Title 40—Protection of Environment--Volume 1
PART 136—GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS
§ 136.1   Applicability.
(a) The procedures prescribed herein shall, except as noted in §§ 136.4, 136.5, and 136.6, be used to perform the measurements indicated whenever the waste constituent specified is required to be measured for:
(1) An application submitted to the Director and/or reports required to be submitted under NPDES permits or other requests for quantitative or qualitative effluent data under parts 122 through 125 of this chapter; and
(2) Reports required to be submitted by dischargers under the NPDES established by parts 124 and 125 of this chapter; and
(3) Certifications issued by States pursuant to section 401 of the Clean Water Act (CWA), as amended.
(b) The procedure prescribed herein and in part 503 of title 40 shall be used to perform the measurements required for an application submitted to the Administrator or to a State for a sewage sludge permit under section 405(f) of the Clean Water Act and for recordkeeping and reporting requirements under part 503 of title 40.
(c) For the purposes of the NPDES program, when more than one test procedure is approved under this part for the analysis of a pollutant or pollutant parameter, the test procedure must be sufficiently sensitive as defined at 40 CFR 122.21(e)(3) and 122.44(i)(1)(iv).
§ 136.2   Definitions.
As used in this part, the term:
(a) Act means the Clean Water Act of 1977, Pub. L. 95-217, 91 Stat. 1566, et seq. (33 U.S.C. 1251 et seq. ) (The Federal Water Pollution Control Act Amendments of 1972 as amended by the Clean Water Act of 1977).
(b) Administrator means the Administrator of the U.S. Environmental Protection Agency.
(c) Regional Administrator means one of the EPA Regional Administrators.
(d) Director means the director as defined in 40 CFR 122.2.
(e) National Pollutant Discharge Elimination System (NPDES) means the national system for the issuance of permits under section 402 of the Act and includes any State or interstate program which has been approved by the Administrator, in whole or in part, pursuant to section 402 of the Act.
(f) Detection limit means the minimum concentration of an analyte (substance) that can be measured and reported with a 99% confidence that the analyte concentration is distinguishable from the method blank results as determined by the procedure set forth at appendix B of this part.
§ 136.3   Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, IF, IG, and IH of this section. The methods listed in Tables IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see paragraph (b) of this section, with the exception of EPA Methods 200.7, 601-613, 624.1, 625.1, 1613, 1624, and 1625. The full texts of Methods 601-613, 624.1, 625.1, 1613, 1624, and 1625 are printed in appendix A of this part, and the full text of Method 200.7 is printed in appendix C of this part. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part. In the event of a conflict between the reporting requirements of 40 CFR parts 122 and 125 and any reporting requirements associated with the methods listed in these tables, the provisions of 40 CFR parts 122 and 125 are controlling and will determine a permittee's reporting requirements. The full texts of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and IH. The date after the method number indicates the latest editorial change of the method. The discharge parameter values for which reports are required must be determined by one of the standard analytical test procedures incorporated by reference and described in Tables IA, IB, IC, ID, IE, IF, IG, and IH or by any alternate test procedure which has been approved by the Administrator under the provisions of paragraph (d) of this section and §§ 136.4 and 136.5. Under certain circumstances (paragraph (c) of this section, § 136.5(a) through (d) or 40 CFR 401.13,) other additional or alternate test procedures may be used.
Table IA—List of Approved Biological Methods for Wastewater and Sewage Sludge
Table IA notes:
1 The method must be specified when results are reported.
2 A 0.45-µm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.
3 Microbiological Methods for Monitoring the Environment, Water and Wastes, EPA/600/8-78/017. 1978. 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 µg/mL of MUG may be used.
15 Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-14-009. September 2014. U.S. EPA.
16 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000 and the MPN calculated from the table provided by the manufacturer.
17 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
18 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc.
19 A description of the mColiBlue24® test is available from Hach Company.
20 Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
21 Method 1603.1: 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-β-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
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 StablCal TM 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.
Table IC—List of Approved Test Procedures for Non-Pesticide Organic Compounds
Table IC notes:
1 All parameters are expressed in micrograms per liter (µg/L) except for Method 1613B, in which the parameters are expressed in picograms per liter (pg/L).
2 The full text of Methods 601-613, 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 Empore TM 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 Pesticides 1
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 α-BHC, γ-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
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
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]
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
Table 1H notes:
1 The method must be specified when results are reported.
2 A 0.45-µm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.
3 Microbiological Methods for Monitoring the Environment, Water and Wastes. EPA/600/8-78/017. 1978. 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 µg/mL of MUG may be used.
13 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000, and the MPN calculated from the table provided by the manufacturer.
14 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 °C, rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
15 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray ®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories Inc.
16 A description of the mColiBlue24® test may be obtained from Hach Company.
17 Subject coliform positive samples determined by 9222B-2015 or other membrane filter procedure to 9222I-2015 using NA-MUG media.
18 Method 1103.2: 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-β-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.
(b) The material listed in this paragraph (b) is incorporated by reference into this section with the approval of the Director of the Federal Register under 5 U.S.C. 552(a) and 1 CFR part 51. All approved incorporation by reference (IBR) material is available for inspection at the EPA and at the National Archives and Records Administration (NARA). Contact the EPA at: EPA's Water Docket, EPA West, 1301 Constitution Avenue NW, Room 3334, Washington, DC 20004; telephone: 202-566-2426; email: docket-customerservice@epa.gov. For information on the availability of this material at NARA, visit www.archives.gov/federal-register/cfr/ibr-locations or email fr.inspection@nara.gov. The material may be obtained from the following sources in this paragraph (b).
(1) Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161
(i) Microbiological Methods for Monitoring the Environment, Water, and Wastes. 1978. EPA/600/8-78/017, Pub. No. PB-290329/A.S.
(A) Part III Analytical Methodology, Section B Total Coliform Methods, page 108. Table IA, Note 3; Table IH, Note 3.
(B) Part III Analytical Methodology, Section B Total Coliform Methods, 2.6.2 Two-Step Enrichment Procedure, page 111. Table IA, Note 3; Table IH, Note 3.
(C) Part III Analytical Methodology, Section B Total Coliform Methods, 4 Most Probable Number (MPN) Method, page 114. Table IA, Note 3; Table IH, Note 3.
(D) Part III Analytical Methodology, Section C Fecal Coliform Methods, 2 Direct Membrane Filter (MF) Method, page 124. Table IA, Note 3; Table IH, Note 3.
(E) Part III, Analytical Methodology, Section C Fecal Coliform Methods, 5 Most Probable Number (MPN) Method, page 132. Table IA, Note 3; Table IH, Note 3.
(F) Part III Analytical Methodology, Section D Fecal Streptococci, 2 Membrane Filter (MF) Method, page 136. Table IA, Note 3; Table IH, Note 3.
(G) Part III Analytical Methodology, Section D Fecal Streptococci, 4 Most Probable Number Method, page 139. Table IA, Note 3; Table IH, Note 3.
(H) Part III Analytical Methodology, Section D Fecal Streptococci, 5 Pour Plate Method, page 143. Table IA, Note 3; Table IH, Note 3.
(ii) [Reserved]
(2) Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i) Method 300.1 (including Errata Cover Sheet, April 27, 1999), Determination of Inorganic Ions in Drinking Water by Ion Chromatography, Revision 1.0, 1997. Table IB, Note 52.
(ii) Method 551, Determination of Chlorination Disinfection Byproducts and Chlorinated Solvents in Drinking Water by Liquid-Liquid Extraction and Gas Chromatography With Electron-Capture Detection. 1990. Table IF.
(3) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available from http://water.epa.gov/scitech/methods/cwa/index.cfm or from the National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Telephone: 800-553-6847.
(i) Methods for the Determination of Inorganic Substances in Environmental Samples. August 1993. EPA/600/R-93/100, Pub. No. PB 94120821. Table IB, Note 52.
(A) Method 180.1, Determination of Turbidity by Nephelometry. Revision 2.0. Table IB, Note 52.
(B) Method 300.0, Determination of Inorganic Anions by Ion Chromatography. Revision 2.1. Table IB, Note 52.
(C) Method 335.4, Determination of Total Cyanide by Semi-Automated Colorimetry. Revision 1.0. Table IB, Notes 52 and 57.
(D) Method 350.1, Determination of Ammonium Nitrogen by Semi-Automated Colorimetry. Revision 2.0. Table IB, Notes 30 and 52.
(E) Method 351.2, Determination of Total Kjeldahl Nitrogen by Semi-Automated Colorimetry. Revision 2.0. Table IB, Note 52.
(F) Method 353.2, Determination of Nitrate-Nitrite Automated Colorimetry. Revision 2.0. Table IB, Note 52.
(G) Method 365.1, Determination of Phosphorus by Automated Colorimetry. Revision 2.0. Table IB, Note 52.
(H) Method 375.2, Determination of Sulfate by Automated Colorimetry. Revision 2.0. Table IB, Note 52.
(I) Method 410.4, Determination of Chemical Oxygen Demand by Semi-Automated Colorimetry. Revision 2.0. Table IB, Note 52.
(ii) Methods for the Determination of Metals in Environmental Samples, Supplement I. May 1994. EPA/600/R-94/111, Pub. No. PB 95125472. Table IB, Note 52.
(A) Method 200.7, Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry. Revision 4.4. Table IB, Note 52.
(B) Method 200.8, Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma Mass Spectrometry. Revision 5.3. Table IB, Note 52.
(C) Method 200.9, Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry. Revision 2.2. Table IB, Note 52.
(D) Method 218.6, Determination of Dissolved Hexavalent Chromium in Drinking Water, Groundwater, and Industrial Wastewater Effluents by Ion Chromatography. Revision 3.3. Table IB, Note 52.
(E) Method 245.1, Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry. Revision 3.0. Table IB, Note 52.
(4) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i) EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry. Revision 4.2, October 2003. EPA/600/R-06/115. Table IB, Note 68.
(ii) EPA Method 525.2, Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry. Revision 2.0, 1995. Table ID, Note 10.
(5) Office of Research and Development, Cincinnati OH. U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from ORD Publications, CERI, U.S. Environmental Protection Agency, Cincinnati OH 45268.
(i) Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol, and Pesticides in Water and Wastewater. 1978. Table IC, Note 3; Table ID, Note 3.
(ii) Methods for Chemical Analysis of Water and Wastes. March 1979. EPA-600/4-79-020. Table IB, Note 1.
(iii) Methods for Chemical Analysis of Water and Wastes. Revised March 1983. EPA-600/4-79-020. Table IB, Note 1.
(A) Method 120.1, Conductance, Specific Conductance, µmhos at 25 °C. Revision 1982. Table IB, Note 1.
(B) Method 130.1, Hardness, Total (mg/L as CaCO 3 ), Colorimetric, Automated EDTA. Issued 1971. Table IB, Note 1.
(C) Method 150.2, pH, Continuous Monitoring (Electrometric). December 1982. Table IB, Note 1.
(D) Method 160.4, Residue, Volatile, Gravimetric, Ignition at 550 °C. Issued 1971. Table IB, Note 1.
(E) Method 206.5, Arsenic, Sample Digestion Prior to Total Arsenic Analysis by Silver Diethyldithiocarbamate or Hydride Procedures. Issued 1978. Table IB, Note 1.
(F) Method 231.2, Gold, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(G) Method 245.2, Mercury, Automated Cold Vapor Technique. Issued 1974. Table IB, Note 1.
(H) Method 252.2, Osmium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(I) Method 253.2, Palladium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(J) Method 255.2, Platinum, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(K) Method 265.2, Rhodium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(L) Method 279.2, Thallium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(M) Method 283.2, Titanium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(N) Method 289.2, Zinc, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.
(O) Method 310.2, Alkalinity, Colorimetric, Automated, Methyl Orange. Revision 1974. Table IB, Note 1.
(P) Method 351.1, Nitrogen, Kjeldahl, Total, Colorimetric, Automated Phenate. Revision 1978. Table IB, Note 1.
(Q) Method 352.1, Nitrogen, Nitrate, Colorimetric, Brucine. Issued 1971. Table IB, Note 1.
(R) Method 365.3, Phosphorus, All Forms, Colorimetric, Ascorbic Acid, Two Reagent. Issued 1978. Table IB, Note 1.
(S) Method 365.4, Phosphorus, Total, Colorimetric, Automated, Block Digestor AA II. Issued 1974. Table IB, Note 1.
(T) Method 410.3, Chemical Oxygen Demand, Titrimetric, High Level for Saline Waters. Revision 1978. Table IB, Note 1.
(U) Method 420.1, Phenolics, Total Recoverable, Spectrophotometric, Manual 4-AAP With Distillation. Revision 1978. Table IB, Note 1.
(iv) Prescribed Procedures for Measurement of Radioactivity in Drinking Water. 1980. EPA-600/4-80-032. Table IE.
(A) Method 900.0, Gross Alpha and Gross Beta Radioactivity. Table IE.
(B) Method 903.0, Alpha-Emitting iRadio Isotopes. Table IE.
(C) Method 903.1, Radium-226, Radon Emanation Technique. Table IE.
(D) Appendix B, Error and Statistical Calculations. Table IE.
(6) Office of Science and Technology, U.S. Environmental Protection Agency, Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.
(i) Method 1625C, Semivolatile Organic Compounds by Isotope Dilution GCMS. 1989. Table IF.
(ii) [Reserved]
(7) Office of Water, U.S. Environmental Protection Agency, Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.
(i) Method 1631, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry. Revision E, August 2002. EPA-821-R-02-019, Pub. No. PB2002-108220. Table IB, Note 43.
(ii) Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate. Revision 1.2, August 2001. EPA 821-B-01-009, Pub. No. PB 2001-108275. Table IB, Note 55.
(iii) In the compendium Analytical Methods for the Determination of Pollutants in Pharmaceutical Manufacturing Industry Wastewaters. July 1998. EPA 821-B-98-016, Pub. No. PB95201679. Table IF, Note 1.
(A) EPA Method 1666, Volatile Organic Compounds Specific to the Pharmaceutical Industry by Isotope Dilution GC/MS. Table IF, Note 1.
(B) EPA Method 1667, Formaldehyde, Isobutyraldehyde, and Furfural by Derivatization Followed by High Performance Liquid Chromatography. Table IF.
(C) Method 1671, Volatile Organic Compounds Specific to the Pharmaceutical Manufacturing Industry by GC/FID. Table IF.
(iv) Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I. Revision I, August 1993. EPA 821-R-93-010A, Pub. No. PB 94121654. Tables ID, IG.
(A) Method 608.1, Organochlorine Pesticides. Table ID, Note 10; Table IG, Note 3.
(B) Method 608.2, Certain Organochlorine Pesticides. Table ID, Note 10; Table IG, Note 3.
(C) Method 614, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.
(D) Method 614.1, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.
(E) Method 615, Chlorinated Herbicides. Table ID, Note 10; Table IG, Note 3.
(F) Method 617, Organohalide Pesticides and PCBs. Table ID, Note 10; Table IG, Note 3.
(G) Method 619, Triazine Pesticides. Table ID, Note 10; Table IG, Note 3.
(H) Method 622, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.
(I) Method 622.1, Thiophosphate Pesticides. Table ID, Note 10; Table IG, Note 3.
(J) Method 627, Dinitroaniline Pesticides. Table ID, Note 10; Table IG, Notes 1 and 3.
(K) Method 629, Cyanazine. Table IG, Note 3.
(L) Method 630, Dithiocarbamate Pesticides. Table IG, Note 3.
(M) Method 630.1, Dithiocarbamate Pesticides. Table IG, Note 3.
(N) Method 631, Benomyl and Carbendazim. Table IG, Note 3.
(O) Method 632, Carbamate and Urea Pesticides. Table ID, Note 10; Table IG, Note 3.
(P) Method 632.1, Carbamate and Amide Pesticides. Table IG, Note 3.
(Q) Method 633, Organonitrogen Pesticides. Table IG, Note 3.
(R) Method 633.1, Neutral Nitrogen-Containing Pesticides. Table IG, Note 3.
(S) Method 637, MBTS and TCMTB. Table IG, Note 3.
(T) Method 644, Picloram. Table IG, Note 3.
(U) Method 645, Certain Amine Pesticides and Lethane. Table IG, Note 3.
(V) Method 1656, Organohalide Pesticides. Table ID, Note 10; Table IG, Notes 1 and 3.
(W) Method 1657, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.
(X) Method 1658, Phenoxy-Acid Herbicides. Table IG, Note 3.
(Y) Method 1659, Dazomet. Table IG, Note 3.
(Z) Method 1660, Pyrethrins and Pyrethroids. Table IG, Note 3.
(AA) Method 1661, Bromoxynil. Table IG, Note 3.
(BB) Ind-01. Methods EV-024 and EV-025, Analytical Procedures for Determining Total Tin and Triorganotin in Wastewater. Table IG, Note 3.
(v) Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume II. August 1993. EPA 821-R-93-010B, Pub. No. PB 94166311. Table IG.
(A) Method 200.9, Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry. Table IG, Note 3.
(B) Method 505, Analysis of Organohalide Pesticides and Commercial Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and Gas Chromatography. Table ID, Note 10; Table IG, Note 3.
(C) Method 507, The Determination of Nitrogen- and Phosphorus-Containing Pesticides in Water by Gas Chromatography with a Nitrogen-Phosphorus Detector. Table ID, Note 10; Table IG, Note 3.
(D) Method 508, Determination of Chlorinated Pesticides in Water by Gas Chromatography with an Electron Capture Detector. Table ID, Note 10; Table IG, Note 3.
(E) Method 515.1, Determination of Chlorinated Acids in Water by Gas Chromatography with an Electron Capture Detector. Table IG, Notes 2 and 3.
(F) Method 515.2, Determination of Chlorinated Acids in Water Using Liquid-Solid Extraction and Gas Chromatography with an Electron Capture Detector. Table IG, Notes 2 and 3.
(G) Method 525.1, Determination of Organic Compounds in Drinking Water by Liquids-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry. Table ID, Note 10; Table IG, Note 3.
(H) Method 531.1, Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization. Table ID, Note 10; Table IG, Note 3.
(I) Method 547, Determination of Glyphosate in Drinking Water by Direct-Aqueous-Injection HPLC, Post-Column Derivatization, and Fluorescence Detection. Table IG, Note 3.
(J) Method 548, Determination of Endothall in Drinking Water by Aqueous Derivatization, Liquid-Solid Extraction, and Gas Chromatography with Electron-Capture Detector. Table IG, Note 3.
(K) Method 548.1, Determination of Endothall in Drinking Water by Ion-Exchange Extraction, Acidic Methanol Methylation and Gas Chromatography/Mass Spectrometry. Table IG, Note 3.
(L) Method 553, Determination of Benzidines and Nitrogen-Containing Pesticides in Water by Liquid-Liquid Extraction or Liquid-Solid Extraction and Reverse Phase High Performance Liquid Chromatography/Particle Beam/Mass Spectrometry Table ID, Note 10; Table IG, Note 3.
(M) Method 555, Determination of Chlorinated Acids in Water by High Performance Liquid Chromatography With a Photodiode Array Ultraviolet Detector. Table IG, Note 3.
(vi) In the compendium Methods for the Determination of Organic Compounds in Drinking Water. Revised July 1991, December 1998. EPA-600/4-88-039, Pub. No. PB92-207703. Table IF.
(A) EPA Method 502.2, Volatile Organic Compounds in Water by Purge and Trap Capillary Column Gas Chromatography with Photoionization and Electrolytic Conductivity Detectors in Series. Table IF.
(B) [Reserved]
(vii) In the compendium Methods for the Determination of Organic Compounds in Drinking Water-Supplement II. August 1992. EPA-600/R-92-129, Pub. No. PB92-207703. Table IF.
(A) EPA Method 524.2, Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry. Table IF.
(B) [Reserved]
(viii) Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, Fifth Edition. October 2002. EPA 821-R-02-012, Pub. No. PB2002-108488. Table IA, Note 26.
(ix) Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition. October 2002. EPA 821-R-02-013, Pub. No. PB2002-108489. Table IA, Note 27.
(x) Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, Third Edition. October 2002. EPA 821-R-02-014, Pub. No. PB2002-108490. Table IA, Note 28.
(8) Office of Water, U.S. Environmental Protection Agency (U.S. EPA), mail code 4303T, 1301 Constitution Avenue NW, Washington, DC 20460; website: www.epa.gov/cwa-methods.
(i) Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry. Revision 2.0, February 2005. EPA-821-R-05-001. Table IB, Note 17.
(ii) 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. Table IH, Note 18.
(iii) Method 1106.2: Enterococci in Water by Membrane Filtration Using membrane- Enterococcus -Esculin Iron Agar (mE-EIA), EPA-821-R-23-007. September 2023. Table IH, Note 22.
(iv) Method 1600.1: Enterococci in Water by Membrane Filtration Using membrane- Enterococcus Indoxyl-β-D-Glucoside Agar (mEI), EPA-821-R-23-006, September 2023. Table 1A, Note 24; Table IH, Note 23.
(v) 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. Table IA, Note 21; Table IH, Note 19.
(vi) Method 1604: Total Coliforms and Escherichia coli ( E. coli ) in Water by Membrane Filtration Using a Simultaneous Detection Technique (MI Medium). September 2002. EPA-821-R-02-024. Table IH, Note 21.
(vii) Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016, Table IA, Notes 25, 26, and 27.
(viii) Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. December 2005. EPA-821-R-05-002. Table IH, Note 26.
(ix) Method 1623.1: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA 816-R-12-001. January 2012. U.S. EPA, Table IH, Notes 25 and 31.
(x) Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality. December 2011. EPA-821-R-09-002. Table IB, Note 69.
(xi) Method 1664, n -Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n -Hexane Extractable Material (SGT-HEM; Nonpolar Material) by Extraction and Gravimetry. Revision A, February 1999. EPA-821-R-98-002. Table IB, Notes 38 and 42.
(xii) Method 1664, n -Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n -Hexane Extractable Material (SGT-HEM; Nonpolar Material) by Extraction and Gravimetry, Revision B, February 2010. EPA-821-R-10-001. Table IB, Notes 38 and 42.
(xiii) Method 1669, Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels. July 1996. Table IB, Note 43.
(xiv) Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using Lauryl Tryptose Broth (LTB) and EC Medium. September 2014. EPA-821-R-14-009.Table IA, Note 15.
(xv) Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. July 2006. EPA 821-R-06-013. Table IA, Note 20.
(xvi) Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. September 2014. EPA 821-R-14-012. Table IA, Note 23.
(9) American National Standards Institute, 1430 Broadway, New York NY 10018.
(i) ANSI. American National Standard on Photographic Processing Effluents. April 2, 1975. Table IB, Note 9.
(ii) [Reserved]
(10) American Public Health Association, 800 I Street, NW, Washington, DC 20001; phone: (202)777-2742, website: www.standardmethods.org.
(i) Standard Methods for the Examination of Water and Wastewater. 14th Edition, 1975. Table IB, Notes 27 and 86.
(ii) Standard Methods for the Examination of Water and Wastewater. 15th Edition, 1980, Table IB, Note 30; Table ID.
(iii) 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. Table IC, Note 6; Table ID, Note 6.
(iv) Standard Methods for the Examination of Water and Wastewater. 18th Edition, 1992. Tables IA, IB, IC, ID, IE, and IH.
(v) Standard Methods for the Examination of Water and Wastewater. 19th Edition, 1995. Tables IA, IB, IC, ID, IE, and IH.
(vi) Standard Methods for the Examination of Water and Wastewater. 20th Edition, 1998. Tables IA, IB, IC, ID, IE, and IH.
(vii) Standard Methods for the Examination of Water and Wastewater. 21st Edition, 2005. Table IB, Notes 17 and 27.
(viii) 2120, Color. Revised September 4, 2021. Table IB.
(ix) 2130, Turbidity. Revised 2020. Table IB.
(x) 2310, Acidity. Revised 2020. Table IB.
(xi) 2320, Alkalinity. Revised 2021. Table IB.
(xii) 2340, Hardness. Revised 2021. Table IB.
(xiii) 2510, Conductivity. Revised 2021. Table IB.
(xiv) 2540, Solids. Revised 2020. Table IB.
(xv) 2550, Temperature. 2010. Table IB.
(xvi) 3111, Metals by Flame Atomic Absorption Spectrometry. Revised 2019. Table IB.
(xvii) 3112, Metals by Cold-Vapor Atomic Absorption Spectrometry. Revised 2020. Table IB.
(xviii) 3113, Metals by Electrothermal Atomic Absorption Spectrometry. Revised 2020. Table IB.
(xix) 3114, Arsenic and Selenium by Hydride Generation/Atomic Absorption Spectrometry. Revised 2020, Table IB.
(xx) 3120, Metals by Plasma Emission Spectroscopy. Revised 2020. Table IB.
(xxi) 3125, Metals by Inductively Coupled Plasma-Mass Spectrometry. Revised 2020. Table IB.
(xxii) 3500-Al, Aluminum. Revised 2020. Table IB.
(xxiii) 3500-As, Arsenic. Revised 2020. Table IB.
(xxiv) 3500-Ca, Calcium. Revised 2020. Table IB.
(xxv) 3500-Cr, Chromium. Revised 2020. Table IB.
(xxvi) 3500-Cu, Copper. Revised 2020. Table IB.
(xxvii) 3500-Fe, Iron. 2011. Table IB.
(xxviii) 3500-Pb, Lead. Revised 2020. Table IB.
(xxix) 3500-Mn, Manganese. Revised 2020. Table IB.
(xxx) 3500-K, Potassium. Revised 2020. Table IB.
(xxxi) 3500-Na, Sodium. Revised 2020. Table IB.
(xxxii) 3500-V, Vanadium. 2011. Table IB.
(xxxiii) 3500-Zn, Zinc. Revised 2020. Table IB.
(xxxiv) 4110, Determination of Anions by Ion Chromatography. Revised 2020. Table IB.
(xxxv) 4140, Inorganic Anions by Capillary Ion Electrophoresis. Revised 2020. Table IB.
(xxxvi) 4500-B, Boron. 2011. Table IB.
(xxxvii) 4500 Cl − , Chloride. Revised 2021. Table IB.
(xxxviii) 4500-Cl, Chlorine (Residual). 2011. Table IB.
(xxxix) 4500-CN − , Cyanide. Revised 2021. Table IB.
(xl) 4500-F − , Fluoride. Revised 2021. Table IB.
(xli) 4500-H + , pH. 2021. Table IB.
(xlii) 4500-NH 3 , Nitrogen (Ammonia). Revised 2021. Table IB.
(xliii) 4500-NO 2 − , Nitrogen (Nitrite). Revised 2021. Table IB.
(xliv) 4500-NO 3 − , Nitrogen (Nitrate). Revised 2019. Table IB.
(xlv) 4500-N (org) , Nitrogen (Organic). Revised 2021. Table IB.
(xlvi) 4500-O, Oxygen (Dissolved). Revised 2021. Table IB.
(xlvii) 4500-P, Phosphorus. Revised 2021. Table IB.
(xlviii) 4500-SiO 2 , Silica. Revised 2021. Table IB.
(xlix) 4500-S 2− , Sulfide. Revised 2021. Table IB.
(l) 4500-SO 3 2− , Sulfite. Revised 2021. Table IB.
(li) 4500-SO 4 2− , Sulfate. Revised 2021. Table IB.
(lii) 5210, Biochemical Oxygen Demand (BOD). Revised 2016. Table IB.
(liii) 5220, Chemical Oxygen Demand (COD). 2011. Table IB.
(liv) 5310, Total Organic Carbon (TOC). Revised 2014. Table IB.
(lv) 5520, Oil and Grease. Revised 2021. Table IB.
(lvi) 5530, Phenols. Revised 2021. Table IB.
(lvii) 5540, Surfactants. Revised 2021. Table IB.
(lviii) 6200, Volatile Organic Compounds. Revised 2020. Table IC.
(lix) 6410, Extractable Base/Neutrals and Acids. Revised 2020. Tables IC and ID.
(lx) 6420, Phenols. Revised 2021. Table IC.
(lxi) 6440, Polynuclear Aromatic Hydrocarbons. Revised 2021. Table IC.
(lxii) 6630, Organochlorine Pesticides. Revised 2021. Table ID.
(lxiii) 6640, Acidic Herbicide Compounds. Revised 2021. Table ID.
(lxiv) 7110, Gross Alpha and Gross Beta Radioactivity (Total, Suspended, and Dissolved). 2000. Table IE.
(lxv) 7500, Radium. 2001. Table IE.
(lxvi) 9213, Recreational Waters. 2007. Table IH.
(lxvii) 9221, Multiple-Tube Fermentation Technique for Members of the Coliform Group. Approved 2014. Table IA, Notes 12, 14; and 33; Table IH, Notes 10, 12, and 32.
(lxviii) 9222, Membrane Filter Technique for Members of the Coliform Group. 2015. Table IA, Note 31; Table IH, Note 17.
(lxix) 9223 Enzyme Substrate Coliform Test. 2016. Table IA; Table IH.
(lxx) 9230 Fecal Enterococcus/Streptococcus Groups. 2013. Table IA, Note 32; Table IH.
(11) The Analyst, The Royal Society of Chemistry, RSC Publishing, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 0WF, United Kingdom. (Also available from most public libraries.)
(i) Spectrophotometric Determination of Ammonia: A Study of a Modified Berthelot Reaction Using Salicylate and Dichloroisocyanurate. Krom, M.D. 105:305-316, April 1980. Table IB, Note 60.
(ii) [Reserved]
(12) Analytical Chemistry, ACS Publications, 1155 Sixteenth St. NW., Washington DC 20036. (Also available from most public libraries.)
(i) Spectrophotometric and Kinetics Investigation of the Berthelot Reaction for the Determination of Ammonia. Patton, C.J. and S.R. Crouch. 49(3):464-469, March 1977. Table IB, Note 60.
(ii) [Reserved]
(13) AOAC International, 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.
(i) Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998.
(A) 920.203, Manganese in Water, Persulfate Method. Table IB, Note 3.
(B) 925.54, Sulfate in Water, Gravimetric Method. Table IB, Note 3.
(C) 973.40, Specific Conductance of Water. Table IB, Note 3.
(D) 973.41, pH of Water. Table IB, Note 3.
(E) 973.43, Alkalinity of Water, Titrimetric Method. Table IB, Note 3.
(F) 973.44, Biochemical Oxygen Demand (BOD) of Water, Incubation Method. Table IB, Note 3.
(G) 973.45, Oxygen (Dissolved) in Water, Titrimetric Methods. Table IB, Note 3.
(H) 973.46, Chemical Oxygen Demand (COD) of Water, Titrimetric Methods. Table IB, Note 3.
(I) 973.47, Organic Carbon in Water, Infrared Analyzer Method. Table IB, Note 3.
(J) 973.48, Nitrogen (Total) in Water, Kjeldahl Method. Table IB, Note 3.
(K) 973.49, Nitrogen (Ammonia) in Water, Colorimetric Method. Table IB, Note 3.
(L) 973.50, Nitrogen (Nitrate) in Water, Brucine Colorimetric Method. Table IB, Note 3.
(M) 973.51, Chloride in Water, Mercuric Nitrate Method. Table IB, Note 3.
(N) 973.52, Hardness of Water. Table IB, Note 3.
(O) 973.53, Potassium in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.
(P) 973.54, Sodium in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.
(Q) 973.55, Phosphorus in Water, Photometric Method. Table IB, Note 3.
(R) 973.56, Phosphorus in Water, Automated Method. Table IB, Note 3.
(S) 974.27, Cadmium, Chromium, Copper, Iron, Lead, Magnesium, Manganese, Silver, Zinc in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.
(T) 977.22, Mercury in Water, Flameless Atomic Absorption Spectrophotometric Method. Table IB, Note 3.
(U) 991.15. Total Coliforms and Escherichia coli in Water Defined Substrate Technology (Colilert) Method. Table IA, Note 10; Table IH, Note 10.
(V) 993.14, Trace Elements in Waters and Wastewaters, Inductively Coupled Plasma-Mass Spectrometric Method. Table IB, Note 3.
(W) 993.23, Dissolved Hexavalent Chromium in Drinking Water, Ground Water, and Industrial Wastewater Effluents, Ion Chromatographic Method. Table IB, Note 3.
(X) 993.30, Inorganic Anions in Water, Ion Chromatographic Method. Table IB, Note 3.
(ii) [Reserved]
(14) Applied and Environmental Microbiology, American Society for Microbiology, 1752 N Street NW., Washington DC 20036. (Also available from most public libraries.)
(i) New Medium for the Simultaneous Detection of Total Coliforms and Escherichia coli in Water. Brenner, K.P., C.C. Rankin, Y.R. Roybal, G.N. Stelma, Jr., P.V. Scarpino, and A.P. Dufour. 59:3534-3544, November 1993. Table IH, Note 21.
(ii) [Reserved]
(15) ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959; phone: (877)909-2786; website: www.astm.org.
(i) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1994. Tables IA, IB, IC, ID, IE, and IH.
(ii) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1996. Tables IA, IB, IC, ID, IE, and IH.
(iii) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1999. Tables IA, IB, IC, ID, IE, and IH.
(iv) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 2000. Tables IA, IB, IC, ID, IE, and IH.
(v) ASTM D511-14, Standard Test Methods for Calcium and Magnesium in Water. Approved October 1, 2014. Table IB.
(vi) ASTM D512-12, Standard Test Methods for Chloride Ion in Water. Approved June 15, 2012. Table IB.
(vii) ASTM D515-88, Test Methods for Phosphorus in Water, March 1989. Table IB.
(viii) ASTM D516-16, Standard Test Method for Sulfate Ion in Water. Approved June 1, 2016. Table IB.
(ix) ASTM D858-17, Standard Test Methods for Manganese in Water. Approved June 1, 2017. Table IB.
(x) ASTM D859-16, Standard Test Method for Silica in Water. Approved June 15, 2016. Table IB.
(xi) ASTM D888-18, Standard Test Methods for Dissolved Oxygen in Water. Approved May 1, 2018. Table IB.
(xii) ASTM D1067-16, Standard Test Methods for Acidity or Alkalinity of Water. Approved June 15, 2016. Table IB.
(xiii) ASTM D1068-15, Standard Test Methods for Iron in Water. Approved October 1, 2015. Table IB.
(xiv) ASTM D1125-95 (Reapproved 1999), Standard Test Methods for Electrical Conductivity and Resistivity of Water. December 1995. Table IB.
(xv) ASTM D1126-17, Standard Test Method for Hardness in Water. Approved December 1, 2017. Table IB.
(xvi) ASTM D1179-16, Standard Test Methods for Fluoride Ion in Water. Approved June 15, 2016. Table IB.
(xvii) ASTM D1246-16, Standard Test Method for Bromide Ion in Water. June 15, 2016. Table IB.
(xviii) ASTM D1252-06 (Reapproved 2012), Standard Test Methods for Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water. Approved June 15, 2012. Table IB.
(xix) ASTM D1253-14, Standard Test Method for Residual Chlorine in Water. Approved January 15, 2014. Table IB.
(xx) ASTM D1293-18, Standard Test Methods for pH of Water. Approved January 15, 2018. Table IB.
(xxi) ASTM D1426-15, Standard Test Methods for Ammonia Nitrogen in Water. Approved March 15, 2015. Table IB.
(xxii) ASTM D1687-17, Standard Test Methods for Chromium in Water. Approved June 1, 2017. Table IB.
(xxiii) ASTM D1688-17, Standard Test Methods for Copper in Water. Approved June 1, 2017. Table IB.
(xxiv) ASTM D1691-17, Standard Test Methods for Zinc in Water. Approved June 1, 2017. Table IB.
(xxv) ASTM D1783-01 (Reapproved 2012), Standard Test Methods for Phenolic Compounds in Water. Approved June 15, 2012. Table IB.
(xxvi) ASTM D1886-14, Standard Test Methods for Nickel in Water. Approved October 1, 2014. Table IB.
(xxvii) ASTM D1889-00, Standard Test Method for Turbidity of Water. October 2000. Table IB.
(xxviii) ASTM D1890-96, Standard Test Method for Beta Particle Radioactivity of Water. April 1996. Table IE.
(xxix) ASTM D1943-96, Standard Test Method for Alpha Particle Radioactivity of Water. April 1996. Table IE.
(xxx) ASTM D1976-20, Standard Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy. Approved May 1, 2020. Table IB.
(xxxi) ASTM D2036-09 (Reapproved 2015), Standard Test Methods for Cyanides in Water. Approved July 15, 2015. Table IB.
(xxxii) ASTM D2330-20, Standard Test Method for Methylene Blue Active Substances. Approved January 1, 2020. Table 1B.
(xxxiii) ASTM D2460-97, Standard Test Method for Alpha-Particle-Emitting Isotopes of Radium in Water. October 1997. Table IE.
(xxxiv) ASTM D2972-15, Standard Tests Method for Arsenic in Water. Approved February 1, 2015. Table IB.
(xxxv) ASTM D3223-17, Standard Test Method for Total Mercury in Water. Approved June 1, 2017. Table IB.
(xxxvi) ASTM D3371-95, Standard Test Method for Nitriles in Aqueous Solution by Gas-Liquid Chromatography, February 1996. Table IF.
(xxxvii) ASTM D3373-17, Standard Test Method for Vanadium in Water. Approved June 1, 2017. Table IB.
(xxxviii) ASTM D3454-97, Standard Test Method for Radium-226 in Water. February 1998. Table IE.
(xxxix) ASTM D3557-17, Standard Test Method for Cadmium in Water. Approved June 1, 2017. Table IB.
(xl) ASTM D3558-15, Standard Test Method for Cobalt in Water. Approved February 1, 2015. Table IB.
(xli) ASTM D3559-15, Standard Test Methods for Lead in Water. Approved June 1, 2015. Table IB.
(xlii) ASTM D3590-17, Standard Test Methods for Total Kjeldahl Nitrogen in Water. Approved June 1, 2017. Table IB.
(xliii) ASTM D3645-15, Standard Test Methods for Beryllium in Water. Approved February 1, 2015. Table IB.
(xliv) ASTM D3695-95, Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography. April 1995. Table IF.
(xlv) ASTM D3859-15, Standard Test Methods for Selenium in Water. Approved March 15, 2015. Table IB.
(xlvi) ASTM D3867-16, Standard Test Method for Nitrite-Nitrate in Water. Approved June 1, 2016. Table IB.
(xlvii) ASTM D4190-15, Standard Test Method for Elements in Water by Direct- Current Plasma Atomic Emission Spectroscopy. Approved February 1, 2015. Table IB.
(xlviii) ASTM D4282-15, Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion. Approved July 15, 2015. Table IB.
(xlix) ASTM D4327-17, Standard Test Method for Anions in Water by Suppressed Ion Chromatography. Approved December 1, 2017. Table IB.
(l) ASTM D4382-18, Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace. Approved February 1, 2018. Table IB.
(li) ASTM D4657-92 (Reapproved 1998), Standard Test Method for Polynuclear Aromatic Hydrocarbons in Water. January 1993. Table IC.
(lii) ASTM D4658-15, Standard Test Method for Sulfide Ion in Water. Approved March 15, 2015. Table IB.
(liii) ASTM D4763-88 (Reapproved 2001), Standard Practice for Identification of Chemicals in Water by Fluorescence Spectroscopy. September 1988. Table IF.
(liv) ASTM D4839-03 (Reapproved 2017), Standard Test Method for Total Carbon and Organic Carbon in Water by Ultraviolet, or Persulfate Oxidation, or Both, and Infrared Detection. Approved December 15, 2017. Table IB.
(lv) ASTM D5257-17, Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography. Approved December 1, 2017. Table IB.
(lvi) ASTM D5259-92, Standard Test Method for Isolation and Enumeration of Enterococci from Water by the Membrane Filter Procedure. October 1992. Table IH, Note 9.
(lvii) ASTM D5392-93, Standard Test Method for Isolation and Enumeration of Escherichia coli in Water by the Two-Step Membrane Filter Procedure. September 1993. Table IH, Note 9.
(lviii) ASTM D5673-16, Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry. Approved February 1, 2016. Table IB.
(lix) ASTM D5907-18, Standard Test Methods for Filterable Matter (Total Dissolved Solids) and Nonfilterable Matter (Total Suspended Solids) in Water. Approved May 1, 2018. Table IB.
(lx) ASTM D6503-99, Standard Test Method for Enterococci in Water Using Enterolert. April 2000. Table IA Note 9, Table IH, Note 9.
(lxi) ASTM. D6508-15, Standard Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. Approved October 1, 2015. Table IB, Note 54.
(lxii) ASTM. D6888-16, Standard Test Method for Available Cyanides with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. Approved February 1, 2016. Table IB, Note 59.
(lxiii) ASTM. D6919-17, Standard Test Method for Determination of Dissolved Alkali and Alkaline Earth Cations and Ammonium in Water and Wastewater by Ion Chromatography. Approved June 1, 2017. Table IB.
(lxiv) ASTM. D7065-17, Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tert -Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry. Approved December 15, 2017. Table IC.
(lxv) ASTM D7237-18, Standard Test Method for Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. Approved December 1, 2018. Table IB.
(lxvi) ASTM D7284-20, Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection. Approved August 1, 2020. Table IB.
(lxvii) ASTM D7365-09a (Reapproved 2015), Standard Practice for Sampling, Preservation and Mitigating Interferences in Water Samples for Analysis of Cyanide. Approved July 15, 2015. Table II, Notes 5 and 6.
(lxviii) ASTM. D7511-12 (Reapproved 2017) e1 , Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection. Approved July 1, 2017. Table IB.
(lxix) ASTM D7573-18a e1 , Standard Test Method for Total Carbon and Organic Carbon in Water by High Temperature Catalytic Combustion and Infrared Detection. Approved December 15, 2018. Table IB.
(lxx) ASTM D7781-14, Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase, Approved April 1, 2014. Table IB.
(16) Bran & Luebbe Analyzing Technologies, Inc., Elmsford NY 10523.
(i) Industrial Method Number 378-75WA, Hydrogen Ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Auto Analyzer II. October 1976. Table IB, Note 21.
(ii) [Reserved]
(17) CEM Corporation, P.O. Box 200, Matthews NC 28106-0200.
(i) Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. Table IB, Note 36.
(ii) [Reserved]
(18) Craig R. Chinchilla, 900 Jorie Blvd., Suite 35, Oak Brook IL 60523. Telephone: 630-645-0600.
(i) Nitrate by Discrete Analysis Easy (1-Reagent) Nitrate Method, (Colorimetric, Automated, 1 Reagent). Revision 1, November 12, 2011. Table IB, Note 62.
(ii) [Reserved]
(19) FIAlab Instruments, Inc., 334 2151 N. Northlake Way, Seattle, WA 98103; phone: (425)376-0450; website: www.flowinjection.com/app-notes/epafialab100.
(i) FIAlab 100, Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis, April 4, 2018. Table IB, Note 82.
(ii) [Reserved]
(20) Hach Company, P.O. Box 389, Loveland CO 80537.
(i) Method 8000, Chemical Oxygen Demand. Hach Handbook of Water Analysis. 1979. Table IB, Note 14.
(ii) Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Table IB, Note 22.
(iii) Method 8009, Zincon Method for Zinc. Hach Handbook for Water Analysis. 1979. Table IB, Note 33.
(iv) Method 8034, Periodate Oxidation Method for Manganese. Hach Handbook for Water Analysis. 1979. Table IB, Note 23.
(v) Method 8506, Bicinchoninate Method for Copper. Hach Handbook of Water Analysis. 1979. Table IB, Note 19.
(vi) Method 8507, Nitrogen, Nitrite—Low Range, Diazotization Method for Water and Wastewater. 1979. Table IB, Note 25.
(vii) Method 10206, Hach Company TNTplus 835/836 Nitrate Method 10206, Spectrophotometric Measurement of Nitrate in Water and Wastewater. Revision 2.1, January 10, 2013. Table IB, Note 75.
(viii) Method 10242, Hach Company TNTplus 880 Total Kjeldahl Nitrogen Method 10242, Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater. Revision 1.1, January 10, 2013. Table IB, Note 76.
(ix) 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. Table IB, Note 63.
(x) m-ColiBlue24® Method, for total Coliforms and E. coli. Revision 2, 1999. Table IA, Note 18; Table IH, Note 17.
(21) IDEXX Laboratories Inc., One Idexx Drive, Westbrook ME 04092.
(i) Colilert. 2013. Table IA, Notes 17 and 18; Table IH, Notes 14, 15 and 16.
(ii) Colilert-18. 2013. Table IA, Notes 17 and 18; Table IH, Notes 14, 15 and 16.
(iii) Enterolert. 2013. Table IA, Note 24; Table IH, Note 12.
(iv) Quanti-Tray Insert and Most Probable Number (MPN) Table. 2013. Table IA, Note 18; Table IH, Notes 14 and 16.
(22) In-Situ Incorporated, 221 E. Lincoln Ave., Ft. Collins CO 80524. Telephone: 970-498-1500.
(i) In-Situ Inc. Method 1002-8-2009, Dissolved Oxygen Measurement by Optical Probe. 2009. Table IB, Note 64.
(ii) In-Situ Inc. Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. Table IB, Note 10.
(iii) In-Situ Inc. Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. Table IB, Note 35.
(23) Journal of Chromatography, Elsevier/North-Holland, Inc., Journal Information Centre, 52 Vanderbilt Avenue, New York NY 10164. (Also available from most public libraries.
(i) Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography. Addison, R.F. and R.G. Ackman. 47(3): 421-426, 1970. Table IB, Note 28.
(ii) [Reserved]
(24) Lachat Instruments, 6645 W. Mill Road, Milwaukee WI 53218, Telephone: 414-358-4200.
(i) 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. Table IB, Note 56.
(ii) [Reserved]
(25) Leck Mitchell, Ph.D., P.E., 656 Independence Valley Dr., Grand Junction CO 81507. Telephone: 970-244-8661.
(i) Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 66.
(ii) Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 65.
(26) MACHEREY-NAGEL GmbH and Co., 2850 Emrick Blvd., Bethlehem, PA 18020; Phone: (888)321-6224.
(i) Method 036/038 NANOCOLOR® COD LR/HR, Spectrophotometric Measurement of Chemical Oxygen Demand in Water and Wastewater, Revision 1.5, May 2018. Table IB, Note 83.
(ii) [Reserved]
(27) Micrology Laboratories, LLC (now known as Roth Bioscience, LLC), 1303 Eisenhower Drive, Goshen, IN 46526; phone: (574)533-3351.
(i) KwikCount TM EC Medium E. coli enzyme substrate test, Rapid Detection of E. coli in Beach Water By KwikCount TM EC Membrane Filtration. 2014. Table IH, Notes 28 and 29.
(ii) [Reserved]
(28) National Council of the Paper Industry for Air and Stream Improvements, Inc. (NCASI), 260 Madison Avenue, New York NY 10016.
(i) NCASI Method TNTP-W10900, Total Nitrogen and Total Phophorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion. June 2011. Table IB, Note 77.
(ii) NCASI Technical Bulletin No. 253, An Investigation of Improved Procedures for Measurement of Mill Effluent and Receiving Water Color. December 1971. Table IB, Note 18.
(iii) NCASI Technical Bulletin No. 803, An Update of Procedures for the Measurement of Color in Pulp Mill Wastewaters. May 2000. Table IB, Note 18.
(29) The Nitrate Elimination Co., Inc. (NECi), 334 Hecla St., Lake Linden NI 49945.
(i) NECi Method N07-0003, Method for Nitrate Reductase Nitrate-Nitrogen Analysis. Revision 9.0. March 2014. Table IB, Note 73.
(ii) [Reserved]
(30) Oceanography International Corporation, 512 West Loop, P.O. Box 2980, College Station TX 77840.
(i) OIC Chemical Oxygen Demand Method. 1978. Table IB, Note 13.
(ii) [Reserved]
(31) OI Analytical, Box 9010, College Station TX 77820-9010.
(i) Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). Copyright 2010. Table IB, Note 59.
(ii) Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. Table IB, Note 39.
(iii) Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. Table IB, Note 40.
(iv) Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. Table IB, Note 41.
(32) ORION Research Corporation, 840 Memorial Drive, Cambridge, Massachusetts 02138.
(i) ORION Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Table IB, Note 16.
(ii) [Reserved]
(33) Pace Analytical Services, LLC, 1800 Elm Street, SE, Minneapolis, MN 55414; phone: (612)656-2240.
(i) 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, May 20, 2022. Table IC, Note 17.
(ii) [Reserved]
(34) SGS AXYS Analytical Services, Ltd., 2045 Mills Road, Sidney, British Columbia, Canada, V8L 5X2; phone: (888)373-0881.
(i) 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-Mass Spectrometry (GC/MS/MS)., Revision 1.0, revised August 2020. Table IC, Note 16.
(ii) [Reserved]
(35) Technicon Industrial Systems, Tarrytown NY 10591.
(i) Industrial Method Number 379-75WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Table IB, Note 7.
(ii) [Reserved]
(36) Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin MA 02038.
(i) Method AES0029. Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986, Revised 1991. Table IB, Note 34.
(ii) [Reserved]
(37) Thermo Scientific, 166 Cummings Center, Beverly MA 01915. Telephone: 1-800-225-1480. www.thermoscientific.com.
(i) Thermo Scientific Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Table IB, Note 67.
(ii) [Reserved]
(38) 3M Corporation, 3M Center Building 220-9E-10, St. Paul MN 55144-1000.
(i) Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk” Test Method 3M 0222. Revised October 28, 1994. Table IC, Note 8; Table ID, Note 8.
(ii) [Reserved]
(39) Timberline Instruments, LLC, 1880 South Flatiron Ct., Unit I, Boulder CO 80301.
(i) Timberline Amonia-001, Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis. June 24, 2011. Table IB, Note 74.
(ii) [Reserved]
(40) U.S. Geological Survey (USGS), U.S. Department of the Interior, Reston, Virginia. Available from USGS Books and Open-File Reports (OFR) Section, Federal Center, Box 25425, Denver, CO 80225; phone: (703)648-5953; website: ww.usgs.gov.
(i) Colorimetric determination of nitrate plus nitrite in water by enzymatic reduction, automated discrete analyzer methods. U.S. Geological Survey Techniques and Methods, Book 5—Laboratory Analysis, Section B—Methods of the National Water Quality Laboratory, Chapter 8. 2011. Table IB, Note 72.
(ii) Techniques and Methods—Book 5, Laboratory Analysis—Section B, Methods of the National Water Quality Laboratory—Chapter 12, Determination of Heat Purgeable and Ambient Purgeable Volatile Organic Compounds in Water by Gas Chromatography/Mass Spectrometry 2016.
(iii) Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, editors, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. Table IB, Note 8.
(iv) 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. 1989. Table IB, Notes 2 and 79.
(v) 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. Table IB, Note 24; Table ID, Note 4.
(vi) OFR 76-177, Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters. 1976. Table IE, Note 2.
(vii) OFR 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. Table ID, Note 14.
(viii) OFR 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by a Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. Table IB, Note 48.
(ix) OFR 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. Table IB, Notes 51 and 80; Table IC, Note 9.
(x) OFR 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. Table IB, Note 46.
(xi) OFR 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. Table ID, Note 9.
(xii) OFR 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. Table ID, Note 11.
(xiii) OFR 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. Table IB, Note 47.
(xiv) OFR 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. Table IC, Note 13.
(xv) OFR 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. Table IB, Notes 50 and 81.
(xvi) OFR 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. Table IB, Note 49.
(xvii) OFR 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. Table IB, Note 45.
(xviii) 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. Table IB, Note 70.
(xix) U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. Table IA, Note 4; Table IH, Note 4.
(xx) Water-Resources Investigation Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry. 2001. Table ID, Note 13.
(xxi) 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. Table IB, Note 71.
(xxii) Water-Resources Investigation 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. Table ID, Note 12.
(xxiii) 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. Table IB, Note 32.
(41) Waters Corporation, 34 Maple Street, Milford MA 01757, Telephone: 508-482-2131, Fax: 508-482-3625.
(i) Method D6508, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. Revision 2, December 2000. Table IB, Note 54.
(ii) [Reserved]
(c) Under certain circumstances, the Director may establish limitations on the discharge of a parameter for which there is no test procedure in this part or in 40 CFR parts 405 through 499. In these instances the test procedure shall be specified by the Director.
(d) Under certain circumstances, the Administrator may approve additional alternate test procedures for nationwide use, upon recommendation by the Alternate Test Procedure Program Coordinator, Washington, DC.
(e) Sample preservation procedures, container materials, and maximum allowable holding times for parameters are cited in Tables IA, IB, IC, ID, IE, IF, IG, and IH are prescribed in Table II. Information in the table takes precedence over information in specific methods or elsewhere. Any person may apply for a change from the prescribed preservation techniques, container materials, and maximum holding times applicable to samples taken from a specific discharge. Applications for such limited use changes may be made by letters to the Regional Alternative Test Procedure (ATP) Program Coordinator or the permitting authority in the Region in which the discharge will occur. Sufficient data should be provided to assure such changes in sample preservation, containers or holding times do not adversely affect the integrity of the sample. The Regional ATP Coordinator or permitting authority will review the application and then notify the applicant and the appropriate State agency of approval or rejection of the use of the alternate test procedure. A decision to approve or deny any request on deviations from the prescribed Table II requirements will be made within 90 days of receipt of the application by the Regional Administrator. An analyst may not modify any sample preservation and/or holding time requirements of an approved method unless the requirements of this section are met.
Table II—Required Containers, Preservation Techniques, and Holding Times
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 ≤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 ≤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 (HNO 3 ) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H 2 SO 4 ) 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 ≤6 °C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine.
13 Extracts may be stored up to 30 days at <0 °C.
14 For the analysis of diphenylnitrosamine, add 0.008% Na 2 S 2 O 3 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% Na 2 S 2 O 3 .
16 Place sufficient ice with the samples in the shipping container to ensure that ice is still present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 °C prior to test initiation.
17 Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48 hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669. If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be filtered in a designated clean area in the field within the time period necessary to maintain sample integrity. A sample that has been collected for determination of total or dissolved trace level mercury must be analyzed within 90 days of sample collection.
18 Aqueous samples must be preserved at ≤6 °C, and should not be frozen unless data demonstrating that sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the regulatory authority. Also, for purposes of NPDES monitoring, the specification of “≤ °C” is used in place of the “4 °C” and “<4 °C” sample temperature requirements listed in some methods. It is not necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three significant figures are specified so that rounding down to 6 °C may not be used to meet the ≤6 °C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than 15 minutes).
19 An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and holding time requirements in the approved metals methods.
20 To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6. The allowance in this footnote supersedes preservation and holding time requirements in the approved hexavalent chromium methods, unless this supersession would compromise the measurement, in which case requirements in the method must be followed.
21 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
22 Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection.
23 For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B aerobically digested, and Class B anaerobically digested.
24 The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-available form of orthophosphorus ( i.e., that which passes through a 0.45-micron filter), hence the requirement to filter the sample immediately upon collection ( i.e., within 15 minutes of collection).
§ 136.4   Application for and approval of alternate test procedures for nationwide use.
(a) A written application for review of an alternate test procedure (alternate method) for nationwide use may be made by letter via email or by hard copy in triplicate to the National Alternate Test Procedure (ATP) Program Coordinator (National Coordinator), Office of Science and Technology (4303T), Office of Water, U.S. Environmental Protection Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460. Any application for an ATP under this paragraph (a) shall:
(1) Provide the name and address of the responsible person or firm making the application.
(2) Identify the pollutant(s) or parameter(s) for which nationwide approval of an alternate test procedure is being requested.
(3) Provide a detailed description of the proposed alternate test procedure, together with references to published or other studies confirming the general applicability of the alternate test procedure for the analysis of the pollutant(s) or parameter(s) in wastewater discharges from representative and specified industrial or other categories.
(4) Provide comparability data for the performance of the proposed alternative test procedure compared to the performance of the reference method.
(b) The National Coordinator may request additional information and analyses from the applicant in order to evaluate whether the alternate test procedure satisfies the applicable requirements of this part.
(c) Approval for nationwide use. (1) After a review of the application and any additional analyses requested from the applicant, the National Coordinator will notify the applicant, in writing, of whether the National Coordinator will recommend approval or disapproval of the alternate test procedure for nationwide use in CWA programs. If the application is not recommended for approval, the National Coordinator may specify what additional information might lead to a reconsideration of the application and notify the Regional Alternate Test Procedure Coordinators of the disapproval recommendation. Based on the National Coordinator's recommended disapproval of a proposed alternate test procedure and an assessment of any current approvals for limited uses for the unapproved method, the Regional ATP Coordinator may decide to withdraw approval of the method for limited use in the Region.
(2) Where the National Coordinator has recommended approval of an applicant's request for nationwide use of an alternate test procedure, the National Coordinator will notify the applicant. The National Coordinator will also notify the Regional ATP Coordinators that they may consider approval of this alternate test procedure for limited use in their Regions based on the information and data provided in the application until the alternate test procedure is approved by publication in a final rule in the Federal Register .
(3) EPA will propose to amend this part to include the alternate test procedure in § 136.3. EPA shall make available for review all the factual bases for its proposal, including the method, any performance data submitted by the applicant and any available EPA analysis of those data.
(4) Following public comment, EPA shall publish in the Federal Register a final decision on whether to amend this part to include the alternate test procedure as an approved analytical method for nationwide use.
(5) Whenever the National Coordinator has recommended approval of an applicant's ATP request for nationwide use, any person may request an approval of the method for limited use under § 136.5 from the EPA Region.
§ 136.5   Approval of alternate test procedures for limited use.
(a) Any person may request the Regional ATP Coordinator to approve the use of an alternate test procedure in the Region.
(b) When the request for the use of an alternate test procedure concerns use in a State with an NPDES permit program approved pursuant to section 402 of the Act, the requestor shall first submit an application for limited use to the Director of the State agency having responsibility for issuance of NPDES permits within such State ( i.e., permitting authority). The Director will forward the application to the Regional ATP Coordinator with a recommendation for or against approval.
(c) Any application for approval of an alternate test procedure for limited use may be made by letter, email or by hard copy. The application shall include the following:
(1) Provide the name and address of the applicant and the applicable ID number of the existing or pending permit(s) and issuing agency for which use of the alternate test procedure is requested, and the discharge serial number.
(2) Identify the pollutant or parameter for which approval of an alternate test procedure is being requested.
(3) Provide justification for using testing procedures other than those specified in Tables IA through IH of § 136.3, or in the NPDES permit.
(4) Provide a detailed description of the proposed alternate test procedure, together with references to published studies of the applicability of the alternate test procedure to the effluents in question.
(5) Provide comparability data for the performance of the proposed alternate test procedure compared to the performance of the reference method.
(d) Approval for limited use. (1) The Regional ATP Coordinator will review the application and notify the applicant and the appropriate State agency of approval or rejection of the use of the alternate test procedure. The approval may be restricted to use only with respect to a specific discharge or facility (and its laboratory) or, at the discretion of the Regional ATP Coordinator, to all dischargers or facilities (and their associated laboratories) specified in the approval for the Region. If the application is not approved, the Regional ATP Coordinator shall specify what additional information might lead to a reconsideration of the application.
(2) The Regional ATP Coordinator will forward a copy of every approval and rejection notification to the National Alternate Test Procedure Coordinator.
§ 136.6   Method modifications and analytical requirements.
(a) Definitions of terms used in this section —(1) Analyst means the person or laboratory using a test procedure (analytical method) in this part.
(2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of interest in an environmental sample.
(3) Determinative technique means the way in which an analyte is identified and quantified (e.g., colorimetry, mass spectrometry).
(4) Equivalent performance means that the modified method produces results that meet or exceed the QC acceptance criteria of the approved method.
(5) Method-defined analyte means an analyte defined solely by the method used to determine the analyte. Such an analyte may be a physical parameter, a parameter that is not a specific chemical, or a parameter that may be comprised of a number of substances. Examples of such analytes include temperature, oil and grease, total suspended solids, total phenolics, turbidity, chemical oxygen demand, and biochemical oxygen demand.
(6) QC means “quality control.”
(b) Method modifications. (1) If the underlying chemistry and determinative technique in a modified method are essentially the same as an approved Part 136 method, then the modified method is an equivalent and acceptable alternative to the approved method provided the requirements of this section are met. However, those who develop or use a modification to an approved (Part 136) method must document that the performance of the modified method, in the matrix to which the modified method will be applied, is equivalent to the performance of the approved method. If such a demonstration cannot be made and documented, then the modified method is not an acceptable alternative to the approved method. Supporting documentation must, if applicable, include the routine initial demonstration of capability and ongoing QC including determination of precision and accuracy, detection limits, and matrix spike recoveries. Initial demonstration of capability typically includes analysis of four replicates of a mid-level standard and a method detection limit study. Ongoing quality control typically includes method blanks, mid-level laboratory control samples, and matrix spikes (QC is as specified in the method). The method is considered equivalent if the quality control requirements in the reference method are achieved. Where the laboratory is using a vendor-supplied method, it is the QC criteria in the reference method, not the vendor's method, that must be met to show equivalency. Where a sample preparation step is required ( i.e., digestion, distillation), QC tests are to be run using standards treated in the same way as the samples. The method user's Standard Operating Procedure (SOP) must clearly document the modifications made to the reference method. Examples of allowed method modifications are listed in this section. If the method user is uncertain whether a method modification is allowed, the Regional ATP Coordinator or Director should be contacted for approval prior to implementing the modification. The method user should also complete necessary performance checks to verify that acceptable performance is achieved with the method modification prior to analyses of compliance samples.
(2) Requirements. The modified method must meet or exceed performance of the approved method(s) for the analyte(s) of interest, as documented by meeting the initial and ongoing quality control requirements in the method.
(i) Requirements for establishing equivalent performance. If the approved method contains QC tests and QC acceptance criteria, the modified method must use these QC tests and the modified method must meet the QC acceptance criteria with the following conditions:
(A) The analyst may only rely on QC tests and QC acceptance criteria in a method if it includes wastewater matrix QC tests and QC acceptance criteria (e.g., matrix spikes) and both initial (start-up) and ongoing QC tests and QC acceptance criteria.
(B) If the approved method does not contain QC tests and QC acceptance criteria or if the QC tests and QC acceptance criteria in the method do not meet the requirements of this section, then the analyst must employ QC tests published in the “equivalent” of a Part 136 method that has such QC, or the essential QC requirements specified at 136.7, as applicable. If the approved method is from a compendium or VCSB and the QA/QC requirements are published in other parts of that organization's compendium rather than within the Part 136 method then that part of the organization's compendium must be used for the QC tests.
(C) In addition, the analyst must perform ongoing QC tests, including assessment of performance of the modified method on the sample matrix (e.g., analysis of a matrix spike/matrix spike duplicate pair for every twenty samples), and analysis of an ongoing precision and recovery sample (e.g., laboratory fortified blank or blank spike) and a blank with each batch of 20 or fewer samples.
(D) If the performance of the modified method in the wastewater matrix or reagent water does not meet or exceed the QC acceptance criteria, the method modification may not be used.
(ii) Requirements for documentation. The modified method must be documented in a method write-up or an addendum that describes the modification(s) to the approved method prior to the use of the method for compliance purposes. The write-up or addendum must include a reference number (e.g., method number), revision number, and revision date so that it may be referenced accurately. In addition, the organization that uses the modified method must document the results of QC tests and keep these records, along with a copy of the method write-up or addendum, for review by an auditor.
(3) Restrictions. An analyst may not modify an approved Clean Water Act analytical method for a method-defined analyte. In addition, an analyst may not modify an approved method if the modification would result in measurement of a different form or species of an analyte. Changes in method procedures are not allowed if such changes would alter the defined chemistry ( i.e., method principle) of the unmodified method. For example, phenol method 420.1 or 420.4 defines phenolics as ferric iron oxidized compounds that react with 4-aminoantipyrine (4-AAP) at pH 10 after being distilled from acid solution. Because total phenolics represents a group of compounds that all react at different efficiencies with 4-AAP, changing test conditions likely would change the behavior of these different phenolic compounds. An analyst may not modify any sample collection, preservation, or holding time requirements of an approved method. Such modifications to sample collection, preservation, and holding time requirements do not fall within the scope of the flexibility allowed at § 136.6. Method flexibility refers to modifications of the analytical procedures used for identification and measurement of the analyte only and does not apply to sample collection, preservation, or holding time procedures, which may only be modified as specified in § 136.3(e).
(4) Allowable changes. Except as noted under paragraph (b)(3) of this section, an analyst may modify an approved test procedure (analytical method) provided that the underlying reactions and principles used in the approved method remain essentially the same, and provided that the requirements of this section are met. If equal or better performance can be obtained with an alternative reagent, then it is allowed. A laboratory wishing to use these modifications must demonstrate acceptable method performance by performing and documenting all applicable initial demonstration of capability and ongoing QC tests and meeting all applicable QC acceptance criteria as described in § 136.7. Some examples of the allowed types of changes, provided the requirements of this section are met include:
(i) Changes between manual method, flow analyzer, and discrete instrumentation.
(ii) Changes in chromatographic columns or temperature programs.
(iii) Changes between automated and manual sample preparation, such as digestions, distillations, and extractions; in-line sample preparation is an acceptable form of automated sample preparation for CWA methods.
(iv) In general, ICP-MS is a sensitive and selective detector for metal analysis; however isobaric interference can cause problems for quantitative determination, as well as identification based on the isotope pattern. Interference reduction technologies, such as collision cells or reaction cells, are designed to reduce the effect of spectroscopic interferences that may bias results for the element of interest. The use of interference reduction technologies is allowed, provided the method performance specifications relevant to ICP-MS measurements are met.
(v) The use of EPA Method 200.2 or the sample preparation steps from EPA Method 1638, including the use of closed-vessel digestion, is allowed for EPA Method 200.8, provided the method performance specifications relevant to the ICP-MS are met.
(vi) Changes in pH adjustment reagents. Changes in compounds used to adjust pH are acceptable as long as they do not produce interference. For example, using a different acid to adjust pH in colorimetric methods.
(vii) Changes in buffer reagents are acceptable provided that the changes do not produce interferences.
(viii) Changes in the order of reagent addition are acceptable provided that the change does not alter the chemistry and does not produce an interference. For example, using the same reagents, but adding them in different order, or preparing them in combined or separate solutions (so they can be added separately), is allowed, provided reagent stability or method performance is equivalent or improved.
(ix) Changes in calibration range (provided that the modified range covers any relevant regulatory limit and the method performance specifications for calibration are met).
(x) Changes in calibration model. (A) Linear calibration models do not adequately fit calibration data with one or two inflection points. For example, vendor-supplied data acquisition and processing software on some instruments may provide quadratic fitting functions to handle such situations. If the calibration data for a particular analytical method routinely display quadratic character, using quadratic fitting functions may be acceptable. In such cases, the minimum number of calibrators for second order fits should be six, and in no case should concentrations be extrapolated for instrument responses that exceed that of the most concentrated calibrator. Examples of methods with nonlinear calibration functions include chloride by SM4500-Cl-E-1997, hardness by EPA Method 130.1, cyanide by ASTM D6888 or OIA1677, Kjeldahl nitrogen by PAI-DK03, and anions by EPA Method 300.0.
(B) As an alternative to using the average response factor, the quality of the calibration may be evaluated using the Relative Standard Error (RSE). The acceptance criterion for the RSE is the same as the acceptance criterion for Relative Standard Deviation (RSD), in the method. RSE is calculated as:
(C) Using the RSE as a metric has the added advantage of allowing the same numerical standard to be applied to the calibration model, regardless of the form of the model. Thus, if a method states that the RSD should be ≤20% for the traditional linear model through the origin, then the RSE acceptance limit can remain ≤20% as well. Similarly, if a method provides an RSD acceptance limit of ≤15%, then that same figure can be used as the acceptance limit for the RSE. The RSE may be used as an alternative to correlation coefficients and coefficients of determination for evaluating calibration curves for any of the methods at part 136. If the method includes a numerical criterion for the RSD, then the same numerical value is used for the RSE. Some older methods do not include any criterion for the calibration curve—for these methods, if RSE is used the value should be ≤20%. Note that the use of the RSE is included as an alternative to the use of the correlation coefficient as a measure of the suitability of a calibration curve. It is not necessary to evaluate both the RSE and the correlation coefficient.
(xi) Changes in equipment such as equipment from a vendor different from the one specified in the method.
(xii) The use of micro or midi distillation apparatus in place of macro distillation apparatus.
(xiii) The use of prepackaged reagents.
(xiv) The use of digital titrators and methods where the underlying chemistry used for the determination is similar to that used in the approved method.
(xv) Use of selected ion monitoring (SIM) mode for analytes that cannot be effectively analyzed in full-scan mode and reach the required sensitivity. False positives are more of a concern when using SIM analysis, so at a minimum, one quantitation and two qualifying ions must be monitored for each analyte (unless fewer than three ions with intensity greater than 15% of the base peak are available). The ratio of each of the two qualifying ions to the quantitation ion must be evaluated and should agree with the ratio observed in an authentic standard within ±20 percent. Analyst judgment must be applied to the evaluation of ion ratios because the ratios can be affected by co-eluting compounds present in the sample matrix. The signal-to-noise ratio of the least sensitive ion should be at least 3:1. Retention time in the sample should match within 0.05 minute of an authentic standard analyzed under identical conditions. Matrix interferences can cause minor shifts in retention time and may be evident as shifts in the retention times of the internal standards. The total scan time should be such that a minimum of eight scans are obtained per chromatographic peak.
(xvi) Changes are allowed in purge-and-trap sample volumes or operating conditions. Some examples are:
(A) Changes in purge time and purge-gas flow rate. A change in purge time and purge-gas flow rate is allowed provided that sufficient total purge volume is used to achieve the required minimum detectible concentration and calibration range for all compounds. In general, a purge rate in the range 20-200 mL/min and a total purge volume in the range 240-880 mL are recommended.
(B) Use of nitrogen or helium as a purge gas, provided that the required sensitivities for all compounds are met.
(C) Sample temperature during the purge state. Gentle heating of the sample during purging (e.g., 40 °C) increases purging efficiency of hydrophilic compounds and may improve sample-to-sample repeatability because all samples are purged under precisely the same conditions.
(D) Trap sorbent. Any trap design is acceptable, provided that the data acquired meet all QC criteria.
(E) Changes to the desorb time. Shortening the desorb time (e.g., from4 minutes to 1 minute) may not affect compound recoveries, and can shorten overall cycle time and significantly reduce the amount of water introduced to the analytical system, thus improving the precision of analysis, especially for water-soluble analytes. A desorb time of four minutes is recommended, however a shorter desorb time may be used, provided that all QC specifications in the method are met.
(F) Use of water management techniques is allowed. Water is always collected on the trap along with the analytes and is a significant interference for analytical systems (GC and GC/MS). Modern water management techniques (e.g., dry purge or condensation points) can remove moisture from the sample stream and improve analytical performance.
(xvii) If the characteristics of a wastewater matrix prevent efficient recovery of organic pollutants and prevent the method from meeting QC requirements, the analyst may attempt to resolve the issue by adding salts to the sample, provided that such salts do not react with or introduce the target pollutant into the sample (as evidenced by the analysis of method blanks, laboratory control samples, and spiked samples that also contain such salts), and that all requirements of paragraph (b)(2) of this section are met. Samples having residual chlorine or other halogen must be dechlorinated prior to the addition of such salts.
(xviii) If the characteristics of a wastewater matrix result in poor sample dispersion or reagent deposition on equipment and prevent the analyst from meeting QC requirements, the analyst may attempt to resolve the issue by adding a inert surfactant that does not affect the chemistry of the method, such as Brij-35 or sodium dodecyl sulfate (SDS), provided that such surfactant does not react with or introduce the target pollutant into the sample (as evidenced by the analysis of method blanks, laboratory control samples, and spiked samples that also contain such surfactant) and that all requirements of paragraph (b)(1) and (b)(2) of this section are met. Samples having residual chlorine or other halogen must be dechlorinated prior to the addition of such surfactant.
(xix) The use of gas diffusion (using pH change to convert the analyte to gaseous form and/or heat to separate an analyte contained in steam from the sample matrix) across a hydrophobic semi-permeable membrane to separate the analyte of interest from the sample matrix may be used in place of manual or automated distillation in methods for analysis such as ammonia, total cyanide, total Kjeldahl nitrogen, and total phenols. These procedures do not replace the digestion procedures specified in the approved methods and must be used in conjunction with those procedures.
(xx) Changes in equipment operating parameters such as the monitoring wavelength of a colorimeter or the reaction time and temperature as needed to achieve the chemical reactions defined in the unmodified CWA method. For example, molybdenum blue phosphate methods have two absorbance maxima, one at about 660 nm and another at about 880 nm. The former is about 2.5 times less sensitive than the latter. Wavelength choice provides a cost-effective, dilution-free means to increase sensitivity of molybdenum blue phosphate methods.
(xxi) Interchange of oxidants, such as the use of titanium oxide in UV-assisted automated digestion of TOC and total phosphorus, as long as complete oxidation can be demonstrated.
(xxii) Use of an axially viewed torch with Method 200.7.
(xxiii) When analyzing metals by inductively coupled plasma-atomic emission spectroscopy, inductively coupled plasma-mass spectrometry, and stabilized temperature graphite furnace atomic absorption, closed-vessel microwave digestion of wastewater samples is allowed as alternative heating source for Method 200.2—“Sample Preparation Procedure for Spectrochemical Determination of Total Recoverable Elements” for the following elements: Aluminum, antimony, arsenic, barium, beryllium, boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, potassium, selenium, silver, sodium, thallium, tin, titanium, vanadium, zinc, provided the performance specifications in the relevant determinative method are met. (Note that this list does not include Mercury.) Each laboratory determining total recoverable metals is required to operate a formal quality control (QC) program. The minimum requirements include initial demonstration of capability, method detection limit (MDL), analysis of reagent blanks, fortified blanks, matrix spike samples, and blind proficiency testing samples, as continuing quality control checks on performance. The laboratory is required to maintain performance records on file that define the quality of the data generated.
(c) The permittee must notify their permitting authority of the intent to use a modified method. Such notification should be of the form “Method xxx has been modified within the flexibility allowed in 40 CFR 136.6.” The permittee may indicate the specific paragraph of § 136.6 allowing the method modification. Specific details of the modification need not be provided, but must be documented in the Standard Operating Procedure (SOP) and maintained by the analytical laboratory that performs the analysis.
§ 136.7   Quality assurance and quality control.
The permittee/laboratory shall use suitable QA/QC procedures when conducting compliance analyses with any part 136 chemical method or an alternative method specified by the permitting authority. These QA/QC procedures are generally included in the analytical method or may be part of the methods compendium for approved Part 136 methods from a consensus organization. For example, Standard Methods contains QA/QC procedures in the Part 1000 section of the Standard Methods Compendium. The permittee/laboratory shall follow these QA/QC procedures, as described in the method or methods compendium. If the method lacks QA/QC procedures, the permittee/laboratory has the following options to comply with the QA/QC requirements:
(a) Refer to and follow the QA/QC published in the “equivalent” EPA method for that parameter that has such QA/QC procedures;
(b) Refer to the appropriate QA/QC section(s) of an approved part 136 method from a consensus organization compendium;
(c)(1) Incorporate the following twelve quality control elements, where applicable, into the laboratory's documented standard operating procedure (SOP) for performing compliance analyses when using an approved part 136 method when the method lacks such QA/QC procedures. One or more of the twelve QC elements may not apply to a given method and may be omitted if a written rationale is provided indicating why the element(s) is/are inappropriate for a specific method.
(i) Demonstration of Capability (DOC);
(ii) Method Detection Limit (MDL);
(iii) Laboratory reagent blank (LRB), also referred to as method blank (MB);
(iv) Laboratory fortified blank (LFB), also referred to as a spiked blank, or laboratory control sample (LCS);
(v) Matrix spike (MS) and matrix spike duplicate (MSD), or laboratory fortified matrix (LFM) and LFM duplicate, may be used for suspected matrix interference problems to assess precision;
(vi) Internal standards (for GC/MS analyses), surrogate standards (for organic analysis) or tracers (for radiochemistry);
(vii) Calibration (initial and continuing), also referred to as initial calibration verification (ICV) and continuing calibration verification (CCV);
(viii) Control charts (or other trend analyses of quality control results);
(ix) Corrective action (root cause analysis);
(x) QC acceptance criteria;
(xi) Definitions of preparation and analytical batches that may drive QC frequencies; and
(xii) Minimum frequency for conducting all QC elements.
(2) These twelve quality control elements must be clearly documented in the written standard operating procedure for each analytical method not containing QA/QC procedures, where applicable.