and organic N | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
Table IB-Metals7 | |||
18. Chromium VI | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, pH = 9.3-9.7 20 | 28 days. |
35. Mercury (CVAA) | P, FP, G | HNO3 to pH [LESS THAN]2 | 28 days. |
35. Mercury (CVAFS) | FP, G; and FP-lined cap 17 | 5 mL/L 12N HCl or 5 mL/L BrCl 17 | 90 days.17 |
3, 5-8, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51, 52, 58-60, 62, 63, 70-72, 74, 75. Metals, except boron, chromium VI, and mercury | P, FP, G | HNO3 to pH [LESS THAN]2, or at least 24 hours prior to analysis 19 | 6 months. |
38. Nitrate | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
39. Nitrate-nitrite | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
40. Nitrite | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
41. Oil and grease | G | Cool to [LESS THAN EQUAL TO]6 °C 18, HCl or H2SO4 to pH [LESS THAN]2 | 28 days. |
42. Organic Carbon | P, FP, G | Cool to [LESS THAN EQUAL TO]6 °C 18, HCl, H2SO4, or H3PO4 to pH [LESS THAN]2 | 28 days. |
44. Orthophosphate | P, FP, G | Cool, to [LESS THAN EQUAL TO]6 °C 18 24 | Filter within 15 minutes; Analyze within 48 hours. |
46. Oxygen, Dissolved Probe | G, Bottle and top | None required | Analyze within 15 minutes. |
47. Winkler | G, Bottle and top | Fix on site and store in dark | 8 hours. |
48. Phenols | G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
49. Phosphorus (elemental) | G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
50. Phosphorus, total | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, H2SO4 to pH [LESS THAN]2 | 28 days. |
53. Residue, total | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days. |
54. Residue, Filterable (TDS) | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days. |
55. Residue, Nonfilterable (TSS) | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days. |
56. Residue, Settleable | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
57. Residue, Volatile | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days. |
61. Silica | P or Quartz | Cool, [LESS THAN EQUAL TO]6 °C 18 | 28 days. |
64. Specific conductance | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 28 days. |
65. Sulfate | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 28 days. |
66. Sulfide | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18, add zinc acetate plus sodium hydroxide to pH [GREATER THAN]9 | 7 days. |
67. Sulfite | P, FP, G | None required | Analyze within 15 minutes. |
68. Surfactants | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
69. Temperature | P, FP, G | None required | Analyze within 15 minutes. |
73. Turbidity | P, FP, G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 48 hours. |
Table IC-Organic Tests8 | |||
13, 18-20, 22, 24, 25, 27, 28, 34-37, 39-43, 45-47, 56, 76, 104, 105, 108-111, 113. Purgeable Halocarbons | G, FP-lined septum | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35, HCl to pH 2 9 | 14 days.9 |
26. 2-Chloroethylvinyl ether | G, FP-lined septum | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35 | 14 days. |
6, 57, 106. Purgeable aromatic hydrocarbons | G, FP-lined septum | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35, HCl to pH 2 9 | 14 days.9 |
3, 4. Acrolein and acrylonitrile | G, FP-lined septum | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O3, pH to 4-5 10 | 14 days.10 |
23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112. Phenols 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O3 | 7 days until extraction, 40 days after extraction. |
7, 38. Benzidines 11 12 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35 | 7 days until extraction.13 |
14, 17, 48, 50-52. Phthalate esters 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days until extraction, 40 days after extraction. |
82-84. Nitrosamines 11 14 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, store in dark, 0.008% Na2S2O35 | 7 days until extraction, 40 days after extraction. |
88-94. PCBs 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18 | 1 year until extraction, 1 year after extraction. |
54, 55, 75, 79. Nitroaromatics and isophorone 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, store in dark, 0.008% Na2S2O35 | 7 days until extraction, 40 days after extraction. |
1, 2, 5, 8-12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, store in dark, 0.008% Na2S2O35 | 7 days until extraction, 40 days after extraction. |
15, 16, 21, 31, 87. Haloethers 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35 | 7 days until extraction, 40 days after extraction. |
29, 35-37, 63-65, 73, 107. Chlorinated hydrocarbons 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days until extraction, 40 days after extraction. |
60-62, 66-72, 85, 86, 95-97, 102, 103. CDDs/CDFs 11 | G | See footnote 11 | See footnote 11. |
Aqueous Samples: Field and Lab Preservation | G | Cool, [LESS THAN EQUAL TO]6 °C 18, 0.008% Na2S2O35, pH [LESS THAN]9 | 1 year. |
Solids and Mixed-Phase Samples: Field Preservation | G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 7 days. |
Tissue Samples: Field Preservation | G | Cool, [LESS THAN EQUAL TO]6 °C 18 | 24 hours. |
Solids, Mixed-Phase, and Tissue Samples: Lab Preservation | G | Freeze, [LESS THAN EQUAL TO]-10 °C | 1 year. |
114-118. Alkylated phenols | G | Cool, [LESS THAN]6 °C, H2SO4 to pH [LESS THAN]2 | 28 days until extraction, 40 days after extraction. |
119. Adsorbable Organic Halides (AOX) | G | Cool, [LESS THAN]6 °C, 0.008% Na2S2O3, HNO3 to pH [LESS THAN]2 | Hold at least 3 days, but not more than 6 months. |
120. Chlorinated Phenolics | G, FP-lined cap | Cool, [LESS THAN]6 °C, 0.008% Na2S2O3, H2SO4 to pH [LESS THAN]2 | 30 days until acetylation, 30 days after acetylation. |
Table ID-Pesticides Tests | |||
1-70. Pesticides 11 | G, FP-lined cap | Cool, [LESS THAN EQUAL TO]6 °C 18, pH 5-9 15 | 7 days until extraction, 40 days after extraction. |
Table IE-Radiological Tests | |||
1-5. Alpha, beta, and radium | P, FP, G | HNO3 to pH [LESS THAN]2 | 6 months. |
Table IH-Bacterial Tests | |||
1, 2. Coliform, total, fecal | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
3.E. coli | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
4. Fecal streptococci | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
5. Enterococci | PA, G | Cool, [LESS THAN]10 °C, 0.008% Na2S2O35 | 8 hours.22 |
Table IH-Protozoan Tests | |||
6. Cryptosporidium | LDPE; field filtration | 1-10 °C | 96 hours.21 |
7. Giardia | LDPE; field filtration | 1-10 °C | 96 hours.21 |
1 "P" is for polyethylene; "FP" is fluoropolymer (polytetrafluoroethylene [PTFE]; Teflon®), or other fluoropolymer, unless stated otherwise in this Table II; "G" is glass; "PA" is any plastic that is made of a sterilizable material (polypropylene or other autoclavable plastic); "LDPE" is low density polyethylene.
2 Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15 minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour composite sample; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), refrigerate the sample at [LESS THAN EQUAL TO]6 °C during collection unless specified otherwise in this Table II or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at [LESS THAN EQUAL TO]6 °C, unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite sample within 15 minutes of collection. If a composite measurement is required but a composite sample would compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations averaged. Alternatively, grab samples may be collected in the field and composited in the laboratory if the compositing procedure produces results equivalent to results produced by arithmetic averaging of results of analysis of individual grab samples. For examples of laboratory compositing procedures, see EPA Method 1664 Rev. A (oil and grease) and the procedures at 40 CFR 141.24(f)(14)(iv) and (v) (volatile organics).
3 When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with the Department of Transportation Hazardous Materials Regulations ( 49 CFR part 172 ). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirement of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater; Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less).
4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before the start of analysis and still be considered valid. Samples may be held for longer periods only if the permittee or monitoring laboratory have data on file to show that, for the specific types of samples under study, the analytes are stable for the longer time, and has received a variance from the Regional ATP Coordinator under § 136.3(e) . For a grab sample, the holding time begins at the time of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), the holding time begins at the time of the end of collection of the composite sample. For a set of grab samples composited in the field or laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain sample stability. See § 136.3(e) for details. The date and time of collection of an individual grab sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and that are all collected on the same calendar date, the date of collection is the date on which the samples are collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected automatically on a given date, the date of collection is the date on which the sample is collected. For a composite sample collected automatically, and that is collected across two calendar dates, the date of collection is the dates of the two days; e.g., November 14-15. For static-renewal toxicity tests, each grab or composite sample may also be used to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after first use, if stored at 0-6 °C, with minimum head space.
5 ASTM D7365-09a (15) specifies treatment options for samples containing oxidants (e.g ., chlorine) for cyanide analyses. Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (23rd edition) addresses dechlorination procedures for microbiological analyses.
6 Sampling, preservation and mitigating interferences in water samples for analysis of cyanide are described in ASTM D7365-09a (15). There may be interferences that are not mitigated by the analytical test methods or D7365-09a (15). Any technique for removal or suppression of interference may be employed, provided the laboratory demonstrates that it more accurately measures cyanide through quality control measures described in the analytical test method. Any removal or suppression technique not described in D7365-09a (15) or the analytical test method must be documented along with supporting data.
7 For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), filter the sample within 15 minutes after completion of collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will be compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically.
8 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
9 If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
10 The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.
11 When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed for optimum safeguard of sample integrity (i.e., use all necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to [LESS THAN EQUAL TO]6 °C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine.
13 Extracts may be stored up to 30 days at [LESS THAN]0 °C.
14 For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours of sampling.
15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
16 Place sufficient ice with the samples in the shipping container to ensure that ice is still present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 °C prior to test initiation.
17 Samples collected for the determination of trace level mercury ([LESS THAN]100 ng/L) using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48 hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669. If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be filtered in a designated clean area in the field within the time period necessary to maintain sample integrity. A sample that has been collected for determination of total or dissolved trace level mercury must be analyzed within 90 days of sample collection.
18 Aqueous samples must be preserved at [LESS THAN EQUAL TO]6 °C, and should not be frozen unless data demonstrating that sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the regulatory authority. Also, for purposes of NPDES monitoring, the specification of "[LESS THAN EQUAL TO] °C" is used in place of the "4 °C" and "[LESS THAN]4 °C" sample temperature requirements listed in some methods. It is not necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three significant figures are specified so that rounding down to 6 °C may not be used to meet the [LESS THAN EQUAL TO]6 °C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than 15 minutes).
19 An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and holding time requirements in the approved metals methods.
20 To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6. The allowance in this footnote supersedes preservation and holding time requirements in the approved hexavalent chromium methods, unless this supersession would compromise the measurement, in which case requirements in the method must be followed.
21 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
22 Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection.
23 For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B aerobically digested, and Class B anaerobically digested.
24 The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-available form of orthophosphorus (i.e., that which passes through a 0.45-micron filter), hence the requirement to filter the sample immediately upon collection (i.e., within 15 minutes of collection).
40 C.F.R. §136.3
For FEDERAL REGISTER citations affecting § 136.3 , see the List of CFR Sections Affected, which appears in the Finding Aids section of the printed volume and at www.govinfo.gov.