Clean Water Act Methods Update Rule for the Analysis of Effluent, 27226-27260 [2021-09596]

Download as PDF 27226 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations ENVIRONMENTAL PROTECTION AGENCY 40 CFR Part 136 [EPA–HQ–OW–2018–0826; FRL–10021–59– OW] RIN 2040–AF84 Clean Water Act Methods Update Rule for the Analysis of Effluent Environmental Protection Agency (EPA). ACTION: Final rule. AGENCY: The Environmental Protection Agency (EPA) is finalizing changes to its test procedures required to be used by industries and municipalities when analyzing the chemical, physical, and biological properties of wastewater and other environmental samples for reporting under EPA’s National Pollutant Discharge Elimination System (NPDES) permit program. The Clean Water Act (CWA) requires EPA to SUMMARY: materials are available electronically through https://www.regulations.gov. FOR FURTHER INFORMATION CONTACT: Meghan Hessenauer, Engineering and Analysis Division (4303T), Office of Water, Environmental Protection Agency, 1200 Pennsylvania Avenue NW, Washington, DC 20460–0001; telephone: 202–566–1040; email: Hessenauer.Meghan@epa.gov. SUPPLEMENTARY INFORMATION: Table of Contents I. General Information II. Overview III. Changes Between the Proposed Rule and the Final Rule IV. Statutory Authority V. Purpose and Summary of Final Rule VI. Statutory and Executive Order Reviews I. General Information A. Does this action apply to me? Entities potentially affected by the requirements of this action include: Category Examples of potentially affected entities State, Territorial, and Indian Tribal Governments. States, territories, and tribes authorized to administer the National Pollutant Discharge Elimination System (NPDES) permitting program; states, territories, and tribes providing certification under CWA section 401; state, territorial, and tribal-owned facilities that must conduct monitoring to comply with NPDES permits. Facilities that must conduct monitoring to comply with NPDES permits. Publicly Owned Treatment Works (POTWs) or other municipality-owned facilities that must conduct monitoring to comply with NPDES permits. Industry ........................................... Municipalities ................................... This table is not exhaustive, but rather provides a guide for readers regarding entities likely to be affected by this action. This table lists types of entities that EPA is now aware of that could potentially be affected by this action. Other types of entities not listed in the table could also be affected. To determine whether your facility is affected by this action, you should carefully examine the applicability language at 40 CFR 122.1 (NPDES purpose and scope), 40 CFR 136.1 (NPDES permits and CWA) and 40 CFR 403.1 (pretreatment standards purpose and applicability). If you have questions regarding the applicability of this action to a particular entity, consult the appropriate person listed in the preceding FOR FURTHER INFORMATION CONTACT section. khammond on DSKJM1Z7X2PROD with RULES2 promulgate these test procedures (analytical methods) for analysis of pollutants. EPA anticipates that these changes will provide increased flexibility for the regulated community in meeting monitoring requirements while improving data quality. In addition, this update to the CWA methods is incorporating technological advances in analytical technology. DATES: This final rule is effective July 19, 2021. ADDRESSES: EPA has established a docket for this action under Docket ID No. EPA–HQ–OW–2018–0826. All documents in the docket are listed on the https://www.regulations.gov website. Although listed in the index, some information is not publicly available, e.g., confidential business information or other information whose disclosure is restricted by statute. Certain other material, such as copyrighted material, is not placed on the internet and will be publicly available only in hard copy form. Publicly available docket II. Overview This preamble describes the reasons for the final rule; the legal authority for the final rule; a summary of the changes and clarifications; and explanation of the abbreviations and acronyms used in this document. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 Abbreviations and Acronyms Used in the Preamble and Rule Text 2-CEVE: 2-Chloroethylvinyl ether AA: Atomic Absorption ADMI: American Dye Manufacturers Institute ASTM: ASTM International 1 ATP: Alternate Test Procedure BHI: Brain heart infusion BOD5: 5-day Biochemical Oxygen Demand CAS: Chemical Abstract Services CATC: Cyanide Amenable to Chlorination CBOD—Carbonaceous Biochemical Oxygen Demand CCB: Continuing calibration blank CCV: Continuing calibration verification CFR: Code of Federal Regulations COD: Chemical Oxygen Demand CWA: Clean Water Act EC-MUG: EC broth with 4methylumbelliferyl-b-D-glucuronide EDTA: Ethylenediaminetetraacetic acid ELAB: Environmental Laboratory Advisory Board EPA: Environmental Protection Agency FLAA: Flame Atomic Absorption Spectroscopy GC: Gas Chromatography GFAA: Graphite Furnace Atomic Absorption Spectroscopy ICP/AES: Inductively Coupled PlasmaAtomic Emission Spectroscopy 1 Formerly known as the American Society for Testing and Materials (ASTM) PO 00000 Frm 00002 Fmt 4701 Sfmt 4700 ICP/MS: Inductively Coupled Plasma-Mass Spectrometry ILI: Independent Laboratories Institute IPR: Initial Precision and Recovery LCS: Laboratory Control Sample MDL: Method Detection Limit MF: Membrane Filtration MgCl2: Magnesium Chloride MPN: Most Probable Number MS/MSD: Matrix Spike/Matrix Spike Duplicate MS: Mass Spectrometry NA-MUG: Nutrient Agar with 4methylumbelliferyl-b-D-glucuronide NECi: A shortened name used by the Nitrate Elimination Company, Inc. NPDES: National Pollutant Discharge Elimination System NTTAA: National Technology Transfer and Advancement Act OPR: Ongoing Precision and Recovery QC: Quality Control STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption SW: Solid Waste TKN: Total Kjeldahl Nitrogen TOC: Total Organic Carbon USGS: United States Geological Survey VCSB: Voluntary Consensus Standards Body III. Changes Between the Proposed Rule and the Final Rule EPA received 25 comments on the October 2019 proposed rule from E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations khammond on DSKJM1Z7X2PROD with RULES2 laboratory associations, commercial labs, state environmental agencies, and various trade associations. None of the comments opposed the promulgation of the proposed methods. Below is a breakout summarizing the comments we received. • All commenters support finalizing this rule. • 12 of the comment letters were outside the scope for the proposed rulemaking or requested a method modification with no underlying data to support the requested change. • Some commenters requested that EPA modify methods developed by external stakeholders (ASTM International, USGS, etc.). However, EPA is only adopting methods as developed by voluntary consensus standard bodies. Comments requesting changes to such methods should be directed to the method developers. • Some commenters noted typographical errors or minor inconsistencies within 40 CFR part 136 that required minor changes (e.g., the wrong citation date in a footnote, methods listed in the wrong section of the 40 CFR part 136). Except as noted below, the content of the final rule is the same as that of the proposed rule. A. Changes in Preamble In the proposed rulemaking, EPA included in Table IA Standard Methods Method 9230D–2013 for the measurement of enterococci but did not include a discussion of this method in the preamble to the proposal. In response to comments, EPA has added a description of the method to Section IV.C of this preamble. Similarly, while the proposal included in Table IB Standard Methods Method 5210B–2016 for the measurement of carbonaceous biochemical oxygen demand (CBOD5), EPA did not discuss approving this method in the preamble to the proposal. The preamble did, however, discuss approval of this method for biochemical oxygen demand (BOD5) and included BOD in Table IB and along with CBOD. In response to comments, EPA has included discussion and the description of the method in Section V.C of this preamble for both BOD and CBOD. In addition, EPA has corrected a typographical error that appeared in the proposed rulemaking regarding Standard Methods Method 2540E–2015 in Section IV.C of this preamble. The correct method, Standard Methods Method 2540F–2015, is now listed in Section IV.C of this preamble. The errata sheets for Whole Effluent Toxicity were not referenced in 40 CFR part 136. In the previous 2017 Methods VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 Update Rule, the errata sheets were approved but not referenced. EPA did not add this to the regulatory test and was a mistake. The errata sheets are now referenced. B. Changes to Table IB EPA has corrected two errors in Table IB of the final rule. In the proposal, EPA listed ASTM Method D1179–16(A) in the wrong row in the Table IB entry for Fluoride. The method is a distillation step and was erroneously listed in the row for colorimetric methods. EPA has corrected Table IB in the final rule. EPA also has corrected the publication date of the Macherey-Nagel Chemical Oxygen Demand method in Footnote 83 to Table IB. In the proposal, the publication date in the footnote was listed as 2008 and has been corrected to 2018. C. Changes to Table II EPA is making a number of conforming changes to the final rule in order to correct inadvertent omissions and errors. In response to a comment that pointed out that EPA did not update Table II to capture the microbiological method changes included in Tables IA and IH, EPA has modified Table II to take account of these changes for the final rule. These changes intended to clarify and correct inadvertent omissions and errors. A commenter pointed out that EPA did not include organic parameter #73, hexachloroethane in Table II. EPA has corrected this error that dates to the Methods Update Rule proposed in 2004. The parameter #73 has been added to the list of chlorinated hydrocarbons in Table II of the final rule. Finally, a typographical error in Table II of the proposed rulemaking resulted in the specifications for four matrices listed under the dioxin and furan (CDDs/CDFs) entry to not be indented. This caused some confusion for commenters. EPA has ensured that Table II in the final rule appears as intended. IV. Statutory Authority EPA is promulgating this regulation under the authorities of sections 301(a), 304(h), and 501(a) of the CWA; 33 U.S.C. 1311(a), 1314(h), and 1361(a). Section 301(a) of the CWA prohibits the discharge of any pollutant into navigable waters unless the discharge complies with, among other provisions, an NPDES permit issued under section 402 of the CWA. Section 304(h) of the CWA requires the Administrator of EPA to ‘‘. . . promulgate guidelines establishing test procedures for the PO 00000 Frm 00003 Fmt 4701 Sfmt 4700 27227 analysis of pollutants that shall include the factors which must be provided in any certification pursuant to [section 401 of the CWA] or permit application pursuant to [section 402 of the CWA].’’ Section 501(a) of the CWA authorizes the Administrator to ‘‘. . . prescribe such regulations as are necessary to carry out this function under [the CWA].’’ EPA generally has codified its test procedure regulations (including analysis and sampling requirements) for CWA programs at 40 CFR part 136, though some requirements are codified in other parts (e.g., 40 CFR chapter I, subchapters N and O). V. Purpose and Summary of Final Rule NPDES permits must include conditions designed to ensure compliance with the technology-based and water quality-based requirements of the CWA, including in many cases, restrictions on the quantity of specific pollutants that can be discharged as well as requirements for pollutant monitoring, measurement and reporting to NPDES authorities. Often, entities have a choice in deciding which approved test procedure they will use for a specific pollutant because EPA has approved the use of more than one method.2 The procedures for the analysis of pollutants required by CWA section 304(h) are a central element of the NPDES permit program. Examples of where these EPA-approved analytical methods must be used include the following: (1) Applications for NPDES permits, (2) sampling or other reports required under NPDES permits, (3) other requests for quantitative or qualitative effluent data under the NPDES regulations, (4) State CWA 401 certifications and (5) sampling and analysis required under EPA’s General Pretreatment Regulations for Existing and New Sources of Pollution, 40 CFR 136.1 and 40 CFR 403.12(b)(5)(v). Periodically, EPA updates the approved methods in 40 CFR part 136. In general, the changes in this final action fall into the following categories. The first is new or revised methods published by the VCSBs or the USGS that are similar to methods previously adopted as EPA-approved methods in 40 CFR part 136. The second category is methods EPA has reviewed under the Agency’s national ATP program and preliminarily concluded are appropriate for nationwide use. Lastly, EPA is finalizing certain corrections or amendments to the text and tables of 40 2 NPDES permit regulations also specify that the approved method needs to be sufficiently sensitive. See 40 CFR 122.21 (e)(3). E:\FR\FM\19MYR2.SGM 19MYR2 27228 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations CFR part 136. EPA is adopting these revisions to improve data quality, update methods to keep current with technology advances, and provide the regulated community with greater flexibility. The following paragraphs provide details on the finalized revisions. A. Changes to 40 CFR 136.3 To Include New Versions of Previously Approved EPA Methods EPA added the revised version of EPA Method 1623 (labeled 1623.1) to Table IH. Method 1623.1 includes updated acceptance criteria for IPR, OPR, and MS/MSD, and clarifications and revisions based on user questions and feedback about Method 1623 over the past 19 years. khammond on DSKJM1Z7X2PROD with RULES2 B. Methods Incorporated by Reference Currently, hundreds of methods and ATPs are incorporated by reference within 40 CFR part 136. In most cases, 40 CFR part 136 contains multiple approved methods for a single pollutant, and regulated entities often have a choice in selecting a method. This final rule contains revisions to VCSB methods that are currently incorporated by reference. Two VCSBs have made such revisions, Standard Methods and ASTM. The finalized VCSB methods are consistent with the requirements of the National Technology Transfer and Advancement Act (NTTAA), under which federal agencies use technical standards developed or adopted by the VCSBs if compliance would not be inconsistent with applicable law or otherwise impracticable (see Section V.I of this preamble). The VCSB methods are available on their respective websites (https://www.standard methods.org/ and www.astm.org) to everyone at a cost determined by the VCSB, generally from $40 to $80. Both organizations also offer memberships or subscriptions that allow unlimited access to their methods. The cost of obtaining these methods is not a significant financial burden for a discharger or environmental laboratory, making the methods reasonably available. Finally, this final rule also includes USGS methods and vendor ATPs, all of which EPA is incorporating by reference. The ATPs and USGS methods are available free of charge on their respective websites (flowinjection.com, mn-net.com, micrologylabs.com and USGS.gov), enabling EPA to conclude that the USGS methods and ATPs incorporated by reference are reasonably available. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 C. Changes to 40 CFR 136.3 To Include New Versions of Approved Standard Methods Methods EPA is approving new versions of Standard Methods methods previously included in 40 CFR part 136. The newer versions clarify the existing methods or make editorial corrections. As was the case with the previous methods update rule (82 FR 40836–40941, August 28, 2017), EPA approves and includes in 40 CFR part 136 only the most recent version of a method published by the Standard Methods Committee. EPA is listing only one version of the method with the year of publication designated by the last four digits in the method number (e.g., SM method 3111 B–2011). The date indicates the date of the specific revision to the method. This allows use of a specific method in any edition of the hard copy publication of Standard Methods for the Examination of Water & Wastewater that includes a method with the same method number and year of publication. The finalized revisions to Standard Methods methods previously approved in 40 CFR part 136 will not affect the performance of the method. The following identifies new versions of previously approved Standard Methods methods that EPA included. Each entry contains the Standard Methods number and date, the parameter, and a brief description of the analytical method. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear. EPA finalized the following changes to Tables IA and IH at 40 CFR part 136: 1. Standard Methods Method 9221 (B, E, F)-2014: Method 9221B–2014 Coliform (total); analyzes for total coliforms in non-potable waters using LTB, all presumptive growth LTB tubes are confirmed in BGLB. Method 9221E– 2014 Coliform (fecal); analyzes all presumptive growth LTB tubes for fecal coliform using EC broth. Method 9221F–2014 E. coli; analyzes all presumptive growth LTB tubes for E. coli using EC–MUG. The number of positive tubes (BGLB, EC broth or EC– MUG) is used to determine the MPN. In response to public comment, EPA is clarifying that Method 9221E–2014 is approved for testing sewage sludge. In Table IA.1, EPA changed Footnote 11 from ‘approved’ to ‘recommended’ in the proposed rulemaking because the 2017 Methods Update Rule erroneously changed the footnote from ‘recommended’ to ‘approved.’ EPA is correcting this error and changing the footnote back to ‘‘recommended’’. EPA has approved all biosolid methods listed in Table 1A.1 for parameter #1, PO 00000 Frm 00004 Fmt 4701 Sfmt 4700 including those listed in Footnote 11. More method validation data is available for EPA Methods 1680 and 1681 than Standard Method 9221. EPA methods are recommended over 9221 and 9222, although all four methods are approved for biosolids. 2. Standard Methods Method 9222 (B, D, I)-2015: Method 9222B–2015 Coliform (total); analyzes for total coliforms in non-potable waters by filtration through a 0.45-mm membrane filter and plated on mEndo or LES Endo agar. Method 9222D–2015 Coliform (fecal); analyzes for fecal coliforms in non-potable waters by filtration through a 0.45-mm membrane filter plated on mFC medium. Method 9222 I–2015 E. coli; membrane filtration (MF), analyzes presumptive positive filters from Method 9222B and 9222D using nutrient agar plates with MUG (NA– MUG) which are examined under a longwave UV lamp. 3. Standard Methods Method 9223B– 2016, E. coli, multiple tube/multiple well: This method analyzes non-potable waters for E. coli using commercially available enzyme substrate media that is mixed with the sample and placed in multiple tubes or multiple well trays, incubated and examined under ambient light for Coliform (total) and under a longwave UV lamp for E. coli. 4. Standard Methods Method 9230 (B,C)-2013: Method 9230B–2013 (Fecal Streptococci) analyzes non-potable waters for streptococci using azide dextrose broth (ADB) Presumptive positive ADB tubes are confirmed by streaking onto bile esculin azide agar (BEA). Method 9230C–2013 Enterococci; analyzes non-potable waters by filtration through a 0.45-mm membrane filter and plated on mE agar. 5. Standard Methods Method 9230D– 2013, Enterococci: This method analyzes non-potable waters using a hydrolyzable substrate (4methylumbelliferyl-+-D-glucoside) to detect enterococci in a multiple-tube or a multi-well format. EPA is promulgating the following changes to Table IB at 40 CFR part 136: 1. Standard Methods Method 2540 series. a. Method 2540B–2015, total solids. A sample aliquot is evaporated in a preweighed evaporating dish at 103–105 °C. Method 2540C–2015 filterable residue (total dissolved solids). The sample aliquot is then filtered through a glass fiber filter, and the filtrate is evaporated on a pre-weighed dish to constant weight at 180 °C. b. Method 2540D–2015 non-filterable residue (total suspended solids). A sample aliquot is filtered through a pre- E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations weighed glass fiber filter which is then dried to constant weight at 103–105 °C. c. Method 2540E–2015 volatile residue (fixed and volatile solids). The residue obtained from the determination of total (Method 2540B), filterable (Method 2540C) or non-filterable residue (Method 2540D) is ignited at 550 °C in a muffle furnace. d. Method 2540F–2015 settleable residue (settleable solids). Settleable matter is measured with an Imhoff cone either volumetrically or gravimetrically. 2. Standard Methods Method 4500– CN¥ (B–G)–2016, cyanide. Cyanides are measured after preliminary treatment of samples to remove interferences (4500– CN¥ B). Manual distillation with magnesium chloride (MgCl2) (4500– CN¥ C) is followed by: Titration with silver nitrate (4500–CN¥ D). Spectrophotometric measurement after cyanide in the alkaline distillate is converted to Cyanogen Chloride (4500– CN¥ E). Potentiometric measurement using an ion selective electrode (4500– CN¥ F). Cyanide amenable to chlorination (CATC) in which a portion of the sample is chlorinated at high pH and cyanide levels in the chlorinated sample are determined after manual distillation followed by titrimetric or spectrophotometric measurement. Amenable cyanide is calculated by the difference between the results for cyanide in the unchlorinated sample and the results for the chlorinated sample (4500–CN¥ G). 3. Standard Methods Method 4500– NO3¥ D–2016. Nitrate (as nitrogen), measured using an ion-selective electrode that develops a potential across a thin, inert membrane holding in place a water-immiscible liquid ion exchanger. 4. Standard Methods Method 4500– NO3¥ (E, F, and H)–2016. Nitrate-nitrite (as nitrogen). Nitrate is reduced to nitrite using a cadmium-copper column, followed by diazotization to form a colored azo dye, which is measured by colorimetry either manually (4500– NO3¥ E) or automated (4500–NO3¥ F); or by reduction of nitrate to nitrite using hydrazine followed by automated colorimetric measurement of nitrite after diazotization (4500–NO3¥ H). 5. Standard Methods Method 4500– NO3¥ (E and F)–2016. Nitrite (as nitrogen). Colorimetric: bypasses the cadmium reduction step and measures nitrite after diazotization either by manual or automated colorimetric analysis. 6. Standard Methods Method 4500–O (B¥F, and G)–2016. Measurement of oxygen (dissolved), using the Winkler iodometric titration procedure with modifications to eliminate or minimize VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 certain interferences if necessary, based on sample type (4500–O B through F), or by use of polarographic or galvanic membrane electrodes (4500–O G). 7. Standard Methods Method 5210 B– 2016., Biochemical oxygen demand (BOD5) and carbonaceous biochemical oxygen demand (CBOD5), dissolved oxygen depletion: The BOD5 test is an indirect measurement of organic matter. It measures the change in dissolved oxygen (DO) concentration caused by microorganisms as they degrade organic matter in a sample held in a stoppered bottle incubated for 5 days in the dark at 20 °C. Nitrification inhibition is recommended for secondary-effluent samples, samples seeded with secondary effluent, and polluted water because nitrogenous compounds can oxidize in such samples. When a nitrification inhibitor is added as directed in 5210B.5e, results are reported as CBOD5. 8. Standard Methods Method 5310 (B, C)–2014. Total organic carbon (TOC), combustion, heated persulfate or UV persulfate oxidation. In method 5310 B– 2014 Combustion, a sample aliquot is combusted, transported in a carrier gas stream and measured via a nondispersive infrared analyzer, or titrated coulometrically. In method 5310C–2014 Persulfate, UV, or heatedpersulfate oxidation method, persulfate oxidizes organic carbon. The produced CO2 is then purged and measured by either nondispersive infrared (NDIR) analyzer, coulometrically titrated, or separated from the liquid stream by a membrane that specifically allows CO2 to pass into high-purity water where the change in the high-purity water’s conductivity corresponds to the amount of CO2 passing the membrane. Lastly, EPA is promulgating one revision to a previously approved Standard Methods method for which the Standard Methods Committee has adopted updates. This modification includes minor changes to method procedures that do not affect the performance of the method. EPA is promulgating the following change to Table IA and Table IH at 40 CFR part 136: Standard Methods Method 9221F– 2014 is an acceptable method for detecting fecal coliforms and E. coli simultaneously. This method analyzes Coliform (fecal) and E. coli using EC broth with 4-methylumbelliferyl-b-Dglucuronide (EC–MUG) with inverted vials and is an MPN method PO 00000 Frm 00005 Fmt 4701 Sfmt 4700 27229 D. Changes to 40 CFR 136.3 To Include New Standard Methods Methods Based on Previously Approved Technologies EPA is promulgating changes based on the National Technology Transfer and Advancement Act of 1995 (NTTAA), Public Law 104–113. This provides that federal agencies and departments must use technical standards developed or adopted by the VCSBs if the use of these standards would not be inconsistent with applicable law or otherwise impracticable. These methods submitted by the Standards Methods Committee are consistent with other methods already approved at 40 CFR part 136. EPA is adding Standard Methods Method 4500–CN¥ N–2016 to Table IB for Cyanide, total. Cyanide is measured after preliminary treatment of samples and manual distillation with magnesium chloride (MgCl2) followed by automated spectrophotometric measurement after conversion to Cyanogen Chloride. This method is similar to the currently approved EPA Method 335.4, USGS Method I–4302– 85, and Lachat Method 10–204–00–1–X, and uses semi-automated spectrophotometric measurement of cyanide. 2. EPA is adding Standard Methods Method 4500–NO3¥ I–2016 to Table IB for combined nitrate-nitrite, nitrite and nitrate by subtraction. Nitrate is reduced to nitrite using a cadmium-copper column followed by diazotization to form an azo dye which is measured by colorimetry. The cadmium reduction column may be by-passed for measurement of nitrite only. The value obtained for nitrite may be subtracted from the value obtained for combined nitrate-nitrite to calculate the concentration of nitrate. This method is similar to the currently approved EPA Method 353.2, Standard Methods Method 4500–NO3¥ F–2011, ASTM Method D3867–04 (A), and USGS Method I–2545–90, and uses automated cadmium reduction and spectrophotometric measurement of nitrite. 3. EPA is adding Standard Methods Method 4500–NO3¥ J–2018 to Table IB for measurement of combined nitratenitrite, nitrite, and for measurement of nitrate by subtraction. Nitrate is reduced to nitrite by an enzymatic reaction. The nitrite is diazotized to yield an azo dye which is measured colorimetrically. The enzyme reduction step may be bypassed for measurement of nitrite singly. The value obtained for nitrite may be subtracted from the value obtained for combined nitrate-nitrite to calculate the concentration of nitrate. E:\FR\FM\19MYR2.SGM 19MYR2 27230 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations This method is similar to the currently approved NECi Method N07–0003, USGS Method I–2547–11, and USGS Method I–2548–11. 4. EPA is adding Standard Methods Method 4500–O H–2016 to Table IB for dissolved oxygen. This method uses a luminescent-based sensor for measurement of dissolved oxygen. The method is similar to the currently approved Hach Method 10360, In-Situ Method 1002–8–2009, and ASTM Method D888–09 (C). khammond on DSKJM1Z7X2PROD with RULES2 E. Changes to 40 CFR 136.3 To Include New Versions of Approved ASTM Methods EPA is approving new versions of ASTM methods previously approved in 40 CFR part 136 for the reasons outlined in the first paragraph of Section IV.C of this preamble. These changes to currently approved ASTM methods in 40 CFR part 136 include minor clarifications and editorial changes, and in some instances, minor changes to method procedures. None of these changes will affect the performance of the method. The following describes the changes to current ASTM methods that EPA is adding to 40 CFR part 136. Each entry contains (in the following order): The ASTM method number (the last two digits in the method number represent the year ASTM published), the parameter, a brief description of the analytical technique, and a brief description of any procedural changes in this revision from the last approved version of the method. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear. EPA is promulgating the following changes to Table IB at 40 CFR part 136: 1. ASTM Method D511–14 (A, B), calcium and magnesium, titrimetric, (EDTA), AA direct aspiration. Method D511–14 A, titrimetric. The pH of the sample is adjusted to 10 (for calcium), then to 12–13 (for magnesium) and titrated with ethylenediamine tetraacetic acid (EDTA) to form complexes with calcium and magnesium ions which react with an indicator to form a colored product. The volume of titrant used to affect the color change is proportional to the concentrations of calcium and magnesium in the sample. Method D511–14 B, AA direct aspiration. The sample is acidified and analyzed by atomic absorption. The concentrations of calcium and magnesium in the samples are proportional to the amount of light absorbed during the analysis and are determined in comparison to a standard curve. This version EPA is VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 adding includes specifications for filter paper. 2. ASTM Method D512–12 chloride ion (A, B), titrimetric (mercuric nitrate), titration (silver nitrate). Method D512– 12A, titrimetric mercuric nitrate. The sample is acidified and titrated with mercuric nitrate in the presence of a diphenylcarbazonebromophenol blue indicator. Method D512–12B, titrimetric silver nitrate. Sample pH is adjusted to phenolphthalein endpoint and titrated with silver nitrate in the presence of potassium chromate. The volume of titrant used to affect the color change in either method is proportional to the concentration of chloride in the sample. This version corrects one term in the chloride calculation. 3. ASTM Method D516–16, sulfate ion, turbidimetric. In this method, sulfate ions are converted to barium sulfate to form a suspension. The turbidity of the suspension is measured with a nephelometer, spectrophotometer, or photoelectric colorimeter, and compared to a standard curve to determine the sulfate concentration in the sample. This version adds specifications for filter paper. 4. ASTM Method D858–17 (A–C), manganese, atomic absorption (AA) direct aspiration, AA furnace. The sample is acid digested and analyzed by direct aspiration atomic absorption or graphite furnace atomic absorption. The concentration of manganese in the sample is proportional to the amount of light absorbed and is determined in comparison to a standard curve. There are no procedural changes. 5. ASTM Method D859–16, silica, colorimetric, manual. In this method, soluble silica in the sample is reacted with molybdate then reduced to form a blue complex in solution. The intensity of the blue complex is determined with a spectrophotometer or filter photometer and the concentration of silica is determined by comparison with a standard curve. There are no procedural changes. 6. ASTM Method D888–12 (A–C) dissolved oxygen, Winkler, electrode, luminescent-based sensor. Method D888–12A measures dissolved oxygen using the Winkler iodometric titration procedure. The volume of titrant used is proportional to the concentration of dissolved oxygen in the sample. Method D888–12B measures dissolved oxygen in the sample with an electrochemical probe that produces an electrical potential which is logarithmically proportional to the concentration of dissolved oxygen in the sample. Method D888–12C measures dissolved oxygen with a luminescence-based sensor probe PO 00000 Frm 00006 Fmt 4701 Sfmt 4700 that employs frequency domain lifetime-based luminescence quenching and signal processing. This version adds information on a two-point calibration and updated performance information from an interlaboratory study to D888– 12C. 7. ASTM Method D1067–16, acidity or alkalinity, electrometric endpoint or phenolphthalein endpoint; electrometric or colorimetric titration to pH 4.5, manual. The acidity or alkalinity of the sample is determined by titration to a specific pH endpoint which is determined by colorimetry or with a pH electrode. The acidity or alkalinity is proportional to the volume of titrant required to affect the pH change. There are no procedural changes. 8. ASTM Method D1068–15 (A–C), iron, AA direct aspiration; AA furnace; colorimetric (Phenanthroline): The sample is acid digested and analyzed by either direct aspiration atomic absorption, graphite furnace atomic absorption, or colorimetry. The concentration of iron in the sample is proportional to the amount of light absorbed and is determined in comparison to a standard curve. The version as promulgated includes specifications for filter paper. 9. ASTM Method D1126–17, hardness, titrimetric (EDTA). The pH of the sample is adjusted, and an indicator is added forming a red color. The mixture is titrated until the color changes from red to blue. The volume of titrant used to affect the color change is proportional to the hardness in the sample. There are no procedural changes. 10. ASTM Method D1179–16 (A, B); fluoride ion, manual distillation, electrode, manual. Method D1179A, manual distillation. The sample is distilled as hydrofluorosilic acid and determined by ion-selective electrode. Method D1179B, electrode. The fluoride ion is determined potentiometrically with an ion-selective electrode in conjunction without sample distillation. There are no procedural changes. 11. ASTM Method D1246–16, bromide ion, electrode. The bromide in the sample is determined potentiometrically with an ion-selective electrode, either through comparison to a standard curve or through a direct readout on the instrument. There are no changes to method procedures. 12. ASTM Method D1252–06 (A, B) (Reapproved 2012), chemical oxygen demand, titrimetric, spectrophotometric. This is the 2012 reapproval of the 2006 ASTM method. Method D1252–06A, titrimetric measures the loss of the hexavalent E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations dichromate ion by reflux digestion followed by titration. The chemical oxygen demand in the sample is determined by comparison to a standard curve. Method D1252–06B, spectrophotometric, uses a spectrophotometer to measure the loss of the hexavalent dichromate ion at 420 nm or the increase in the trivalent chromium ion at 600 nm, after closed digestion and determines the chemical oxygen demand by comparison to a standard curve. There are no procedural changes. 13. ASTM Method D1253–14, residual chlorine, amperometric direct. The concentration of chlorine in the sample is determined by titration with phenylarsine oxide, using an amperometric probe that responds to chlorine to determine when the titration is complete. The chlorine concentration in the sample is proportional to the volume of titrant used. There are no procedural changes. 14. ASTM Method D1426–15 (A, B), ammonia nitrogen, Nesslerization, electrode. Method D1426A, Nesslerization. An aliquot is Nesslerized, and the ammonia content determined colorimetrically. Method D1426B, electrode. Ammonia is potentiometricly determined using a gas-permeable ion-selective electrode, either through comparison to a standard curve or through a direct readout on the instrument using. A lengthy section of QC requirements was added to the Nesslerization procedure (D1426A) that parallels the QC discussion that was already in the B procedure. Both procedures added information on use of commercially prepared standards and filter paper. 15. ASTM Method D1687–17 (A–C), chromium (total) and dissolved hexavalent chromium, colorimetric (diphenyl-carbazide); AA direct aspiration; AA furnace. Method D1687– 17A, chromium (dissolved) measures dissolved hexavalent chromium by reacting it with diphenylcarbohydrazide to produce a reddishpurple color that is measured with a spectrophotometer or filter photometer. The concentration in the sample is proportional to the intensity of the color. Method D1687–17B, chromium (total). The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D1687–17C, chromium (total). The sample is acid digested and analyzed by graphite furnace atomic absorption. The concentration of total chromium in the sample is proportional to the amount of light absorbed during the analysis and is determined in comparison to a standard curve. The changes mirror those for the VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 other metal methods. The QC frequencies for method blank, continuing calibration verification (CCV), continuing calibration blank (CCB), matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples. 16. ASTM Method D1688–17 (A–C), copper, AA direct aspiration, AA furnace. The sample is acid digested and analyzed by direct aspiration atomic absorption (D1688–17A and B) or graphite furnace atomic absorption (D1688–17B). The concentration of copper in the sample is proportional to the amount of light absorbed and is determined in comparison to a standard curve. The changes mirror those for the other metal methods. The changes EPA is promulgating also clarify the requirements for a multi-point calibration by discussing it in the calibration section as well as the QC section of all three procedures. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples. 17. ASTM Method D1691–17 (A, B), zinc, AA direct aspiration. Method D1691–17A. The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D1691–17B. The sample is processed by chelationextraction and analyzed by atomic absorption. The concentration of zinc in the sample is proportional to the amount of light absorbed and is determined in comparison to a standard curve. The changes mirror those for the other metal methods. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples. 18. ASTM Method D1783–01 (A, B) (Reapproved 2012), phenols, manual distillation followed by manual colorimetric (4AAP). The sample is distilled, the distillate pH is adjusted to 10.0, and reacted with 4aminoantipyrine to form a colored product. In Method D1783–01A, the colored product is extracted from the sample with chloroform and measured with a photometer at 460 nm. In Method D1783–01B, the colored product is measured without extraction, using a photometer at 510 nm. The concentration of phenolics is determined in comparison to a standard curve. There are no procedural changes. 19. ASTM Method D1886–14 (A–C), nickel AA direct aspiration, chelation extraction AA and AA furnace. Method D1886–14A. The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D1886–14B. The sample is acid digested and the PO 00000 Frm 00007 Fmt 4701 Sfmt 4700 27231 nickel chelated and extracted. The extract is analyzed by direct aspiration atomic absorption. Method D1886–14C. The sample is acid digested and analyzed by graphite furnace atomic absorption. The concentration of nickel in the sample is proportional to the amount of light absorbed during the analysis and is determined in comparison to a standard curve. The changes mirror those for the other metal methods. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratory-defined batch of up to 20 samples. 20. ASTM Method D2036–09 (A, B) (Reapproved 2015). D2036–09 A (total cyanide). Manual distillation followed by gas diffusion amperometry, titrimetric, spectrophotometric, ion chromatography, ion selective electrode. D2036–09 B (available (amenable) cyanide) Manual distillation followed by titrimetric or spectrophotometric. The cyanide in the sample is distilled and trapped in a sodium hydroxide solution. Method D2036–09A, the cyanide is treated with strong acid and a catalyst during distillation and measured by titration, gas diffusion amperometry, spectrophotometry, ionselective electrode, ion chromatography, or flow injection analysis. Method D2036–09B—cyanide amenable to chlorination is determined by comparing the results for one sample aliquot analyzed for total cyanide and a second aliquot that is treated with calcium hypochlorite prior to analysis by Method D2036–09A. There are no procedural changes. 21. ASTM Method D2972–15 (A–C), arsenic, colorimetric, AA gaseous hydride, AA furnace. The sample is digested with nitric and sulfuric acids. Method D2972–15A. Arsenic is trapped in a solution of silver diethyldithiocarbamate in pyridine which produces a red-colored product that is analyzed photometrically by comparison to a standard curve. Method D2972–15B. Arsenic in the digested sample is determined by hydride generation atomic absorption. Method D2972–15C. Arsenic in the digested sample is determined by graphite furnace atomic absorption. The changes mirror those for the other metal methods. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratory-defined batch of up to 20 samples. 22. ASTM Method D3223–17, total mercury, cold vapor, manual. Mercury in the sample is converted to the mercuric ion, which is reduced to elemental mercury, purged from the E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 27232 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations sample, and analyzed by cold vapor atomic absorption. The changes mirror those for the other metals methods, but this version changes the acceptance limit for the CCV from 10% to 15% and adds a requirement for a CCB. Given that the most comparable EPA procedure, Method 245.1, does not include a CCV requirement or an acceptance limit, the change of the acceptance limit from 10% to 15% in the revised ASTM method represents a requirement that is more stringent than that required in EPA’s procedure. 23. ASTM Method D3373–17, vanadium, AA furnace. The sample is digested with nitric acid and analyzed by graphite furnace atomic absorption. The concentration of vanadium in the sample is proportional to the amount of light absorbed during the graphite furnace atomic absorption analysis and is determined in comparison to a standard curve. The changes mirror those for the other metals methods. The changes clarify the requirements for a multi-point calibration by discussing it in the calibration section as well as the QC section of all three procedures. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples. 24. ASTM Method D3557–17 (A–D), cadmium, AA direct aspiration, voltammetry, AA furnace. Method D3557–17A—the sample is acid digested and analyzed by direct aspiration atomic absorption. Method D3557–17B the sample is acid digested, the digestate is chelated and extracted. The extract analyzed by direct aspiration atomic absorption. Method D3557–17C—the sample is acid digested and analyzed by differential pulse anodic stripping voltammetry. Method D3557–17D. The sample is digested with nitric acid and analyzed by graphite furnace atomic absorption. The concentration of cadmium in the sample is determined in comparison to a standard curve. The changes mirror those for the other metals methods. The changes also clarify requirements for a multi-point calibration by discussing it in the calibration section as well as the QC section of all three procedures. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples, as opposed to 10 samples previously. 25. ASTM Method D3558–15 (A–C), cobalt, AA direct aspiration, chelation extraction AA, and AA furnace. Method D3558–15A.The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D3558– 15B.The sample is acid digested, VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 chelated and extracted. The extract is analyzed by direct aspiration atomic absorption. Method D3558–15C. The sample is acid digested and analyzed by graphite furnace atomic absorption. The concentration of cobalt in the sample is proportional to the amount of light absorbed during the analysis and is determined in comparison to a standard curve. The changes mirror those for the other metals methods. The changes also clarify the requirements for a multipoint calibration by discussing it in the calibration section as well as the QC section of all three procedures. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratorydefined batch of up to 20 samples, as opposed to 10 samples previously. 26. ASTM Method D3559–15 (A–D), lead, AA direct aspiration, voltammetry, AA furnace. Method D3559–15A. The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D3559–15B. The sample is acid digested, chelated and extracted. The extract is analyzed by direct aspiration atomic absorption. Method D3559–15C. The sample is acid digested and analyzed by differential pulse anodic stripping voltammetry. Method D3559– 15D. The sample is digested with nitric acid and analyzed by graphite furnace atomic absorption. The changes mirror those for the other metals methods. The changes also clarify the requirements for a multi-point calibration by discussing it in the calibration section as well as the QC section of all three procedures. It also adds a new section with the QC requirements to the direct AA procedure that was already present in the AA furnace portion of this procedure (D3559–15 D). 27. ASTM Method D3590–17 (A, B), total Kjeldahl nitrogen, manual digestion and distillation or gas diffusion; semi-automated block digester colorimetric (distillation not required). Method D3590–17A. The sample is chemically processed to covert nitrogenous compounds to ammonia, then distilled or subjected to a gas diffusion system which releases the ammonia for analysis by colorimetry, titrimetry, or potentiometry. Method D3590–17B. The digestion and distillation are accomplished by a semi-automated system and the resulting ammonia is determined by colorimetry of the salicylate/nitroprusside Berthelot reaction product. This version changes the acceptance limit for the CCV from 10% to 15% and adds a requirement for a CCB. Given that neither the approved Standard Methods method for measuring ammonia after the TKN PO 00000 Frm 00008 Fmt 4701 Sfmt 4700 digestion, nor the comparable EPA Method 350.1, include a CCV requirement or an acceptance limit, the change of the acceptance limit from 10% to 15% in the revised ASTM method represents a requirement that is more stringent than that required in other approved procedures. 28. ASTM Method D3645–15, beryllium (A, B), AA direct aspiration AA furnace. Method D3645–15A. The sample is acid digested and analyzed by direct aspiration atomic absorption. Method D3645–15B. The sample is digested with nitric acid and analyzed by graphite furnace atomic absorption. This version adds specifications for filter paper. The changes also clarify the requirements for a three-point calibration by discussing it in the calibration section as well as the QC section of both procedures. It also adds a new section with the QC requirements to the direct aspiration AA procedure that was already present in the AA furnace portion of this procedure (D3645–15B). 29. ASTM Method D3859–15 (A, B), selenium, AA gaseous hydride, AA furnace. Method D3859–15A. The selenium in the sample is converted to gaseous selenium hydride, which is then analyzed by flame atomic absorption. Method D3859–15B. The selenium in the sample is converted to gaseous selenium hydride and analyzed by graphite furnace atomic absorption. The changes to the gaseous hydride portion of the method clarify the requirement for a 6-point calibration curve by discussing it in the calibration section as well as the QC section. The version adds an updated discussion of block digesters. The QC frequencies for method blank, CCV, CCB, matrix spike, and duplicate analyses are now based on a laboratory-defined batch, as opposed to an otherwise undefined ‘‘batch.’’ The GFAA portion contains similar editorial and technical changes. Technical changes also include specifications for filter paper. The calibration requirement for three standards has been clarified by discussing it in the calibration section as well as the QC section. 30. ASTM Method D3867–16 (A, B) nitrate-nitrite, nitrite and nitrate; automated cadmium reduction, manual cadmium reduction, bypass cadmium reduction and subtraction. The combination of nitrate and nitrite in the sample is determined by reducing the nitrate to nitrite using a cadmiumcopper column, diazotizing and analyzing in either a manual or automated spectrophotometric system. A second aliquot of the sample can be analyzed without use of the cadmium E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations reduction column to determine the concentration of nitrate by difference. The changes add more detailed QC requirements, including specifically calling out the laboratory control sample (LCS), method blank, and matrix spike analyses. The 2016 version adds specifications for filter paper. It also changes the LCS frequency from 10% of samples to once per batch (up to 20) and sets the CCB and CCV frequencies at 10%. 31. ASTM Method D4190–15, dissolved elements and total recoverable elements, direct current plasma. The concentrations of various metal elements are determined by acidifying an aliquot of the sample and analyzing it by direct current plasma spectrometry, monitoring a specific wavelength of light for each element. There is one change that adds a requirement to run at least four calibration standards for all metals, as opposed to running four standards for only lithium to demonstrate linearity. 32. ASTM Method D4282–15, free cyanide, manual micro-diffusion and colorimetry. The sample is treated and allows for free cyanide to diffuse into a sodium hydroxide solution. An aliquot of that solution is treated to form a colored product that is measured with a spectrophotometer at 580 nm. There are no procedural changes. 33. ASTM Method D4327–17, inorganic anions (fluoride, bromide, chloride, nitrite, nitrate, orthophosphate, and sulfate), ion chromatography. An aliquot of the sample in injected into an ion chromatograph equipped with an anion exchange column and a conductivity detector. The anions are identified based on their retention times and concentrations are determined by comparison to a standard curve. Changes include updating the equipment and reagent descriptions to reflect more modern instrumentation, such as the use of hydroxide eluents and eluent regeneration systems. 34. ASTM Method D4382–18, barium, AA furnace. The sample is digested with nitric acid and analyzed by graphite furnace atomic absorption. The only procedural change is to the description of the hot block digester equipment. The new version specifies the capability to heat samples between 65 and 95 degrees C, instead of ‘‘approximately 95 degrees C.’’ That change recognizes the operational characteristics of hot block digesters that will experience a temperature drop below 95 degrees when samples are added. EPA has concluded that this should not adversely affect use of this method for barium. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 35. ASTM Method D4658–15, sulfide ion, ion selective electrode. The sample is treated with a sulfide antioxidant buffer to create a highly alkaline solution. Sulfide in the sample is measured potentiometrically with an ion-selective electrode. There are no procedural changes. 36. ASTM Method D4839–03 (Reapproved 2017), total organic carbon; heated persulfate or UV persulfate oxidation. The sample is sparged with an inert gas to remove dissolved inorganic carbon and then treated with persulfate and either heat or UV radiation to convert organic carbon to carbon dioxide. The carbon dioxide is measured with an infra-red detector. There are no procedural changes. 37. ASTM Method D5257–17, dissolved hexavalent chromium, ion chromatography. The sample is filtered and buffered, and an aliquot injected into an ion chromatograph that separates hexavalent chromium from other ions. The eluent from the chromatograph is treated with an acidic solution of diphenylcarbohydrazide to form a violet-colored product that is measured with a photometric detector at 530 nm. The changes also include a few additional cautions and recommendations. 38. ASTM Method D5673–16, dissolved elements and totalrecoverable elements, ICP/MS. The sample is acid digested and analyzed by inductively coupled plasma/mass spectrometry. Gold was added to the list of target analytes. Some of the changes address the analysis of gold. 39. ASTM Method D6508–15, inorganic anions (fluoride, bromide, chloride, nitrite, nitrate, orthophosphate, and sulfate), capillary ion electrophoresis with indirect UV detection. An aliquot of the sample is injected into a capillary ion electrophoresis instrument where the anions are separated in an applied electric field through a fused silica capillary. The analytes are detected by a UV detector and their concentrations are determined by comparison to a standard curve. There are no procedural changes. 40. ASTM Method D6888–16, available cyanide, flow injection and ligand exchange, followed by gas diffusion amperometry. An aliquot of the sample is introduced into a flow injection analysis instrument, where available cyanide is acidified to form hydrogen cyanide which diffuses through a hydrophobic gas diffusion membrane into an alkaline solution and is detected amperometrically with a silver electrode. This version adds a new mixed ligand exchange reagent, but PO 00000 Frm 00009 Fmt 4701 Sfmt 4700 27233 also retains the original two ligand reagents that had to be mixed together during the testing. 41. ASTM Method D6919–17, inorganic alkali and alkaline earth cations and ammonium (ammonium, calcium magnesium, potassium and sodium), ion chromatography. An aliquot of the sample is injected into an ion chromatograph equipped with a cation exchange column and a conductivity detector. The cations are identified based on their retention times and concentrations are determined by comparison to a standard curve. There are no procedural changes. 42. ASTM Method D7237–15 A, free cyanide, flow injection, followed by gas diffusion amperometry. An aliquot of the sample is introduced into a flow injection analysis instrument, where it mixes with a phosphate buffer to release hydrogen cyanide which diffuses through a hydrophobic gas diffusion membrane into an alkaline solution and is detected amperometrically with a silver electrode. There are a few additions and changes to the newer version of note. These include changing the applicable range of the method in Section 1.4 at the low end, from 2 to 500 mg/L to 5 to 500 mg/L. New information about interferences from floatation reagents has been added to Section 6.3. New materials in Section 8 discuss alternative reagents or concentrations. 43. ASTM Method D7284–13 (Reapproved 2017), total cyanide, manual distillation with MgCl2 followed by flow injection, gas diffusion amperometry. The sample is distilled with acid and a magnesium chloride catalyst to release cyanide to a sodium hydroxide solution. An aliquot of the sodium hydroxide solution is introduced into a flow injection analysis instrument, where it is acidified, and the hydrogen cyanide diffuses through a hydrophobic gas diffusion membrane into an alkaline solution and is detected amperometrically with a silver electrode. There are no procedural changes. 44. ASTM Method D7511–12 (Reapproved 2017), total cyanide, segmented flow injection, in-line ultraviolet digestion, followed by gas diffusion amperometry. The sample is introduced into a segmented flow injection analysis instrument, where UV light releases cyanide from cyanide complexes. The sample is then acidified in the instrument and the produced cyanide gas is detected amperometrically with a silver electrode. There are no procedural changes. 45. ASTM Method D7573–09 (Reapproved 2017), total organic carbon, E:\FR\FM\19MYR2.SGM 19MYR2 27234 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations combustion. The sample is sparged with an inert gas to remove dissolved inorganic carbon, acidified, and then combusted at high temperature convert organic carbon to carbon dioxide. The carbon dioxide is measured with an infra-red detector. There are no procedural changes. EPA is promulgating the following changes to Table IC at 40 CFR part 136: 1. ASTM Method D7065–17, nonylphenol, bisphenol A, p-tertoctylphenol, nonylphenol monoethoxylate, nonylphenol diethoxylate, gas chromatography/mass spectrometry (GC/MS). The sample is extracted with methylene chloride and the extract is injected into a gas chromatograph-mass spectrometer. The target analytes are identified by retention time and mass spectra and quantified using internal standards and a calibration curve. There are a large number of editorial and structural changes in the document, and a new QC section has been added. khammond on DSKJM1Z7X2PROD with RULES2 F. Changes to 40 CFR 136.3 To Include a New ASTM Method Based on Previously Approved Technologies EPA is promulgating these changes in furtherance of the National Technology Transfer and Advancement Act of 1995 (NTTAA), Public Law 104–113, that provides that federal agencies and departments shall use technical standards developed or adopted by the VCSBs if compliance would not be inconsistent with applicable law or otherwise impracticable. This method submitted by ASTM is consistent with other already approved methods. EPA is adding ASTM Method D7781– 14 to Table IB for nitrate-nitrite, nitrite (bypass the enzymatic reduction step) and nitrate by subtraction. Nitrate is reduced to nitrite by an enzymatic reaction. The nitrite is diazotized to yield an azo dye which is measured colorimetrically. The enzyme reduction step may be by-passed for measurement of nitrite singly. The value obtained for nitrite may be subtracted from the value obtained for combined nitrate-nitrite to calculate the concentration of nitrate. This method is similar to the currently approved NECi Method N07–0003, USGS Method I–2547–11, and USGS Method I–2548–11. G. Changes to 40 CFR 136.3 To Include New United States Geological Survey (USGS) Inorganic Methods Based on Previously Approved Technologies 1. EPA is adding USGS Method I– 2057–85 titled ‘‘Anions, ion-exchange chromatographic, automated,’’ to Table IB for bromide. Method I–2057–85 is an ion chromatography method that lists VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 several target analytes: Bromide, chloride, fluoride, nitrate, nitrite, orthophosphate, and sulfate. These are the same target analytes found in EPA Methods 300.0 (Part A) and 300.1 (Part A). Both EPA methods are approved in 40 CFR part 136 for the target analytes listed in the methods. USGS Method I– 2057–85 is similar to EPA Method 300.0, in that it uses ion chromatography with a sodium bicarbonate/sodium carbonate eluent and has the same target analyte list. The two methods specify different columns and eluent concentrations but rely on essentially the same underlying chemistry and determinative technique as other ion chromatography methods approved at 40 CFR part 136 for measurement of bromide. That is, the sample is introduced into an ion chromatograph. The anions of interest are separated and measured, using a system comprised of a guard column, analytical column, suppressor device, and conductivity detector. 2. EPA is adding USGS Method I– 2522–90 titled ‘‘Nitrogen, ammonia, colorimetry, salicylate-hypochlorite, automated-segmented flow’’ to Table IB for ammonia. USGS Method I–2522–90 uses the same underlying chemistry and determinative technique as other methods approved at 40 CFR part 136 for measurement of ammonia. The method is similar to other approved methods, such as EPA Method 350.1, Standard Methods Method 4500–NH3 G, and USGS Method I–4523–85, which rely on the Berthelot reaction. USGS Method I–2522–90 uses a modified version of the Berthelot reaction in which salicylate and hypochlorite react with ammonia in the presence of ferricyanide ions to form the salicylic analog of indophenol blue dye. The resulting color is directly proportional to the concentration of ammonia present and is measured using automated spectrophotometry. This is a welldocumented modification to the Berthelot reaction used in EPA Method 351 and is specifically allowed in Table IB. 3. EPA is adding USGS Method I– 2540–90 titled ‘‘Nitrogen, nitrite, colorimetry, diazotization, automatedsegmented flow’’ to Table IB for nitrite. USGS Method I–2540–90 employs the same underlying chemistry and determinative technique as other methods approved at 40 CFR part 136 for measurement of nitrite. The method is similar to other methods approved at 40 CFR part 136 for measurement of nitrite, including USGS Method I–4540– 85, which uses an automated-segmented flow analyzer (Technicon AA II). Method I–2540–90, nitrite reacts with PO 00000 Frm 00010 Fmt 4701 Sfmt 4700 sulfanilamide under acidic conditions to form a diazo compound which is coupled with N-1naphthylethylenediamine dihydrochloride to form a red compound, the absorbance of which is measured using an automatedsegmented flow, spectrophotometry. 4. EPA is adding USGS Method I– 2601–90 titled ‘‘Phosphorus, orthophosphate, colorimetry, phosphomolybdate, automatedsegmented flow’’ to Table IB for orthophosphate. USGS Method I–2601– 90 employs the same underlying chemistry and determinative technique as other methods approved in 40 CFR part 136 for measurement of orthophosphate. Orthophosphate reacts with ammonium molybdate in acidic solution to form phosphomolybdic acid, which upon reduction with ascorbic acid produces an intensely blue complex the absorbance of which is measured using automated spectrophotometry. Antimony potassium tartrate is added to increase the rate of reduction. The method is similar to other approved methods, such as USGS Method I–4601–85 which uses an automated-segmented flow analyzer (Technicon AA II). The submitted USGS Method I–2601–90 also uses an automated-segmented flow analyzer (Alpkem rapid flow analyzer). It should be noted that the approved USGS Method I–4601–85 has two parameter codes listed: a. Phosphorus, orthophosphate, dissolved, I–2601–85 (mg/L as P); and b. Phosphorus, orthophosphate, total, I–4601–85 (mg/L as P). Although USGS Method I–4601–85 is listed in Table IB, samples to be used for measurement of orthophosphate are to be filtered upon collection as provided in Table II. Therefore, the correct parameter code listed for the method should have been I–2601–85. I–2601–90 is just an updated version of that method (parameter code). In Section 3— Interferences, USGS Method I–2601–85 states: ‘‘Because as phosphorus is easily adsorbed on sediment, the orthophosphate recovered from the supernatant solution above a watersuspended sediment after some time has elapsed may be less than the orthophosphate that would have been determined in the filtrate from a sample filtered at the time of collection. The amount recovered may also depend on the type of sediment (clay, sand, etc.).’’ 5. EPA is adding USGS Method I–4472–97 titled ‘‘Metals, Acid Digestion, Whole-Water Recoverable, inductively coupled plasma-mass spectrometry’’ to Table IB for certain E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations khammond on DSKJM1Z7X2PROD with RULES2 metals by ICP/MS. USGS Method I– 4472–97 is an ICP/MS method that was previously listed under the same method number as the USGS ICP/AES Method I–4471–97 and was split out and assigned a unique method number by USGS in 2003. EPA is adding this to Table IB on the line for ICP/MS and replace USGS Method I–4471–97 as an approved method for measurement of the following 16 elements: Aluminum, antimony, barium, beryllium, cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, selenium, silver, thallium and zinc. USGS Method I–4472–97 relies on the same underlying chemistry and determinative technique as other ICP/ MS methods approved at 40 CFR part 136 for measurement of the same 16 elements (e.g., EPA Method 200.8 and Standard Methods Method 3125 B) where analytes in the sample are solubilized by gentle refluxing with acids and then measured using inductively coupled plasma-mass spectrometry. H. Changes to 40 CFR 136.3 To Include New United States Geological Survey (USGS) Organic Methods Based on Previously Approved Technologies 1. EPA is adding USGS Method O– 4127–96 titled ‘‘Determination of 86 Volatile Organic Compounds in Water by Gas Chromatography/Mass Spectrometry, Including Detections Less Than Reporting Limits’’ to Table IC for certain organic compounds. USGS Method O–4127–96 relies on the same underlying chemistry and determinative technique as other methods approved at 40 CFR part 136 for measurement of the analytes. Volatile organic compounds are extracted by purging with helium, collected on a sorbent trap, thermally desorbed, separated by a gas chromatographic capillary column, and finally determined by a quadrupole mass spectrometer operated in full-scan mode. Compound identification is confirmed by the gas chromatographic retention time and by the resultant mass spectrum, typically identified by three unique ions. 2. EPA is adding USGS Method O– 4436–16 titled ‘‘Determination of Heat Purgeable and Ambient Purgeable Volatile Organic Compounds in Water by Gas Chromatography/Mass Spectrometry’’ to Table IC for certain organic compounds. USGS Method O– 4436–16 relies on the same underlying chemistry and determinative technique as other methods approved at 40 CFR part 136 for measurement of the analytes. Volatile organic compounds are extracted from a water sample and compounds are trapped in a tube VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 containing suitable sorbent materials and then thermally desorbed into a capillary gas chromatographic column interfaced to a mass spectrometer system. Selected compounds are identified by using strict qualification criteria, which include analyzing standard reference materials and comparing retention times and relative ratios of the mass spectra. Compounds are quantitated using internal standard procedures. I. Changes to 40 CFR 136.3 To Include Alternate Test Procedures (ATPs) To promote method innovation, EPA maintains a program that allows method developers to apply for EPA review and potential approval of an alternative method to an existing EPA approved method. This ATP program is described for CWA applications at 40 CFR 136.4 and 136.5. EPA is promulgating three ATPs for nationwide use. Based on EPA’s review, the performance of these ATPs is equally effective as other methods already approved for measurement. The ATP applicants supplied EPA with study reports that contain the data from their validation studies that support EPA’s conclusion that the ATPs are equally effective to currently approved methods. These study reports and the letters documenting EPA’s review are contained as supporting documents within the docket for this final rule. These new methods include: FIAlab Method 100, ‘‘Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis,’’ MACHEREYNAGEL GmbH and Co. Method 036/038 NANOCOLOR® COD LR/HR, ‘‘Spectrophotometric Measurement of Chemical Oxygen Demand in Water and Wastewater,’’ and Micrology Laboratories, LLC. KwikCountTM EC Medium Escherichia coli (E. coli) enzyme substrate test, ‘‘Rapid Detection of E. coli in Beach Water by KwikCountTM EC Membrane Filtration.’’ Descriptions of these new methods are as follows: 1. FIAlab Instruments, Inc. Method 100, ‘‘Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis,’’ dated April 4, 2018 (FIAlab Instruments, Inc. 2018a). FIAlab Method 100 uses automated flow injection analysis with gas diffusion and fluorescence detector analysis to determine concentrations of ammonia in wastewater, ambient water, and Kjeldahl digestates. FIAlab Method 100 can be obtained from FIAlab Instruments, Inc., 2151 N Northlake PO 00000 Frm 00011 Fmt 4701 Sfmt 4700 27235 Way, Seattle, WA 98103. Telephone: 425–376–0450. 2. 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, dated, May 2018 (MACHEREY-NAGEL GmbH and Co. 2018a). MACHEREY-NAGEL Method 036/038 NANOCOLOR® COD LR/HR is a manual method that uses spectrophotometry to measure chemical oxygen demand in wastewater. MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR® COD LR/HR, can be obtained from MACHEREY-NAGEL GmbH and Co., 2850 Emrick Blvd., Bethlehem, PA 18020. Telephone: 888–321–6224. 3. Micrology Laboratories LLC. KwikCountTM EC Medium E. coli enzyme substrate test, ‘‘Rapid Detection of E. coli in Beach Water by KwikCountTM EC Membrane Filtration’’ uses a membrane filtration procedure for rapid detection and enumeration of E. coli in ambient water. The KwikCountTM EC Medium E. coli enzyme substrate test can be obtained from Micrology Laboratories, LLC, 1303 Eisenhower Drive, Goshen, IN 46526. Telephone: 574–533–3351. J. Changes to 40 CFR 136.3, Tables IA, IB, and IH EPA is promulgating the following changes to 40 CFR 136.3, Tables IA and IH: 1. Table IA: Moving Colilert-18 from Parameter #1 Coliform (fecal), number per 100 mL or number per gram dry weight, to Parameter #2 Coliform (fecal), (number per 100 mL), to eliminate confusion as to whether it is approved for sewage sludge in addition to wastewater. 2. Table IA: Adding E. coli, number per 100 mL¥MF, two-step, Standard Methods Method 9222 B/9222 I, to the table along with footnote 31 ‘‘Subject coliform positive samples determined by 9222 B–2015 or other membrane filter procedure to 9222 I–2015 using NA–MUG media.’’ The method was inadvertently omitted from Table IA when Table IA was split into two tables (IA and IH) in an earlier rulemaking; the addition corrects that error. 3. Table IA: Revising Parameter #2 Coliform (fecal), deleting ‘‘in presence of chlorine,’’ number per 100 mL. The phrase ‘‘in the presence of chlorine’’ caused confusion because the methods cited were the same for the analyte/ matrix combination that did not state ‘‘in the presence of chlorine.’’ The approved methods did not change. E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 27236 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 4. Table IA: Deleting Parameter #4 Coliform (total) in presence of chlorine, number per 100 mL. Except for ‘‘MF with enrichment,’’ all the methods were duplicative (e.g., Parameters #3 and #4). No approved methods for coliform (total) were removed from Table IA. 5. Table IH: Deleting Parameters #2 Coliform (fecal) in presence of chlorine, number per 100 mL and #4 Coliform (total) in presence of chlorine, number per 100 mL. Except for ‘‘MF with enrichment’’ for coliform (total), all the methods were duplicative (e.g., Parameters #1 and #2). In addition to the methods being duplicative, Table IH is for ambient water which would not be expected to contain chlorine. No approved methods for coliform (fecal) or coliform (total) were removed from Table IH. The remaining parameters are renumbered. 6. Tables IA and IH: Revising footnote 13 to Table IA and footnote 12 to Table IH as follows ‘‘These tests are collectively known as defined enzyme substrate tests.’’ The remaining text, ‘‘where, for example, a substrate is used to detect the enzyme b-glucuronidase produced by E. coli’’ has been deleted because the example has caused some confusion to stakeholders. 7. Tables IA and IH: Adding QuantiTray®/2000 as an option to footnotes 13 (IH), 15 (IH), 16 (IA) and 18 (IA). The addition of Quanti-Tray®/2000 is to address matrices with high bacterial concentrations and to ensure Tables IA and IH are accurate and consistent. 8. Tables IA and IH: Adding footnote 30 to Table IA and footnote 27 to Table IH to specify a verification procedure. The footnotes contain the following language: ‘‘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.’’ Adding the footnotes addresses the change in Standard Methods Method 9222 B–2015 that stated that five typical and five atypical colonies should be verified per membrane, which could be burdensome to laboratories analyzing samples other than drinking water. In most cases, analysis of ambient waters and wastewaters could result in multiple plates per sample with typical and atypical colonies, whereas drinking water analyses would seldom result in any typical or atypical colonies. In addition, the language in footnotes 29 (IA) and 26 (IH), was revised as follows VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 ‘‘the medium’’ was replaced with ‘‘positive samples’’ for clarity and consistency. 9. Tables IA and IH: Adding footnote 32 to Table IA and footnote 30 to Table IH. The footnotes contain the following language ‘‘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 & 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.’’ 10. Updating the Aquatic Toxicity Table to include the editorial correction from publex to pulex and adding the common names of the genus and species. 11. Table IH: Deleting ‘‘or number per gram dry weight’’ from Parameter #1. Table IH is specifically for ambient waters, which does not require reporting results on a per gram dry weight basis. 12. Table IH: Adding the Alternate Test Procedure KwikCountTM EC for E. coli, number per 100 mL under ‘‘Other.’’ 13. Table IH: Adding EPA Method 1623.1 for Parameters 6 and 7. EPA Method 1623.1 includes updated acceptance criteria for IPR, OPR, and MS/MSD, and clarifications and revisions based on the use of EPA Method 1623 and technical support questions over the past 19 years. EPA is approving the use of both methods 1623 and 1623.1 for Parameters 6 and 7. 14. Table IH: Deleting footnote 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.’’ Table IH is specifically for ambient waters, so the footnote is not applicable. The remaining footnotes are renumbered accordingly. 15. Table IH: Revising footnote 20, to reference only EPA Method 1604. The literature reference was deleted from the footnote because it resulted in confusion as to whether EPA Method 1604 provided all the necessary information required by stakeholders to conduct analyses of ambient waters under the CWA. K. Changes to Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times EPA is updating footnote 6 to the preservation and holding time requirements for cyanide to cite the latest version of ASTM method D7365– 09a that was reapproved in 2015. The recommended sampling and preservation procedures in the ASTM PO 00000 Frm 00012 Fmt 4701 Sfmt 4700 method have not changed since 2009, but the change to footnote 6 will simplify identification of the current method that is available from ASTM International. EPA is adding a call-out to footnote 9 to the preservation and holding time requirements for the purgeable halocarbons entry. This will allow the flexibility to collect a single sample with no acidification to be used for analysis of both purgeable halocarbons and purgeable aromatic hydrocarbons within seven days of collection, or to collect a single sample with acidification to be used for analysis of both purgeable halocarbons (except 2– CEVE) and purgeable aromatic hydrocarbons within the 14-day maximum holding time specified in Table II for both classes of compounds. The added flexibility is consistent with historical requirements for preservation in 40 CFR part 136 and holding time requirements in other EPA program methods, such as the SW–846 methods in the Office of Land and Emergency Management. This is part of EPA’s ongoing effort to harmonize methods between EPA programs, as requested by the Environmental Laboratory Advisory Board (ELAB). Footnote 9 to Table II states: ‘‘If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.’’ L. Changes to 40 CFR 136.6 Method Modifications and Analytical Requirements In response to requests from ELAB and the Independent Laboratories Institute, EPA is adding a new paragraph (b)(4)(xviii) to 40 CFR 136.6 that explicitly allows the use of closedvessel microwave digestion as a modification to the approved metals digestion procedure that does not require prior approval. Microwave digestion has the same fundamental chemistry as a hot plate digestion, both the microwave and hot plate serve the same function as heat sources. VI. Statutory and Executive Order Reviews A. Executive Order 12866: Regulatory Planning and Review and Executive Order 13563: Improving Regulation and Regulatory Review This rule is not a significant regulatory action and was therefore not submitted to the Office of Management and Budget (OMB) for interagency review under this E.O. B. Paperwork Reduction Act This action does not impose an information collection burden under the E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations Paperwork Reduction Act. This rule does not impose any information collection, reporting, or recordkeeping requirements. This rule merely adds or revises CWA test procedures. C. Regulatory Flexibility Act I certify that this action would not have a significant economic impact on a substantial number of small entities under the Regulatory Flexibility Act. This action will not impose any requirements on small entities. This action would approve new and revised versions of CWA testing procedures. Generally, these changes have a positive impact on small entities by increasing method flexibility, thereby allowing entities to reduce costs by choosing more cost-effective methods. In general, EPA expects the final revisions will lead to few, if any, increased costs. As explained previously, most of the changes clarify or improve the instructions in the method, update the technology used in the method, improve the QC instructions, make editorial corrections, or reflect the most recent approval year of an already approved method. In some cases, they would add alternatives to currently approved methods for a particular analyte (e.g., Method N07–0003 for Nitrate Reductase Nitrate-Nitrogen Analysis). Because these methods would be alternatives rather than requirements, there are no direct costs associated with this proposal. EPA finalized methods that would be incorporated by reference. If a permittee elected to use these methods, they could incur a small cost associated with obtaining these methods from the listed sources. See Section IV.B of this preamble. D. Unfunded Mandates Reform Act This action does not contain any unfunded mandate as described in the Unfunded Mandates Reform Act, 2 U.S.C. 1531–1538, and does not significantly or uniquely affect small governments. The action imposes no enforceable duty on any state, local or tribal governments or the private sector. khammond on DSKJM1Z7X2PROD with RULES2 E. Executive Order 13132: Federalism This final rule does not have federalism implications. It will not have substantial direct effects on the states, on the relationship between the national government and the states, or on the distribution of power and responsibilities among the various levels of government. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 F. Executive Order 13175: Consultation and Coordination With Indian Tribal Governments This final rule does not have tribal implications as specified in Executive Order 13175. This rule merely approves new and revised versions of test procedures. EPA has concluded that the final rule would not lead to any costs to any tribal governments, and in the event there are any, EPA projects they would be minimal. Thus, Executive Order 13175 does not apply to this action. G. Executive Order 13045: Protection of Children From Environmental Health Risks and Safety Risks EPA interprets Executive Order 13045 as applying only to those regulatory actions that concern environmental health or safety risks that EPA has reason to believe may disproportionately affect children, per the definition of ‘‘covered regulatory action’’ in section 2–202 of the Executive Order. This action is not subject to Executive Order 13045 because it does not concern an environmental health risk or safety risk. H. Executive Order 13211: Actions That Significantly Affect Energy Supply, Distribution, or Use This action is not subject to Executive Order 13211 because it is not a significant regulatory action under Executive Order 12866. I. National Technology Transfer and Advancement Act of 1995 This action involves technical standards. EPA is approving the use of technical standards developed and recommended by the Standard Methods Committee and ASTM International for use in compliance monitoring where EPA determined that those standards meet the needs of CWA programs. As described above, the final rule is consistent with the NTTAA. J. Executive Order 12898: Federal Actions To Address Environmental Justice in Minority Populations and Low-Income Populations EPA has concluded that this action will not have potential disproportionately high and adverse human health or environmental effects on minority, low-income or indigenous populations. L. Congressional Review Act This action is subject to the Congressional Review Act and EPA will submit a rule report to each House of the Congress and to the Comptroller General of the United States. This action PO 00000 Frm 00013 Fmt 4701 Sfmt 4700 27237 is not a ‘‘major rule’’ as defined by 5 U.S.C. 804(2). List of Subjects in 40 CFR Part 136 Environmental protection, Incorporation by reference, Reporting and recordkeeping requirements, Test procedures, Water pollution control. Michael S. Regan, Administrator. For the reasons set out in the preamble, the EPA amends 40 CFR part 136 as follows: PART 136—GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS 1. The authority citation for part 136 continues to read as follows: ■ Authority: Secs. 301, 304(h), 307 and 501(a), 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). 2. Amend § 136.3: a. In paragraph (a): i. In the introductory text, in the seventh sentence, by removing the word ‘‘year’’ and adding in its place the word ‘‘date’’, and removing from the last sentence the text ‘‘(paragraph (c) of this section, in § 136.5(a) through (d) or 40 CFR 401.13)’’ and adding in its place the text ‘‘paragraph (c) of this section, § 136.5(a) through (d) or 40 CFR 401.13,’’ respectively; ■ ii. By revising tables IA, IB, IC, and IH; ■ b. In paragraph (b) by: ■ i. Revising the introductory text; paragraph (b)(8) introductory text, and paragraphs (b)(8)(ix) through (xv); ■ ii. Adding paragraph (b)(8)(xvi); ■ iii. Revising paragraphs (b)(10)(xiv), (xxxix), (xliv), (xlvi), (lii), (liv), and (lxvii) through (lxx), (b)(15)(v), (vi), (viii) through (xiii), (xv) through (xix), (xxi) through (xxvi), (xxxi), (xxxiv), (xxxv), (xxxvii), (xxxix) through (xliii), (xlv) through (l), (lii), (liv), (lv), (lviii), (lxi) through (lxvi), (lxviii), and (lxix); ■ iv. Adding paragraph (b)(15)(lxx); ■ v. Redesignating paragraphs (b)(25) through (36) as paragraphs (b)(28) through (39); ■ vi. Redesignating paragraphs (b)(19) through (24) as paragraphs (b)(20) through (25); ■ vii. Adding new paragraphs (b)(19), (26), and (27); ■ viii. Revising the newly redesignated paragraphs (b)(38)(ii) through (xxi); ■ ix. Adding paragraphs (b)(38)(xxii) and (xxiii); and ■ c. By revising table II in paragraph (e). The revisions and additions read as follows: ■ ■ ■ E:\FR\FM\19MYR2.SGM 19MYR2 27238 § 136.3 * * Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations Identification of test procedures. * * * TABLE IA—LIST OF APPROVED BIOLOGICAL METHODS FOR WASTEWATER AND SEWAGE SLUDGE Method 1 Parameter and units EPA Standard methods AOAC, ASTM, USGS Other Bacteria 1. Coliform (fecal), number per 100 mL or number per gram dry weight. 2. Coliform (fecal), number per 100 mL 3. Coliform (total), number per 100 mL 4. E. coli, number per 100 mL ............. 5. Fecal streptococci, number per 100 mL. 6. Enterococci, number per 100 mL .... 7. Salmonella, number per gram dry weight 11. Most Probable Number (MPN), 5 tube, 3 dilution, or. Membrane filter (MF) 2 5, single step MPN, 5 tube, 3 dilution, or ................ p. 132,3 1680,11 15 1681 11 20. p. 124 3 ................ p. 132 3 ................ Multiple tube/multiple well, or ........... .............................. MF 2 5, single step 5 ........................... MPN, 5 tube, 3 dilution, or ................ MF 2 5, single step or two step .......... MF 2 5, with enrichment ..................... MPN 6 8 16 multiple tube, or ............... p. 124 3 ................ p. 114 3 ................ p. 108 3 ................ p. 111 3 ................ .............................. multiple tube/multiple well, or ........... .............................. MF 2 5 6 7 8, two step, or ..................... .............................. Single step ........................................ MPN, 5 tube, 3 dilution, or ................ 1603 21 ................. p. 139 3 ................ MF 2, or ............................................. Plate count ........................................ MPN, 5 tube, 3 dilution, or ................ MPN 6 8, multiple tube/multiple well, or. MF 2 5 6 7 8 single step or ................... Plate count ........................................ MPN multiple tube ............................ p. 136 3 ................ p. 143 3. p. 139 3 ................ .............................. 1600 24 ................. p. 143 3. 1682 22. 9221 E–2014. 9222 D–2015 29 ......... 9221 E–2014; 9221 F–2014 33. .................................... 9222 D–2015 29. 9221 B–2014. 9222 B–2015 30 ......... 9222 B–2015 30. 9221 B2014/9221 F– 2014 12 14 33. 9223 B–2016 13 ......... 9222 B–2015/9222 I– 2015 31. .................................... 9230 B–2013. B–0050–85 4. .............................. B–0025–85 4. 991.15 10 .............. Colilert® 13 18 Colilert-18® 13 17 18 .............................. m-ColiBlue24®.19 9230 C–2013 32 ......... B–0055–85 4. 9230 B–2013. 9230 D–2013 ............. D6503–99 9 .......... 9230 C–2013 32. Aquatic Toxicity 8. Toxicity, acute, fresh water organisms, LC50, percent effluent. 9. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC50, percent effluent. 10. Toxicity, chronic, fresh water organisms, NOEC or IC25, percent effluent. khammond on DSKJM1Z7X2PROD with RULES2 11. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC25, percent effluent. Water flea, Cladoceran, Ceriodaphnia dubia acute. Water fleas, Cladocerans, Daphnia pulex and Daphnia magna acute. Fish, Fathead minnow, Pimephales promelas, and Bannerfin shiner, Cyprinella leedsi, acute. Fish, Rainbow trout, Oncorhynchus mykiss, and brook trout, Salvelinus fontinalis, acute. Mysid, Mysidopsis bahia, acute ........ Fish, Sheepshead minnow, Cyprinodon variegatus, acute. Fish, Silverside, Menidia beryllina, Menidia menidia, and Menidia peninsulae, acute. Fish, Fathead minnow, Pimephales promelas, larval survival and growth. Fish, Fathead minnow, Pimephales promelas, embryo-larval survival and teratogenicity. Water flea, Cladoceran, Ceriodaphnia dubia, survival and reproduction. Green alga, Selenastrum capricornutum, growth. Fish, Sheepshead minnow, Cyprinodon variegatus, larval survival and growth. Fish, Sheepshead minnow, Cyprinodon variegatus, embryolarval survival and teratogenicity. Fish, Inland silverside, Menidia beryllina, larval survival and growth. Mysid, Mysidopsis bahia, survival, growth, and fecundity. Sea urchin, Arbacia punctulata, fertilization. 2002.0 25. 2021.0 25. 2000.0 25. 2019.0 25. 2007.0 25. 2004.0 25. 2006.0 25. 1000.0 26. 1001.0 26. 1002.0 26. 1003.0 26. 1004.0 27. 1005.0 27. 1006.0 27. 1007.0 27. 1008.0 27. Table IA notes: 1 The method must be specified when results are reported. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00014 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM Colilert18®.13 18 28 19MYR2 Enterolert®.13 23 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27239 2 A 0.45-μm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth. 3 Microbiological Methods for Monitoring the Environment, Water and Wastes, EPA/600/8–78/017. 1978. U.S. EPA. 4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS. 5 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies. 6 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample. 7 When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results. 8 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines. 9 Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International. 10 Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International. 11 Recommended for enumeration of target organism in sewage sludge. 12 The multiple-tube fermentation test is used in 9221B.2–2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis. 13 These tests are collectively known as defined enzyme substrate tests. 14 After prior enrichment in a presumptive medium for total coliform using 9221B.2–2014, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F–2014. Commercially available EC–MUG media or EC media supplemented in the laboratory with 50 μg/mL of MUG may be used. 15 Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA–821–R– 14–009. September 2014. U.S. EPA. 16 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000 and the MPN calculated from the table provided by the manufacturer. 17 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples. 18 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc. 19 A description of the mColiBlue24® test is available from Hach Company. 20 Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using A–1 Medium, EPA–821–R–06–013. July 2006. U.S. EPA. 21 Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified mTEC), EPA– 821–R–14–010. September 2014. U.S. EPA. 22 Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA–821–R–14–012. September 2014. U.S. EPA. 23 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc. 24 Method 1600: Enterococci in Water by Membrane Filtration Using Membrane-Enterococcus Indoxyl-b-D-Glucoside Agar (mEI), EPA–821–R–14–011. September 2014. U.S. EPA. 25 Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA–821–R–02–012. Fifth Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016. 26 Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA–821–R–02–013. Fourth Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016. 27 Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA–821–R–02–014. Third Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821–R–02–012–ES. December 2016. 28 To use Colilert-18® to assay for fecal coliforms, the incubation temperature is 44.5 ± 0.2 °C, and a water bath incubator is used. 29 On a monthly basis, at least ten blue colonies from positive samples must be verified using Lauryl Tryptose Broth and EC broth, followed by count adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications should be done from randomized sample sources. 30 On a monthly basis, at least ten sheen colonies from positive samples must be verified using lauryl tryptose broth and brilliant green lactose bile broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using lauryl tryptose broth. Where possible, verifications should be done from randomized sample sources. 31 Subject coliform positive samples determined by 9222 B–2015 or other membrane filter procedure to 9222 I–2015 using NA–MUG media. 32 Verification of colonies by incubation of BHI agar at 10 ± 0.5 °C for 48 ± 3 h is optional. As per the Errata to the 23rd Edition of Standard Methods for the Examination of Water and Wastewater ‘‘Growth on a BHI agar plate incubated at 10 ± 0.5 °C for 48 ± 3 h is further verification that the colony belongs to the genus Enterococcus.’’ 33 9221 F.2–2014 allows for simultaneous detection of E. coli and thermotolerant fecal coliforms by adding inverted vials to EC–MUG; the inverted vials collect gas produced by thermotolerant fecal coliforms. TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES Parameter Methodology 58 EPA 52 Standard methods 84 ASTM 1. Acidity, as CaCO3, mg/L. 2. Alkalinity, as CaCO3, mg/L. Electrometric endpoint or phenolphthalein endpoint. Electrometric or Colorimetric titration to pH 4.5, Manual. Automatic .................................................... Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. ................................... 2310 B–2011 ............ D1067–16 ................. I–1020–85.2 ................................... 2320 B–2011 ............ D1067–16 ................. 973.43,3 I–1030–85.2 310.2 (Rev. 1974) 1 .. ................................... ................................... I–2030–85.2 ................................... 3111 D–2011 or 3111 E–2011. 3113 B–2010. ................................... I–3051–85.2 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... 3500–Al B–2011. 4500–NH3 B–2011 ... D4190–15 ................. 993.14,3 I–4472– 97.81 See footnote.34 ................................... 973.49.3 ................................... 4500–NH3 C–2011. 4500–NH3 D–2011 or E–2011. D1426–15 (A) ........... 973.49,3 I–3520–85.2 3. Aluminum—Total,4 mg/L. AA furnace .................................................. STGFAA ...................................................... khammond on DSKJM1Z7X2PROD with RULES2 ICP/AES 36 ................................................... ICP/MS ........................................................ 4. Ammonia (as N), mg/L. VerDate Sep<11>2014 Direct Current Plasma (DCP) 36 .................. Colorimetric (Eriochrome cyanine R) .......... Manual distillation 6 or gas diffusion (pH > 11), followed by any of the following: Nesslerization .............................................. Titration ....................................................... Electrode ..................................................... 17:42 May 18, 2021 Jkt 253001 PO 00000 ................................... 200.9, Rev. 2.2 (1994)/ 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... 350.1, Rev. 2.0 (1993). ................................... ................................... ................................... Frm 00015 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM D1426–15 (B). 19MYR2 USGS/AOAC/other 27240 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 EPA 52 Standard methods 84 ASTM Manual phenate, salicylate, or other substituted phenols in Berthelot reactionbased methods. Automated phenate, salicylate, or other substituted phenols in Berthelot reactionbased methods. Automated electrode ................................... Ion Chromatography ................................... Automated gas diffusion, followed by conductivity cell analysis. Automated gas diffusion followed by fluorescence detector analysis. Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA furnace .................................................. STGFAA ...................................................... ................................... 4500–NH3 F–2011 ... ................................... See footnote.60 350.1,30 Rev. 2.0 (1993). 4500–NH3 G–2011 4500–NH3 H–2011. ................................... I–4523–85,2 I–2522– 90.80 ................................... ................................... ................................... ................................... ................................... ................................... ................................... D6919–17. ................................... See footnote.7 ................................... ................................... ................................... ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). 206.5 (Issued 1978) 1. ................................... 3111 B–2011. 3113 B–2010. Parameter 5. Antimony—Total,4 mg/L. ICP/AES 36 ................................................... ICP/MS ........................................................ 6. Arsenic-Total,4 mg/L Digestion,4 followed by any of the following: AA gaseous hydride .................................... AA furnace .................................................. STGFAA ...................................................... ICP/AES 36 ................................................... ICP/MS ........................................................ 7. Barium-Total,4 mg/L Colorimetric (SDDC) ................................... Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA furnace .................................................. ICP/AES 36 ................................................... ICP/MS ........................................................ 8. Beryllium—Total,4 mg/L. DCP 36 ......................................................... Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. STGFAA ...................................................... D1976–12. 3125 B–2011 ............ D5673–16 ................. 993.14,3 I–4472– 97.81 3114 B–2011 or 3114 C–2011. 3113 B–2010 ............ D2972–15 (B) ........... I–3062–85.2 D2972–15 (C) ........... I–4063–98.49 3120 B–2011 ............ D1976–12. 3125 B–2011 ............ D5673–16 ................. 3500–As B–2011 ...... D2972–15 (A) ........... ................................... ................................... 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... 3111 D–2011 ............ 3113 B–2010 ............ 3120 B–2011 ............ ................................... D4382–18. ................................... I–3084–85.2 3125 B–2011 ............ D5673–16 ................. ................................... ................................... 993.14,3 I–4472– 97.81 See footnote.34 ................................... 3111 D–2011 or 3111 E–2011. 3113 B–2010 ............ D3645–15 (A) ........... I–3095–85.2 D3645–15 (B). 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 993.14,3 I–4472– 97.81 See footnote.34 ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... 993.14,3 I–4020– 05.70 I–3060–85.2 I–4471–97.50 D5673–16 ................. DCP ............................................................. Colorimetric (aluminon) ............................... Dissolved Oxygen Depletion ....................... ................................... See footnote.61. 5210 B–2016 85 ........ D4190–15 ................. Colorimetric (curcumin) ............................... ................................... 4500–B B–2011 ....... ................................... 973.44,3 p. 17,9 I– 1578–78,8 See footnote.10, 63 I–3112–85.2 ICP/AES ...................................................... 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997). ................................... 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... ................................... 4110 B–2011, C– 2011, D–2011. D4190–15 ................. D1246–16 ................. D4327–17 ................. S7ee footnote.34 I–1125–85.2 993.30,3 I–2057– 85.79 4140 B–2011 ............ D6508–15 ................. D6508, Rev. 2.54 3111 B–2011 or 3111 C–2011. D3557–17 (A or B) ... 974.27,3 p. 37,9 I– 3135–85 2 or I– 3136–85.2 ICP/MS ........................................................ khammond on DSKJM1Z7X2PROD with RULES2 3120 B–2011 ............ 3125 B–2011 ............ ICP/MS ........................................................ 11. Bromide, mg/L ....... DCP ............................................................. Electrode ..................................................... Ion Chromatography ................................... 12. Cadmium—Total,4 mg/L. CIE/UV ........................................................ Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. VerDate Sep<11>2014 Timberline Ammonia001.74 FIAlab100.82 ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ICP/AES ...................................................... 9. Biochemical oxygen demand (BOD5), mg/ L. 10. Boron—Total,37 mg/L. USGS/AOAC/other 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00016 ................................... Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM ................................... 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27241 TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 EPA 52 Standard methods 84 ASTM AA furnace .................................................. STGFAA ...................................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... 3113 B–2010 ............ D3557–17 (D) ........... I–4138–89.51 3120 B–2011 ............ D1976–12 ................. I–1472–85 2 or I– 4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... ................................... 3500–Cd–D–1990. D4190–15 ................. D3557–17 (C). 993.14,3 I–4472– 97.81 See footnote.34 3111 B–2011 ............ 3120 B–2011 ............ D511–14 (B) ............. ................................... I–3152–85.2 I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... 3500-Ca B–2011 ...... ................................... 5210 B–2016 85 ........ ................................... D511–14 (A). D6919–17. ................................... See footnote.34 5220 B–2011 or C– 2011. 5220 D–2011 ............ D1252–06(12) (A) ..... Parameter ICP/AES 36 ................................................... ICP/MS ........................................................ 13. Calcium—Total,4 mg/L. DCP 36 ......................................................... Voltammetry 11 ............................................. Colorimetric (Dithizone) ............................... Digestion,4 followed by any of the following: AA direct aspiration ..................................... ICP/AES ...................................................... ICP/MS ........................................................ DCP ............................................................. Titrimetric (EDTA) ....................................... Ion Chromatography ................................... Dissolved Oxygen Depletion with nitrification inhibitor. 14. Carbonaceous biochemical oxygen demand (CBOD5), mg/ L12. 15. Chemical oxygen Titrimetric ..................................................... demand (COD), mg/L. Spectrophotometric, manual or automatic .. 16. Chloride, mg/L ....... 17. Chlorine-Total residual, mg/L. 17A. Chlorine-Free Available, mg/L. 18. Chromium VI dissolved, mg/L. 19. Chromium—Total,4 mg/L. D512–12 (B) ............. D512–12 (A) ............. ................................... ................................... CIE/UV ........................................................ Amperometric direct .................................... 4140 B–2011 ............ 4500–Cl D–2011 ...... D6508–15 ................. D1253–14. D6508, Rev. 2.54 Amperometric direct (low level) .................. Iodometric direct .......................................... Back titration ether end-point 15 .................. DPD–FAS .................................................... Spectrophotometric, DPD ........................... Electrode ..................................................... Amperometric direct .................................... ................................... ................................... ................................... ................................... ................................... ................................... ................................... 4500-Cl E–2011. 4500-Cl B–2011. 4500-Cl C–2011. 4500–Cl F–2011. 4500–Cl G–2011. ................................... 4500–Cl D–2011 ...... ................................... D1253–14. See footnote.16 Amperometric direct (low level) .................. DPD–FAS .................................................... Spectrophotometric, DPD ........................... 0.45-micron filtration followed by any of the following: AA chelation-extraction ............................... Ion Chromatography ................................... ................................... ................................... ................................... 4500–Cl E–2011. 4500-Cl F–2011. 4500-Cl G–2011. ................................... 218.6, Rev. 3.3 (1994). ................................... 3111 C–2011 ............ 3500-Cr C–2011 ....... ................................... D5257–17 ................. I–1232–85.2 993.23.3 3500–Cr B–2011 ...... D1687–17 (A) ........... I–1230–85.2 3111 B–2011 ............ 3111 C–2011. 3113 B–2010 ............ D1687–17 (B) ........... 974.27,3 I–3236–85.2 D1687–17 (C) ........... I–3233–93.46 3120 B–2011 ............ D1976–12. 3125 B–2011 ............ D5673–16 ................. ................................... 3500–Cr B–2011. D4190–15 ................. 993.14,3 I–4020– 05 70 I–4472–97.81 See footnote.34 3111 B–2011 or 3111 C–2011. 3113 B–2010 ............ D3558–15 (A or B) ... p. 37,9 I–3239–85.2 D3558–15 (C) ........... I–4243–89.51 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 Colorimetric (diphenyl-carbazide) ............... Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA chelation-extraction ............................... AA furnace .................................................. STGFAA ...................................................... khammond on DSKJM1Z7X2PROD with RULES2 DCP 36 ......................................................... Colorimetric (diphenyl-carbazide) ............... Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. STGFAA ...................................................... ICP/AES ...................................................... 17:42 May 18, 2021 Jkt 253001 PO 00000 ................................... ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003),68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ................................... 200.9, Rev. 2.2 (1994). 200.7, Rev. 4.4 (1994). Frm 00017 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM D1252–06(12) (B) ..... 973.46,3 p. 17,9 I– 3560–85.2 See footnotes.13 14 83, I–3561–85.2 I–1183–85.2 973.51,3 I–1184–85.2 I–1187–85.2 I–2187–85.2 4500–Cl–B–2011 ...... 4500–Cl–C–2011 ..... ................................... 4500–Cl–E–2011 ...... 4500–Cl–D–2011. ................................... 4110 B–2011 or 4110 C–2011. Titrimetric: (silver nitrate) ............................ (Mercuric nitrate) ......................................... Colorimetric: manual ................................... Automated (ferricyanide) ............................. Potentiometric Titration ............................... Ion Selective Electrode ............................... Ion Chromatography ................................... ICP/MS ........................................................ VerDate Sep<11>2014 410.3 (Rev. 1978) 1 .. See footnote.35 63 410.4, Rev. 2.0 (1993). ................................... ................................... ................................... ................................... ................................... ................................... 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997). ................................... ................................... ICP/AES 36 ................................................... 20. Cobalt—Total,4 mg/ L. ................................... 200.5, Rev 4.2 (2003);68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ................................... USGS/AOAC/other D512–12 (C). D4327–17 ................. 19MYR2 993.30,3 I–2057– 90.51 27242 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 EPA 52 Standard methods 84 ASTM USGS/AOAC/other ICP/MS ........................................................ 200.8, Rev. 5.4 (1994). ................................... ................................... 3125 B–2011 ............ D5673–16 ................. ................................... 2120 F–2011 78. D4190–15 ................. 993.14,3 I–4020– 05 70 I–4472–97.81 See footnote.34 Platinum cobalt visual comparison ............. Spectrophotometric ..................................... Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. ................................... ................................... 2120 B–2011 ............ ................................... ................................... ................................... I–1250–85.2 See footnote 18 ................................... 3111 B–2011 or 3111 C–2011. D1688–17 (A or B) ... AA furnace .................................................. STGFAA ...................................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ................................... 3113 B–2010 ............ D1688–17 (C) ........... 974.27,3 p. 37,9 I– 3270–85 2 or I– 3271–85.2 I–4274–89.51 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... 3500-Cu B–2011. 3500-Cu C–2011 ...... ................................... D4190–15 ................. 993.14,3 I–4020– 05,70, I–4472–97.81 See footnote.34 ................................... ................................... See footnote.19 Kelada-01.55 ................................... ................................... D7511–12(17). 335.4, Rev. 1.0 (1993) 57. ................................... 4500–CN–B–2016 and C–2016. ................................... ................................... ................................... 335.4, Rev. 1.0 (1993) 57. ................................... ................................... ................................... 4500–CN–D–2016 .... 4500–CN–E–2016 .... 4500–CN–N–2016 .... D2036–09(15)(A), D7284–13(17). D2036–09(15)(A) D7284–13(17). D2036–09(15)(A) ...... D2036–09(15)(A) ...... ................................... ................................... 4500–CN–F–2016 .... 4500–CN–G–2016 .... D2036–09(15)(A). D2036–09(15)(A). D2036–09(15)(B). ................................... ................................... D6888–16 ................. OIA–1677–09.44 ................................... ................................... ................................... Kelada-01.55 ................................... ................................... D7237–15 (A) ........... OIA–1677–09.44 ................................... ................................... ................................... 4500–F–B–2011 ....... D4282–15. D1179–16 (A). ................................... ................................... ................................... ................................... 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997). ................................... 4500–F–C–2011 ....... ................................... 4500–F–D–2011. 4500–F–E–2011. 4110 B–2011 or C– 2011. D1179–16 (B). ................................... I–4327–85.2 D4327–17 ................. 993.30.3 4140 B–2011 ............ D6508–15 ................. D6508, Rev. 2.54 ................................... 231.2 (Issued 1978) 1 200.8, Rev. 5.4 (1994). ................................... 130.1 (Issued 1971) 1. ................................... 3111 B–2011. 3113 B–2010. 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... ................................... See footnote.34 2340 C–2011 ............ D1126–17 ................. 973.52B 3, I–1338– 85.2 Parameter 21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity 22. Copper—Total,4 mg/L. DCP ............................................................. Colorimetric (ADMI) ..................................... ICP/AES 36 ................................................... ICP/MS ........................................................ 23. Cyanide—Total, mg/L. DCP 36 ......................................................... Colorimetric (Neocuproine) ......................... Colorimetric (Bathocuproine) ...................... Automated UV digestion/distillation and Colorimetry. Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometry. Manual distillation with MgCl2, followed by any of the following: Flow Injection, gas diffusion amperometry Titrimetric ..................................................... Spectrophotometric, manual ....................... Semi-Automated 20 ...................................... 24. Cyanide-Available, mg/L. 24.A Cyanide-Free, mg/L. 25. Fluoride—Total, mg/L. 26. Gold—Total,4 mg/L 27. Hardness—Total, as CaCO3, mg/L. Ion Chromatography ................................... Ion Selective Electrode ............................... Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl2, followed by Titrimetric or Spectrophotometric. Flow injection and ligand exchange, followed by gas diffusion amperometry 59. Automated Distillation and Colorimetry (no UV digestion). Flow Injection, followed by gas diffusion amperometry. Manual micro-diffusion and colorimetry ...... Manual distillation,6 followed by any of the following: Electrode, manual ....................................... Electrode, automated .................................. Colorimetric, (SPADNS) .............................. Automated complexone .............................. Ion Chromatography ................................... CIE/UV ........................................................ Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/MS ........................................................ DCP ............................................................. Automated colorimetric ............................... khammond on DSKJM1Z7X2PROD with RULES2 Titrimetric (EDTA) ....................................... 28. Hydrogen ion (pH), pH units. VerDate Sep<11>2014 10–204–00–1–X.56 p. 22.9 I–3300–85.2 10–204–00–1–X,56 I– 4302–85.2 Ca plus Mg as their carbonates, by any approved method for Ca and Mg (See Parameters 13 and 33), provided that the sum of the lowest point of quantitation for Ca and Mg is below the NPDES permit requirement for Hardness. Electrometric measurement ........................ ................................... 2340 B–2011. ................................... 4500–H+ B–2011 ...... D1293–99 (A or B) ... 973.41,3 I–1586–85.2 Automated electrode ................................... 150.2 (Dec. 1982) 1 .. ................................... ................................... See footnote,21 I– 2587–85.2 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00018 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27243 TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Parameter Methodology 58 29. Iridium—Total,4 mg/ L. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. 30. Iron—Total,4 mg/L EPA 52 ICP/MS ........................................................ Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA furnace .................................................. STGFAA ...................................................... ICP/AES 36 ................................................... ICP/MS ........................................................ DCP 36 31. Kjeldahl Nitrogen 5—Total, (as N), mg/L. ......................................................... Colorimetric (Phenanthroline) ..................... Manual digestion 20 and distillation or gas diffusion, followed by any of the following: Titration ....................................................... Nesslerization .............................................. Electrode ..................................................... Semi-automated phenate ............................ Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods. Automated gas diffusion, followed by conductivity cell analysis. Automated gas diffusion followed by fluorescence detector analysis. Standard methods 84 ASTM USGS/AOAC/other D1068–15 (A) ........... 974.27,3 I–3381–85.2 ................................... 235.2 (Issued 1978) 1. ................................... 3111 B–2011. ................................... 3111 B–2011 o 3111 C–2011. 3113 B–2010 ............ D1068–15 (B). 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 D4190–15 ................. D1068–15 (C) ........... D3590–17 (A) ........... See footnote.34 See footnote.22 I–4515–91.45 ................................... D1426–15 (A). D1426–15 (B). 973.48.3 350.1, Rev. 2.0 (1993). ................................... ................................... 3500–Fe B–2011 ...... 4500–Norg B–2011 or C–2011 and 4500– NH3 B–2011. 4500–NH3 C–2011 ... ................................... 4500–NH3 D–2011 or E–2011. 4500–NH3 G–2011 4500–NH3 H–2011. 4500–NH3 F–2011 ... ................................... See footnote.60 ................................... ................................... ................................... ................................... ................................... ................................... Timberline Ammonia001.74 FIAlab 100.82 ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ................................... ................................... ................................... 3125 B–2011. Automated Methods for TKN that do not require manual distillation 32. Lead—Total,4 mg/L Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation). Semi-automated block digestor colorimetric (distillation not required). Block digester, followed by Auto distillation and Titration. Block digester, followed by Auto distillation and Nesslerization. Block Digester, followed by Flow injection gas diffusion (distillation not required). Digestion with peroxdisulfate, followed by Spectrophotometric (2,6-dimethyl phenol). Digestion with persulfate, followed by Colorimetric. Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. 351.1 (Rev. 1978) 1 .. ................................... ................................... I–4551–78.8 351.2, Rev. 2.0 (1993). ................................... 4500–Norg D–2011 ... D3590–17 (B) ........... I–4515–91 45 ................................... ................................... See footnote.39 ................................... ................................... ................................... See footnote.40 ................................... ................................... ................................... See footnote.41 ................................... ................................... ................................... Hach 10242.76 ................................... ................................... ................................... NCASI TNTP W10900.77 ................................... D3559–15 (A or B) ... 974.27,3 I–3399–85.2 AA furnace .................................................. STGFAA ...................................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... 3111 B–2011 or 3111 C–2011. 3113 B–2010 ............ D3559–15 (D) ........... I–4403–89.51 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... ................................... 3500–Pb B–2011. D4190–15 ................. D3559–15 (C). 993.14,3 I–4472– 97.81 See footnote.34 3111 B–2011 ............ 3120 B–2011 ............ D511–14 (B) ............. D1976–12 ................. 974.27,3 I–3447–85.2 I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... ................................... ................................... D6919–17. See footnote.34 ICP/AES 36 ................................................... ICP/MS ........................................................ khammond on DSKJM1Z7X2PROD with RULES2 33. Magnesium— Total,4 mg/L. DCP 36 ......................................................... Voltammetry 11 ............................................. Colorimetric (Dithizone) ............................... Digestion,4 followed by any of the following: AA direct aspiration ..................................... ICP/AES ...................................................... ICP/MS ........................................................ 34. Manganese— Total,4 mg/L. VerDate Sep<11>2014 DCP ............................................................. Ion Chromatography ................................... Digestion,4 followed by any of the following: 17:42 May 18, 2021 Jkt 253001 PO 00000 ................................... 200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... Frm 00019 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 27244 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 EPA 52 Standard methods 84 ASTM USGS/AOAC/other AA direct aspiration 36 ................................. AA furnace .................................................. STGFAA ...................................................... ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... 245.1, Rev. 3.0 (1994). 245.2 (Issued 1974) 1. 245.7 Rev. 2.0 (2005) 17. 1631E 43. 3111 B–2011 ............ 3113 B–2010 ............ D858–17 (A or B) ..... D858–17 (C). 974.27,3 I–3454–85.2 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... 3500–Mn B–2011 ..... ................................... 3112 B–2011 ............ D4190–15 ................. ................................... ................................... D3223–17 ................. 993.14,3 I–4472– 97.81 See footnote.34 920.203.3 See footnote.23 977.22,3 I–3462–85.2 ................................... ................................... I–4464–01.71 ................................... ................................... 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... 3111 D–2011 ............ 3113 B–2010 ............ 3120 B–2011 ............ ................................... ................................... D1976–12 ................. I–3490–85.2 I–3492–96.47 I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... ................................... 993.14,3 I–4472– 97.81 See footnote.34 ................................... 3111 B–2011 or 3111 C–2011. 3113 B–2010 ............ D1886–14 (A or B) ... I–3499–85 2 D1886–14 (C) ........... I–4503–89.51 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... 4110 B–2011 or C– 2011. D4190–15 ................. D4327–17 ................. 993.14,3 I–4020– 05 70 I–4472–97.81 See footnote.34 993.30.3 4140 B–2011 ............ 4500–NO3 D–2016. ................................... D6508–15 ................. D6508, Rev. 2.54 ................................... ................................... ................................... ................................... 973.50,3 419D1 thnsp;7, p. 28.9 Hach 10206 75 ................................... 4500–NO3–E–2016 .. D3867–16 (B). 353.2, Rev. 2.0 (1993). ................................... ................................... 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997). ................................... ................................... 4500–NO3–F–2016 4500–NO3–I–2016. 4500–NO3–H–2016. ................................... 4110 B–2011 or C– 2011. D3867–16 (A) ........... I–2545–90.51 ................................... D4327–17 ................. See footnote.62 993.30.3 4140 B–2011 ............ ................................... D6508–15 ................. D7781–14 ................. D6508, Rev. 2.54 I–2547–11.72 I–2548–11.72 N07–0003.73 Hach 10206.75 See footnote.25 I–4540–85,2 See footnote.62 I–2540– 90.80 I–4545–85.2 Parameter ICP/AES 36 ................................................... ICP/MS ........................................................ 35. Mercury—Total, mg/L. DCP 36 ......................................................... Colorimetric (Persulfate) ............................. Colorimetric (Periodate) .............................. Cold vapor, Manual ..................................... Cold vapor, Automated ............................... 36. Molybdenum— Total,4 mg/L. Cold vapor atomic fluorescence spectrometry (CVAFS). Purge and Trap CVAFS .............................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/AES ...................................................... ICP/MS ........................................................ 37. Nickel—Total,4 mg/L ............................. DCP ............................................................. Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA furnace .................................................. STGFAA ...................................................... ICP/AES 36 ................................................... ICP/MS ........................................................ 38. Nitrate (as N), mg/L DCP 36 ......................................................... Ion Chromatography ................................... CIE/UV ........................................................ Ion Selective Electrode ............................... Colorimetric (Brucine sulfate) ...................... 39. Nitrate-nitrite (as N), mg/L. Spectrophotometric (2,6-dimethylphenol) ... Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40). Cadmium reduction, Manual ....................... Cadmium reduction, Automated ................. Automated hydrazine .................................. Reduction/Colorimetric ................................ Ion Chromatography ................................... CIE/UV ........................................................ Enzymatic reduction, followed by automated colorimetric determination. khammond on DSKJM1Z7X2PROD with RULES2 40. Nitrite (as N), mg/L Enzymatic reduction, followed by manual colorimetric determination. Spectrophotometric (2,6-dimethylphenol) ... Spectrophotometric: Manual ....................... Automated (Diazotization) ........................... Automated (*bypass cadmium reduction) ... Manual (*bypass cadmium or enzymatic reduction). Ion Chromatography ................................... CIE/UV ........................................................ Automated (*bypass Enzymatic reduction) VerDate Sep<11>2014 ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997). ................................... ................................... 352.1 (Issued 1971) 1 19:30 May 18, 2021 Jkt 253001 PO 00000 ................................... 4500–NO3–J–2018. ................................... ................................... ................................... ................................... 4500–NO2–B–2011 .. ................................... ................................... ................................... ................................... 353.2, Rev. 2.0 (1993). ................................... 4500–NO3–F–2016 4500–NO3–I–2016. 4500–NO3– E–2016, 4500–NO3–J–2018. 4110 B–2011 or C– 2011. D3867–16 (A) ........... D4327–17 ................. 993.30.3 4140 B–2011 ............ ................................... D6508–15 ................. D7781–14 ................. D6508, Rev. 2.54 I–2547–11 72 I–2548– 11 72 N07–0003.73 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997). ................................... ................................... Frm 00020 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM D3867–16 (B). 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27245 TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 Parameter 41. Oil and grease— Total recoverable, mg/L. 42. Organic carbon— Total (TOC), mg/L. 43. Organic nitrogen (as N), mg/L. 44. Ortho-phosphate (as P), mg/L. EPA 52 Hexane extractable material (HEM): nHexane extraction and gravimetry. 1664 Rev. A; 1664 Rev. B 42. 5520 B–2011 38. Silica gel treated HEM (SGT–HEM): Silica gel treatment and gravimetry. Combustion ................................................. 1664 Rev. A; 1664 Rev. B 42. 5520 B–2011 38 and 5520 F–2011 38. 5310 B–2014 ............ Heated persulfate or UV persulfate oxidation. Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4). Ascorbic acid method: ................................... Automated ................................................... 47. Palladium—Total,4 mg/L. 48. Phenols, mg/L ....... 5310 C–2014 5310 D–2011. D4839–03(17) .......... 973.47,3, p. 14.24 365.1, Rev. 2.0 (1993). ................................... 365.3 (Issued 1978) 1. 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997). ................................... 4500–P F–2011 or G–2011. 4500–P E–2011 ....... ................................... D515–88 (A) ............. 973.56,3 I–4601–85,2 I–2601–90.80 973.55.3 4110 B–2011 or C– 2011. D4327–17 ................. 993.30.3 4140 B–2011 ............ D6508–15 ................. D6508, Rev. 2.54 3111 D–2011. Winkler (Azide modification) ....................... ................................... 252.2 (Issued 1978) 1. ................................... 4500–O (B–F)–2016 D888–12 (A) ............. Electrode ..................................................... Luminescence-Based Sensor ..................... ................................... ................................... 4500–O G–2016 ....... 4500–O H–2016 ....... D888–12 (B) ............. D888–12 (C) ............. 973.45B,3 I–1575– 78.8 I–1576–78.8 See footnote.63 See footnote.64 ................................... 253.2 (Issued 1978) 1. ................................... ................................... 420.1 (Rev. 1978) 1 .. 3111 B–2011. 420.1 (Rev. 1978) 1 .. 5530 D–2010 27 ........ D1783–01(12) (A or B). 420.4 Rev. 1.0 (1993). ................................... ................................... ................................... See footnote.28 ................................... 4500–P B (5)–2011 .. ................................... 973.55.3 365.3 (Issued 1978) 1 365.1 Rev. 2.0 (1993). 200.7, Rev. 4.4 (1994). 365.4 (Issued 1974) 1 4500–P E–2011 ....... 4500–P (F–H)–2011 D515–88 (A). ................................... 973.56,3 I–4600–85.2 3120 B–2011 ............ ................................... I–4471–97.50 ................................... D515–88 (B) ............. I–4610–91.48 ................................... ................................... ................................... NCASI TNTP W10900.77 ................................... 255.2 (Issued 1978) 1. ................................... ................................... 3111 B–2011. ................................... See footnote.34 3111 B–2011 ............ 3120 B–2011. ................................... 973.53,3 I–3630–85.2 3125 B–2011 ............ D5673–16 ................. 993.14.3 Flame photometric ...................................... Electrode ..................................................... Ion Chromatography ................................... Gravimetric, 103–105° ................................ ................................... 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... ................................... 3500–K B–2011. 3500–K C–2011. ................................... 2540 B–2015 ............ D6919–17. ................................... I–3750–85.2 Gravimetric, 180° ........................................ ................................... 2540 C–2015 ............ D5907–13 ................. I–1750–85.2 Gravimetric, 103–105° post-washing of residue. ................................... 2540 D–2015 ............ D5907–13 ................. I–3765–85.2 CIE/UV ........................................................ Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/MS ........................................................ DCP ............................................................. Manual distillation,26 followed by any of the following: Colorimetric (4AAP) manual ....................... Automated colorimetric (4AAP) ................... 49. Phosphorus (elemental), mg/L. 50. Phosphorus—Total, mg/L. Gas-liquid chromatography ......................... Digestion,20 followed by any of the following: Manual ......................................................... Automated ascorbic acid reduction ............. ICP/AES 4 36 ................................................ 51. Platinum—Total,4 mg/L. 52. Potassium—Total,4 mg/L. Semi-automated block digestor (TKP digestion). Digestion with persulfate, followed by Colorimetric. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/MS ........................................................ DCP ............................................................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... ICP/AES ...................................................... khammond on DSKJM1Z7X2PROD with RULES2 ICP/MS ........................................................ 53. Residue—Total, mg/L. 54. Residue—filterable, mg/L. 55. Residue—non-filterable (TSS), mg/L. VerDate Sep<11>2014 USGS/AOAC/other 973.47,3 p. 14.24 Ion Chromatography ................................... 46. Oxygen, dissolved, mg/L. ASTM D7573–09(17) ........... Manual, single-reagent ................................ Manual, two-reagent ................................... 45. Osmium—Total,4 mg/L. Standard methods 84 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00021 Fmt 4701 Sfmt 4700 3125 B–2011. ................................... 5530 B–2010 ............ 3125 B–2011. ................................... E:\FR\FM\19MYR2.SGM ................................... D1783–01(12). 19MYR2 See footnote.34 27246 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Methodology 58 EPA 52 Volumetric (Imhoff cone), or gravimetric ..... ................................... 2540 F–2015. Gravimetric, 550° ........................................ 160.4 (Issued 1971) 1 2540 E–2015 ............ ................................... 265.2 (Issued 1978) 1. ................................... 3111 B–2011. Parameter 56. Residue—settleable, ml/L. 57. Residue—Volatile, mg/L. 58. Rhodium—Total,4 mg/L. 59. Ruthenium—Total,4 mg/L. 60. Selenium—Total,4 mg/L. Digestion,4 followed by any of the following: AA direct aspiration, or ............................... AA furnace .................................................. ICP/MS ........................................................ Digestion,4 followed by any of the following: AA direct aspiration, or ............................... AA furnace .................................................. ICP/MS ........................................................ Digestion,4 followed by any of the following: AA furnace .................................................. STGFAA ...................................................... ICP/AES 36 ................................................... ICP/MS ........................................................ ................................... 267.2 1. ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). AA gaseous hydride .................................... 61. Silica—Dissolved,37 mg/L. 0.45-micron filtration followed by any of the following: Colorimetric, Manual ................................... Automated (Molybdosilicate) ....................... ICP/AES ...................................................... ICP/MS ........................................................ 62. Silver—Total,4 31 mg/L. ICP/AES ...................................................... ICP/MS ........................................................ DCP ............................................................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... ICP/AES ...................................................... ICP/MS ........................................................ 64. Specific conductance, micromhos/cm at 25 °C. 65. Sulfate (as SO4), mg/L. 200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). Digestion,4 thnsp;29 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. STGFAA ...................................................... 63. Sodium—Total,4 mg/L. ................................... ................................... DCP ............................................................. Flame photometric ...................................... Ion Chromatography ................................... Wheatstone bridge ...................................... Automated colorimetric ............................... ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... ................................... 120.1 (Rev. 1982) 1 .. 375.2, Rev. 2.0 (1993). Gravimetric .................................................. khammond on DSKJM1Z7X2PROD with RULES2 Turbidimetric ................................................ Ion Chromatography ................................... 66. Sulfide (as S), mg/L 67. Sulfite (as SO3), mg/L. 68. Surfactants, mg/L .. VerDate Sep<11>2014 Standard methods 84 I–3753–85.2 3113 B–2010 ............ D3859–15 (B) ........... I–4668–98.49 3120 B–2011 ............ D1976–12. 3125 B–2011 ............ D5673–16 ................. 3114 B–2011, or 3114 C–2011. D3859–15 (A) ........... 993.14,3 I–4020– 05 70 I–4472–97.81 I–3667–85.2 4500-SiO2 C–2011 ... 4500–SiO2 E–2011 or F–2011. 3120 B–2011 ............ D859–16 ................... ................................... I–1700–85.2 I–2700–85.2 ................................... I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 3111 B–2011 or 3111 C–2011. 3113 B–2010 ............ ................................... ................................... 974.27,3 p. 37,9 I– 3720–85.2 I–4724–89.51 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... ................................... 993.14,3 I–4472– 97.81 See footnote.34 3111 B–2011 ............ 3120 B–2011 ............ ................................... ................................... 973.54,3 I–3735–85.2 I–4471–97.50 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... 3500–Na B–2011. ................................... 2510 B–2011 ............ ................................... See footnote.34 D6919–17. D1125–95(99) (A) ..... 973.40,3 I–2781–85.2 3125 B–2011. 3111 B–2011. 3125 B–2011. 4500–SO42 F–2011 or G–2011. 4500–SO42–C–2011 or D–2011. 4500–SO42–E–2011 4110 B–2011 or C– 2011. CIE/UV ........................................................ Sample Pretreatment .................................. Titrimetric (iodine) ....................................... Colorimetric (methylene blue) ..................... Ion Selective Electrode ............................... Titrimetric (iodine-iodate) ............................ ................................... ................................... ................................... ................................... 4140 B–2011 ............ 4500–S2¥ B, C– 2011. 4500–S–F–2011 ....... 4500–S2¥ D–2011. 4500–S–G–2011 ...... 4500–SO32–B–2011. Colorimetric (methylene blue) ..................... ................................... 5540 C–2011 ............ Jkt 253001 PO 00000 Frm 00022 Fmt 4701 Sfmt 4700 USGS/AOAC/other ................................... ................................... 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997). ................................... ................................... 19:30 May 18, 2021 ASTM E:\FR\FM\19MYR2.SGM 925.54.3 D516–16. D4327–17 ................. 993, I–4020– 05 70.303 D6508–15 ................. D6508, Rev. 2.54 ................................... I–3840–85.2 D4658–15. D2330–02. 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27247 TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued Parameter Methodology 58 EPA 52 Standard methods 84 ASTM 69. Temperature, °C .... 70. Thallium-Total,4 mg/L. Thermometric .............................................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. STGFAA ...................................................... ................................... 2550 B–2010 ............ ................................... ................................... 279.2 (Issued 1978) 1 200.9, Rev. 2.2 (1994). 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). 3111 B–2011. 3113 B–2010. ICP/AES ...................................................... ICP/MS ........................................................ 71. Tin-Total,4 mg/L ..... Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. STGFAA ...................................................... ICP/AES ...................................................... ICP/MS ........................................................ 72. Titanium-Total,4 mg/L. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/AES ...................................................... ICP/MS ........................................................ 73. Turbidity, NTU 53 ... 74. Vanadium-Total,4 mg/L. DCP ............................................................. Nephelometric ............................................. Digestion,4 followed by any of the following: AA direct aspiration ..................................... AA furnace .................................................. ICP/AES ...................................................... ICP/MS ........................................................ 75. Zinc-Total,4 mg/L ... DCP ............................................................. Colorimetric (Gallic Acid) ............................ Digestion,4 followed by any of the following: AA direct aspiration 36 ................................. AA furnace .................................................. ICP/AES 36 ................................................... ICP/MS ........................................................ khammond on DSKJM1Z7X2PROD with RULES2 76. Acid Mine Drainage DCP 36 ......................................................... Colorimetric (Zincon) ................................... ...................................................................... USGS/AOAC/other See footnote.32 3120 B–2011 ............ D1976–12. 3125 B–2011 ............ D5673–16 ................. 993.14,3 I–4471– 97 50 I–4472–97.81 ................................... ................................... 200.9, Rev. 2.2 (1994). 200.5, Rev. 4.2 (2003) 68; 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). 3111 B–2011 ............ 3113 B–2010. ................................... I–3850–78.8 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... 283.2 (Issued 1978) 1. 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... 180.1, Rev. 2.0 (1993). 3111 D–2011. 3125 B–2011 ............ D5673–16 ................. 993.14.3 ................................... 2130 B–2011 ............ ................................... D1889–00 ................. See footnote.34 I–3860–852 See footnote.65 See footnote.66 See footnote.67 ................................... ................................... 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... 3111 D–2011. 3113 B–2010 ............ 3120 B–2011 ............ D3373–17. D1976–12 ................. 3125 B–2011 ............ D5673–16 ................. ................................... 3500–V B–2011. D4190–15 ................. 3111 B–2011 or 3111 C–2011. D1691–17 (A or B) ... 974.27,3 p. 37,9 I– 3900–85.2 3120 B–2011 ............ D1976–12 ................. I–4471–97.50 3125 B–2011 ............ D5673–16 ................. ................................... 3500 Zn B–2011 ....... D4190–15 ................. ................................... 993.14,3 I–4020– 05 70 I–4472–97.81 See footnote.34 See footnote.33 ................................... 289.2 (Issued 1978) 1. 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994). 200.8, Rev. 5.4 (1994). ................................... ................................... 1627 69. I–4471–97 50 993.14,3 I–4020– 05.70 See footnote.34 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 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. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00023 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 27248 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 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 ) must not be confused with the traditional BOD test method which measures ‘‘total 5-day BOD.’’ The addi5 5 tion of the nitrification inhibitor is not a procedural option but must be included to report the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger’s permit specifically states CBOD5 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 Chromatography, 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 Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory. 30 The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method-specified quality control acceptance criteria are met. 31 For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water. 32 ‘‘Water Temperature-Influential Factors, Field Measurement and Data Presentation,’’ Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1. 1975. USGS. 33 Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company. 34 Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised 1991. Thermo Jarrell Ash Corporation. 35 In-Situ Method 1004–8–2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated. 36 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. CEM Corporation 37 When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. 38 Only use n-hexane (n-Hexane—85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of other extraction solvents is prohibited. 39 Method PAI–DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical. 40 Method PAI–DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical. 41 Method PAI–DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical. 42 Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT–HEM; Non-polar Material) by Extraction and Gravimetry. EPA–821–R–98–002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT–HEM; Non-polar Material) by Extraction and Gravimetry. EPA–821–R–10–001. 43 Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA–821–R–02–019. Revision E. August 2002, U.S. EPA. The application of clean techniques described in EPA’s Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels, EPA–821–R–96–011, are recommended to preclude contamination at low-level, trace metal determinations. 44 Method OIA–1677–09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical. 45 Open File Report 00–170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS. 46 Open File Report 93–449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS. 47 Open File Report 97–198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS. 48 Open File Report 92–146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS. 49 Open File Report 98–639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS. 50 Open File Report 98–165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS. 51 Open File Report 93–125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS. 52 Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in U.S. EPA. May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, EPA/600/R–94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in Environmental Samples, EPA/600/R–93/100. EPA Method 300.1 is U.S. EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography. 53 Styrene divinyl benzene beads (e.g., AMCO–AEPA–1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin. 54 Method D6508–15, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. 2015. ASTM VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00024 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27249 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. U.S. 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 335.4–1, reconstitute particulate that is filtered with the sample prior to distillation. 58 Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ‘‘followed by’’ analysis with a method, approved digestion and/or distillation are required prior to analysis. 59 Samples analyzed for available cyanide using OI Analytical method OIA–1677–09 or ASTM method D6888–16 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 and CBOD . Revi5 5 sion 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD). 64 In-Situ Method 1002–8–2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated. 65 Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell. 66 Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell. 67 Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific. 68 EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/600/ R–06/115. Revision 4.2, October 2003. U.S. EPA. 69 Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA–821–R–09–002. December 2011. U.S. 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 U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. A11989, Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, 1989. 80 Methods I–2522–90, I–2540–90, and I–2601–90 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–1472–97, 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 Instruments, Inc. Method 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 (2017); Part 3000 Methods, Metals, 3020 (2017); Part 4000 Methods, Inorganic Nonmetallic Constituents, 4020 (2014); Part 5000 Methods, and Aggregate Organic Constituents, 5020 (2017). 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 BOD5. 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%. • Any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L. TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS Parameter 1 Method EPA 2 7 1. Acenaphthene ................................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. Spectrophotometric .................... GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... 603. 624.1,4 1624B. 603. 624.1,4 1624B ...... 610. 625.1, 1625B ........ 610 ....................... 602 ....................... 624.1, 1624B ........ ............................... 2. Acenaphthylene ............................... 3. Acrolein ............................................ 4. Acrylonitrile ...................................... khammond on DSKJM1Z7X2PROD with RULES2 5. Anthracene ...................................... 6. Benzene .......................................... 7. Benzidine ......................................... 8. Benzo(a)anthracene ........................ VerDate Sep<11>2014 19:30 May 18, 2021 Jkt 253001 PO 00000 625.1,5 1625B ...... 605. 610. 625.1, 1625B ........ 610 ....................... Frm 00025 Fmt 4701 Standard methods ASTM 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. ............................... ............................... O–4127–96. 13 6410 B–2000 ........ 6440 B–2005 ........ 6200 C–2011. 6200 B–2011 ........ ............................... ............................... D4657–92 (98). See footnote 9, p. 27. ............................... ............................... O–4127–96 13, O–4436–16.14 See footnote 3, p.1. ............................... D4657–92 (98). See footnote 9, p. 27. Other 6410 B–2000. 6410 B–2000 ........ 6440 B–2005 ........ Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 27250 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued ASTM 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... ............................... ............................... D4657–92 (98). ............................... ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 6200 6200 6200 6200 6200 6200 B–2000 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ ............................... See footnote 9, p. 27. ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 6410 6200 6200 6420 6410 6200 6200 6200 6200 B–2000 ........ C–2011 ........ B–2011 ........ B–2000. B–2000 ........ C–2011 ........ B–2011 ........ C–2011. B–2011 ........ ............................... ............................... ............................... See footnote 9, p. 27. See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... ............................... ............................... See footnote 9, p. 27. See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... O–4127–96.13 6200 6200 6200 6200 C–2011 ........ B–2011 ........ C–2011. B–2011 ........ ............................... ............................... See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 6410 B–2000 ........ 6420 B–2000. 6410 B–2000 ........ ............................... See footnote 9, p. 27. ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 6440 6200 6200 6200 6200 B–2000 ........ B–2005 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ ............................... D4657–92 (98). See footnote 9, p. 27. ............................... O–4127–96 13, O–4436–16.14 ............................... See footnote, 9 p. 27; O–4127–96,13 O–4436–16.14 601, 602 ............... 624.1, 1625B ........ 601, 602 ............... 624.1, 1625B ........ 6200 6200 6200 6200 C–2011. B–2011 ........ C–2011. B–2011 ........ ............................... See footnote 9, p. 27; O–4127–96.13 ............................... See footnote,9 p. 27; O–4127–96,13 O–4436–16.14 625.1, 1625B ........ 605. 601. ............................... 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 604 ....................... 625.1, 1625B ........ 6410 B–2000. ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... See footnote 9, p. 27. Method EPA 2 7 9. Benzo(a)pyrene ............................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... ............................... ............................... 606. 625.1, 1625B ........ 611. 625.1, 1625B ........ 611. 625.1, 1625B ........ 606. 625.1, 1625B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 611. 625.1, 1625B ........ 601 ....................... 624.1, 1624B ........ 604 ....................... 625.1, 1625B ........ 601, 602 ............... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601. 624.1, 1624B. 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 612. 625.1, 1625B ........ 604 ....................... 625.1, 1625B ........ 611. 625.1, 1625B ........ 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... 601 ....................... 624.1, 1624B ........ 601, 602 ............... 624.1, 1625B ........ GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. 10. Benzo(b)fluoranthene .................... 11. Benzo(g,h,i)perylene ..................... 12. Benzo(k)fluoranthene .................... 13. Benzyl chloride .............................. 14. Butyl benzyl phthalate ................... 15. bis(2-Chloroethoxy) methane ........ 16. bis(2-Chloroethyl) ether ................. 17. bis(2-Ethylhexyl) phthalate ............ 18. Bromodichloromethane ................. 19. Bromoform ..................................... 20. Bromomethane .............................. 21. 4-Bromophenyl phenyl ether ......... 22. Carbon tetrachloride ...................... 23. 4-Chloro-3-methyl phenol .............. 24. Chlorobenzene .............................. 25. Chloroethane ................................. 26. 2-Chloroethylvinyl ether ................. 27. Chloroform ..................................... 28. Chloromethane .............................. 29. 2-Chloronaphthalene ..................... 30. 2-Chlorophenol .............................. 31. 4-Chlorophenyl phenyl ether ......... 32. Chrysene ....................................... 33. Dibenzo(a,h)anthracene ................ 34. Dibromochloromethane ................. 35. 1,2-Dichlorobenzene ..................... 36. 1,3-Dichlorobenzene ..................... 37. 1,4-Dichlorobenzene ..................... 38. 3,3′-Dichlorobenzidine ................... 39. Dichlorodifluoromethane ................ khammond on DSKJM1Z7X2PROD with RULES2 Standard methods Parameter 1 40. 1,1-Dichloroethane ........................ 41. 1,2-Dichloroethane ........................ 42. 1,1-Dichloroethene ........................ 43. trans-1,2-Dichloroethene ............... 44. 2,4-Dichlorophenol ........................ VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00026 Fmt 4701 6200 6200 6200 6200 6200 6200 6200 6200 6200 6420 6410 C–2011 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ B–2000.. B–2000 ........ Sfmt 4700 E:\FR\FM\19MYR2.SGM Other See footnote 3, p. 130. See footnote 6, p. S102. 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27251 TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued Parameter 1 Method EPA 2 7 45. 1,2-Dichloropropane ...................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC/MS .................. 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 606. 625.1, 1625B ........ 604 ....................... 625.1, 1625B ........ 606. 625.1, 1625B ........ 606. 625.1, 1625B ........ 606. 625.1, 1625B ........ 604 ....................... 625.1, 1625B ........ 609. 625.1, 1625B ........ 609. 625.1, 1625B ........ ............................... ............................... 602 ....................... 624.1, 1624B ........ 610. 625.1, 1625B ........ 610 ....................... 610. 625.1, 1625B ........ 610 ....................... 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC/MS .................. 612. 625.1, 1625B ........ 612. 625.1, 1625B ........ 612. 625.1,5 1625B ...... 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC/MS .................. 1613B. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ 612. 625.1, 1625B ........ 610. 625.1, 1625B ........ 610 ....................... 609. 625.1, 1625B ........ 601 ....................... 624.1, 1624B ........ 604 ....................... 625.1, 1625B ........ 610. 625.1, 1625B ........ 610 ....................... 609. 625.1, 1625B ........ ............................... 604 ....................... 625.1, 1625B ........ 604 ....................... 625.1, 1625B ........ 607. 46. cis-1,3-Dichloropropene ................ 47. trans-1,3-Dichloropropene ............. 48. Diethyl phthalate ............................ 49. 2,4-Dimethylphenol ........................ 50. Dimethyl phthalate ......................... 51. Di-n-butyl phthalate ....................... 52. Di-n-octyl phthalate ....................... 53. 2, 4-Dinitrophenol .......................... 54. 2,4-Dinitrotoluene .......................... 55. 2,6-Dinitrotoluene .......................... 56. Epichlorohydrin .............................. 57. Ethylbenzene ................................. 58. Fluoranthene ................................. 59. Fluorene ........................................ 60. 1,2,3,4,6,7,8-Heptachlorodibenzofuran. 61. 1,2,3,4,7,8,9-Heptachlorodibenzofuran. 62. 1,2,3,4,6,7,8-Heptachloro-dibenzop-dioxin. 63. Hexachlorobenzene ....................... 64. Hexachlorobutadiene ..................... 65. Hexachlorocyclopentadiene .......... 66. 1,2,3,4,7,8-Hexachlorodibenzofuran. 67. 1,2,3,6,7,8-Hexachlorodibenzofuran. 68. 1,2,3,7,8,9-Hexachlorodibenzofuran. 69. 2,3,4,6,7,8-Hexachlorodibenzofuran. 70. 1,2,3,4,7,8-Hexachloro-dibenzo-pdioxin. 71. 1,2,3,6,7,8-Hexachloro-dibenzo-pdioxin. 72. 1,2,3,7,8,9-Hexachloro-dibenzo-pdioxin. 73. Hexachloroethane ......................... 74. Indeno(1,2,3-c,d) pyrene ............... 75. Isophorone ..................................... 76. Methylene chloride ........................ 77. 2-Methyl-4,6-dinitrophenol ............. khammond on DSKJM1Z7X2PROD with RULES2 78. Naphthalene .................................. 79. Nitrobenzene ................................. 80. 2-Nitrophenol ................................. 81. 4-Nitrophenol ................................. 82. N-Nitrosodimethylamine ................ VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00027 Fmt 4701 Standard methods 6200 6200 6200 6200 6200 6200 C–2011. B–2011 ........ C–2011. B–2011 ........ C–2011. B–2011 ........ ASTM Other ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 6410 B–2000 ........ 6420 B–2000. 6410 B–2000 ........ ............................... See footnote 9, p. 27. ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote,9, p. 27. 6410 B–2000 ........ 6420 B–2000 ........ 6410 B–2000. ............................... ............................... See footnote,9 p. 27. See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... ............................... 6200 C–2011. 6200 B–2011 ........ ............................... ............................... ............................... See footnote 9, p. 27. See footnote 3, p. 130. See footnote 6, p. S102. ............................... O–4127–96,13 O–4436–16.14 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... See footnote,9 p. 27; O–4127–96.13 6410 B–2000 ........ ............................... See footnote,9 p. 27; O–4127–96.13 6410 B–2000 ........ ............................... See footnote 9, p. 27; O–4127–96.13 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. 6410 6200 6200 6420 6410 B–2000 ........ C–2011 ........ B–2011 ........ B–2000. B–2000 ........ ............................... ............................... ............................... See footnote 9, p. 27. See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005. ............................... See footnote 9, p. 27. 6410 B–2000 ........ ............................... 6420 B–2000. 6410 B–2000 ........ 6420 B–2000. 6410 B–2000 ........ ............................... D4657–92 (98). See footnote 9, p. 27. ............................... See footnote 9, p. 27. ............................... See footnote 9, p. 27. Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 27252 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued Parameter 1 83. N-Nitrosodi-n-propylamine ............. 84. N-Nitrosodiphenylamine ................ 85. Octachlorodibenzofuran ................ 86. Octachlorodibenzo-p-dioxin ........... 87. 2,2′-oxybis(1-chloropropane) 12 [also known as bis(2-Chloro-1methylethyl) ether]. 88. PCB–1016 ..................................... 89. PCB–1221 ..................................... 90. PCB–1232 ..................................... 91. PCB–1242 ..................................... 92. PCB–1248 ..................................... 93. PCB–1254 ..................................... 94. PCB–1260 ..................................... 95. 1,2,3,7,8-Pentachlorodibenzofuran. 96. 2,3,4,7,8-Pentachlorodibenzofuran. 97. 1,2,3,7,8-Pentachloro-dibenzo-pdioxin. 98. Pentachlorophenol ......................... 99. Phenanthrene ................................ 100. Phenol ......................................... 101. Pyrene ......................................... 102. 2,3,7,8-Tetrachloro-dibenzofuran 103. 2,3,7,8-Tetrachloro-dibenzo-pdioxin. 104. 1,1,2,2-Tetrachloroethane ........... 105. Tetrachloroethene ....................... 106. Toluene ........................................ 107. 1,2,4-Trichlorobenzene ................ 108. 1,1,1-Trichloroethane .................. 109. 1,1,2-Trichloroethane .................. 110. Trichloroethene ............................ 111. Trichlorofluoromethane ................ 112. 2,4,6-Trichlorophenol ................... khammond on DSKJM1Z7X2PROD with RULES2 113. Vinyl chloride ............................... 114. Nonylphenol ................................. 115. Bisphenol A (BPA) ...................... 116. p-tert-Octylphenol (OP) ............... 117. Nonylphenol Monoethoxylate (NP1EO). 118. Nonylphenol Diethoxylate (NP2EO). 119. Adsorbable Organic Halides (AOX). 120. Chlorinated Phenolics ................. Method EPA 2 7 Standard methods ASTM GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC/MS .................. GC/MS .................. GC ........................ 625.1,5 1625B ...... 607. 625.1,5 1625B ...... 607. 625.1,5 1625B ...... 1613B.10 1613B.10 611. 6410 B–2000 ........ ............................... See footnote,9 p. 27. 6410 B–2000 ........ ............................... See footnote,9 p. 27. 6410 B–2000 ........ ............................... See footnote,9 p. 27. GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC/MS .................. 625.1, 1625B ........ 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 608.3 .................... 625.1 .................... 1613B. 6410 B–2000 ........ ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... 6410 B–2000. ............................... ............................... See footnote 9, p. 27. See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 ............................... See footnote 3, p. 43; See footnote.8 GC/MS .................. 1613B. GC/MS .................. 1613B. GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC ........................ GC/MS .................. GC ........................ GC/MS .................. HPLC .................... GC/MS .................. GC/MS .................. 6420 B–2000 ........ 6410 B–2000 ........ ............................... ............................... See footnote 3, p. 140. See footnote 9, p. 27. 6410 6440 6420 6410 B–2000 ........ B–2005 ........ B–2000. B–2000 ........ ............................... D4657–92 (98). See footnote 9, p. 27. ............................... See footnote 9, p. 27. 6410 B–2000 ........ 6440 B–2005 ........ ............................... D4657–92 (98). See footnote 9, p. 27. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. 604 ....................... 625.1, 1625B ........ 610. 625.1, 1625B ........ 610 ....................... 604 ....................... 625.1, 1625B ........ 610. 625.1, 1625B ........ 610 ....................... 1613B.10 613, 625.1,5a 1613B. 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 602 ....................... 624.1, 1624B ........ 612 ....................... 625.1, 1625B ........ 6200 C–2011 ........ 6200 B–2011 ........ 6200 C–2011 ........ 6200 B–2011 ........ 6200 C–2011. 6200 B–2011 ........ ............................... 6410 B–2000 ........ ............................... ............................... ............................... ............................... See footnote 3, p. 130. O–4127–96.13 See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... ............................... ............................... O–4127–96 13, O–4436–16.14 See footnote 3, p. 130. See footnote,9 p. 27; O–4127–96,13 O–4436–16.14 GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC ........................ GC/MS .................. GC/MS .................. GC/MS .................. GC/MS .................. GC/MS .................. 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1, 1624B ........ 601 ....................... 624.1 .................... 604 ....................... 625.1, 1625B ........ 601 ....................... 624.1, 1624B ........ ............................... ............................... ............................... ............................... 6200 C–2011. 6200 B–2011 ........ 6200 C–2011 ........ 6200 B–2011 ........ 6200 C–2011. 6200 B–2011 ........ 6200 C–2011. 6200 B–2011 ........ 6420 B–2000. 6410 B–2000 ........ 6200 C–2011. 6200 B–2011 ........ ............................... ............................... ............................... ............................... ............................... ............................... ............................... O–4127–96 13, O–4436–16.14 See footnote 3, p. 130. O–4127–96 13, O–4436–16.14 ............................... O–4127–96 13, O–4436–16.14 ............................... O–4127–96.13 ............................... See footnote 9, p. 27. ............................... D7065–17. D7065–17. D7065–17. D7065–17. O–4127–96 13, O–4436–16.14 GC/MS .................. ............................... ............................... D7065–17. Adsorption and Coulometric Titration. In Situ Acetylation and GC/MS. 1650.11 Other 1653.11 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). VerDate Sep<11>2014 19:30 May 18, 2021 Jkt 253001 PO 00000 Frm 00028 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27253 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. 5a Method 625.1 screening only. 6 Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA). 7 Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601–603, 1624B, and 1625B in accordance with procedures in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624.1 and 625.1 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the quality control (QC) acceptance criteria in the pertinent method, analytical results for that parameter in the unspiked sample are suspect. The results should be reported but cannot be used to demonstrate regulatory compliance. If the method does not contain QC acceptance criteria, control limits of ± three standard deviations around the mean of a minimum of five replicate measurements must be used. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited. 8 Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk. Revised October 28, 1994. 3M Corporation. 9 Method O–3116–87 is in Open File Report 93–125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS. 10 Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in appendix A to this part and at https://www.epa.gov/cwa-methods/approved-cwa-test-methods-organic-compounds. 11 Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997 U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS. Revision A, 1997 U.S. EPA. The full text for both of these methods is provided at appendix A in part 430 of this chapter, The Pulp, Paper, and Paperboard Point Source Category. 12 The compound was formerly inaccurately labeled as 2,2′-oxybis(2-chloropropane) and bis(2-chloroisopropyl) ether. Some versions of Methods 611, and 1625 inaccurately list the analyte as ‘‘bis(2-chloroisopropyl)ether,’’ but use the correct CAS number of 108–60–1. 13 Method O–4127–96, U.S. Geological Survey Open-File Report 97–829, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory— Determination of 86 volatile organic compounds in water by gas chromatography/mass spectrometry, including detections less than reporting limits,1998, USGS. 14 Method O–4436–16 U.S. Geological Survey Techniques and Methods, book 5, chap. B12, Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry, 2016, USGS. * * * * * TABLE IH—LIST OF APPROVED MICROBIOLOGICAL METHODS FOR AMBIENT WATER Method 1 Parameter and units EPA Standard methods AOAC, ASTM, USGS Other Bacteria 1. Coliform (fecal), number per 100 mL. Most Probable Number (MPN), 5 tube, 3 dilution, or. Membrane filter (MF) 2, single step ............. MPN, 5 tube, 3 dilution, or .......................... MF 2, single step or two step ...................... MF 2 with enrichment ................................... MPN 5 7 13, multiple tube, or ........................ p. ..................... p. 114 3 ..................... 3 p. 108 ..................... p. 111 3 ..................... ................................... Multiple tube/multiple well, or ...................... ................................... MF 2 5 6 7, two step, or ................................. 1103.1 18 ................... Single step .................................................. 1603 19, 1604 20 ........ MPN, 5 tube, 3 dilution, or .......................... MF 2, or ........................................................ Plate count .................................................. MPN 5 7, multiple tube/multiple well, or ....... MF 2 5 6 7 two step, or .................................. Single step, or ............................................. Plate count .................................................. p. 139 3 ..................... p. 136 3 ..................... p. 143 3. ................................... 1106.1 22. 1600 23 ...................... p. 143 3. 6. Cryptosporidium ...... Filtration/IMS/FA .......................................... 1622 24, 7. Giardia ..................... Filtration/IMS/FA .......................................... 2. Coliform (total), number per 100 mL. 3. E. coli, number per 100 mL. 4. Fecal streptococci, number per 100 mL. 5. Enterococci, number per 100 mL. p. 132 3 ..................... 124 3 9221 E–2014, 9221 F–2014 32. 9222 D–2015 26 ........ 9221 B–2014 ............ 9222 B–2015 27 ........ 9222 B– 2015 27. 9221 B.3–2014/9221 F–2014 10 12 32. 9223 B–2016 11 ........ B–0050–85 4. B–0025–85 4. 991.15 9 .................... 9222 B–2015/9222 I– 2015 17, 9213 D– 2007. ................................... D5392–93 8. 9230 B–2013 ............ 9230 C–2013 30 ........ B–0055–85 4. 9230 D–2013 ............ 9230 C–2013 30 ........ 9230 C–2013 30. D6503–99 8 ............... D5259–92 8 ............... ................................... Colilert® 11 15, Colilert-18®.11 14 15 m-ColiBlue24® 16, KwikCountTM EC. 28 29 Enterolert®.11 21 khammond on DSKJM1Z7X2PROD with RULES2 Protozoa 1623 25, 1623.1 25 31. 1623 25, 1623.1 25 31. 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. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00029 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 27254 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations khammond on DSKJM1Z7X2PROD with RULES2 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 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA–821–R–10–002. March 2010. US EPA. 19 Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified mTEC), EPA– 821–R–14–010. September 2014. 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 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE–EIA), EPA–821–R–09–015. December 2009. US EPA. 23 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b-D-Glucoside Agar (mEI), EPA–821–R–14–011. September 2014. 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 KwikCountTM EC may be obtained from Micrology Laboratories 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) Certain material 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 material may be inspected at EPA’s Water Docket, EPA West, 1301 Constitution Avenue NW, Room 3334, Washington, DC 20004, (Telephone: 202–566–2426). It is also available for inspection at National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202–741–6030, or go to: https:// www.archives.gov/federal-register/cfr/ ibr-locations.html. * * * * * (8) Office of Water, U.S. Environmental Protection Agency, Washington, DC (U.S. EPA). Available at https://www.epa.gov/cwa-methods. * * * * * (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, Note 25. (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 VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 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 MultipleTube 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 MultipleTube 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 PO 00000 Frm 00030 Fmt 4701 Sfmt 4700 (MSRV) Medium. September 2014. EPA 821–R–14–012. Table IA, Note 23. * * * * * (10) * * * (xiv) 2540, solids. 2015. Table IB. * * * * * (xxxix) 4500–CN¥, Cyanide. 2016. Table IB. * * * * * (xliv) 4500–NO3¥, Nitrogen (Nitrate). 2016. Table IB. * * * * * (xlvi) 4500–O, Oxygen (Dissolved). 2016. Table IB. * * * * * (lii) 5210, Biochemical Oxygen Demand (BOD). 2016. Table IB. * * * * * (liv) 5310, Total Organic Carbon (TOC). 2014. Table IB. * * * * * (lxvii) 9221 Multiple-Tube Fermentation Technique for Members of the Coliform Group. 2014. Table IA, Notes 12 and 14; Table IH, Notes 10 and 12. (lxviii) 9222, Membrane Filter Technique for Members of the Coliform Group. 2015. Table IA; Table IH, Note 17. E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations (lxix) 9223 Enzyme Substrate Coliform Test. 2016. Table IA; Table IH. (lxx) 9230 Fecal Enterococcus/ Streptococcus Groups. 2013. Table IA; Table IH. * * * * * (15) * * * (v) ASTM D511–14, Standard Test Methods for Calcium and Magnesium in Water. November 2014. Table IB. (vi) ASTM D512–12, Standard Test Methods for Chloride Ion in Water. July 2012. Table IB. * * * * * (viii) ASTM D516–16, Standard Test Method for Sulfate Ion in Water, June 2016. Table IB. (ix) ASTM D858–17, Standard Test Methods for Manganese in Water. June 2017. Table IB. (x) ASTM D859–16, Standard Test Method for Silica in Water. June 2016. Table IB. (xi) ASTM D888–12, Standard Test Methods for Dissolved Oxygen in Water. March 2012. Table IB. (xii) ASTM D1067–16, Standard Test Methods for Acidity or Alkalinity of Water. June 2016. Table IB. (xiii) ASTM D1068–15, Standard Test Methods for Iron in Water. October 2015. Table IB. * * * * * (xv) ASTM D1126–17, Standard Test Method for Hardness in Water. December 2017. Table IB. (xvi) ASTM D1179–16, Standard Test Methods for Fluoride Ion in Water. June 2016. Table IB. (xvii) ASTM D1246–16, Standard Test Method for Bromide Ion in Water. June 2016. Table IB. (xviii) ASTM D1252–06 (Reapproved 2012), Standard Test Methods for Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water. June 2012. Table IB. (xix) ASTM D1253–14, Standard Test Method for Residual Chlorine in Water. February 2014. Table IB. * * * * * (xxi) ASTM D1426–15, Standard Test Methods for Ammonia Nitrogen in Water. April 2015. Table IB. (xxii) ASTM D1687–17, Standard Test Methods for Chromium in Water. July 2017. Table IB. (xxiii) ASTM D1688–17, Standard Test Methods for Copper in Water. July 2017. Table IB. (xxiv) ASTM D1691–17, Standard Test Methods for Zinc in Water. June 2017. Table IB. (xxv) ASTM D1783–01 (Reapproved 2012), Standard Test Methods for Phenolic Compounds in Water. August 2012. Table IB. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 (xxvi) ASTM D1886–14, Standard Test Methods for Nickel in Water. November 2014. Table IB. * * * * * (xxxi) ASTM D2036–09 (Reapproved 2015), Standard Test Methods for Cyanides in Water. July 2015. Table IB. * * * * * (xxxiv) ASTM D2972–15, Standard Tests Method for Arsenic in Water. March 2015. Table IB. (xxxv) ASTM D3223–17, Standard Test Method for Total Mercury in Water. June 2017. Table IB. * * * * * (xxxvii) ASTM D3373–17, Standard Test Method for Vanadium in Water. June 2017. Table IB. * * * * * (xxxix) ASTM D3557–17, Standard Test Method for Cadmium in Water. June 2017. Table IB. (xl) ASTM D3558–15, Standard Test Method for Cobalt in Water. March 2015. Table IB. (xli) ASTM D3559–15, Standard Test Methods for Lead in Water. October 2015. Table IB. (xlii) ASTM D3590–17, Standard Test Methods for Total Kjeldahl Nitrogen in Water. June 2017. Table IB. (xliii) ASTM D3645–15, Standard Test Methods for Beryllium in Water. March 2015. Table IB. * * * * * (xlv) ASTM D3859–15, Standard Test Methods for Selenium in Water. April 2015. Table IB. (xlvi) ASTM D3867–16, Standard Test Method for Nitrite-Nitrate in Water. June 2016. Table IB. (xlvii) ASTM D4190–15, Standard Test Method for Elements in Water by Direct- Current Plasma Atomic Emission Spectroscopy. March 2015. Table IB. (xlviii) ASTM D4282–15, Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion. July 2015. Table IB. (xlix) ASTM D4327–17, Standard Test Method for Anions in Water by Suppressed Ion Chromatography. December 2017. Table IB. (l) ASTM D4382–18, Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace. May 2018. Table IB. * * * * * (lii) ASTM D4658–15, Standard Test Method for Sulfide Ion in Water. April 2015. Table IB. * * * * * (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. December 2017. Table IB. PO 00000 Frm 00031 Fmt 4701 Sfmt 4700 27255 (lv) ASTM D5257–17, Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography. December 2017. Table IB. * * * * * (lviii) ASTM D5673–16, Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry. February 2016. Table IB. * * * * * (lxi) ASTM. D6508–15, Standard Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. October 2015. Table IB, Note 54. (lxii) ASTM. D6888–16, Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. June 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. June 2017. Table IB. (lxiv) ASTM. D7065–17, Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tertOctylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry. January 2018. Table IC. (lxv) ASTM. D7237–15a, Standard Test Method for Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. June 2015. Table IB. (lxvi) ASTM. D7284–13 (Reapproved 2017), Standard Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas Diffusion Separation and Amperometric Detection. July 2017. Table IB. * * * * * (lxviii) ASTM. D7511–12 (Reapproved 2017), Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection. July 2017. Table IB. (lxix) ASTM. D7573–09 (Reapproved 2017), Standard Test Method for Total Carbon and Organic Carbon in Water by High Temperature Catalytic Combustion and Infrared Detection, February 2017. Table IB. (lxx) ASTM D7781–14 Standard Test Method for Nitrate-Nitrite in Water by Nitrate Reductase, May 2014. Table IB. * * * * * E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 27256 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations (19) FIAlab Instruments, Inc., 2151 N. Northlake Way, Seattle, WA 98103. Telephone: 425–376–0450. (i) Method 100, Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector Analysis, April 4, 2018. Table IB, Note 82. (ii) [Reserved] * * * * * (26) MACHEREY-NAGEL GmbH and Co., 2850 Emrick Blvd. Bethlehem, PA 18020. Telephone: 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, 1303 Eisenhower Drive, Goshen, IN 46526. Telephone: 574–533–3351. (i) KwikCountTM EC Medium E. coli enzyme substrate test, Rapid Detection of E. coli in Beach Water By KwikCountTM EC Membrane Filtration. 2014. Table IH, Notes 28 and 29. (ii) [Reserved] * * * * * (38) * * * (ii) Determination of Heat Purgeable and Ambient Purgeable Volatile Organic Compounds in Water by Gas Chromatography/Mass Spectrometry. Chapter 12 of Section B, Methods of the National Water Quality Laboratory, of Book 5, Laboratory Analysis. 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 VerDate Sep<11>2014 19:30 May 18, 2021 Jkt 253001 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, Note 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. 1999. 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 WholeWater 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 PO 00000 Frm 00032 Fmt 4701 Sfmt 4700 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. * * * * * (e) * * * E:\FR\FM\19MYR2.SGM 19MYR2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27257 TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES Container 1 Parameter number/name Preservation 2 3 Maximum holding time 4 Table IA—Bacterial Tests 1–4. Coliform, total, fecal, and E. coli. 5. Fecal streptococci ...................... 6. Enterococci ................................ 7. Salmonella ................................. PA, G ............................................ Cool, <10 °C, 0.008% Na2S2O3 5 8 hours.22 23 PA, G ............................................ PA, G ............................................ PA, G ............................................ Cool, <10 °C, 0.008% Na2S2O3 5 Cool, <10 °C, 0.008% Na2S2O3 5 Cool, <10 °C, 0.008% Na2S2O3 5 8 hours.22 8 hours.22 8 hours.22 Table IA—Aquatic Toxicity Tests 8–11. Toxicity, acute and chronic .. P, FP, G ........................................ Cool, ≤6 °C 16 ................................ 36 hours. Table IB—Inorganic Tests 1. Acidity ........................................ 2. Alkalinity ..................................... 4. Ammonia .................................... 9. Biochemical oxygen demand ..... 10. Boron ....................................... 11. Bromide ................................... 14. Biochemical oxygen demand, carbonaceous. 15. Chemical oxygen demand ....... 16. Chloride ................................... 17. Chlorine, total residual ............. 21. Color ........................................ 23–24. Cyanide, total or available (or CATC) and free. P, P, P, P, P, P, P, FP, G ........................................ FP, G ........................................ FP, G ........................................ FP, G ........................................ FP, or Quartz ........................... FP, G ........................................ FP G ......................................... Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18, H2SO4 to pH <2 ... Cool, ≤6 °C 18 ................................ HNO3 to pH <2 ............................. None required ............................... Cool, ≤6 °C 18 ................................ 14 days. 14 days. 28 days. 48 hours. 6 months. 28 days. 48 hours. P, P, P, P, P, FP, G ........................................ FP, G ........................................ G .............................................. FP, G ........................................ FP, G ........................................ 28 days. 28 days. Analyze within 15 minutes. 48 hours. 14 days. 25. 27. 28. 31, P P, P, P, ................................................... FP, G ........................................ FP, G ........................................ FP, G ........................................ Cool, ≤6 °C 18, H2SO4 to pH <2 ... None required ............................... None required ............................... Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18, NaOH to pH >10 5 6, reducing agent if oxidizer present. None required ............................... HNO3 or H2SO4 to pH <2 ............ None required ............................... Cool, ≤6 °C 18, H2SO4 to pH <2 ... Fluoride .................................... Hardness ................................. Hydrogen ion (pH) ................... 43. Kjeldahl and organic N ...... 28 days. 6 months. Analyze within 15 minutes. 28 days. khammond on DSKJM1Z7X2PROD with RULES2 Table IB—Metals 7 18. Chromium VI ............................ 35. Mercury (CVAA) ....................... 35. Mercury (CVAFS) .................... 3, 5–8, 12, 13, 19, 20, 22, 26, 29, 30, 32–34, 36, 37, 45, 47, 51, 52, 58–60, 62, 63, 70–72, 74, 75. Metals, except boron, chromium VI, and mercury. 38. Nitrate ...................................... 39. Nitrate-nitrite ............................ 40. Nitrite ....................................... 41. Oil and grease ......................... P, FP, G ........................................ P, FP, G ........................................ FP, G; and FP-lined cap 17 ........... P, FP, G ........................................ Cool, ≤6 °C 18, pH = 9.3–9.7 20 ..... HNO3 to pH <2 ............................. 5 mL/L 12N HCl or 5 mL/L BrCl 17 HNO3 to pH <2, or at least 24 hours prior to analysis 19. 28 days. 28 days. 90 days.17 6 months. P, P, P, G 48 28 48 28 42. Organic Carbon ....................... P, FP, G ........................................ 44. Orthophosphate ....................... P, FP, G ........................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18, H2SO4 to pH <2 ... Cool, ≤6 °C 18 ................................ Cool to ≤6 °C 18, HCl or H2SO4 to pH <2. Cool to ≤6 °C 18, HCl, H2SO4, or H3PO4 to pH <2. Cool, to ≤6 °C 18 24 ........................ 46. 47. 48. 49. 50. 53. 54. 55. 56. 57. 61. 64. 65. 66. Oxygen, Dissolved Probe ........ Winkler ..................................... Phenols .................................... Phosphorus (elemental) ........... Phosphorus, total ..................... Residue, total ........................... Residue, Filterable (TDS) ........ Residue, Nonfilterable (TSS) ... Residue, Settleable ................. Residue, Volatile ...................... Silica ........................................ Specific conductance ............... Sulfate ...................................... Sulfide ...................................... G, Bottle and top .......................... G, Bottle and top .......................... G ................................................... G ................................................... P, FP, G ........................................ P, FP, G ........................................ P, FP, G ........................................ P, FP, G ........................................ P, FP, G ........................................ P, FP, G ........................................ P or Quartz ................................... P, FP, G ........................................ P, FP, G ........................................ P, FP, G ........................................ 67. 68. 69. 73. Sulfite ....................................... Surfactants ............................... Temperature ............................ Turbidity ................................... P, P, P, P, VerDate Sep<11>2014 17:42 May 18, 2021 FP, G ........................................ FP, G ........................................ FP, G ........................................ ................................................... FP, FP, FP, FP, Jkt 253001 G G G G ........................................ ........................................ ........................................ ........................................ PO 00000 Frm 00033 Fmt 4701 None required ............................... Fix on site and store in dark ........ Cool, ≤6 °C 18, H2SO4 to pH <2 ... Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18, H2SO4 to pH <2 ... Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18 ................................ Cool, ≤6 °C 18, add zinc acetate plus sodium hydroxide to pH >9. None required ............................... Cool, ≤6 °C 18 ................................ None required ............................... Cool, ≤6 °C 18 ................................ Sfmt 4700 E:\FR\FM\19MYR2.SGM hours. days. hours. days. 28 days. Filter within 15 minutes; Analyze within 48 hours. Analyze within 15 minutes. 8 hours. 28 days. 48 hours. 28 days. 7 days. 7 days. 7 days. 48 hours. 7 days. 28 days. 28 days. 28 days. 7 days. Analyze within 15 minutes. 48 hours. Analyze within 15 minutes. 48 hours. 19MYR2 27258 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued Container 1 Parameter number/name Preservation 2 3 Maximum holding time 4 Table IC—Organic Tests 8 13, 18–20, 22, 24, 25, 27, 28, 34– 37, 39–43, 45–47, 56, 76, 104, 105, 108–111, 113. Purgeable Halocarbons. 26. 2-Chloroethylvinyl ether ........... 6, 57, 106. Purgeable aromatic hydrocarbons. 3, 4. Acrolein and acrylonitrile ....... G, FP-lined septum ...................... Cool, ≤6 °C 18, 0.008% Na2S2O3 5, HCl to pH 2 9. 14 days.9 G, FP-lined septum ...................... G, FP-lined septum ...................... Na2S2O3 5 Na2S2O3 5, 14 days. 14 days.9 Na2S2O3, 14 days.10 23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112. Phenols 11. 7, 38. Benzidines 11 12 .................... 14, 17, 48, 50–52. Phthalate esters 11. 82–84. Nitrosamines 11 14 .............. G, FP-lined cap ............................ Cool, ≤6 °C 18, 0.008% Cool, ≤6 °C 18, 0.008% HCl to pH 2 9. Cool, ≤6 °C 18, 0.008% pH to 4–5 10. Cool, ≤6 °C 18, 0.008% Na2S2O3 .. G, FP-lined cap ............................ G, FP-lined cap ............................ Cool, ≤6 °C 18, 0.008% Na2S2O3 5 Cool, ≤6 °C 18 ................................ G, FP-lined cap ............................ 88–94. PCBs 11 .............................. G, FP-lined cap ............................ Cool, ≤6 °C 18, store in dark, 0.008% Na2S2O3 5. Cool, ≤6 °C 18 ................................ 54, 55, 75, 79. Nitroaromatics and isophorone 11. 1, 2, 5, 8–12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons 11. 15, 16, 21, 31, 87. Haloethers 11 ... G, FP-lined cap ............................ 7 days until extraction, 40 days after extraction. 7 days until extraction.13 7 days until extraction, 40 days after extraction. 7 days until extraction, 40 days after extraction. 1 year until extraction, 1 year after extraction. 7 days until extraction, 40 days after extraction. 7 days until extraction, 40 days after extraction. G, FP-lined septum ...................... G, FP-lined cap ............................ Cool, ≤6 °C 18, store in dark, 0.008% Na2S2O3 5. Cool, ≤6 °C 18, store in dark, 0.008% Na2S2O3 5. G, FP-lined cap ............................ Cool, ≤6 °C 18, 0.008% Na2S2O3 5 29, 35–37, 63–65, 73, 107. Chlorinated hydrocarbons 11. 60–62, 66–72, 85, 86, 95–97, 102, 103. CDDs/CDFs 11. G, FP-lined cap ............................ Cool, ≤6 °C 18 ................................ G ................................................... See footnote 11 ............................ Aqueous Samples: Field and Lab Preservation. Solids and Mixed-Phase Samples: Field Preservation. Tissue Samples: Field Preservation. Solids, Mixed-Phase, and Tissue Samples: Lab Preservation. 114–118. Alkylated phenols .......... G ................................................... G ................................................... Cool, ≤6 °C 18, 0.008% Na2S2O3 5, pH <9. Cool, ≤6 °C 18 ................................ 7 days. G ................................................... Cool, ≤6 °C 18 ................................ 24 hours. G ................................................... Freeze, ≤¥10 °C .......................... 1 year. G ................................................... Cool, <6 °C, H2SO4 to pH <2 ....... 119. Adsorbable Organic Halides (AOX). 120. Chlorinated Phenolics ............ G ................................................... Cool, <6 °C, 0.008% Na2S2O3, HNO3 to pH <2. Cool, <6 °C, 0.008% Na2S2O3, H2SO4 to pH <2. 28 days until extraction, 40 days after extraction. Hold at least 3 days, but not more than 6 months. 30 days until acetylation, 30 days after acetylation. G, FP-lined cap ............................ 7 days until extraction, 40 days after extraction. 7 days until extraction, 40 days after extraction. See footnote 11. 1 year. Table ID—Pesticides Tests 1–70. Pesticides 11 ......................... G, FP-lined cap ............................ Cool, ≤6 °C 18, pH 5–9 15 .............. 7 days until extraction, 40 days after extraction. Table IE—Radiological Tests 1–5. Alpha, beta, and radium ........ P, FP, G ........................................ HNO3 to pH <2 ............................. 6 months. khammond on DSKJM1Z7X2PROD with RULES2 Table IH—Bacterial Tests 1, 2. Coliform, total, fecal ............... 3.E. coli .......................................... 4. Fecal streptococci ...................... 5. Enterococci ................................ PA, PA, PA, PA, G G G G ............................................ ............................................ ............................................ ............................................ Cool, Cool, Cool, Cool, <10 °C, <10 °C, <10 °C, <10 °C, 0.008% 0.008% 0.008% 0.008% Na2S2O3 5 Na2S2O3 5 Na2S2O3 5 Na2S2O3 5 8 8 8 8 hours.22 hours.22 hours.22 hours.22 Table IH—Protozoan Tests 6. Cryptosporidium ......................... 7. Giardia ....................................... LDPE; field filtration ...................... LDPE; field filtration ...................... 1–10 °C ......................................... 1–10 °C ......................................... 96 hours.21 96 hours.21 1 ’’P’’ is for polyethylene; ‘‘FP’’ is fluoropolymer (polytetrafluoroethylene [PTFE]; Teflon®), or other fluoropolymer, unless stated otherwise in this Table II; ‘‘G’’ is glass; ‘‘PA’’ is any plastic that is made of a sterilizable material (polypropylene or other autoclavable plastic); ‘‘LDPE’’ is low density polyethylene. VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00034 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 khammond on DSKJM1Z7X2PROD with RULES2 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 27259 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 (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less). 4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before the start of analysis and still be considered valid. Samples may be held for longer periods only if the permittee or monitoring laboratory have data on file to show that, for the specific types of samples under study, the analytes are stable for the longer time, and has received a variance from the Regional ATP Coordinator under § 136.3(e). For a grab sample, the holding time begins at the time of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, appendix E), the holding time begins at the time of the end of collection of the composite sample. For a set of grab samples composited in the field or laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain sample stability. See § 136.3(e) for details. The date and time of collection of an individual grab sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and that are all collected on the same calendar date, the date of collection is the date on which the samples are collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the date of collection is the dates of the two days; e.g., November 14–15. For a composite sample collected automatically on a given date, the date of collection is the date on which the sample is collected. For a composite sample collected automatically, and that is collected across two calendar dates, the date of collection is the dates of the two days; e.g., November 14–15. For static-renewal toxicity tests, each grab or composite sample may also be used to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after first use, if stored at 0– 6 °C, with minimum head space. 5 ASTM D7365–09a 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 S O and adjust pH to 7–10 with NaOH within 24 hours of sampling. 2 2 3 15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3. 16 Place sufficient ice with the samples in the shipping container to ensure that ice is still present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 °C prior to test initiation. 17 Samples collected for the determination of trace level mercury (<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). VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 PO 00000 Frm 00035 Fmt 4701 Sfmt 4700 E:\FR\FM\19MYR2.SGM 19MYR2 27260 Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations 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). 3. Amend § 136.6 by adding paragraph (b)(4)(xxiii) to read as follows: ■ § 136.6 Method modifications and analytical requirements. * * * * (b) * * * (4) * * * (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 khammond on DSKJM1Z7X2PROD with RULES2 * VerDate Sep<11>2014 17:42 May 18, 2021 Jkt 253001 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 PO 00000 Frm 00036 Fmt 4701 Sfmt 9990 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. * * * * * [FR Doc. 2021–09596 Filed 5–18–21; 8:45 am] BILLING CODE 6560–50–P E:\FR\FM\19MYR2.SGM 19MYR2

Agencies

ENVIRONMENTAL PROTECTION AGENCY

[Federal Register Volume 86, Number 95 (Wednesday, May 19, 2021)]
[Rules and Regulations]
[Pages 27226-27260]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2021-09596]



[[Page 27225]]

Vol. 86

Wednesday,

No. 95

May 19, 2021

Part III





Environmental Protection Agency





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40 CFR Part 136





Clean Water Act Methods Update Rule for the Analysis of Effluent; Final 
Rule

Federal Register / Vol. 86 , No. 95 / Wednesday, May 19, 2021 / Rules 
and Regulations

[[Page 27226]]


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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 136

[EPA-HQ-OW-2018-0826; FRL-10021-59-OW]
RIN 2040-AF84


Clean Water Act Methods Update Rule for the Analysis of Effluent

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: The Environmental Protection Agency (EPA) is finalizing 
changes to its test procedures required to be used by industries and 
municipalities when analyzing the chemical, physical, and biological 
properties of wastewater and other environmental samples for reporting 
under EPA's National Pollutant Discharge Elimination System (NPDES) 
permit program. The Clean Water Act (CWA) requires EPA to promulgate 
these test procedures (analytical methods) for analysis of pollutants. 
EPA anticipates that these changes will provide increased flexibility 
for the regulated community in meeting monitoring requirements while 
improving data quality. In addition, this update to the CWA methods is 
incorporating technological advances in analytical technology.

DATES: This final rule is effective July 19, 2021.

ADDRESSES: EPA has established a docket for this action under Docket ID 
No. EPA-HQ-OW-2018-0826. All documents in the docket are listed on the 
https://www.regulations.gov website. Although listed in the index, some 
information is not publicly available, e.g., confidential business 
information or other information whose disclosure is restricted by 
statute. Certain other material, such as copyrighted material, is not 
placed on the internet and will be publicly available only in hard copy 
form. Publicly available docket materials are available electronically 
through https://www.regulations.gov.

FOR FURTHER INFORMATION CONTACT:  Meghan Hessenauer, Engineering and 
Analysis Division (4303T), Office of Water, Environmental Protection 
Agency, 1200 Pennsylvania Avenue NW, Washington, DC 20460-0001; 
telephone: 202-566-1040; email: [email protected].

SUPPLEMENTARY INFORMATION: 

Table of Contents

I. General Information
II. Overview
III. Changes Between the Proposed Rule and the Final Rule
IV. Statutory Authority
V. Purpose and Summary of Final Rule
VI. Statutory and Executive Order Reviews

I. General Information

A. Does this action apply to me?

    Entities potentially affected by the requirements of this action 
include:

------------------------------------------------------------------------
                                      Examples of potentially affected
             Category                             entities
------------------------------------------------------------------------
State, Territorial, and Indian      States, territories, and tribes
 Tribal Governments.                 authorized to administer the
                                     National Pollutant Discharge
                                     Elimination System (NPDES)
                                     permitting program; states,
                                     territories, and tribes providing
                                     certification under CWA section
                                     401; state, territorial, and tribal-
                                     owned facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
Industry..........................  Facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
Municipalities....................  Publicly Owned Treatment Works
                                     (POTWs) or other municipality-owned
                                     facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
------------------------------------------------------------------------

    This table is not exhaustive, but rather provides a guide for 
readers regarding entities likely to be affected by this action. This 
table lists types of entities that EPA is now aware of that could 
potentially be affected by this action. Other types of entities not 
listed in the table could also be affected. To determine whether your 
facility is affected by this action, you should carefully examine the 
applicability language at 40 CFR 122.1 (NPDES purpose and scope), 40 
CFR 136.1 (NPDES permits and CWA) and 40 CFR 403.1 (pretreatment 
standards purpose and applicability). If you have questions regarding 
the applicability of this action to a particular entity, consult the 
appropriate person listed in the preceding FOR FURTHER INFORMATION 
CONTACT section.

II. Overview

    This preamble describes the reasons for the final rule; the legal 
authority for the final rule; a summary of the changes and 
clarifications; and explanation of the abbreviations and acronyms used 
in this document.

Abbreviations and Acronyms Used in the Preamble and Rule Text

2-CEVE: 2-Chloroethylvinyl ether
AA: Atomic Absorption
ADMI: American Dye Manufacturers Institute
ASTM: ASTM International \1\
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    \1\ Formerly known as the American Society for Testing and 
Materials (ASTM)
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ATP: Alternate Test Procedure
BHI: Brain heart infusion
BOD5: 5-day Biochemical Oxygen Demand
CAS: Chemical Abstract Services
CATC: Cyanide Amenable to Chlorination
CBOD--Carbonaceous Biochemical Oxygen Demand
CCB: Continuing calibration blank
CCV: Continuing calibration verification
CFR: Code of Federal Regulations
COD: Chemical Oxygen Demand
CWA: Clean Water Act
EC-MUG: EC broth with 4-methylumbelliferyl-[beta]-D-glucuronide
EDTA: Ethylenediaminetetraacetic acid
ELAB: Environmental Laboratory Advisory Board
EPA: Environmental Protection Agency
FLAA: Flame Atomic Absorption Spectroscopy
GC: Gas Chromatography
GFAA: Graphite Furnace Atomic Absorption Spectroscopy
ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy
ICP/MS: Inductively Coupled Plasma-Mass Spectrometry
ILI: Independent Laboratories Institute
IPR: Initial Precision and Recovery
LCS: Laboratory Control Sample
MDL: Method Detection Limit
MF: Membrane Filtration
MgCl2: Magnesium Chloride
MPN: Most Probable Number
MS/MSD: Matrix Spike/Matrix Spike Duplicate
MS: Mass Spectrometry
NA-MUG: Nutrient Agar with 4-methylumbelliferyl-[beta]-D-glucuronide
NECi: A shortened name used by the Nitrate Elimination Company, Inc.
NPDES: National Pollutant Discharge Elimination System
NTTAA: National Technology Transfer and Advancement Act
OPR: Ongoing Precision and Recovery
QC: Quality Control
STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption
SW: Solid Waste
TKN: Total Kjeldahl Nitrogen
TOC: Total Organic Carbon
USGS: United States Geological Survey
VCSB: Voluntary Consensus Standards Body

III. Changes Between the Proposed Rule and the Final Rule

    EPA received 25 comments on the October 2019 proposed rule from

[[Page 27227]]

laboratory associations, commercial labs, state environmental agencies, 
and various trade associations. None of the comments opposed the 
promulgation of the proposed methods. Below is a breakout summarizing 
the comments we received.
     All commenters support finalizing this rule.
     12 of the comment letters were outside the scope for the 
proposed rulemaking or requested a method modification with no 
underlying data to support the requested change.
     Some commenters requested that EPA modify methods 
developed by external stakeholders (ASTM International, USGS, etc.). 
However, EPA is only adopting methods as developed by voluntary 
consensus standard bodies. Comments requesting changes to such methods 
should be directed to the method developers.
     Some commenters noted typographical errors or minor 
inconsistencies within 40 CFR part 136 that required minor changes 
(e.g., the wrong citation date in a footnote, methods listed in the 
wrong section of the 40 CFR part 136). Except as noted below, the 
content of the final rule is the same as that of the proposed rule.

A. Changes in Preamble

    In the proposed rulemaking, EPA included in Table IA Standard 
Methods Method 9230D-2013 for the measurement of enterococci but did 
not include a discussion of this method in the preamble to the 
proposal. In response to comments, EPA has added a description of the 
method to Section IV.C of this preamble.
    Similarly, while the proposal included in Table IB Standard Methods 
Method 5210B-2016 for the measurement of carbonaceous biochemical 
oxygen demand (CBOD5), EPA did not discuss approving this 
method in the preamble to the proposal. The preamble did, however, 
discuss approval of this method for biochemical oxygen demand 
(BOD5) and included BOD in Table IB and along with CBOD. In 
response to comments, EPA has included discussion and the description 
of the method in Section V.C of this preamble for both BOD and CBOD.
    In addition, EPA has corrected a typographical error that appeared 
in the proposed rulemaking regarding Standard Methods Method 2540E-2015 
in Section IV.C of this preamble. The correct method, Standard Methods 
Method 2540F-2015, is now listed in Section IV.C of this preamble.
    The errata sheets for Whole Effluent Toxicity were not referenced 
in 40 CFR part 136. In the previous 2017 Methods Update Rule, the 
errata sheets were approved but not referenced. EPA did not add this to 
the regulatory test and was a mistake. The errata sheets are now 
referenced.

B. Changes to Table IB

    EPA has corrected two errors in Table IB of the final rule. In the 
proposal, EPA listed ASTM Method D1179-16(A) in the wrong row in the 
Table IB entry for Fluoride. The method is a distillation step and was 
erroneously listed in the row for colorimetric methods. EPA has 
corrected Table IB in the final rule.
    EPA also has corrected the publication date of the Macherey-Nagel 
Chemical Oxygen Demand method in Footnote 83 to Table IB. In the 
proposal, the publication date in the footnote was listed as 2008 and 
has been corrected to 2018.

C. Changes to Table II

    EPA is making a number of conforming changes to the final rule in 
order to correct inadvertent omissions and errors.
    In response to a comment that pointed out that EPA did not update 
Table II to capture the microbiological method changes included in 
Tables IA and IH, EPA has modified Table II to take account of these 
changes for the final rule. These changes intended to clarify and 
correct inadvertent omissions and errors.
    A commenter pointed out that EPA did not include organic parameter 
#73, hexachloroethane in Table II. EPA has corrected this error that 
dates to the Methods Update Rule proposed in 2004. The parameter #73 
has been added to the list of chlorinated hydrocarbons in Table II of 
the final rule.
    Finally, a typographical error in Table II of the proposed 
rulemaking resulted in the specifications for four matrices listed 
under the dioxin and furan (CDDs/CDFs) entry to not be indented. This 
caused some confusion for commenters. EPA has ensured that Table II in 
the final rule appears as intended.

IV. Statutory Authority

    EPA is promulgating this regulation under the authorities of 
sections 301(a), 304(h), and 501(a) of the CWA; 33 U.S.C. 1311(a), 
1314(h), and 1361(a). Section 301(a) of the CWA prohibits the discharge 
of any pollutant into navigable waters unless the discharge complies 
with, among other provisions, an NPDES permit issued under section 402 
of the CWA. Section 304(h) of the CWA requires the Administrator of EPA 
to ``. . . promulgate guidelines establishing test procedures for the 
analysis of pollutants that shall include the factors which must be 
provided in any certification pursuant to [section 401 of the CWA] or 
permit application pursuant to [section 402 of the CWA].'' Section 
501(a) of the CWA authorizes the Administrator to ``. . . prescribe 
such regulations as are necessary to carry out this function under [the 
CWA].'' EPA generally has codified its test procedure regulations 
(including analysis and sampling requirements) for CWA programs at 40 
CFR part 136, though some requirements are codified in other parts 
(e.g., 40 CFR chapter I, subchapters N and O).

V. Purpose and Summary of Final Rule

    NPDES permits must include conditions designed to ensure compliance 
with the technology-based and water quality-based requirements of the 
CWA, including in many cases, restrictions on the quantity of specific 
pollutants that can be discharged as well as requirements for pollutant 
monitoring, measurement and reporting to NPDES authorities. Often, 
entities have a choice in deciding which approved test procedure they 
will use for a specific pollutant because EPA has approved the use of 
more than one method.\2\
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    \2\ NPDES permit regulations also specify that the approved 
method needs to be sufficiently sensitive. See 40 CFR 122.21 (e)(3).
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    The procedures for the analysis of pollutants required by CWA 
section 304(h) are a central element of the NPDES permit program. 
Examples of where these EPA-approved analytical methods must be used 
include the following: (1) Applications for NPDES permits, (2) sampling 
or other reports required under NPDES permits, (3) other requests for 
quantitative or qualitative effluent data under the NPDES regulations, 
(4) State CWA 401 certifications and (5) sampling and analysis required 
under EPA's General Pretreatment Regulations for Existing and New 
Sources of Pollution, 40 CFR 136.1 and 40 CFR 403.12(b)(5)(v).
    Periodically, EPA updates the approved methods in 40 CFR part 136. 
In general, the changes in this final action fall into the following 
categories. The first is new or revised methods published by the VCSBs 
or the USGS that are similar to methods previously adopted as EPA-
approved methods in 40 CFR part 136. The second category is methods EPA 
has reviewed under the Agency's national ATP program and preliminarily 
concluded are appropriate for nationwide use. Lastly, EPA is finalizing 
certain corrections or amendments to the text and tables of 40

[[Page 27228]]

CFR part 136. EPA is adopting these revisions to improve data quality, 
update methods to keep current with technology advances, and provide 
the regulated community with greater flexibility. The following 
paragraphs provide details on the finalized revisions.

A. Changes to 40 CFR 136.3 To Include New Versions of Previously 
Approved EPA Methods

    EPA added the revised version of EPA Method 1623 (labeled 1623.1) 
to Table IH. Method 1623.1 includes updated acceptance criteria for 
IPR, OPR, and MS/MSD, and clarifications and revisions based on user 
questions and feedback about Method 1623 over the past 19 years.

B. Methods Incorporated by Reference

    Currently, hundreds of methods and ATPs are incorporated by 
reference within 40 CFR part 136. In most cases, 40 CFR part 136 
contains multiple approved methods for a single pollutant, and 
regulated entities often have a choice in selecting a method. This 
final rule contains revisions to VCSB methods that are currently 
incorporated by reference. Two VCSBs have made such revisions, Standard 
Methods and ASTM. The finalized VCSB methods are consistent with the 
requirements of the National Technology Transfer and Advancement Act 
(NTTAA), under which federal agencies use technical standards developed 
or adopted by the VCSBs if compliance would not be inconsistent with 
applicable law or otherwise impracticable (see Section V.I of this 
preamble). The VCSB methods are available on their respective websites 
(https://www.standardmethods.org/ and www.astm.org) to everyone at a 
cost determined by the VCSB, generally from $40 to $80. Both 
organizations also offer memberships or subscriptions that allow 
unlimited access to their methods. The cost of obtaining these methods 
is not a significant financial burden for a discharger or environmental 
laboratory, making the methods reasonably available. Finally, this 
final rule also includes USGS methods and vendor ATPs, all of which EPA 
is incorporating by reference. The ATPs and USGS methods are available 
free of charge on their respective websites (flowinjection.com, mn-net.com, micrologylabs.com and USGS.gov), enabling EPA to conclude that 
the USGS methods and ATPs incorporated by reference are reasonably 
available.

C. Changes to 40 CFR 136.3 To Include New Versions of Approved Standard 
Methods Methods

    EPA is approving new versions of Standard Methods methods 
previously included in 40 CFR part 136. The newer versions clarify the 
existing methods or make editorial corrections. As was the case with 
the previous methods update rule (82 FR 40836-40941, August 28, 2017), 
EPA approves and includes in 40 CFR part 136 only the most recent 
version of a method published by the Standard Methods Committee. EPA is 
listing only one version of the method with the year of publication 
designated by the last four digits in the method number (e.g., SM 
method 3111 B-2011). The date indicates the date of the specific 
revision to the method. This allows use of a specific method in any 
edition of the hard copy publication of Standard Methods for the 
Examination of Water & Wastewater that includes a method with the same 
method number and year of publication.
    The finalized revisions to Standard Methods methods previously 
approved in 40 CFR part 136 will not affect the performance of the 
method. The following identifies new versions of previously approved 
Standard Methods methods that EPA included. Each entry contains the 
Standard Methods number and date, the parameter, and a brief 
description of the analytical method. The methods listed below are 
organized according to the table at 40 CFR part 136 in which they 
appear.
    EPA finalized the following changes to Tables IA and IH at 40 CFR 
part 136:
    1. Standard Methods Method 9221 (B, E, F)-2014: Method 9221B-2014 
Coliform (total); analyzes for total coliforms in non-potable waters 
using LTB, all presumptive growth LTB tubes are confirmed in BGLB. 
Method 9221E-2014 Coliform (fecal); analyzes all presumptive growth LTB 
tubes for fecal coliform using EC broth. Method 9221F-2014 E. coli; 
analyzes all presumptive growth LTB tubes for E. coli using EC-MUG. The 
number of positive tubes (BGLB, EC broth or EC-MUG) is used to 
determine the MPN. In response to public comment, EPA is clarifying 
that Method 9221E-2014 is approved for testing sewage sludge. In Table 
IA.1, EPA changed Footnote 11 from `approved' to `recommended' in the 
proposed rulemaking because the 2017 Methods Update Rule erroneously 
changed the footnote from `recommended' to `approved.' EPA is 
correcting this error and changing the footnote back to 
``recommended''. EPA has approved all biosolid methods listed in Table 
1A.1 for parameter #1, including those listed in Footnote 11. More 
method validation data is available for EPA Methods 1680 and 1681 than 
Standard Method 9221. EPA methods are recommended over 9221 and 9222, 
although all four methods are approved for biosolids.
    2. Standard Methods Method 9222 (B, D, I)-2015: Method 9222B-2015 
Coliform (total); analyzes for total coliforms in non-potable waters by 
filtration through a 0.45-[micro]m membrane filter and plated on mEndo 
or LES Endo agar. Method 9222D-2015 Coliform (fecal); analyzes for 
fecal coliforms in non-potable waters by filtration through a 0.45-
[micro]m membrane filter plated on mFC medium. Method 9222 I-2015 E. 
coli; membrane filtration (MF), analyzes presumptive positive filters 
from Method 9222B and 9222D using nutrient agar plates with MUG (NA-
MUG) which are examined under a longwave UV lamp.
    3. Standard Methods Method 9223B-2016, E. coli, multiple tube/
multiple well: This method analyzes non-potable waters for E. coli 
using commercially available enzyme substrate media that is mixed with 
the sample and placed in multiple tubes or multiple well trays, 
incubated and examined under ambient light for Coliform (total) and 
under a longwave UV lamp for E. coli.
    4. Standard Methods Method 9230 (B,C)-2013: Method 9230B-2013 
(Fecal Streptococci) analyzes non-potable waters for streptococci using 
azide dextrose broth (ADB) Presumptive positive ADB tubes are confirmed 
by streaking onto bile esculin azide agar (BEA). Method 9230C-2013 
Enterococci; analyzes non-potable waters by filtration through a 0.45-
[micro]m membrane filter and plated on mE agar.
    5. Standard Methods Method 9230D-2013, Enterococci: This method 
analyzes non-potable waters using a hydrolyzable substrate (4-
methylumbelliferyl-[szlig]-D-glucoside) to detect enterococci in a 
multiple-tube or a multi-well format.
    EPA is promulgating the following changes to Table IB at 40 CFR 
part 136:
    1. Standard Methods Method 2540 series.
    a. Method 2540B-2015, total solids. A sample aliquot is evaporated 
in a pre-weighed evaporating dish at 103-105 [deg]C. Method 2540C-2015 
filterable residue (total dissolved solids). The sample aliquot is then 
filtered through a glass fiber filter, and the filtrate is evaporated 
on a pre-weighed dish to constant weight at 180 [deg]C.
    b. Method 2540D-2015 non-filterable residue (total suspended 
solids). A sample aliquot is filtered through a pre-

[[Page 27229]]

weighed glass fiber filter which is then dried to constant weight at 
103-105 [deg]C.
    c. Method 2540E-2015 volatile residue (fixed and volatile solids). 
The residue obtained from the determination of total (Method 2540B), 
filterable (Method 2540C) or non-filterable residue (Method 2540D) is 
ignited at 550 [deg]C in a muffle furnace.
    d. Method 2540F-2015 settleable residue (settleable solids). 
Settleable matter is measured with an Imhoff cone either volumetrically 
or gravimetrically.
    2. Standard Methods Method 4500-CN^- (B-G)-2016, cyanide. 
Cyanides are measured after preliminary treatment of samples to remove 
interferences (4500-CN^- B). Manual distillation with 
magnesium chloride (MgCl2) (4500-CN^- C) is 
followed by: Titration with silver nitrate (4500-CN^- D). 
Spectrophotometric measurement after cyanide in the alkaline distillate 
is converted to Cyanogen Chloride (4500-CN^- E). 
Potentiometric measurement using an ion selective electrode (4500-
CN^- F). Cyanide amenable to chlorination (CATC) in which a 
portion of the sample is chlorinated at high pH and cyanide levels in 
the chlorinated sample are determined after manual distillation 
followed by titrimetric or spectrophotometric measurement. Amenable 
cyanide is calculated by the difference between the results for cyanide 
in the unchlorinated sample and the results for the chlorinated sample 
(4500-CN^- G).
    3. Standard Methods Method 4500-NO3^- D-2016. 
Nitrate (as nitrogen), measured using an ion-selective electrode that 
develops a potential across a thin, inert membrane holding in place a 
water-immiscible liquid ion exchanger.
    4. Standard Methods Method 4500-NO3^- (E, F, 
and H)-2016. Nitrate-nitrite (as nitrogen). Nitrate is reduced to 
nitrite using a cadmium-copper column, followed by diazotization to 
form a colored azo dye, which is measured by colorimetry either 
manually (4500-NO3^- E) or automated (4500-
NO3^- F); or by reduction of nitrate to nitrite 
using hydrazine followed by automated colorimetric measurement of 
nitrite after diazotization (4500-NO3^- H).
    5. Standard Methods Method 4500-NO3^- (E and 
F)-2016. Nitrite (as nitrogen). Colorimetric: bypasses the cadmium 
reduction step and measures nitrite after diazotization either by 
manual or automated colorimetric analysis.
    6. Standard Methods Method 4500-O (B^-F, and G)-2016. 
Measurement of oxygen (dissolved), using the Winkler iodometric 
titration procedure with modifications to eliminate or minimize certain 
interferences if necessary, based on sample type (4500-O B through F), 
or by use of polarographic or galvanic membrane electrodes (4500-O G).
    7. Standard Methods Method 5210 B-2016., Biochemical oxygen demand 
(BOD5) and carbonaceous biochemical oxygen demand 
(CBOD5), dissolved oxygen depletion: The BOD5 
test is an indirect measurement of organic matter. It measures the 
change in dissolved oxygen (DO) concentration caused by microorganisms 
as they degrade organic matter in a sample held in a stoppered bottle 
incubated for 5 days in the dark at 20 [deg]C. Nitrification inhibition 
is recommended for secondary-effluent samples, samples seeded with 
secondary effluent, and polluted water because nitrogenous compounds 
can oxidize in such samples. When a nitrification inhibitor is added as 
directed in 5210B.5e, results are reported as CBOD5.
    8. Standard Methods Method 5310 (B, C)-2014. Total organic carbon 
(TOC), combustion, heated persulfate or UV persulfate oxidation. In 
method 5310 B-2014 Combustion, a sample aliquot is combusted, 
transported in a carrier gas stream and measured via a nondispersive 
infrared analyzer, or titrated coulometrically. In method 5310C-2014 
Persulfate, UV, or heated-persulfate oxidation method, persulfate 
oxidizes organic carbon. The produced CO2 is then purged and 
measured by either nondispersive infrared (NDIR) analyzer, 
coulometrically titrated, or separated from the liquid stream by a 
membrane that specifically allows CO2 to pass into high-
purity water where the change in the high-purity water's conductivity 
corresponds to the amount of CO2 passing the membrane.
    Lastly, EPA is promulgating one revision to a previously approved 
Standard Methods method for which the Standard Methods Committee has 
adopted updates. This modification includes minor changes to method 
procedures that do not affect the performance of the method. EPA is 
promulgating the following change to Table IA and Table IH at 40 CFR 
part 136:
    Standard Methods Method 9221F-2014 is an acceptable method for 
detecting fecal coliforms and E. coli simultaneously. This method 
analyzes Coliform (fecal) and E. coli using EC broth with 4-
methylumbelliferyl-[beta]-D-glucuronide (EC-MUG) with inverted vials 
and is an MPN method

D. Changes to 40 CFR 136.3 To Include New Standard Methods Methods 
Based on Previously Approved Technologies

    EPA is promulgating changes based on the National Technology 
Transfer and Advancement Act of 1995 (NTTAA), Public Law 104-113. This 
provides that federal agencies and departments must use technical 
standards developed or adopted by the VCSBs if the use of these 
standards would not be inconsistent with applicable law or otherwise 
impracticable. These methods submitted by the Standards Methods 
Committee are consistent with other methods already approved at 40 CFR 
part 136.
    EPA is adding Standard Methods Method 4500-CN^- N-2016 to 
Table IB for Cyanide, total. Cyanide is measured after preliminary 
treatment of samples and manual distillation with magnesium chloride 
(MgCl2) followed by automated spectrophotometric measurement 
after conversion to Cyanogen Chloride. This method is similar to the 
currently approved EPA Method 335.4, USGS Method I-4302-85, and Lachat 
Method 10-204-00-1-X, and uses semi-automated spectrophotometric 
measurement of cyanide.
    2. EPA is adding Standard Methods Method 4500-
NO3^- I-2016 to Table IB for combined nitrate-
nitrite, nitrite and nitrate by subtraction. Nitrate is reduced to 
nitrite using a cadmium-copper column followed by diazotization to form 
an azo dye which is measured by colorimetry. The cadmium reduction 
column may be by-passed for measurement of nitrite only. The value 
obtained for nitrite may be subtracted from the value obtained for 
combined nitrate-nitrite to calculate the concentration of nitrate. 
This method is similar to the currently approved EPA Method 353.2, 
Standard Methods Method 4500-NO3^- F-2011, ASTM 
Method D3867-04 (A), and USGS Method I-2545-90, and uses automated 
cadmium reduction and spectrophotometric measurement of nitrite.
    3. EPA is adding Standard Methods Method 4500-
NO3^- J-2018 to Table IB for measurement of 
combined nitrate-nitrite, nitrite, and for measurement of nitrate by 
subtraction. Nitrate is reduced to nitrite by an enzymatic reaction. 
The nitrite is diazotized to yield an azo dye which is measured 
colorimetrically. The enzyme reduction step may be by-passed for 
measurement of nitrite singly. The value obtained for nitrite may be 
subtracted from the value obtained for combined nitrate-nitrite to 
calculate the concentration of nitrate.

[[Page 27230]]

This method is similar to the currently approved NECi Method N07-0003, 
USGS Method I-2547-11, and USGS Method I-2548-11.
    4. EPA is adding Standard Methods Method 4500-O H-2016 to Table IB 
for dissolved oxygen. This method uses a luminescent-based sensor for 
measurement of dissolved oxygen. The method is similar to the currently 
approved Hach Method 10360, In-Situ Method 1002-8-2009, and ASTM Method 
D888-09 (C).

E. Changes to 40 CFR 136.3 To Include New Versions of Approved ASTM 
Methods

    EPA is approving new versions of ASTM methods previously approved 
in 40 CFR part 136 for the reasons outlined in the first paragraph of 
Section IV.C of this preamble. These changes to currently approved ASTM 
methods in 40 CFR part 136 include minor clarifications and editorial 
changes, and in some instances, minor changes to method procedures. 
None of these changes will affect the performance of the method. The 
following describes the changes to current ASTM methods that EPA is 
adding to 40 CFR part 136. Each entry contains (in the following 
order): The ASTM method number (the last two digits in the method 
number represent the year ASTM published), the parameter, a brief 
description of the analytical technique, and a brief description of any 
procedural changes in this revision from the last approved version of 
the method. The methods listed below are organized according to the 
table at 40 CFR part 136 in which they appear.
    EPA is promulgating the following changes to Table IB at 40 CFR 
part 136:
    1. ASTM Method D511-14 (A, B), calcium and magnesium, titrimetric, 
(EDTA), AA direct aspiration. Method D511-14 A, titrimetric. The pH of 
the sample is adjusted to 10 (for calcium), then to 12-13 (for 
magnesium) and titrated with ethylenediamine tetraacetic acid (EDTA) to 
form complexes with calcium and magnesium ions which react with an 
indicator to form a colored product. The volume of titrant used to 
affect the color change is proportional to the concentrations of 
calcium and magnesium in the sample. Method D511-14 B, AA direct 
aspiration. The sample is acidified and analyzed by atomic absorption. 
The concentrations of calcium and magnesium in the samples are 
proportional to the amount of light absorbed during the analysis and 
are determined in comparison to a standard curve. This version EPA is 
adding includes specifications for filter paper.
    2. ASTM Method D512-12 chloride ion (A, B), titrimetric (mercuric 
nitrate), titration (silver nitrate). Method D512-12A, titrimetric 
mercuric nitrate. The sample is acidified and titrated with mercuric 
nitrate in the presence of a diphenylcarbazonebromophenol blue 
indicator. Method D512-12B, titrimetric silver nitrate. Sample pH is 
adjusted to phenolphthalein endpoint and titrated with silver nitrate 
in the presence of potassium chromate. The volume of titrant used to 
affect the color change in either method is proportional to the 
concentration of chloride in the sample. This version corrects one term 
in the chloride calculation.
    3. ASTM Method D516-16, sulfate ion, turbidimetric. In this method, 
sulfate ions are converted to barium sulfate to form a suspension. The 
turbidity of the suspension is measured with a nephelometer, 
spectrophotometer, or photoelectric colorimeter, and compared to a 
standard curve to determine the sulfate concentration in the sample. 
This version adds specifications for filter paper.
    4. ASTM Method D858-17 (A-C), manganese, atomic absorption (AA) 
direct aspiration, AA furnace. The sample is acid digested and analyzed 
by direct aspiration atomic absorption or graphite furnace atomic 
absorption. The concentration of manganese in the sample is 
proportional to the amount of light absorbed and is determined in 
comparison to a standard curve. There are no procedural changes.
    5. ASTM Method D859-16, silica, colorimetric, manual. In this 
method, soluble silica in the sample is reacted with molybdate then 
reduced to form a blue complex in solution. The intensity of the blue 
complex is determined with a spectrophotometer or filter photometer and 
the concentration of silica is determined by comparison with a standard 
curve. There are no procedural changes.
    6. ASTM Method D888-12 (A-C) dissolved oxygen, Winkler, electrode, 
luminescent-based sensor. Method D888-12A measures dissolved oxygen 
using the Winkler iodometric titration procedure. The volume of titrant 
used is proportional to the concentration of dissolved oxygen in the 
sample. Method D888-12B measures dissolved oxygen in the sample with an 
electrochemical probe that produces an electrical potential which is 
logarithmically proportional to the concentration of dissolved oxygen 
in the sample. Method D888-12C measures dissolved oxygen with a 
luminescence-based sensor probe that employs frequency domain lifetime-
based luminescence quenching and signal processing. This version adds 
information on a two-point calibration and updated performance 
information from an interlaboratory study to D888-12C.
    7. ASTM Method D1067-16, acidity or alkalinity, electrometric 
endpoint or phenolphthalein endpoint; electrometric or colorimetric 
titration to pH 4.5, manual. The acidity or alkalinity of the sample is 
determined by titration to a specific pH endpoint which is determined 
by colorimetry or with a pH electrode. The acidity or alkalinity is 
proportional to the volume of titrant required to affect the pH change. 
There are no procedural changes.
    8. ASTM Method D1068-15 (A-C), iron, AA direct aspiration; AA 
furnace; colorimetric (Phenanthroline): The sample is acid digested and 
analyzed by either direct aspiration atomic absorption, graphite 
furnace atomic absorption, or colorimetry. The concentration of iron in 
the sample is proportional to the amount of light absorbed and is 
determined in comparison to a standard curve. The version as 
promulgated includes specifications for filter paper.
    9. ASTM Method D1126-17, hardness, titrimetric (EDTA). The pH of 
the sample is adjusted, and an indicator is added forming a red color. 
The mixture is titrated until the color changes from red to blue. The 
volume of titrant used to affect the color change is proportional to 
the hardness in the sample. There are no procedural changes.
    10. ASTM Method D1179-16 (A, B); fluoride ion, manual distillation, 
electrode, manual. Method D1179A, manual distillation. The sample is 
distilled as hydrofluorosilic acid and determined by ion-selective 
electrode. Method D1179B, electrode. The fluoride ion is determined 
potentiometrically with an ion-selective electrode in conjunction 
without sample distillation. There are no procedural changes.
    11. ASTM Method D1246-16, bromide ion, electrode. The bromide in 
the sample is determined potentiometrically with an ion-selective 
electrode, either through comparison to a standard curve or through a 
direct readout on the instrument. There are no changes to method 
procedures.
    12. ASTM Method D1252-06 (A, B) (Reapproved 2012), chemical oxygen 
demand, titrimetric, spectrophotometric. This is the 2012 reapproval of 
the 2006 ASTM method. Method D1252-06A, titrimetric measures the loss 
of the hexavalent

[[Page 27231]]

dichromate ion by reflux digestion followed by titration. The chemical 
oxygen demand in the sample is determined by comparison to a standard 
curve. Method D1252-06B, spectrophotometric, uses a spectrophotometer 
to measure the loss of the hexavalent dichromate ion at 420 nm or the 
increase in the trivalent chromium ion at 600 nm, after closed 
digestion and determines the chemical oxygen demand by comparison to a 
standard curve. There are no procedural changes.
    13. ASTM Method D1253-14, residual chlorine, amperometric direct. 
The concentration of chlorine in the sample is determined by titration 
with phenylarsine oxide, using an amperometric probe that responds to 
chlorine to determine when the titration is complete. The chlorine 
concentration in the sample is proportional to the volume of titrant 
used. There are no procedural changes.
    14. ASTM Method D1426-15 (A, B), ammonia nitrogen, Nesslerization, 
electrode. Method D1426A, Nesslerization. An aliquot is Nesslerized, 
and the ammonia content determined colorimetrically. Method D1426B, 
electrode. Ammonia is potentiometricly determined using a gas-permeable 
ion-selective electrode, either through comparison to a standard curve 
or through a direct readout on the instrument using. A lengthy section 
of QC requirements was added to the Nesslerization procedure (D1426A) 
that parallels the QC discussion that was already in the B procedure. 
Both procedures added information on use of commercially prepared 
standards and filter paper.
    15. ASTM Method D1687-17 (A-C), chromium (total) and dissolved 
hexavalent chromium, colorimetric (diphenyl-carbazide); AA direct 
aspiration; AA furnace. Method D1687-17A, chromium (dissolved) measures 
dissolved hexavalent chromium by reacting it with diphenyl-
carbohydrazide to produce a reddish-purple color that is measured with 
a spectrophotometer or filter photometer. The concentration in the 
sample is proportional to the intensity of the color. Method D1687-17B, 
chromium (total). The sample is acid digested and analyzed by direct 
aspiration atomic absorption. Method D1687-17C, chromium (total). The 
sample is acid digested and analyzed by graphite furnace atomic 
absorption. The concentration of total chromium in the sample is 
proportional to the amount of light absorbed during the analysis and is 
determined in comparison to a standard curve. The changes mirror those 
for the other metal methods. The QC frequencies for method blank, 
continuing calibration verification (CCV), continuing calibration blank 
(CCB), matrix spike, and duplicate analyses are now based on a 
laboratory-defined batch of up to 20 samples.
    16. ASTM Method D1688-17 (A-C), copper, AA direct aspiration, AA 
furnace. The sample is acid digested and analyzed by direct aspiration 
atomic absorption (D1688-17A and B) or graphite furnace atomic 
absorption (D1688-17B). The concentration of copper in the sample is 
proportional to the amount of light absorbed and is determined in 
comparison to a standard curve. The changes mirror those for the other 
metal methods. The changes EPA is promulgating also clarify the 
requirements for a multi-point calibration by discussing it in the 
calibration section as well as the QC section of all three procedures. 
The QC frequencies for method blank, CCV, CCB, matrix spike, and 
duplicate analyses are now based on a laboratory-defined batch of up to 
20 samples.
    17. ASTM Method D1691-17 (A, B), zinc, AA direct aspiration. Method 
D1691-17A. The sample is acid digested and analyzed by direct 
aspiration atomic absorption. Method D1691-17B. The sample is processed 
by chelation-extraction and analyzed by atomic absorption. The 
concentration of zinc in the sample is proportional to the amount of 
light absorbed and is determined in comparison to a standard curve. The 
changes mirror those for the other metal methods. The QC frequencies 
for method blank, CCV, CCB, matrix spike, and duplicate analyses are 
now based on a laboratory-defined batch of up to 20 samples.
    18. ASTM Method D1783-01 (A, B) (Reapproved 2012), phenols, manual 
distillation followed by manual colorimetric (4AAP). The sample is 
distilled, the distillate pH is adjusted to 10.0, and reacted with 4-
aminoantipyrine to form a colored product. In Method D1783-01A, the 
colored product is extracted from the sample with chloroform and 
measured with a photometer at 460 nm. In Method D1783-01B, the colored 
product is measured without extraction, using a photometer at 510 nm. 
The concentration of phenolics is determined in comparison to a 
standard curve. There are no procedural changes.
    19. ASTM Method D1886-14 (A-C), nickel AA direct aspiration, 
chelation extraction AA and AA furnace. Method D1886-14A. The sample is 
acid digested and analyzed by direct aspiration atomic absorption. 
Method D1886-14B. The sample is acid digested and the nickel chelated 
and extracted. The extract is analyzed by direct aspiration atomic 
absorption. Method D1886-14C. The sample is acid digested and analyzed 
by graphite furnace atomic absorption. The concentration of nickel in 
the sample is proportional to the amount of light absorbed during the 
analysis and is determined in comparison to a standard curve. The 
changes mirror those for the other metal methods. The QC frequencies 
for method blank, CCV, CCB, matrix spike, and duplicate analyses are 
now based on a laboratory-defined batch of up to 20 samples.
    20. ASTM Method D2036-09 (A, B) (Reapproved 2015). D2036-09 A 
(total cyanide). Manual distillation followed by gas diffusion 
amperometry, titrimetric, spectrophotometric, ion chromatography, ion 
selective electrode. D2036-09 B (available (amenable) cyanide) Manual 
distillation followed by titrimetric or spectrophotometric. The cyanide 
in the sample is distilled and trapped in a sodium hydroxide solution. 
Method D2036-09A, the cyanide is treated with strong acid and a 
catalyst during distillation and measured by titration, gas diffusion 
amperometry, spectrophotometry, ion-selective electrode, ion 
chromatography, or flow injection analysis. Method D2036-09B--cyanide 
amenable to chlorination is determined by comparing the results for one 
sample aliquot analyzed for total cyanide and a second aliquot that is 
treated with calcium hypochlorite prior to analysis by Method D2036-
09A. There are no procedural changes.
    21. ASTM Method D2972-15 (A-C), arsenic, colorimetric, AA gaseous 
hydride, AA furnace. The sample is digested with nitric and sulfuric 
acids. Method D2972-15A. Arsenic is trapped in a solution of silver 
diethyldithiocarbamate in pyridine which produces a red-colored product 
that is analyzed photometrically by comparison to a standard curve. 
Method D2972-15B. Arsenic in the digested sample is determined by 
hydride generation atomic absorption. Method D2972-15C. Arsenic in the 
digested sample is determined by graphite furnace atomic absorption. 
The changes mirror those for the other metal methods. The QC 
frequencies for method blank, CCV, CCB, matrix spike, and duplicate 
analyses are now based on a laboratory-defined batch of up to 20 
samples.
    22. ASTM Method D3223-17, total mercury, cold vapor, manual. 
Mercury in the sample is converted to the mercuric ion, which is 
reduced to elemental mercury, purged from the

[[Page 27232]]

sample, and analyzed by cold vapor atomic absorption. The changes 
mirror those for the other metals methods, but this version changes the 
acceptance limit for the CCV from 10% to 15% and adds a requirement for 
a CCB. Given that the most comparable EPA procedure, Method 245.1, does 
not include a CCV requirement or an acceptance limit, the change of the 
acceptance limit from 10% to 15% in the revised ASTM method represents 
a requirement that is more stringent than that required in EPA's 
procedure.
    23. ASTM Method D3373-17, vanadium, AA furnace. The sample is 
digested with nitric acid and analyzed by graphite furnace atomic 
absorption. The concentration of vanadium in the sample is proportional 
to the amount of light absorbed during the graphite furnace atomic 
absorption analysis and is determined in comparison to a standard 
curve. The changes mirror those for the other metals methods. The 
changes clarify the requirements for a multi-point calibration by 
discussing it in the calibration section as well as the QC section of 
all three procedures. The QC frequencies for method blank, CCV, CCB, 
matrix spike, and duplicate analyses are now based on a laboratory-
defined batch of up to 20 samples.
    24. ASTM Method D3557-17 (A-D), cadmium, AA direct aspiration, 
voltammetry, AA furnace. Method D3557-17A--the sample is acid digested 
and analyzed by direct aspiration atomic absorption. Method D3557-17B 
the sample is acid digested, the digestate is chelated and extracted. 
The extract analyzed by direct aspiration atomic absorption. Method 
D3557-17C--the sample is acid digested and analyzed by differential 
pulse anodic stripping voltammetry. Method D3557-17D. The sample is 
digested with nitric acid and analyzed by graphite furnace atomic 
absorption. The concentration of cadmium in the sample is determined in 
comparison to a standard curve. The changes mirror those for the other 
metals methods. The changes also clarify requirements for a multi-point 
calibration by discussing it in the calibration section as well as the 
QC section of all three procedures. The QC frequencies for method 
blank, CCV, CCB, matrix spike, and duplicate analyses are now based on 
a laboratory-defined batch of up to 20 samples, as opposed to 10 
samples previously.
    25. ASTM Method D3558-15 (A-C), cobalt, AA direct aspiration, 
chelation extraction AA, and AA furnace. Method D3558-15A.The sample is 
acid digested and analyzed by direct aspiration atomic absorption. 
Method D3558-15B.The sample is acid digested, chelated and extracted. 
The extract is analyzed by direct aspiration atomic absorption. Method 
D3558-15C. The sample is acid digested and analyzed by graphite furnace 
atomic absorption. The concentration of cobalt in the sample is 
proportional to the amount of light absorbed during the analysis and is 
determined in comparison to a standard curve. The changes mirror those 
for the other metals methods. The changes also clarify the requirements 
for a multi-point calibration by discussing it in the calibration 
section as well as the QC section of all three procedures. The QC 
frequencies for method blank, CCV, CCB, matrix spike, and duplicate 
analyses are now based on a laboratory-defined batch of up to 20 
samples, as opposed to 10 samples previously.
    26. ASTM Method D3559-15 (A-D), lead, AA direct aspiration, 
voltammetry, AA furnace. Method D3559-15A. The sample is acid digested 
and analyzed by direct aspiration atomic absorption. Method D3559-15B. 
The sample is acid digested, chelated and extracted. The extract is 
analyzed by direct aspiration atomic absorption. Method D3559-15C. The 
sample is acid digested and analyzed by differential pulse anodic 
stripping voltammetry. Method D3559-15D. The sample is digested with 
nitric acid and analyzed by graphite furnace atomic absorption. The 
changes mirror those for the other metals methods. The changes also 
clarify the requirements for a multi-point calibration by discussing it 
in the calibration section as well as the QC section of all three 
procedures. It also adds a new section with the QC requirements to the 
direct AA procedure that was already present in the AA furnace portion 
of this procedure (D3559-15 D).
    27. ASTM Method D3590-17 (A, B), total Kjeldahl nitrogen, manual 
digestion and distillation or gas diffusion; semi-automated block 
digester colorimetric (distillation not required). Method D3590-17A. 
The sample is chemically processed to covert nitrogenous compounds to 
ammonia, then distilled or subjected to a gas diffusion system which 
releases the ammonia for analysis by colorimetry, titrimetry, or 
potentiometry. Method D3590-17B. The digestion and distillation are 
accomplished by a semi-automated system and the resulting ammonia is 
determined by colorimetry of the salicylate/nitroprusside Berthelot 
reaction product. This version changes the acceptance limit for the CCV 
from 10% to 15% and adds a requirement for a CCB. Given that neither 
the approved Standard Methods method for measuring ammonia after the 
TKN digestion, nor the comparable EPA Method 350.1, include a CCV 
requirement or an acceptance limit, the change of the acceptance limit 
from 10% to 15% in the revised ASTM method represents a requirement 
that is more stringent than that required in other approved procedures.
    28. ASTM Method D3645-15, beryllium (A, B), AA direct aspiration AA 
furnace. Method D3645-15A. The sample is acid digested and analyzed by 
direct aspiration atomic absorption. Method D3645-15B. The sample is 
digested with nitric acid and analyzed by graphite furnace atomic 
absorption. This version adds specifications for filter paper. The 
changes also clarify the requirements for a three-point calibration by 
discussing it in the calibration section as well as the QC section of 
both procedures. It also adds a new section with the QC requirements to 
the direct aspiration AA procedure that was already present in the AA 
furnace portion of this procedure (D3645-15B).
    29. ASTM Method D3859-15 (A, B), selenium, AA gaseous hydride, AA 
furnace. Method D3859-15A. The selenium in the sample is converted to 
gaseous selenium hydride, which is then analyzed by flame atomic 
absorption. Method D3859-15B. The selenium in the sample is converted 
to gaseous selenium hydride and analyzed by graphite furnace atomic 
absorption. The changes to the gaseous hydride portion of the method 
clarify the requirement for a 6-point calibration curve by discussing 
it in the calibration section as well as the QC section. The version 
adds an updated discussion of block digesters. The QC frequencies for 
method blank, CCV, CCB, matrix spike, and duplicate analyses are now 
based on a laboratory-defined batch, as opposed to an otherwise 
undefined ``batch.'' The GFAA portion contains similar editorial and 
technical changes. Technical changes also include specifications for 
filter paper. The calibration requirement for three standards has been 
clarified by discussing it in the calibration section as well as the QC 
section.
    30. ASTM Method D3867-16 (A, B) nitrate-nitrite, nitrite and 
nitrate; automated cadmium reduction, manual cadmium reduction, bypass 
cadmium reduction and subtraction. The combination of nitrate and 
nitrite in the sample is determined by reducing the nitrate to nitrite 
using a cadmium-copper column, diazotizing and analyzing in either a 
manual or automated spectrophotometric system. A second aliquot of the 
sample can be analyzed without use of the cadmium

[[Page 27233]]

reduction column to determine the concentration of nitrate by 
difference. The changes add more detailed QC requirements, including 
specifically calling out the laboratory control sample (LCS), method 
blank, and matrix spike analyses. The 2016 version adds specifications 
for filter paper. It also changes the LCS frequency from 10% of samples 
to once per batch (up to 20) and sets the CCB and CCV frequencies at 
10%.
    31. ASTM Method D4190-15, dissolved elements and total recoverable 
elements, direct current plasma. The concentrations of various metal 
elements are determined by acidifying an aliquot of the sample and 
analyzing it by direct current plasma spectrometry, monitoring a 
specific wavelength of light for each element. There is one change that 
adds a requirement to run at least four calibration standards for all 
metals, as opposed to running four standards for only lithium to 
demonstrate linearity.
    32. ASTM Method D4282-15, free cyanide, manual micro-diffusion and 
colorimetry. The sample is treated and allows for free cyanide to 
diffuse into a sodium hydroxide solution. An aliquot of that solution 
is treated to form a colored product that is measured with a 
spectrophotometer at 580 nm. There are no procedural changes.
    33. ASTM Method D4327-17, inorganic anions (fluoride, bromide, 
chloride, nitrite, nitrate, orthophosphate, and sulfate), ion 
chromatography. An aliquot of the sample in injected into an ion 
chromatograph equipped with an anion exchange column and a conductivity 
detector. The anions are identified based on their retention times and 
concentrations are determined by comparison to a standard curve. 
Changes include updating the equipment and reagent descriptions to 
reflect more modern instrumentation, such as the use of hydroxide 
eluents and eluent regeneration systems.
    34. ASTM Method D4382-18, barium, AA furnace. The sample is 
digested with nitric acid and analyzed by graphite furnace atomic 
absorption. The only procedural change is to the description of the hot 
block digester equipment. The new version specifies the capability to 
heat samples between 65 and 95 degrees C, instead of ``approximately 95 
degrees C.'' That change recognizes the operational characteristics of 
hot block digesters that will experience a temperature drop below 95 
degrees when samples are added. EPA has concluded that this should not 
adversely affect use of this method for barium.
    35. ASTM Method D4658-15, sulfide ion, ion selective electrode. The 
sample is treated with a sulfide antioxidant buffer to create a highly 
alkaline solution. Sulfide in the sample is measured potentiometrically 
with an ion-selective electrode. There are no procedural changes.
    36. ASTM Method D4839-03 (Reapproved 2017), total organic carbon; 
heated persulfate or UV persulfate oxidation. The sample is sparged 
with an inert gas to remove dissolved inorganic carbon and then treated 
with persulfate and either heat or UV radiation to convert organic 
carbon to carbon dioxide. The carbon dioxide is measured with an infra-
red detector. There are no procedural changes.
    37. ASTM Method D5257-17, dissolved hexavalent chromium, ion 
chromatography. The sample is filtered and buffered, and an aliquot 
injected into an ion chromatograph that separates hexavalent chromium 
from other ions. The eluent from the chromatograph is treated with an 
acidic solution of diphenylcarbohydrazide to form a violet-colored 
product that is measured with a photometric detector at 530 nm. The 
changes also include a few additional cautions and recommendations.
    38. ASTM Method D5673-16, dissolved elements and total-recoverable 
elements, ICP/MS. The sample is acid digested and analyzed by 
inductively coupled plasma/mass spectrometry. Gold was added to the 
list of target analytes. Some of the changes address the analysis of 
gold.
    39. ASTM Method D6508-15, inorganic anions (fluoride, bromide, 
chloride, nitrite, nitrate, orthophosphate, and sulfate), capillary ion 
electrophoresis with indirect UV detection. An aliquot of the sample is 
injected into a capillary ion electrophoresis instrument where the 
anions are separated in an applied electric field through a fused 
silica capillary. The analytes are detected by a UV detector and their 
concentrations are determined by comparison to a standard curve. There 
are no procedural changes.
    40. ASTM Method D6888-16, available cyanide, flow injection and 
ligand exchange, followed by gas diffusion amperometry. An aliquot of 
the sample is introduced into a flow injection analysis instrument, 
where available cyanide is acidified to form hydrogen cyanide which 
diffuses through a hydrophobic gas diffusion membrane into an alkaline 
solution and is detected amperometrically with a silver electrode. This 
version adds a new mixed ligand exchange reagent, but also retains the 
original two ligand reagents that had to be mixed together during the 
testing.
    41. ASTM Method D6919-17, inorganic alkali and alkaline earth 
cations and ammonium (ammonium, calcium magnesium, potassium and 
sodium), ion chromatography. An aliquot of the sample is injected into 
an ion chromatograph equipped with a cation exchange column and a 
conductivity detector. The cations are identified based on their 
retention times and concentrations are determined by comparison to a 
standard curve. There are no procedural changes.
    42. ASTM Method D7237-15 A, free cyanide, flow injection, followed 
by gas diffusion amperometry. An aliquot of the sample is introduced 
into a flow injection analysis instrument, where it mixes with a 
phosphate buffer to release hydrogen cyanide which diffuses through a 
hydrophobic gas diffusion membrane into an alkaline solution and is 
detected amperometrically with a silver electrode. There are a few 
additions and changes to the newer version of note. These include 
changing the applicable range of the method in Section 1.4 at the low 
end, from 2 to 500 [micro]g/L to 5 to 500 [micro]g/L. New information 
about interferences from floatation reagents has been added to Section 
6.3. New materials in Section 8 discuss alternative reagents or 
concentrations.
    43. ASTM Method D7284-13 (Reapproved 2017), total cyanide, manual 
distillation with MgCl2 followed by flow injection, gas 
diffusion amperometry. The sample is distilled with acid and a 
magnesium chloride catalyst to release cyanide to a sodium hydroxide 
solution. An aliquot of the sodium hydroxide solution is introduced 
into a flow injection analysis instrument, where it is acidified, and 
the hydrogen cyanide diffuses through a hydrophobic gas diffusion 
membrane into an alkaline solution and is detected amperometrically 
with a silver electrode. There are no procedural changes.
    44. ASTM Method D7511-12 (Reapproved 2017), total cyanide, 
segmented flow injection, in-line ultraviolet digestion, followed by 
gas diffusion amperometry. The sample is introduced into a segmented 
flow injection analysis instrument, where UV light releases cyanide 
from cyanide complexes. The sample is then acidified in the instrument 
and the produced cyanide gas is detected amperometrically with a silver 
electrode. There are no procedural changes.
    45. ASTM Method D7573-09 (Reapproved 2017), total organic carbon,

[[Page 27234]]

combustion. The sample is sparged with an inert gas to remove dissolved 
inorganic carbon, acidified, and then combusted at high temperature 
convert organic carbon to carbon dioxide. The carbon dioxide is 
measured with an infra-red detector. There are no procedural changes.
    EPA is promulgating the following changes to Table IC at 40 CFR 
part 136:
    1. ASTM Method D7065-17, nonylphenol, bisphenol A, p-tert-
octylphenol, nonylphenol monoethoxylate, nonylphenol diethoxylate, gas 
chromatography/mass spectrometry (GC/MS). The sample is extracted with 
methylene chloride and the extract is injected into a gas 
chromatograph-mass spectrometer. The target analytes are identified by 
retention time and mass spectra and quantified using internal standards 
and a calibration curve. There are a large number of editorial and 
structural changes in the document, and a new QC section has been 
added.

F. Changes to 40 CFR 136.3 To Include a New ASTM Method Based on 
Previously Approved Technologies

    EPA is promulgating these changes in furtherance of the National 
Technology Transfer and Advancement Act of 1995 (NTTAA), Public Law 
104-113, that provides that federal agencies and departments shall use 
technical standards developed or adopted by the VCSBs if compliance 
would not be inconsistent with applicable law or otherwise 
impracticable. This method submitted by ASTM is consistent with other 
already approved methods.
    EPA is adding ASTM Method D7781-14 to Table IB for nitrate-nitrite, 
nitrite (bypass the enzymatic reduction step) and nitrate by 
subtraction. Nitrate is reduced to nitrite by an enzymatic reaction. 
The nitrite is diazotized to yield an azo dye which is measured 
colorimetrically. The enzyme reduction step may be by-passed for 
measurement of nitrite singly. The value obtained for nitrite may be 
subtracted from the value obtained for combined nitrate-nitrite to 
calculate the concentration of nitrate. This method is similar to the 
currently approved NECi Method N07-0003, USGS Method I-2547-11, and 
USGS Method I-2548-11.

G. Changes to 40 CFR 136.3 To Include New United States Geological 
Survey (USGS) Inorganic Methods Based on Previously Approved 
Technologies

    1. EPA is adding USGS Method I-2057-85 titled ``Anions, ion-
exchange chromatographic, automated,'' to Table IB for bromide. Method 
I-2057-85 is an ion chromatography method that lists several target 
analytes: Bromide, chloride, fluoride, nitrate, nitrite, 
orthophosphate, and sulfate. These are the same target analytes found 
in EPA Methods 300.0 (Part A) and 300.1 (Part A). Both EPA methods are 
approved in 40 CFR part 136 for the target analytes listed in the 
methods. USGS Method I-2057-85 is similar to EPA Method 300.0, in that 
it uses ion chromatography with a sodium bicarbonate/sodium carbonate 
eluent and has the same target analyte list. The two methods specify 
different columns and eluent concentrations but rely on essentially the 
same underlying chemistry and determinative technique as other ion 
chromatography methods approved at 40 CFR part 136 for measurement of 
bromide. That is, the sample is introduced into an ion chromatograph. 
The anions of interest are separated and measured, using a system 
comprised of a guard column, analytical column, suppressor device, and 
conductivity detector.
    2. EPA is adding USGS Method I-2522-90 titled ``Nitrogen, ammonia, 
colorimetry, salicylate-hypochlorite, automated-segmented flow'' to 
Table IB for ammonia. USGS Method I-2522-90 uses the same underlying 
chemistry and determinative technique as other methods approved at 40 
CFR part 136 for measurement of ammonia. The method is similar to other 
approved methods, such as EPA Method 350.1, Standard Methods Method 
4500-NH3 G, and USGS Method I-4523-85, which rely on the Berthelot 
reaction. USGS Method I-2522-90 uses a modified version of the 
Berthelot reaction in which salicylate and hypochlorite react with 
ammonia in the presence of ferricyanide ions to form the salicylic 
analog of indophenol blue dye. The resulting color is directly 
proportional to the concentration of ammonia present and is measured 
using automated spectrophotometry. This is a well-documented 
modification to the Berthelot reaction used in EPA Method 351 and is 
specifically allowed in Table IB.
    3. EPA is adding USGS Method I-2540-90 titled ``Nitrogen, nitrite, 
colorimetry, diazotization, automated-segmented flow'' to Table IB for 
nitrite. USGS Method I-2540-90 employs the same underlying chemistry 
and determinative technique as other methods approved at 40 CFR part 
136 for measurement of nitrite. The method is similar to other methods 
approved at 40 CFR part 136 for measurement of nitrite, including USGS 
Method I-4540-85, which uses an automated-segmented flow analyzer 
(Technicon AA II). Method I-2540-90, nitrite reacts with sulfanilamide 
under acidic conditions to form a diazo compound which is coupled with 
N-1-naphthylethylenediamine dihydrochloride to form a red compound, the 
absorbance of which is measured using an automated-segmented flow, 
spectrophotometry.
    4. EPA is adding USGS Method I-2601-90 titled ``Phosphorus, 
orthophosphate, colorimetry, phosphomolybdate, automated-segmented 
flow'' to Table IB for orthophosphate. USGS Method I-2601-90 employs 
the same underlying chemistry and determinative technique as other 
methods approved in 40 CFR part 136 for measurement of orthophosphate. 
Orthophosphate reacts with ammonium molybdate in acidic solution to 
form phosphomolybdic acid, which upon reduction with ascorbic acid 
produces an intensely blue complex the absorbance of which is measured 
using automated spectrophotometry. Antimony potassium tartrate is added 
to increase the rate of reduction. The method is similar to other 
approved methods, such as USGS Method I-4601-85 which uses an 
automated-segmented flow analyzer (Technicon AA II). The submitted USGS 
Method I-2601-90 also uses an automated-segmented flow analyzer (Alpkem 
rapid flow analyzer). It should be noted that the approved USGS Method 
I-4601-85 has two parameter codes listed:
    a. Phosphorus, orthophosphate, dissolved, I-2601-85 (mg/L as P); 
and
    b. Phosphorus, orthophosphate, total, I-4601-85 (mg/L as P).

Although USGS Method I-4601-85 is listed in Table IB, samples to be 
used for measurement of orthophosphate are to be filtered upon 
collection as provided in Table II. Therefore, the correct parameter 
code listed for the method should have been I-2601-85. I-2601-90 is 
just an updated version of that method (parameter code). In Section 3--
Interferences, USGS Method I-2601-85 states: ``Because as phosphorus is 
easily adsorbed on sediment, the orthophosphate recovered from the 
supernatant solution above a water-suspended sediment after some time 
has elapsed may be less than the orthophosphate that would have been 
determined in the filtrate from a sample filtered at the time of 
collection. The amount recovered may also depend on the type of 
sediment (clay, sand, etc.).''
    5. EPA is adding USGS Method I-4472-97 titled ``Metals, Acid 
Digestion, Whole-Water Recoverable, inductively coupled plasma-mass 
spectrometry'' to Table IB for certain

[[Page 27235]]

metals by ICP/MS. USGS Method I-4472-97 is an ICP/MS method that was 
previously listed under the same method number as the USGS ICP/AES 
Method I-4471-97 and was split out and assigned a unique method number 
by USGS in 2003. EPA is adding this to Table IB on the line for ICP/MS 
and replace USGS Method I-4471-97 as an approved method for measurement 
of the following 16 elements: Aluminum, antimony, barium, beryllium, 
cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, 
selenium, silver, thallium and zinc. USGS Method I-4472-97 relies on 
the same underlying chemistry and determinative technique as other ICP/
MS methods approved at 40 CFR part 136 for measurement of the same 16 
elements (e.g., EPA Method 200.8 and Standard Methods Method 3125 B) 
where analytes in the sample are solubilized by gentle refluxing with 
acids and then measured using inductively coupled plasma-mass 
spectrometry.

H. Changes to 40 CFR 136.3 To Include New United States Geological 
Survey (USGS) Organic Methods Based on Previously Approved Technologies

    1. EPA is adding USGS Method O-4127-96 titled ``Determination of 86 
Volatile Organic Compounds in Water by Gas Chromatography/Mass 
Spectrometry, Including Detections Less Than Reporting Limits'' to 
Table IC for certain organic compounds. USGS Method O-4127-96 relies on 
the same underlying chemistry and determinative technique as other 
methods approved at 40 CFR part 136 for measurement of the analytes. 
Volatile organic compounds are extracted by purging with helium, 
collected on a sorbent trap, thermally desorbed, separated by a gas 
chromatographic capillary column, and finally determined by a 
quadrupole mass spectrometer operated in full-scan mode. Compound 
identification is confirmed by the gas chromatographic retention time 
and by the resultant mass spectrum, typically identified by three 
unique ions.
    2. EPA is adding USGS Method O-4436-16 titled ``Determination of 
Heat Purgeable and Ambient Purgeable Volatile Organic Compounds in 
Water by Gas Chromatography/Mass Spectrometry'' to Table IC for certain 
organic compounds. USGS Method O-4436-16 relies on the same underlying 
chemistry and determinative technique as other methods approved at 40 
CFR part 136 for measurement of the analytes. Volatile organic 
compounds are extracted from a water sample and compounds are trapped 
in a tube containing suitable sorbent materials and then thermally 
desorbed into a capillary gas chromatographic column interfaced to a 
mass spectrometer system. Selected compounds are identified by using 
strict qualification criteria, which include analyzing standard 
reference materials and comparing retention times and relative ratios 
of the mass spectra. Compounds are quantitated using internal standard 
procedures.

I. Changes to 40 CFR 136.3 To Include Alternate Test Procedures (ATPs)

    To promote method innovation, EPA maintains a program that allows 
method developers to apply for EPA review and potential approval of an 
alternative method to an existing EPA approved method. This ATP program 
is described for CWA applications at 40 CFR 136.4 and 136.5. EPA is 
promulgating three ATPs for nationwide use. Based on EPA's review, the 
performance of these ATPs is equally effective as other methods already 
approved for measurement. The ATP applicants supplied EPA with study 
reports that contain the data from their validation studies that 
support EPA's conclusion that the ATPs are equally effective to 
currently approved methods. These study reports and the letters 
documenting EPA's review are contained as supporting documents within 
the docket for this final rule. These new methods include: FIAlab 
Method 100, ``Determination of Inorganic Ammonia by Continuous Flow Gas 
Diffusion and Fluorescence Detector Analysis,'' MACHEREY-NAGEL GmbH and 
Co. Method 036/038 NANOCOLOR[supreg] COD LR/HR, ``Spectrophotometric 
Measurement of Chemical Oxygen Demand in Water and Wastewater,'' and 
Micrology Laboratories, LLC. KwikCount^TM EC Medium 
Escherichia coli (E. coli) enzyme substrate test, ``Rapid Detection of 
E. coli in Beach Water by KwikCount^TM EC Membrane 
Filtration.'' Descriptions of these new methods are as follows:
    1. FIAlab Instruments, Inc. Method 100, ``Determination of 
Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence 
Detector Analysis,'' dated April 4, 2018 (FIAlab Instruments, Inc. 
2018a). FIAlab Method 100 uses automated flow injection analysis with 
gas diffusion and fluorescence detector analysis to determine 
concentrations of ammonia in wastewater, ambient water, and Kjeldahl 
digestates. FIAlab Method 100 can be obtained from FIAlab Instruments, 
Inc., 2151 N Northlake Way, Seattle, WA 98103. Telephone: 425-376-0450.
    2. MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR[supreg] COD 
LR/HR, ``Spectrophotometric Measurement of Chemical Oxygen Demand in 
Water and Wastewater,'' Revision 1.5, dated, May 2018 (MACHEREY-NAGEL 
GmbH and Co. 2018a). MACHEREY-NAGEL Method 036/038 NANOCOLOR[supreg] 
COD LR/HR is a manual method that uses spectrophotometry to measure 
chemical oxygen demand in wastewater. MACHEREY-NAGEL GmbH and Co. 
Method 036/038 NANOCOLOR[supreg] COD LR/HR, can be obtained from 
MACHEREY-NAGEL GmbH and Co., 2850 Emrick Blvd., Bethlehem, PA 18020. 
Telephone: 888-321-6224.
    3. Micrology Laboratories LLC. KwikCount^TM EC Medium E. 
coli enzyme substrate test, ``Rapid Detection of E. coli in Beach Water 
by KwikCount^TM EC Membrane Filtration'' uses a membrane 
filtration procedure for rapid detection and enumeration of E. coli in 
ambient water. The KwikCount^TM EC Medium E. coli enzyme 
substrate test can be obtained from Micrology Laboratories, LLC, 1303 
Eisenhower Drive, Goshen, IN 46526. Telephone: 574-533-3351.

J. Changes to 40 CFR 136.3, Tables IA, IB, and IH

    EPA is promulgating the following changes to 40 CFR 136.3, Tables 
IA and IH:
    1. Table IA: Moving Colilert-18 from Parameter #1 Coliform (fecal), 
number per 100 mL or number per gram dry weight, to Parameter #2 
Coliform (fecal), (number per 100 mL), to eliminate confusion as to 
whether it is approved for sewage sludge in addition to wastewater.
    2. Table IA: Adding E. coli, number per 100 mL-MF, two-step, 
Standard Methods Method 9222 B/9222 I, to the table along with footnote 
31 ``Subject coliform positive samples determined by 9222 B-2015 or 
other membrane filter procedure to 9222 I-2015 using NA-MUG media.'' 
The method was inadvertently omitted from Table IA when Table IA was 
split into two tables (IA and IH) in an earlier rulemaking; the 
addition corrects that error.
    3. Table IA: Revising Parameter #2 Coliform (fecal), deleting ``in 
presence of chlorine,'' number per 100 mL. The phrase ``in the presence 
of chlorine'' caused confusion because the methods cited were the same 
for the analyte/matrix combination that did not state ``in the presence 
of chlorine.'' The approved methods did not change.

[[Page 27236]]

    4. Table IA: Deleting Parameter #4 Coliform (total) in presence of 
chlorine, number per 100 mL. Except for ``MF with enrichment,'' all the 
methods were duplicative (e.g., Parameters #3 and #4). No approved 
methods for coliform (total) were removed from Table IA.
    5. Table IH: Deleting Parameters #2 Coliform (fecal) in presence of 
chlorine, number per 100 mL and #4 Coliform (total) in presence of 
chlorine, number per 100 mL. Except for ``MF with enrichment'' for 
coliform (total), all the methods were duplicative (e.g., Parameters #1 
and #2). In addition to the methods being duplicative, Table IH is for 
ambient water which would not be expected to contain chlorine. No 
approved methods for coliform (fecal) or coliform (total) were removed 
from Table IH. The remaining parameters are renumbered.
    6. Tables IA and IH: Revising footnote 13 to Table IA and footnote 
12 to Table IH as follows ``These tests are collectively known as 
defined enzyme substrate tests.'' The remaining text, ``where, for 
example, a substrate is used to detect the enzyme [beta]-glucuronidase 
produced by E. coli'' has been deleted because the example has caused 
some confusion to stakeholders.
    7. Tables IA and IH: Adding Quanti-Tray[supreg]/2000 as an option 
to footnotes 13 (IH), 15 (IH), 16 (IA) and 18 (IA). The addition of 
Quanti-Tray[supreg]/2000 is to address matrices with high bacterial 
concentrations and to ensure Tables IA and IH are accurate and 
consistent.
    8. Tables IA and IH: Adding footnote 30 to Table IA and footnote 27 
to Table IH to specify a verification procedure. The footnotes contain 
the following language: ``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.'' Adding the footnotes addresses the change in Standard 
Methods Method 9222 B-2015 that stated that five typical and five 
atypical colonies should be verified per membrane, which could be 
burdensome to laboratories analyzing samples other than drinking water. 
In most cases, analysis of ambient waters and wastewaters could result 
in multiple plates per sample with typical and atypical colonies, 
whereas drinking water analyses would seldom result in any typical or 
atypical colonies. In addition, the language in footnotes 29 (IA) and 
26 (IH), was revised as follows ``the medium'' was replaced with 
``positive samples'' for clarity and consistency.
    9. Tables IA and IH: Adding footnote 32 to Table IA and footnote 30 
to Table IH. The footnotes contain the following language 
``Verification of colonies by incubation of BHI agar at 10  
0.5 [deg]C for 48  3 h is optional.'' As per the Errata to 
the 23rd Edition of Standard Methods for the Examination of Water & 
Wastewater, ``Growth on a BHI agar plate incubated at 10  
0.5 [deg]C for 48  3 h is further verification that the 
colony belongs to the genus Enterococcus.''
    10. Updating the Aquatic Toxicity Table to include the editorial 
correction from publex to pulex and adding the common names of the 
genus and species.
    11. Table IH: Deleting ``or number per gram dry weight'' from 
Parameter #1. Table IH is specifically for ambient waters, which does 
not require reporting results on a per gram dry weight basis.
    12. Table IH: Adding the Alternate Test Procedure 
KwikCount^TM EC for E. coli, number per 100 mL under 
``Other.''
    13. Table IH: Adding EPA Method 1623.1 for Parameters 6 and 7. EPA 
Method 1623.1 includes updated acceptance criteria for IPR, OPR, and 
MS/MSD, and clarifications and revisions based on the use of EPA Method 
1623 and technical support questions over the past 19 years. EPA is 
approving the use of both methods 1623 and 1623.1 for Parameters 6 and 
7.
    14. Table IH: Deleting footnote 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.'' Table IH is specifically for ambient waters, so the 
footnote is not applicable. The remaining footnotes are renumbered 
accordingly.
    15. Table IH: Revising footnote 20, to reference only EPA Method 
1604. The literature reference was deleted from the footnote because it 
resulted in confusion as to whether EPA Method 1604 provided all the 
necessary information required by stakeholders to conduct analyses of 
ambient waters under the CWA.

K. Changes to Table II at 40 CFR 136.3(e) to Required Containers, 
Preservation Techniques, and Holding Times

    EPA is updating footnote 6 to the preservation and holding time 
requirements for cyanide to cite the latest version of ASTM method 
D7365-09a that was reapproved in 2015. The recommended sampling and 
preservation procedures in the ASTM method have not changed since 2009, 
but the change to footnote 6 will simplify identification of the 
current method that is available from ASTM International.
    EPA is adding a call-out to footnote 9 to the preservation and 
holding time requirements for the purgeable halocarbons entry. This 
will allow the flexibility to collect a single sample with no 
acidification to be used for analysis of both purgeable halocarbons and 
purgeable aromatic hydrocarbons within seven days of collection, or to 
collect a single sample with acidification to be used for analysis of 
both purgeable halocarbons (except 2-CEVE) and purgeable aromatic 
hydrocarbons within the 14-day maximum holding time specified in Table 
II for both classes of compounds. The added flexibility is consistent 
with historical requirements for preservation in 40 CFR part 136 and 
holding time requirements in other EPA program methods, such as the SW-
846 methods in the Office of Land and Emergency Management. This is 
part of EPA's ongoing effort to harmonize methods between EPA programs, 
as requested by the Environmental Laboratory Advisory Board (ELAB).
    Footnote 9 to Table II states: ``If the sample is not adjusted to 
pH 2, then the sample must be analyzed within seven days of sampling.''

L. Changes to 40 CFR 136.6 Method Modifications and Analytical 
Requirements

    In response to requests from ELAB and the Independent Laboratories 
Institute, EPA is adding a new paragraph (b)(4)(xviii) to 40 CFR 136.6 
that explicitly allows the use of closed-vessel microwave digestion as 
a modification to the approved metals digestion procedure that does not 
require prior approval. Microwave digestion has the same fundamental 
chemistry as a hot plate digestion, both the microwave and hot plate 
serve the same function as heat sources.

VI. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review and Executive 
Order 13563: Improving Regulation and Regulatory Review

    This rule is not a significant regulatory action and was therefore 
not submitted to the Office of Management and Budget (OMB) for 
interagency review under this E.O.

B. Paperwork Reduction Act

    This action does not impose an information collection burden under 
the

[[Page 27237]]

Paperwork Reduction Act. This rule does not impose any information 
collection, reporting, or recordkeeping requirements. This rule merely 
adds or revises CWA test procedures.

C. Regulatory Flexibility Act

    I certify that this action would not have a significant economic 
impact on a substantial number of small entities under the Regulatory 
Flexibility Act. This action will not impose any requirements on small 
entities. This action would approve new and revised versions of CWA 
testing procedures. Generally, these changes have a positive impact on 
small entities by increasing method flexibility, thereby allowing 
entities to reduce costs by choosing more cost-effective methods. In 
general, EPA expects the final revisions will lead to few, if any, 
increased costs. As explained previously, most of the changes clarify 
or improve the instructions in the method, update the technology used 
in the method, improve the QC instructions, make editorial corrections, 
or reflect the most recent approval year of an already approved method. 
In some cases, they would add alternatives to currently approved 
methods for a particular analyte (e.g., Method N07-0003 for Nitrate 
Reductase Nitrate-Nitrogen Analysis). Because these methods would be 
alternatives rather than requirements, there are no direct costs 
associated with this proposal. EPA finalized methods that would be 
incorporated by reference. If a permittee elected to use these methods, 
they could incur a small cost associated with obtaining these methods 
from the listed sources. See Section IV.B of this preamble.

D. Unfunded Mandates Reform Act

    This action does not contain any unfunded mandate as described in 
the Unfunded Mandates Reform Act, 2 U.S.C. 1531-1538, and does not 
significantly or uniquely affect small governments. The action imposes 
no enforceable duty on any state, local or tribal governments or the 
private sector.

E. Executive Order 13132: Federalism

    This final rule does not have federalism implications. It will not 
have substantial direct effects on the states, on the relationship 
between the national government and the states, or on the distribution 
of power and responsibilities among the various levels of government.

F. Executive Order 13175: Consultation and Coordination With Indian 
Tribal Governments

    This final rule does not have tribal implications as specified in 
Executive Order 13175. This rule merely approves new and revised 
versions of test procedures. EPA has concluded that the final rule 
would not lead to any costs to any tribal governments, and in the event 
there are any, EPA projects they would be minimal. Thus, Executive 
Order 13175 does not apply to this action.

G. Executive Order 13045: Protection of Children From Environmental 
Health Risks and Safety Risks

    EPA interprets Executive Order 13045 as applying only to those 
regulatory actions that concern environmental health or safety risks 
that EPA has reason to believe may disproportionately affect children, 
per the definition of ``covered regulatory action'' in section 2-202 of 
the Executive Order. This action is not subject to Executive Order 
13045 because it does not concern an environmental health risk or 
safety risk.

H. Executive Order 13211: Actions That Significantly Affect Energy 
Supply, Distribution, or Use

    This action is not subject to Executive Order 13211 because it is 
not a significant regulatory action under Executive Order 12866.

I. National Technology Transfer and Advancement Act of 1995

    This action involves technical standards. EPA is approving the use 
of technical standards developed and recommended by the Standard 
Methods Committee and ASTM International for use in compliance 
monitoring where EPA determined that those standards meet the needs of 
CWA programs. As described above, the final rule is consistent with the 
NTTAA.

J. Executive Order 12898: Federal Actions To Address Environmental 
Justice in Minority Populations and Low-Income Populations

    EPA has concluded that this action will not have potential 
disproportionately high and adverse human health or environmental 
effects on minority, low-income or indigenous populations.

L. Congressional Review Act

    This action is subject to the Congressional Review Act and EPA will 
submit a rule report to each House of the Congress and to the 
Comptroller General of the United States. This action is not a ``major 
rule'' as defined by 5 U.S.C. 804(2).

List of Subjects in 40 CFR Part 136

    Environmental protection, Incorporation by reference, Reporting and 
recordkeeping requirements, Test procedures, Water pollution control.

Michael S. Regan,
Administrator.

    For the reasons set out in the preamble, the EPA amends 40 CFR part 
136 as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS 
OF POLLUTANTS

0
1. The authority citation for part 136 continues to read as follows:

    Authority: Secs. 301, 304(h), 307 and 501(a), 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).


0
2. Amend Sec.  136.3:
0
a. In paragraph (a):
0
i. In the introductory text, in the seventh sentence, by removing the 
word ``year'' and adding in its place the word ``date'', and removing 
from the last sentence the text ``(paragraph (c) of this section, in 
Sec.  136.5(a) through (d) or 40 CFR 401.13)'' and adding in its place 
the text ``paragraph (c) of this section, Sec.  136.5(a) through (d) or 
40 CFR 401.13,'' respectively;
0
ii. By revising tables IA, IB, IC, and IH;
0
b. In paragraph (b) by:
0
i. Revising the introductory text; paragraph (b)(8) introductory text, 
and paragraphs (b)(8)(ix) through (xv);
0
ii. Adding paragraph (b)(8)(xvi);
0
iii. Revising paragraphs (b)(10)(xiv), (xxxix), (xliv), (xlvi), (lii), 
(liv), and (lxvii) through (lxx), (b)(15)(v), (vi), (viii) through 
(xiii), (xv) through (xix), (xxi) through (xxvi), (xxxi), (xxxiv), 
(xxxv), (xxxvii), (xxxix) through (xliii), (xlv) through (l), (lii), 
(liv), (lv), (lviii), (lxi) through (lxvi), (lxviii), and (lxix);
0
iv. Adding paragraph (b)(15)(lxx);
0
v. Redesignating paragraphs (b)(25) through (36) as paragraphs (b)(28) 
through (39);
0
vi. Redesignating paragraphs (b)(19) through (24) as paragraphs (b)(20) 
through (25);
0
vii. Adding new paragraphs (b)(19), (26), and (27);
0
viii. Revising the newly redesignated paragraphs (b)(38)(ii) through 
(xxi);
0
ix. Adding paragraphs (b)(38)(xxii) and (xxiii); and
0
c. By revising table II in paragraph (e).
    The revisions and additions read as follows:

[[Page 27238]]

Sec.  136.3   Identification of test procedures.

* * * * *

                                     Table IA--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                 Method \1\                   EPA              Standard methods      AOAC, ASTM, USGS            Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Bacteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Coliform (fecal), number per     Most Probable Number        p. 132,3 1680,11 15    9221 E-2014..........
 100 mL or number per gram dry       (MPN), 5 tube, 3            1681 11 20.
 weight.                             dilution, or.
                                    Membrane filter (MF) 2 5,   p. 124 3.............  9222 D-2015 29.......  B-0050-85 4.........
                                     single step.
2. Coliform (fecal), number per     MPN, 5 tube, 3 dilution,    p. 132 3.............  9221 E-2014; 9221 F-
 100 mL.                             or.                                                2014 33.
                                    Multiple tube/multiple      .....................  .....................  ....................  Colilert-
                                     well, or.                                                                                       18[supreg].13 18 28
                                    MF 2 5, single step 5.....  p. 124 3.............  9222 D-2015 29.......
3. Coliform (total), number per     MPN, 5 tube, 3 dilution,    p. 114 3.............  9221 B-2014..........
 100 mL.                             or.
                                    MF 2 5, single step or two  p. 108 3.............  9222 B-2015 30.......  B-0025-85 4.........
                                     step.
                                    MF 2 5, with enrichment...  p. 111 3.............  9222 B-2015 30.......
4. E. coli, number per 100 mL.....  MPN 6 8 16 multiple tube,   .....................  9221 B2014/9221 F-
                                     or.                                                2014 12 14 33.
                                    multiple tube/multiple      .....................  9223 B-2016 13.......  991.15 10...........  Colilert[supreg] 13
                                     well, or.                                                                                       18
                                                                                                                                    Colilert-18[supreg]
                                                                                                                                     13 17 18
                                    MF 2 5 6 7 8, two step, or  .....................  9222 B-2015/9222 I-
                                                                                        2015 31.
                                    Single step...............  1603 21..............  .....................  ....................  m-
                                                                                                                                     ColiBlue24[supreg].
                                                                                                                                     19
5. Fecal streptococci, number per   MPN, 5 tube, 3 dilution,    p. 139 3.............  9230 B-2013..........
 100 mL.                             or.
                                    MF 2, or..................  p. 136 3.............  9230 C-2013 32.......  B-0055-85 4.........
                                    Plate count...............  p. 143 3.............
6. Enterococci, number per 100 mL.  MPN, 5 tube, 3 dilution,    p. 139 3.............  9230 B-2013..........
                                     or.
                                    MPN 6 8, multiple tube/     .....................  9230 D-2013..........  D6503-99 9..........  Enterolert[supreg].1
                                     multiple well, or.                                                                              3 23
                                    MF 2 5 6 7 8 single step    1600 24..............  9230 C-2013 32.......
                                     or.
                                    Plate count...............  p. 143 3.............
7. Salmonella, number per gram dry  MPN multiple tube.........  1682 22..............
 weight 11.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                    Aquatic Toxicity
--------------------------------------------------------------------------------------------------------------------------------------------------------
8. Toxicity, acute, fresh water     Water flea, Cladoceran,     2002.0 25............
 organisms, LC50, percent effluent.  Ceriodaphnia dubia acute.
                                    Water fleas, Cladocerans,   2021.0 25............
                                     Daphnia pulex and Daphnia
                                     magna acute.
                                    Fish, Fathead minnow,       2000.0 25............
                                     Pimephales promelas, and
                                     Bannerfin shiner,
                                     Cyprinella leedsi, acute.
                                    Fish, Rainbow trout,        2019.0 25............
                                     Oncorhynchus mykiss, and
                                     brook trout, Salvelinus
                                     fontinalis, acute.
9. Toxicity, acute, estuarine and   Mysid, Mysidopsis bahia,    2007.0 25.
 marine organisms of the Atlantic    acute.                     2004.0 25............
 Ocean and Gulf of Mexico, LC50,    Fish, Sheepshead minnow,    2006.0 25............
 percent effluent.                   Cyprinodon variegatus,
                                     acute.
                                    Fish, Silverside, Menidia
                                     beryllina, Menidia
                                     menidia, and Menidia
                                     peninsulae, acute.
10. Toxicity, chronic, fresh water  Fish, Fathead minnow,       1000.0 26............
 organisms, NOEC or IC25, percent    Pimephales promelas,
 effluent.                           larval survival and
                                     growth.
                                    Fish, Fathead minnow,       1001.0 26............
                                     Pimephales promelas,
                                     embryo-larval survival
                                     and teratogenicity.
                                    Water flea, Cladoceran,     1002.0 26............
                                     Ceriodaphnia dubia,
                                     survival and reproduction.
                                    Green alga, Selenastrum     1003.0 26............
                                     capricornutum, growth.
11. Toxicity, chronic, estuarine    Fish, Sheepshead minnow,    1004.0 27.
 and marine organisms of the         Cyprinodon variegatus,     .....................
 Atlantic Ocean and Gulf of          larval survival and        .....................
 Mexico, NOEC or IC25, percent       growth.                    1005.0 27............
 effluent.                          Fish, Sheepshead minnow,
                                     Cyprinodon variegatus,
                                     embryo-larval survival
                                     and teratogenicity.
                                    Fish, Inland silverside,    1006.0 27............
                                     Menidia beryllina, larval
                                     survival and growth.
                                    Mysid, Mysidopsis bahia,    1007.0 27............
                                     survival, growth, and
                                     fecundity.
                                    Sea urchin, Arbacia         1008.0 27............
                                     punctulata, fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:
\1\ The method must be specified when results are reported.

[[Page 27239]]

 
\2\ A 0.45-[micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water and Wastes, EPA/600/8-78/017. 1978. U.S. EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
  organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
  results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
\11\ Recommended for enumeration of target organism in sewage sludge.
\12\ The multiple-tube fermentation test is used in 9221B.2-2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.
\13\ These tests are collectively known as defined enzyme substrate tests.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.2-2014, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2014. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\15\ Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-
  14-009. September 2014. U.S. EPA.
\16\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000 and the MPN calculated from the table provided by the manufacturer.
\17\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\18\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories, Inc.
\19\ A description of the mColiBlue24[supreg] test is available from Hach Company.
\20\ Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
\21\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified
  mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.
\22\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014.
  U.S. EPA.
\23\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\24\ Method 1600: Enterococci in Water by Membrane Filtration Using Membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-14-011.
  September 2014. U.S. EPA.
\25\ Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA-821-R-02-012. Fifth Edition,
  October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\26\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA-821-R-02-013. Fourth Edition,
  October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\27\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA-821-R-02-014. Third
  Edition, October 2002. U.S. EPA; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\28\ To use Colilert-18[supreg] to assay for fecal coliforms, the incubation temperature is 44.5  0.2 [deg]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 [deg]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 [deg]C for 48
   3 h is further verification that the colony belongs to the genus Enterococcus.''
\33\ 9221 F.2-2014 allows for simultaneous detection of E. coli and thermotolerant fecal coliforms by adding inverted vials to EC-MUG; the inverted
  vials collect gas produced by thermotolerant fecal coliforms.


                                                  Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                   Methodology \58\              EPA \52\        Standard methods \84\          ASTM             USGS/AOAC/other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L........  Electrometric endpoint or   .....................  2310 B-2011..........  D1067-16............  I-1020-85.\2\
                                     phenolphthalein endpoint.
2. Alkalinity, as CaCO3, mg/L.....  Electrometric or            .....................  2320 B-2011..........  D1067-16............  973.43,\3\ I-1030-
                                     Colorimetric titration to                                                                       85.\2\
                                     pH 4.5, Manual.
                                    Automatic.................  310.2 (Rev. 1974) \1\  .....................  ....................  I-2030-85.\2\
3. Aluminum--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 D-2011 or 3111 E- ....................  I-3051-85.\2\
                                                                                        2011.
                                    AA furnace................  .....................  3113 B-2010.
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994)/
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    Direct Current Plasma       .....................  .....................  D4190-15............  See footnote.\34\
                                     (DCP) \36\.
                                    Colorimetric (Eriochrome    .....................  3500-Al B-2011.
                                     cyanine R).
4. Ammonia (as N), mg/L...........  Manual distillation \6\ or  350.1, Rev. 2.0        4500-NH3 B-2011......  ....................  973.49.\3\
                                     gas diffusion (pH > 11),    (1993).
                                     followed by any of the
                                     following:
                                    Nesslerization............  .....................  .....................  D1426-15 (A)........  973.49,\3\ I-3520-
                                                                                                                                     85.\2\
                                    Titration.................  .....................  4500-NH3 C-2011.
                                    Electrode.................  .....................  4500-NH3 D-2011 or E-  D1426-15 (B).
                                                                                        2011.

[[Page 27240]]

 
                                    Manual phenate,             .....................  4500-NH3 F-2011......  ....................  See footnote.\60\
                                     salicylate, or other
                                     substituted phenols in
                                     Berthelot reaction-based
                                     methods.
                                    Automated phenate,          350.1,\30\ Rev. 2.0    4500-NH3 G-2011 4500-  ....................  I-4523-85,\2\ I-2522-
                                     salicylate, or other        (1993).                NH3 H-2011.                                  90.\80\
                                     substituted phenols in
                                     Berthelot reaction-based
                                     methods.
                                    Automated electrode.......  .....................  .....................  ....................  See footnote.\7\
                                    Ion Chromatography........  .....................  .....................  D6919-17.
                                    Automated gas diffusion,    .....................  .....................  ....................  Timberline Ammonia-
                                     followed by conductivity                                                                        001.\74\
                                     cell analysis.
                                    Automated gas diffusion     .....................  .....................  ....................  FIAlab100.\82\
                                     followed by fluorescence
                                     detector analysis.
5. Antimony--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011.
                                    AA furnace................  .....................  3113 B-2010.
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12.
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
6. Arsenic-Total,\4\ mg/L.........  Digestion,\4\ followed by   206.5 (Issued 1978)
                                     any of the following:       \1\.
                                    AA gaseous hydride........  .....................  3114 B-2011 or 3114 C- D2972-15 (B)........  I-3062-85.\2\
                                                                                        2011.
                                    AA furnace................  .....................  3113 B-2010..........  D2972-15 (C)........  I-4063-98.\49\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12.
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-
                                                                 (1994).                                                             05.\70\
                                    Colorimetric (SDDC).......  .....................  3500-As B-2011.......  D2972-15 (A)........  I-3060-85.\2\
7. Barium-Total,\4\ mg/L..........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 D-2011..........  ....................  I-3084-85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D4382-18.
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  ....................  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP \36\..................  .....................  .....................  ....................  See footnote.\34\
8. Beryllium--Total,\4\ mg/L......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 D-2011 or 3111 E- D3645-15 (A)........  I-3095-85.\2\
                                                                                        2011.
                                    AA furnace................  .....................  3113 B-2010..........  D3645-15 (B).
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES...................  200.5, Rev 4.2         3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP.......................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (aluminon)...  .....................  See footnote.\61\.
9. Biochemical oxygen demand        Dissolved Oxygen Depletion  .....................  5210 B-2016 \85\.....  ....................  973.44,\3\ p. 17,\9\
 (BOD5), mg/L.                                                                                                                       I-1578-78,\8\ See
                                                                                                                                     footnote.\10, 63\
10. Boron--Total,\37\ mg/L........  Colorimetric (curcumin)...  .....................  4500-B B-2011........  ....................  I-3112-85.\2\
                                    ICP/AES...................  200.5, Rev 4.2         3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  D4190-15............  S7ee footnote.\34\
11. Bromide, mg/L.................  Electrode.................  .....................  .....................  D1246-16............  I-1125-85.\2\
                                    Ion Chromatography........  300.0, Rev 2.1 (1993)  4110 B-2011, C-2011,   D4327-17............  993.30,\3\ I-2057-
                                                                 and 300.1, Rev 1.0     D-2011.                                      85.\79\
                                                                 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
12. Cadmium--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 or 3111 C- D3557-17 (A or B)...  974.27,\3\ p. 37,\9\
                                                                                        2011.                                        I-3135-85 \2\ or I-
                                                                                                                                     3136-85.\2\

[[Page 27241]]

 
                                    AA furnace................  .....................  3113 B-2010..........  D3557-17 (D)........  I-4138-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12............  I-1472-85 \2\ or I-
                                                                 (2003); \68\ 200.7,                                                 4471-97.\50\
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Voltammetry \11\..........  .....................  .....................  D3557-17 (C).
                                    Colorimetric (Dithizone)..  .....................  3500-Cd-D-1990.
13. Calcium--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011..........  D511-14 (B).........  I-3152-85.\2\
                                    ICP/AES...................  200.5, Rev 4.2         3120 B-2011..........  ....................  I-4471-97.\50\
                                                                 (2003);\68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
                                    Titrimetric (EDTA)........  .....................  3500-Ca B-2011.......  D511-14 (A).
                                    Ion Chromatography........  .....................  .....................  D6919-17.
14. Carbonaceous biochemical        Dissolved Oxygen Depletion  .....................  5210 B-2016 \85\.....  ....................  See footnote.35 63
 oxygen demand (CBOD5), mg/L\12\.    with nitrification
                                     inhibitor.
15. Chemical oxygen demand (COD),   Titrimetric...............  410.3 (Rev. 1978) \1\  5220 B-2011 or C-2011  D1252-06(12) (A)....  973.46,\3\ p. 17,\9\
 mg/L.                                                                                                                               I-3560-85.\2\
                                    Spectrophotometric, manual  410.4, Rev. 2.0        5220 D-2011..........  D1252-06(12) (B)....  See footnotes.13 14
                                     or automatic.               (1993).                                                             83, I-3561-85.\2\
16. Chloride, mg/L................  Titrimetric: (silver        .....................  4500-Cl-B-2011.......  D512-12 (B).........  I-1183-85.\2\
                                     nitrate).
                                    (Mercuric nitrate)........  .....................  4500-Cl-C-2011.......  D512-12 (A).........  973.51,\3\ I-1184-
                                                                                                                                     85.\2\
                                    Colorimetric: manual......  .....................  .....................  ....................  I-1187-85.\2\
                                    Automated (ferricyanide)..  .....................  4500-Cl-E-2011.......  ....................  I-2187-85.\2\
                                    Potentiometric Titration..  .....................  4500-Cl-D-2011.
                                    Ion Selective Electrode...  .....................  .....................  D512-12 (C).
                                    Ion Chromatography........  300.0, Rev 2.1 (1993)  4110 B-2011 or 4110 C- D4327-17............  993.30,\3\ I-2057-
                                                                 and 300.1, Rev 1.0     2011.                                        90.\51\
                                                                 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
17. Chlorine-Total residual, mg/L.  Amperometric direct.......  .....................  4500-Cl D-2011.......  D1253-14.
                                    Amperometric direct (low    .....................  4500-Cl E-2011.
                                     level).
                                    Iodometric direct.........  .....................  4500-Cl B-2011.
                                    Back titration ether end-   .....................  4500-Cl C-2011.
                                     point \15\.
                                    DPD-FAS...................  .....................  4500-Cl F-2011.
                                    Spectrophotometric, DPD...  .....................  4500-Cl G-2011.
                                    Electrode.................  .....................  .....................  ....................  See footnote.\16\
17A. Chlorine-Free Available, mg/L  Amperometric direct.......  .....................  4500-Cl D-2011.......  D1253-14.
                                    Amperometric direct (low    .....................  4500-Cl E-2011.
                                     level).
                                    DPD-FAS...................  .....................  4500-Cl F-2011.
                                    Spectrophotometric, DPD...  .....................  4500-Cl G-2011.
18. Chromium VI dissolved, mg/L...  0.45-micron filtration
                                     followed by any of the
                                     following:
                                    AA chelation-extraction...  .....................  3111 C-2011..........  ....................  I-1232-85.\2\
                                    Ion Chromatography........  218.6, Rev. 3.3        3500-Cr C-2011.......  D5257-17............  993.23.\3\
                                                                 (1994).
                                    Colorimetric (diphenyl-     .....................  3500-Cr B-2011.......  D1687-17 (A)........  I-1230-85.\2\
                                     carbazide).
19. Chromium--Total,\4\ mg/L......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011..........  D1687-17 (B)........  974.27,\3\ I-3236-
                                                                                                                                     85.\2\
                                    AA chelation-extraction...  .....................  3111 C-2011.
                                    AA furnace................  .....................  3113 B-2010..........  D1687-17 (C)........  I-3233-93.\46\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12.
                                                                 (2003),\68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-05
                                                                 (1994).                                                             \70\ I-4472-97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (diphenyl-     .....................  3500-Cr B-2011.
                                     carbazide).
20. Cobalt--Total,\4\ mg/L........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011 or 3111 C- D3558-15 (A or B)...  p. 37,\9\ I-3239-
                                                                                        2011.                                        85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D3558-15 (C)........  I-4243-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES...................  200.7, Rev. 4.4        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (1994).

[[Page 27242]]

 
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-05
                                                                 (1994).                                                             \70\ I-4472-97.\81\
                                    DCP.......................  .....................  .....................  D4190-15............  See footnote.\34\
21. Color, platinum cobalt units    Colorimetric (ADMI).......  .....................  2120 F-2011 \78\.
 or dominant wavelength, hue,
 luminance purity
                                    Platinum cobalt visual      .....................  2120 B-2011..........  ....................  I-1250-85.\2\
                                     comparison.
                                    Spectrophotometric........  .....................  .....................  ....................  See footnote \18\
22. Copper--Total,\4\ mg/L........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 or 3111 C- D1688-17 (A or B)...  974.27,\3\ p. 37,\9\
                                                                                        2011.                                        I-3270-85 \2\ or I-
                                                                                                                                     3271-85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D1688-17 (C)........  I-4274-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-
                                                                 (1994).                                                             05,\70\, I-4472-
                                                                                                                                     97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (Neocuproine)  .....................  3500-Cu B-2011.
                                    Colorimetric                .....................  3500-Cu C-2011.......  ....................  See footnote.\19\
                                     (Bathocuproine).
23. Cyanide--Total, mg/L..........  Automated UV digestion/     .....................  .....................  ....................  Kelada-01.\55\
                                     distillation and
                                     Colorimetry.
                                    Segmented Flow Injection,   .....................  .....................  D7511-12(17).
                                     In-Line Ultraviolet
                                     Digestion, followed by
                                     gas diffusion amperometry.
                                    Manual distillation with    335.4, Rev. 1.0        4500-CN-B-2016 and C-  D2036-09(15)(A),      10-204-00-1-X.\56\
                                     MgCl2, followed by any of   (1993) \57\.           2016.                  D7284-13(17).
                                     the following:
                                    Flow Injection, gas         .....................  .....................  D2036-09(15)(A)
                                     diffusion amperometry.                                                    D7284-13(17).
                                    Titrimetric...............  .....................  4500-CN-D-2016.......  D2036-09(15)(A).....  p. 22.\9\
                                    Spectrophotometric, manual  .....................  4500-CN-E-2016.......  D2036-09(15)(A).....  I-3300-85.\2\
                                    Semi-Automated \20\.......  335.4, Rev. 1.0        4500-CN-N-2016.......  ....................  10-204-00-1-X,\56\ I-
                                                                 (1993) \57\.                                                        4302-85.\2\
                                    Ion Chromatography........  .....................  .....................  D2036-09(15)(A).
                                    Ion Selective Electrode...  .....................  4500-CN-F-2016.......  D2036-09(15)(A).
24. Cyanide-Available, mg/L.......  Cyanide Amenable to         .....................  4500-CN-G-2016.......  D2036-09(15)(B).
                                     Chlorination (CATC);
                                     Manual distillation with
                                     MgCl2, followed by
                                     Titrimetric or
                                     Spectrophotometric.
                                    Flow injection and ligand   .....................  .....................  D6888-16............  OIA-1677-09.\44\
                                     exchange, followed by gas
                                     diffusion amperometry
                                     \59\.
                                    Automated Distillation and  .....................  .....................  ....................  Kelada-01.\55\
                                     Colorimetry (no UV
                                     digestion).
24.A Cyanide-Free, mg/L...........  Flow Injection, followed    .....................  .....................  D7237-15 (A)........  OIA-1677-09.\44\
                                     by gas diffusion
                                     amperometry.
                                    Manual micro-diffusion and  .....................  .....................  D4282-15.
                                     colorimetry.
25. Fluoride--Total, mg/L.........  Manual distillation,\6\     .....................  4500-F-B-2011........  D1179-16 (A).
                                     followed by any of the
                                     following:
                                    Electrode, manual.........  .....................  4500-F-C-2011........  D1179-16 (B).
                                    Electrode, automated......  .....................  .....................  ....................  I-4327-85.\2\
                                    Colorimetric, (SPADNS)....  .....................  4500-F-D-2011.
                                    Automated complexone......  .....................  4500-F-E-2011.
                                    Ion Chromatography........  300.0, Rev 2.1 (1993)  4110 B-2011 or C-2011  D4327-17............  993.30.\3\
                                                                 and 300.1, Rev 1.0
                                                                 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
26. Gold--Total,\4\ mg/L..........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011.
                                    AA furnace................  231.2 (Issued 1978)    3113 B-2010.
                                                                 \1\.
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
27. Hardness--Total, as CaCO3, mg/  Automated colorimetric....  130.1 (Issued 1971)
 L.                                                              \1\.
                                    Titrimetric (EDTA)........  .....................  2340 C-2011..........  D1126-17............  973.52B \3\, I-1338-
                                                                                                                                     85.\2\
                                    Ca plus Mg as their         .....................  2340 B-2011.
                                     carbonates, by any
                                     approved method for Ca
                                     and Mg (See Parameters 13
                                     and 33), provided that
                                     the sum of the lowest
                                     point of quantitation for
                                     Ca and Mg is below the
                                     NPDES permit requirement
                                     for Hardness.
28. Hydrogen ion (pH), pH units...  Electrometric measurement.  .....................  4500-H\+\ B-2011.....  D1293-99 (A or B)...  973.41,\3\ I-1586-
                                                                                                                                     85.\2\
                                    Automated electrode.......  150.2 (Dec. 1982) \1\  .....................  ....................  See footnote,\21\ I-
                                                                                                                                     2587-85.\2\

[[Page 27243]]

 
29. Iridium--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011.
                                    AA furnace................  235.2 (Issued 1978)
                                                                 \1\.
                                    ICP/MS....................  .....................  3125 B-2011.
30. Iron--Total,\4\ mg/L..........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 o 3111 C-  D1068-15 (A)........  974.27,\3\ I-3381-
                                                                                        2011.                                        85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D1068-15 (B).
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric                .....................  3500-Fe B-2011.......  D1068-15 (C)........  See footnote.\22\
                                     (Phenanthroline).
31. Kjeldahl Nitrogen \5\--Total,   Manual digestion \20\ and   .....................  4500-Norg B-2011 or C- D3590-17 (A)........  I-4515-91.\45\
 (as N), mg/L.                       distillation or gas                                2011 and 4500-NH3 B-
                                     diffusion, followed by                             2011.
                                     any of the following:
                                    Titration.................  .....................  4500-NH3 C-2011......  ....................  973.48.\3\
                                    Nesslerization............  .....................  .....................  D1426-15 (A).
                                    Electrode.................  .....................  4500-NH3 D-2011 or E-  D1426-15 (B).
                                                                                        2011.
                                    Semi-automated phenate....  350.1, Rev. 2.0        4500-NH3 G-2011 4500-
                                                                 (1993).                NH3 H-2011.
                                    Manual phenate,             .....................  4500-NH3 F-2011......  ....................  See footnote.\60\
                                     salicylate, or other
                                     substituted phenols in
                                     Berthelot reaction based
                                     methods.
                                    Automated gas diffusion,    .....................  .....................  ....................  Timberline Ammonia-
                                     followed by conductivity                                                                        001.\74\
                                     cell analysis.
                                    Automated gas diffusion     .....................  .....................  ....................  FIAlab 100.\82\
                                     followed by fluorescence
                                     detector analysis.
                                   ---------------------------------------------------------------------------------------------------------------------
                                    Automated Methods for TKN that do not require manual distillation
                                   ---------------------------------------------------------------------------------------------------------------------
                                    Automated phenate,          351.1 (Rev. 1978) \1\  .....................  ....................  I-4551-78.\8\
                                     salicylate, or other
                                     substituted phenols in
                                     Berthelot reaction based
                                     methods colorimetric
                                     (auto digestion and
                                     distillation).
                                    Semi-automated block        351.2, Rev. 2.0        4500-Norg D-2011.....  D3590-17 (B)........  I-4515-91 \45\
                                     digestor colorimetric       (1993).
                                     (distillation not
                                     required).
                                    Block digester, followed    .....................  .....................  ....................  See footnote.\39\
                                     by Auto distillation and
                                     Titration.
                                    Block digester, followed    .....................  .....................  ....................  See footnote.\40\
                                     by Auto distillation and
                                     Nesslerization.
                                    Block Digester, followed    .....................  .....................  ....................  See footnote.\41\
                                     by Flow injection gas
                                     diffusion (distillation
                                     not required).
                                    Digestion with              .....................  .....................  ....................  Hach 10242.\76\
                                     peroxdisulfate, followed
                                     by Spectrophotometric
                                     (2,6-dimethyl phenol).
                                    Digestion with persulfate,  .....................  .....................  ....................  NCASI TNTP
                                     followed by Colorimetric.                                                                       W10900.\77\
32. Lead--Total,\4\ mg/L..........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 or 3111 C- D3559-15 (A or B)...  974.27,\3\ I-3399-
                                                                                        2011.                                        85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D3559-15 (D)........  I-4403-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Voltammetry \11\..........  .....................  .....................  D3559-15 (C).
                                    Colorimetric (Dithizone)..  .....................  3500-Pb B-2011.
33. Magnesium--Total,\4\ mg/L.....  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011..........  D511-14 (B).........  974.27,\3\ I-3447-
                                                                                                                                     85.\2\
                                    ICP/AES...................  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003) \68\; 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
                                    Ion Chromatography........  .....................  .....................  D6919-17.
34. Manganese--Total,\4\ mg/L.....  Digestion,\4\ followed by
                                     any of the following:

[[Page 27244]]

 
                                    AA direct aspiration \36\.  .....................  3111 B-2011..........  D858-17 (A or B)....  974.27,\3\ I-3454-
                                                                                                                                     85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  D858-17 (C).
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (Persulfate).  .....................  3500-Mn B-2011.......  ....................  920.203.\3\
                                    Colorimetric (Periodate)..  .....................  .....................  ....................  See footnote.\23\
35. Mercury--Total, mg/L..........  Cold vapor, Manual........  245.1, Rev. 3.0        3112 B-2011..........  D3223-17............  977.22,\3\ I-3462-
                                                                 (1994).                                                             85.\2\
                                    Cold vapor, Automated.....  245.2 (Issued 1974)
                                                                 \1\.
                                    Cold vapor atomic           245.7 Rev. 2.0 (2005)  .....................  ....................  I-4464-01.\71\
                                     fluorescence spectrometry   \17\.
                                     (CVAFS).
                                    Purge and Trap CVAFS......  1631E \43\.
36. Molybdenum--Total,\4\ mg/L....  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 D-2011..........  ....................  I-3490-85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  ....................  I-3492-96.\47\
                                    ICP/AES...................  200.7, Rev. 4.4        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
37. Nickel--Total,\4\               Digestion,\4\ followed by
mg/L..............................   any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 or 3111 C- D1886-14 (A or B)...  I-3499-85 \2\
                                                                                        2011.
                                    AA furnace................  .....................  3113 B-2010..........  D1886-14 (C)........  I-4503-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-05
                                                                 (1994).                                                             \70\ I-4472-97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
38. Nitrate (as N), mg/L..........  Ion Chromatography........  300.0, Rev. 2.1        4110 B-2011 or C-2011  D4327-17............  993.30.\3\
                                                                 (1993) and 300.1,
                                                                 Rev. 1.0 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
                                    Ion Selective Electrode...  .....................  4500-NO3 D-2016.
                                    Colorimetric (Brucine       352.1 (Issued 1971)    .....................  ....................  973.50,\3\ 419D\1
                                     sulfate).                   \1\.                                                                7\, p. 28.\9\
                                    Spectrophotometric (2,6-    .....................  .....................  ....................  Hach 10206 \75\
                                     dimethylphenol).
                                    Nitrate-nitrite N minus
                                     Nitrite N (See parameters
                                     39 and 40).
39. Nitrate-nitrite (as N), mg/L..  Cadmium reduction, Manual.  .....................  4500-NO3-E-2016......  D3867-16 (B).
                                    Cadmium reduction,          353.2, Rev. 2.0        4500-NO3-F-2016 4500-  D3867-16 (A)........  I-2545-90.\51\
                                     Automated.                  (1993).                NO3-I-2016.
                                    Automated hydrazine.......  .....................  4500-NO3-H-2016.
                                    Reduction/Colorimetric....  .....................  .....................  ....................  See footnote.\62\
                                    Ion Chromatography........  300.0, Rev. 2.1        4110 B-2011 or C-2011  D4327-17............  993.30.\3\
                                                                 (1993) and 300.1,
                                                                 Rev. 1.0 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
                                    Enzymatic reduction,        .....................  .....................  D7781-14............  I-2547-11.\72\
                                     followed by automated                                                                          I-2548-11.\72\
                                     colorimetric                                                                                   N07-0003.\73\
                                     determination.
                                    Enzymatic reduction,        .....................  4500-NO3-J-2018.
                                     followed by manual
                                     colorimetric
                                     determination.
                                    Spectrophotometric (2,6-    .....................  .....................  ....................  Hach 10206.\75\
                                     dimethylphenol).
40. Nitrite (as N), mg/L..........  Spectrophotometric: Manual  .....................  4500-NO2-B-2011......  ....................  See footnote.\25\
                                    Automated (Diazotization).  .....................  .....................  ....................  I-4540-85,\2\ See
                                                                                                                                     footnote.\62\ I-
                                                                                                                                     2540-90.\80\
                                    Automated (*bypass cadmium  353.2, Rev. 2.0        4500-NO3-F-2016 4500-  D3867-16 (A)........  I-4545-85.\2\
                                     reduction).                 (1993).                NO3-I-2016.
                                    Manual (*bypass cadmium or  .....................  4500-NO3- E-2016,      D3867-16 (B).
                                     enzymatic reduction).                              4500-NO3-J-2018.
                                    Ion Chromatography........  300.0, Rev. 2.1        4110 B-2011 or C-2011  D4327-17............  993.30.\3\
                                                                 (1993) and 300.1,
                                                                 Rev. 1.0 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
                                    Automated (*bypass          .....................  .....................  D7781-14............  I-2547-11 \72\ I-
                                     Enzymatic reduction).                                                                           2548-11 \72\ N07-
                                                                                                                                     0003.\73\

[[Page 27245]]

 
41. Oil and grease--Total           Hexane extractable          1664 Rev. A; 1664      5520 B-2011 \38\.
 recoverable, mg/L.                  material (HEM): n-Hexane    Rev. B \42\.
                                     extraction and gravimetry.
                                    Silica gel treated HEM      1664 Rev. A; 1664      5520 B-2011 \38\ and
                                     (SGT-HEM): Silica gel       Rev. B \42\.           5520 F-2011 \38\.
                                     treatment and gravimetry.
42. Organic carbon--Total (TOC),    Combustion................                         5310 B-2014..........  D7573-09(17)........  973.47,\3\ p.
 mg/L.                                                                                                                               14.\24\
                                    Heated persulfate or UV     .....................  5310 C-2014 5310 D-    D4839-03(17)........  973.47,\3,\ p.
                                     persulfate oxidation.                              2011.                                        14.\24\
43. Organic nitrogen (as N), mg/L.  Total Kjeldahl N
                                     (Parameter 31) minus
                                     ammonia N (Parameter 4).
44. Ortho-phosphate (as P), mg/L..  Ascorbic acid method:
                                    Automated.................  365.1, Rev. 2.0        4500-P F-2011 or G-    ....................  973.56,\3\ I-4601-
                                                                 (1993).                2011.                                        85,\2\ I-2601-
                                                                                                                                     90.\80\
                                    Manual, single-reagent....  .....................  4500-P E-2011........  D515-88 (A).........  973.55.\3\
                                    Manual, two-reagent.......  365.3 (Issued 1978)
                                                                 \1\.
                                    Ion Chromatography........  300.0, Rev. 2.1        4110 B-2011 or C-2011  D4327-17............  993.30.\3\
                                                                 (1993) and 300.1,
                                                                 Rev. 1.0 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
45. Osmium--Total,\4\ mg/L........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 D-2011.
                                    AA furnace................  252.2 (Issued 1978)
                                                                 \1\.
46. Oxygen, dissolved, mg/L.......  Winkler (Azide              .....................  4500-O (B-F)-2016....  D888-12 (A).........  973.45B,\3\ I-1575-
                                     modification).                                                                                  78.\8\
                                    Electrode.................  .....................  4500-O G-2016........  D888-12 (B).........  I-1576-78.\8\
                                    Luminescence-Based Sensor.  .....................  4500-O H-2016........  D888-12 (C).........  See footnote.\63\
                                                                                                                                     See footnote.\64\
47. Palladium--Total,\4\ mg/L.....  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011.
                                    AA furnace................  253.2 (Issued 1978)
                                                                 \1\.
                                    ICP/MS....................  .....................  3125 B-2011.
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
48. Phenols, mg/L.................  Manual distillation,\26\    420.1 (Rev. 1978) \1\  5530 B-2010..........  D1783-01(12).
                                     followed by any of the
                                     following:
                                    Colorimetric (4AAP) manual  420.1 (Rev. 1978) \1\  5530 D-2010 \27\.....  D1783-01(12) (A or
                                                                                                               B).
                                    Automated colorimetric      420.4 Rev. 1.0 (1993)
                                     (4AAP).
49. Phosphorus (elemental), mg/L..  Gas-liquid chromatography.  .....................  .....................  ....................  See footnote.\28\
50. Phosphorus--Total, mg/L.......  Digestion,\20\ followed by  .....................  4500-P B (5)-2011....  ....................  973.55.\3\
                                     any of the following:
                                    Manual....................  365.3 (Issued 1978)    4500-P E-2011........  D515-88 (A).
                                                                 \1\.
                                    Automated ascorbic acid     365.1 Rev. 2.0 (1993)  4500-P (F-H)-2011....  ....................  973.56,\3\ I-4600-
                                     reduction.                                                                                      85.\2\
                                    ICP/AES 4 36..............  200.7, Rev. 4.4        3120 B-2011..........  ....................  I-4471-97.\50\
                                                                 (1994).
                                    Semi-automated block        365.4 (Issued 1974)    .....................  D515-88 (B).........  I-4610-91.\48\
                                     digestor (TKP digestion).   \1\.
                                    Digestion with persulfate,  .....................  .....................  ....................  NCASI TNTP
                                     followed by Colorimetric.                                                                       W10900.\77\
51. Platinum--Total,\4\ mg/L......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011.
                                    AA furnace................  255.2 (Issued 1978)
                                                                 \1\.
                                    ICP/MS....................  .....................  3125 B-2011.
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
52. Potassium--Total,\4\ mg/L.....  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011..........  ....................  973.53,\3\ I-3630-
                                                                                                                                     85.\2\
                                    ICP/AES...................  200.7, Rev. 4.4        3120 B-2011.
                                                                 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    Flame photometric.........  .....................  3500-K B-2011.
                                    Electrode.................  .....................  3500-K C-2011.
                                    Ion Chromatography........  .....................  .....................  D6919-17.
53. Residue--Total, mg/L..........  Gravimetric, 103-105[deg].  .....................  2540 B-2015..........  ....................  I-3750-85.\2\
54. Residue--filterable, mg/L.....  Gravimetric, 180[deg].....  .....................  2540 C-2015..........  D5907-13............  I-1750-85.\2\
55. Residue--non-filterable (TSS),  Gravimetric, 103-105[deg]   .....................  2540 D-2015..........  D5907-13............  I-3765-85.\2\
 mg/L.                               post-washing of residue.

[[Page 27246]]

 
56. Residue--settleable, ml/L.....  Volumetric (Imhoff cone),   .....................  2540 F-2015.
                                     or gravimetric.
57. Residue--Volatile, mg/L.......  Gravimetric, 550[deg].....  160.4 (Issued 1971)    2540 E-2015..........  ....................  I-3753-85.\2\
                                                                 \1\.
58. Rhodium--Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration, or..  .....................  3111 B-2011.
                                    AA furnace................  265.2 (Issued 1978)
                                                                 \1\.
                                    ICP/MS....................  .....................  3125 B-2011.
59. Ruthenium--Total,\4\ mg/L.....  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration, or..  .....................  3111 B-2011.
                                    AA furnace................  267.2 \1\.
                                    ICP/MS....................  .....................  3125 B-2011.
60. Selenium--Total,\4\ mg/L......  Digestion,\4\ followed by
                                     any of the following:
                                    AA furnace................  .....................  3113 B-2010..........  D3859-15 (B)........  I-4668-98.\49\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES \36\..............  200.5, Rev 4.2         3120 B-2011..........  D1976-12.
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-05
                                                                 (1994).                                                             \70\ I-4472-97.\81\
                                    AA gaseous hydride........                         3114 B-2011, or 3114   D3859-15 (A)........  I-3667-85.\2\
                                                                                        C-2011.
61. Silica--Dissolved,\37\ mg/L...  0.45-micron filtration
                                     followed by any of the
                                     following:
                                    Colorimetric, Manual......  .....................  4500-SiO2 C-2011.....  D859-16.............  I-1700-85.\2\
                                    Automated                   .....................  4500-SiO2 E-2011 or F- ....................  I-2700-85.\2\
                                     (Molybdosilicate).                                 2011.
                                    ICP/AES...................  200.5, Rev. 4.2        3120 B-2011..........  ....................  I-4471-97.\50\
                                                                 (2003) \68\; 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
62. Silver--Total,4 31 mg/L.......  Digestion,\4 29\ followed
                                     by any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011 or 3111 C- ....................  974.27,\3\ p. 37,\9\
                                                                                        2011.                                        I-3720-85.\2\
                                    AA furnace................  .....................  3113 B-2010..........  ....................  I-4724-89.\51\
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES...................  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4472-
                                                                 (1994).                                                             97.\81\
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
63. Sodium--Total,\4\ mg/L........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011..........  ....................  973.54,\3\ I-3735-
                                                                                                                                     85.\2\
                                    ICP/AES...................  200.5, Rev. 4.2        3120 B-2011..........  ....................  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
                                    Flame photometric.........  .....................  3500-Na B-2011.
                                    Ion Chromatography........  .....................  .....................  D6919-17.
64. Specific conductance,           Wheatstone bridge.........  120.1 (Rev. 1982) \1\  2510 B-2011..........  D1125-95(99) (A)....  973.40,\3\ I-2781-
 micromhos/cm at 25 [deg]C.                                                                                                          85.\2\
65. Sulfate (as SO4), mg/L........  Automated colorimetric....  375.2, Rev. 2.0        4500-SO4\2\ F-2011 or
                                                                 (1993).                G-2011.
                                    Gravimetric...............                         4500-SO4\2\-C-2011 or                        925.54.\3\
                                                                                        D-2011.
                                    Turbidimetric.............  .....................  4500-SO4\2\-E-2011...  D516-16.
                                    Ion Chromatography........  300.0, Rev. 2.1        4110 B-2011 or C-2011  D4327-17............  993, I-4020-05
                                                                 (1993) and 300.1,                                                   \70\.303
                                                                 Rev. 1.0 (1997).
                                    CIE/UV....................  .....................  4140 B-2011..........  D6508-15............  D6508, Rev. 2.\54\
66. Sulfide (as S), mg/L..........  Sample Pretreatment.......  .....................  4500-S2- B, C-2011.
                                    Titrimetric (iodine)......  .....................  4500-S-F-2011........  ....................  I-3840-85.\2\
                                    Colorimetric (methylene     .....................  4500-S2- D-2011.
                                     blue).
                                    Ion Selective Electrode...  .....................  4500-S-G-2011........  D4658-15.
67. Sulfite (as SO3), mg/L........  Titrimetric (iodine-        .....................  4500-SO3\2\-B-2011.
                                     iodate).
68. Surfactants, mg/L.............  Colorimetric (methylene     .....................  5540 C-2011..........  D2330-02.
                                     blue).

[[Page 27247]]

 
69. Temperature, [deg]C...........  Thermometric..............  .....................  2550 B-2010..........  ....................  See footnote.\32\
70. Thallium-Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011.
                                    AA furnace................  279.2 (Issued 1978)    3113 B-2010.
                                                                 \1\.
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES...................  200.7, Rev. 4.4        3120 B-2011..........  D1976-12.
                                                                 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4471-97
                                                                 (1994).                                                             \50\ I-4472-97.\81\
71. Tin-Total,\4\ mg/L............  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 B-2011..........  ....................  I-3850-78.\8\
                                    AA furnace................  .....................  3113 B-2010.
                                    STGFAA....................  200.9, Rev. 2.2
                                                                 (1994).
                                    ICP/AES...................  200.5, Rev. 4.2
                                                                 (2003) \68\; 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
72. Titanium-Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 D-2011.
                                    AA furnace................  283.2 (Issued 1978)
                                                                 \1\.
                                    ICP/AES...................  200.7, Rev. 4.4
                                                                 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14.\3\
                                                                 (1994).
                                    DCP.......................  .....................  .....................  ....................  See footnote.\34\
73. Turbidity, NTU \53\...........  Nephelometric.............  180.1, Rev. 2.0        2130 B-2011..........  D1889-00............  I-3860-85\2\
                                                                 (1993).                                                            See footnote.\65\
                                                                                                                                    See footnote.\66\
                                                                                                                                    See footnote.\67\
74. Vanadium-Total,\4\ mg/L.......  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration......  .....................  3111 D-2011.
                                    AA furnace................  .....................  3113 B-2010..........  D3373-17.
                                    ICP/AES...................  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97 \50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-
                                                                 (1994).                                                             05.\70\
                                    DCP.......................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (Gallic Acid)  .....................  3500-V B-2011.
75. Zinc-Total,\4\ mg/L...........  Digestion,\4\ followed by
                                     any of the following:
                                    AA direct aspiration \36\.  .....................  3111 B-2011 or 3111 C- D1691-17 (A or B)...  974.27,\3\ p. 37,\9\
                                                                                        2011.                                        I-3900-85.\2\
                                    AA furnace................  289.2 (Issued 1978)
                                                                 \1\.
                                    ICP/AES \36\..............  200.5, Rev. 4.2        3120 B-2011..........  D1976-12............  I-4471-97.\50\
                                                                 (2003); \68\ 200.7,
                                                                 Rev. 4.4 (1994).
                                    ICP/MS....................  200.8, Rev. 5.4        3125 B-2011..........  D5673-16............  993.14,\3\ I-4020-05
                                                                 (1994).                                                             \70\ I-4472-97.\81\
                                    DCP \36\..................  .....................  .....................  D4190-15............  See footnote.\34\
                                    Colorimetric (Zincon).....  .....................  3500 Zn B-2011.......  ....................  See footnote.\33\
76. Acid Mine Drainage............  ..........................  1627 \69\.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB Notes:
\1\ Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.
\2\ Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological
  Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.
\3\ Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC
  International.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion
  procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable
  form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations, a digestion using nitric acid (as specified in
  Section 4.1.3 of Methods for Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to
  gentle acid refluxing, and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption (FLAA) determinations, a
  combination acid (nitric and hydrochloric acids) digestion is preferred, prior to analysis. The approved total recoverable digestion is described as
  Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in
  EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain
  elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic
  absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required, and, in all cases the referenced
  method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission
  spectrometry (ICP-AES), the direct current plasma (DCP) technique or EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS), use
  EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in 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.

[[Page 27248]]

 
\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 (CBOD5) must not be confused with the traditional BOD5 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 CBOD5 parameter. A discharger whose permit
  requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's
  permit specifically states CBOD5 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 Chromatography,
  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 Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
  approved method is satisfactory.
\30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method-
  specified quality control acceptance criteria are met.
\31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in
  solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2
  to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent
  the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with
  reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as
  well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the
  cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ ``Water Temperature-Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 1, Chapter D1. 1975. USGS.
\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\ Method D6508-15, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate
  Electrolyte. 2015. ASTM

[[Page 27249]]

 
\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.
  U.S. 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 335.4-1, reconstitute particulate that is filtered with the sample prior to
  distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method,
  approved digestion and/or distillation are required prior to analysis.
\59\ Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-16 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 BOD5 and CBOD5.
  Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for
  measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).
\64\ In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\65\ Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\66\ Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\67\ Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.
\68\ EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/
  600/R-06/115. Revision 4.2, October 2003. U.S. EPA.
\69\ Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. U.S. 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 U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. A11989, Methods for Determination of Inorganic
  Substances in Water and Fluvial Sediments, 1989.
\80\ Methods I-2522-90, I-2540-90, and I-2601-90 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-1472-97, 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 Instruments, Inc. Method 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[supreg] 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 (2017); Part 3000
  Methods, Metals, 3020 (2017); Part 4000 Methods, Inorganic Nonmetallic Constituents, 4020 (2014); Part 5000 Methods, and Aggregate Organic
  Constituents, 5020 (2017). 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 BOD5. 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%.
 Any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L.


                                     Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
          Parameter \1\                    Method                EPA \2\ \7\            Standard methods               ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
2. Acenaphthylene...............  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
3. Acrolein.....................  GC.....................  603....................
                                  GC/MS..................  624.1,\4\ 1624B........
4. Acrylonitrile................  GC.....................  603....................
                                  GC/MS..................  624.1,\4\ 1624B........  .......................  .......................  O-4127-96. \13\
5. Anthracene...................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
6. Benzene......................  GC.....................  602....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
7. Benzidine....................  Spectrophoto-            .......................  .......................  .......................  See footnote \3\,
                                  metric.................                                                                              p.1.
                                  GC/MS..................  625.1,\5\ 1625B........  6410 B-2000............
                                  HPLC...................  605....................
8. Benzo(a)anthracene...........  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........

[[Page 27250]]

 
9. Benzo(a)pyrene...............  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
10. Benzo(b)fluoranthene........  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
11. Benzo(g,h,i)perylene........  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
12. Benzo(k)fluoranthene........  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
13. Benzyl chloride.............  GC.....................  .......................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  .......................  .......................  .......................  See footnote \6\,
                                                                                                                                       p. S102.
14. Butyl benzyl phthalate......  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
15. bis(2-Chloroethoxy) methane.  GC.....................  611....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
16. bis(2-Chloroethyl) ether....  GC.....................  611....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
17. bis(2-Ethylhexyl) phthalate.  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
18. Bromodichloromethane........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
19. Bromoform...................  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
20. Bromomethane................  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
21. 4-Bromophenyl phenyl ether..  GC.....................  611....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
22. Carbon tetrachloride........  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
23. 4-Chloro-3-methyl phenol....  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
24. Chlorobenzene...............  GC.....................  601, 602...............  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
25. Chloroethane................  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96.\13\
26. 2-Chloroethylvinyl ether....  GC.....................  601....................
                                  GC/MS..................  624.1, 1624B...........
27. Chloroform..................  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
28. Chloromethane...............  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
29. 2-Chloronaphthalene.........  GC.....................  612....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
30. 2-Chlorophenol..............  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
31. 4-Chlorophenyl phenyl ether.  GC.....................  611....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
32. Chrysene....................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
33. Dibenzo(a,h)anthracene......  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
34. Dibromochloromethane........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
35. 1,2-Dichlorobenzene.........  GC.....................  601, 602...............  6200 C-2011............
                                  GC/MS..................  624.1, 1625B...........  6200 B-2011............  .......................  See footnote, \9\
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96,\13\ O-4436-
                                                                                                                                       16.\14\
36. 1,3-Dichlorobenzene.........  GC.....................  601, 602...............  6200 C-2011............
                                  GC/MS..................  624.1, 1625B...........  6200 B-2011............  .......................  See footnote \9\,
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96.\13\
37. 1,4-Dichlorobenzene.........  GC.....................  601, 602...............  6200 C-2011............
                                  GC/MS..................  624.1, 1625B...........  6200 B-2011............  .......................  See footnote,\9\
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96,\13\ O-4436-
                                                                                                                                       16.\14\
38. 3,3'-Dichlorobenzidine......  GC/MS..................  625.1, 1625B...........  6410 B-2000............
                                  HPLC...................  605....................
39. Dichlorodifluoromethane.....  GC.....................  601....................
                                  GC/MS..................  .......................  6200 C-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
40. 1,1-Dichloroethane..........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
41. 1,2-Dichloroethane..........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
42. 1,1-Dichloroethene..........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
43. trans-1,2-Dichloroethene....  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
44. 2,4-Dichlorophenol..........  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.

[[Page 27251]]

 
45. 1,2-Dichloropropane.........  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
46. cis-1,3-Dichloropropene.....  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
47. trans-1,3-Dichloropropene...  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
48. Diethyl phthalate...........  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
49. 2,4-Dimethylphenol..........  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
50. Dimethyl phthalate..........  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
51. Di-n-butyl phthalate........  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote,\9\,
                                                                                                                                       p. 27.
52. Di-n-octyl phthalate........  GC.....................  606....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27.
53. 2, 4-Dinitrophenol..........  GC.....................  604....................  6420 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............
54. 2,4-Dinitrotoluene..........  GC.....................  609....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
55. 2,6-Dinitrotoluene..........  GC.....................  609....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
56. Epichlorohydrin.............  GC.....................  .......................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  .......................  .......................  .......................  See footnote \6\,
                                                                                                                                       p. S102.
57. Ethylbenzene................  GC.....................  602....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96,\13\ O-
                                                                                                                                       4436-16.\14\
58. Fluoranthene................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
59. Fluorene....................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
60. 1,2,3,4,6,7,8-Heptachloro-    GC/MS..................  1613B..................
 dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro-    GC/MS..................  1613B..................
 dibenzofuran.
62. 1,2,3,4,6,7,8-Heptachloro-    GC/MS..................  1613B..................
 dibenzo-p-dioxin.
63. Hexachlorobenzene...........  GC.....................  612....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
64. Hexachlorobutadiene.........  GC.....................  612....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96.\13\
65. Hexachlorocyclopentadiene...  GC.....................  612....................
                                  GC/MS..................  625.1,\5\ 1625B........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96.\13\
66. 1,2,3,4,7,8-Hexachloro-       GC/MS..................  1613B..................
 dibenzofuran.
67. 1,2,3,6,7,8-Hexachloro-       GC/MS..................  1613B..................
 dibenzofuran.
68. 1,2,3,7,8,9-Hexachloro-       GC/MS..................  1613B..................
 dibenzofuran.
69. 2,3,4,6,7,8-Hexachloro-       GC/MS..................  1613B..................
 dibenzofuran.
70. 1,2,3,4,7,8-Hexachloro-       GC/MS..................  1613B..................
 dibenzo-p-dioxin.
71. 1,2,3,6,7,8-Hexachloro-       GC/MS..................  1613B..................
 dibenzo-p-dioxin.
72. 1,2,3,7,8,9-Hexachloro-       GC/MS..................  1613B..................
 dibenzo-p-dioxin.
73. Hexachloroethane............  GC.....................  612....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96.\13\
74. Indeno(1,2,3-c,d) pyrene....  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
75. Isophorone..................  GC.....................  609....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
76. Methylene chloride..........  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
77. 2-Methyl-4,6-dinitrophenol..  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
78. Naphthalene.................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............
79. Nitrobenzene................  GC.....................  609....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  .......................  .......................  D4657-92 (98)..........
80. 2-Nitrophenol...............  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
81. 4-Nitrophenol...............  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
82. N-Nitrosodimethylamine......  GC.....................  607....................

[[Page 27252]]

 
                                  GC/MS..................  625.1,\5\ 1625B........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27.
83. N-Nitrosodi-n-propylamine...  GC.....................  607....................
                                  GC/MS..................  625.1,\5\ 1625B........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27.
84. N-Nitrosodiphenylamine......  GC.....................  607....................
                                  GC/MS..................  625.1,\5\ 1625B........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27.
85. Octachlorodibenzofuran......  GC/MS..................  1613B.\10\
86. Octachlorodibenzo-p-dioxin..  GC/MS..................  1613B.\10\
87. 2,2'-oxybis(1-chloropropane)  GC.....................  611....................
 \12\ [also known as bis(2-
 Chloro-1-methylethyl) ether].
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
88. PCB-1016....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
89. PCB-1221....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
90. PCB-1232....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
91. PCB-1242....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
92. PCB-1248....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
93. PCB-1254....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
94. PCB-1260....................  GC.....................  608.3..................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 43; See
                                                                                                                                       footnote.\8\
                                  GC/MS..................  625.1..................  6410 B-2000............
95. 1,2,3,7,8-Pentachloro-        GC/MS..................  1613B..................
 dibenzofuran.
96. 2,3,4,7,8-Pentachloro-        GC/MS..................  1613B..................
 dibenzofuran.
97. 1,2,3,7,8-Pentachloro-        GC/MS..................  1613B..................
 dibenzo-p-dioxin.
98. Pentachlorophenol...........  GC.....................  604....................  6420 B-2000............  .......................  See footnote \3\,
                                                                                                                                       p. 140.
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
99. Phenanthrene................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
100. Phenol.....................  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
101. Pyrene.....................  GC.....................  610....................
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
                                  HPLC...................  610....................  6440 B-2005............  D4657-92 (98)..........
102. 2,3,7,8-Tetrachloro-         GC/MS..................  1613B.\10\
 dibenzofuran.
103. 2,3,7,8-Tetrachloro-dibenzo- GC/MS..................  613, 625.1,\5a\ 1613B..
 p-dioxin.
104. 1,1,2,2-Tetrachloroethane..  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96.\13\
105. Tetrachloroethene..........  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
106. Toluene....................  GC.....................  602....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
107. 1,2,4-Trichlorobenzene.....  GC.....................  612....................  .......................  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote,\9\
                                                                                                                                       p. 27; O-4127-
                                                                                                                                       96,\13\ O-4436-
                                                                                                                                       16.\14\
108. 1,1,1-Trichloroethane......  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
109. 1,1,2-Trichloroethane......  GC.....................  601....................  6200 C-2011............  .......................  See footnote \3\,
                                                                                                                                       p. 130.
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
110. Trichloroethene............  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
111. Trichlorofluoromethane.....  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1..................  6200 B-2011............  .......................  O-4127-96.\13\
112. 2,4,6-Trichlorophenol......  GC.....................  604....................  6420 B-2000............
                                  GC/MS..................  625.1, 1625B...........  6410 B-2000............  .......................  See footnote \9\,
                                                                                                                                       p. 27.
113. Vinyl chloride.............  GC.....................  601....................  6200 C-2011............
                                  GC/MS..................  624.1, 1624B...........  6200 B-2011............  .......................  O-4127-96 \13\, O-
                                                                                                                                       4436-16.\14\
114. Nonylphenol................  GC/MS..................  .......................  .......................  D7065-17...............
115. Bisphenol A (BPA)..........  GC/MS..................  .......................  .......................  D7065-17...............
116. p-tert-Octylphenol (OP)....  GC/MS..................  .......................  .......................  D7065-17...............
117. Nonylphenol Monoethoxylate   GC/MS..................  .......................  .......................  D7065-17...............
 (NP1EO).
118. Nonylphenol Diethoxylate     GC/MS..................  .......................  .......................  D7065-17...............
 (NP2EO).
119. Adsorbable Organic Halides   Adsorption and           1650.\11\
 (AOX).                            Coulometric Titration.
120. Chlorinated Phenolics......  In Situ Acetylation and  1653.\11\
                                   GC/MS.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([micro]g/L) except for Method 1613B, in which the parameters are expressed in picograms per
  liter (pg/L).

[[Page 27253]]

 
\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.
\5a\ Method 625.1 screening 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.

* * * * *

                                          Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                 Method \1\                   EPA              Standard methods      AOAC, ASTM, USGS            Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Bacteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Coliform (fecal), number per     Most Probable Number        p. 132 3.............  9221 E-2014, 9221 F-
 100 mL.                             (MPN), 5 tube, 3                                   2014 32.
                                     dilution, or.
                                    Membrane filter (MF) 2,     p. 124 3.............  9222 D-2015 26.......  B-0050-85 4.........
                                     single step.
2. Coliform (total), number per     MPN, 5 tube, 3 dilution,    p. 114 3.............  9221 B-2014..........  B-0025-85 4.........
 100 mL.                             or.                        p. 108 3.............  9222 B-2015 27.......
                                    MF 2, single step or two
                                     step.
                                    MF 2 with enrichment......  p. 111 3.............  9222 B- 2015 27......
3. E. coli, number per 100 mL.....  MPN 5 7 13, multiple tube,  .....................  9221 B.3-2014/9221 F-
                                     or.                                                2014 10 12 32.
                                    Multiple tube/multiple      .....................  9223 B-2016 11.......  991.15 9............  Colilert[supreg] 11
                                     well, or.                                                                                       15, Colilert-
                                                                                                                                     18[supreg].11 14 15
                                    MF 2 5 6 7, two step, or..  1103.1 18............  9222 B-2015/9222 I-    D5392-93 8..........
                                                                                        2015 17, 9213 D-2007.
                                    Single step...............  1603 19, 1604 20.....  .....................  ....................  m-ColiBlue24[supreg]
                                                                                                                                     16, KwikCountTM EC.
                                                                                                                                     28 29
4. Fecal streptococci, number per   MPN, 5 tube, 3 dilution,    p. 139 3.............  9230 B-2013..........  B-0055-85 4.........
 100 mL.                             or.                        p. 136 3.............  9230 C-2013 30.......
                                    MF 2, or..................
                                    Plate count...............  p. 143 3.............
5. Enterococci, number per 100 mL.  MPN 5 7, multiple tube/     .....................  9230 D-2013..........  D6503-99 8..........  Enterolert[supreg].1
                                     multiple well, or.         1106.1 22............  9230 C-2013 30.......  D5259-92 8..........   1 21
                                    MF 2 5 6 7 two step, or...
                                    Single step, or...........  1600 23..............  9230 C-2013 30.......
                                    Plate count...............  p. 143 3.............
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Protozoa
--------------------------------------------------------------------------------------------------------------------------------------------------------
6. Cryptosporidium................  Filtration/IMS/FA.........  1622 24, 1623 25,
                                                                 1623.1 25 31.
7. Giardia........................  Filtration/IMS/FA.........  1623 25, 1623.1 25 31
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1H notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water and Wastes. EPA/600/8-78/017. 1978. US EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\6\ When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may
  contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
  comparability of results.
\7\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\8\ Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.
\9\ Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.

[[Page 27254]]

 
\10\ The multiple-tube fermentation test is used in 9221B.3-2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.
\11\ These tests are collectively known as defined enzyme substrate tests.
\12\ After prior enrichment in a presumptive medium for total coliform using 9221B.3-2014, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2014. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\13\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\14\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C, rather than the 24 h required for the Colilert[supreg] test, and is recommended for marine water samples.
\15\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories Inc.
\16\ A description of the mColiBlue24[supreg] 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 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-10-
  002. March 2010. US EPA.
\19\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified
  mTEC), EPA-821-R-14-010. September 2014. 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[supreg] test may be obtained from IDEXX Laboratories Inc.
\22\ Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), EPA-821-R-09-015. December 2009.
  US EPA.
\23\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-14-011.
  September 2014. 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 KwikCountTM EC may be obtained from Micrology Laboratories 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 [deg]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 [deg]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) Certain material 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 material may be inspected 
at EPA's Water Docket, EPA West, 1301 Constitution Avenue NW, Room 
3334, Washington, DC 20004, (Telephone: 202-566-2426). It is also 
available for inspection at National Archives and Records 
Administration (NARA). For information on the availability of this 
material at NARA, call 202-741-6030, or go to: https://www.archives.gov/federal-register/cfr/ibr-locations.html.
* * * * *
    (8) Office of Water, U.S. Environmental Protection Agency, 
Washington, DC (U.S. EPA). Available at https://www.epa.gov/cwa-methods.
* * * * *
    (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, 
Note 25.
    (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.
* * * * *
    (10) * * *
    (xiv) 2540, solids. 2015. Table IB.
* * * * *
    (xxxix) 4500-CN-, Cyanide. 2016. Table IB.
* * * * *
    (xliv) 4500-NO3-, Nitrogen (Nitrate). 2016. Table IB.
* * * * *
    (xlvi) 4500-O, Oxygen (Dissolved). 2016. Table IB.
* * * * *
    (lii) 5210, Biochemical Oxygen Demand (BOD). 2016. Table IB.
* * * * *
    (liv) 5310, Total Organic Carbon (TOC). 2014. Table IB.
* * * * *
    (lxvii) 9221 Multiple-Tube Fermentation Technique for Members of 
the Coliform Group. 2014. Table IA, Notes 12 and 14; Table IH, Notes 10 
and 12.
    (lxviii) 9222, Membrane Filter Technique for Members of the 
Coliform Group. 2015. Table IA; Table IH, Note 17.

[[Page 27255]]

    (lxix) 9223 Enzyme Substrate Coliform Test. 2016. Table IA; Table 
IH.
    (lxx) 9230 Fecal Enterococcus/Streptococcus Groups. 2013. Table IA; 
Table IH.
* * * * *
    (15) * * *
    (v) ASTM D511-14, Standard Test Methods for Calcium and Magnesium 
in Water. November 2014. Table IB.
    (vi) ASTM D512-12, Standard Test Methods for Chloride Ion in Water. 
July 2012. Table IB.
* * * * *
    (viii) ASTM D516-16, Standard Test Method for Sulfate Ion in Water, 
June 2016. Table IB.
    (ix) ASTM D858-17, Standard Test Methods for Manganese in Water. 
June 2017. Table IB.
    (x) ASTM D859-16, Standard Test Method for Silica in Water. June 
2016. Table IB.
    (xi) ASTM D888-12, Standard Test Methods for Dissolved Oxygen in 
Water. March 2012. Table IB.
    (xii) ASTM D1067-16, Standard Test Methods for Acidity or 
Alkalinity of Water. June 2016. Table IB.
    (xiii) ASTM D1068-15, Standard Test Methods for Iron in Water. 
October 2015. Table IB.
* * * * *
    (xv) ASTM D1126-17, Standard Test Method for Hardness in Water. 
December 2017. Table IB.
    (xvi) ASTM D1179-16, Standard Test Methods for Fluoride Ion in 
Water. June 2016. Table IB.
    (xvii) ASTM D1246-16, Standard Test Method for Bromide Ion in 
Water. June 2016. Table IB.
    (xviii) ASTM D1252-06 (Reapproved 2012), Standard Test Methods for 
Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water. June 2012. 
Table IB.
    (xix) ASTM D1253-14, Standard Test Method for Residual Chlorine in 
Water. February 2014. Table IB.
* * * * *
    (xxi) ASTM D1426-15, Standard Test Methods for Ammonia Nitrogen in 
Water. April 2015. Table IB.
    (xxii) ASTM D1687-17, Standard Test Methods for Chromium in Water. 
July 2017. Table IB.
    (xxiii) ASTM D1688-17, Standard Test Methods for Copper in Water. 
July 2017. Table IB.
    (xxiv) ASTM D1691-17, Standard Test Methods for Zinc in Water. June 
2017. Table IB.
    (xxv) ASTM D1783-01 (Reapproved 2012), Standard Test Methods for 
Phenolic Compounds in Water. August 2012. Table IB.
    (xxvi) ASTM D1886-14, Standard Test Methods for Nickel in Water. 
November 2014. Table IB.
* * * * *
    (xxxi) ASTM D2036-09 (Reapproved 2015), Standard Test Methods for 
Cyanides in Water. July 2015. Table IB.
* * * * *
    (xxxiv) ASTM D2972-15, Standard Tests Method for Arsenic in Water. 
March 2015. Table IB.
    (xxxv) ASTM D3223-17, Standard Test Method for Total Mercury in 
Water. June 2017. Table IB.
* * * * *
    (xxxvii) ASTM D3373-17, Standard Test Method for Vanadium in Water. 
June 2017. Table IB.
* * * * *
    (xxxix) ASTM D3557-17, Standard Test Method for Cadmium in Water. 
June 2017. Table IB.
    (xl) ASTM D3558-15, Standard Test Method for Cobalt in Water. March 
2015. Table IB.
    (xli) ASTM D3559-15, Standard Test Methods for Lead in Water. 
October 2015. Table IB.
    (xlii) ASTM D3590-17, Standard Test Methods for Total Kjeldahl 
Nitrogen in Water. June 2017. Table IB.
    (xliii) ASTM D3645-15, Standard Test Methods for Beryllium in 
Water. March 2015. Table IB.
* * * * *
    (xlv) ASTM D3859-15, Standard Test Methods for Selenium in Water. 
April 2015. Table IB.
    (xlvi) ASTM D3867-16, Standard Test Method for Nitrite-Nitrate in 
Water. June 2016. Table IB.
    (xlvii) ASTM D4190-15, Standard Test Method for Elements in Water 
by Direct- Current Plasma Atomic Emission Spectroscopy. March 2015. 
Table IB.
    (xlviii) ASTM D4282-15, Standard Test Method for Determination of 
Free Cyanide in Water and Wastewater by Microdiffusion. July 2015. 
Table IB.
    (xlix) ASTM D4327-17, Standard Test Method for Anions in Water by 
Suppressed Ion Chromatography. December 2017. Table IB.
    (l) ASTM D4382-18, Standard Test Method for Barium in Water, Atomic 
Absorption Spectrophotometry, Graphite Furnace. May 2018. Table IB.
* * * * *
    (lii) ASTM D4658-15, Standard Test Method for Sulfide Ion in Water. 
April 2015. Table IB.
* * * * *
    (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. December 2017. Table IB.
    (lv) ASTM D5257-17, Standard Test Method for Dissolved Hexavalent 
Chromium in Water by Ion Chromatography. December 2017. Table IB.
* * * * *
    (lviii) ASTM D5673-16, Standard Test Method for Elements in Water 
by Inductively Coupled Plasma--Mass Spectrometry. February 2016. Table 
IB.
* * * * *
    (lxi) ASTM. D6508-15, Standard Test Method for Determination of 
Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion 
Electrophoresis and Chromate Electrolyte. October 2015. Table IB, Note 
54.
    (lxii) ASTM. D6888-16, Standard Test Method for Available Cyanide 
with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing 
Gas Diffusion Separation and Amperometric Detection. June 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. June 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. January 2018. Table IC.
    (lxv) ASTM. D7237-15a, Standard Test Method for Free Cyanide with 
Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and 
Amperometric Detection. June 2015. Table IB.
    (lxvi) ASTM. D7284-13 (Reapproved 2017), Standard Test Method for 
Total Cyanide in Water by Micro Distillation followed by Flow Injection 
Analysis with Gas Diffusion Separation and Amperometric Detection. July 
2017. Table IB.
* * * * *
    (lxviii) ASTM. D7511-12 (Reapproved 2017), Standard Test Method for 
Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet 
Digestion and Amperometric Detection. July 2017. Table IB.
    (lxix) ASTM. D7573-09 (Reapproved 2017), Standard Test Method for 
Total Carbon and Organic Carbon in Water by High Temperature Catalytic 
Combustion and Infrared Detection, February 2017. Table IB.
    (lxx) ASTM D7781-14 Standard Test Method for Nitrate-Nitrite in 
Water by Nitrate Reductase, May 2014. Table IB.
* * * * *

[[Page 27256]]

    (19) FIAlab Instruments, Inc., 2151 N. Northlake Way, Seattle, WA 
98103. Telephone: 425-376-0450.
    (i) Method 100, Determination of Inorganic Ammonia by Continuous 
Flow Gas Diffusion and Fluorescence Detector Analysis, April 4, 2018. 
Table IB, Note 82.
    (ii) [Reserved]
* * * * *
    (26) MACHEREY-NAGEL GmbH and Co., 2850 Emrick Blvd. Bethlehem, PA 
18020. Telephone: 888-321-6224.
    (i) Method 036/038 NANOCOLOR[supreg] 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, 1303 Eisenhower Drive, Goshen, IN 
46526. Telephone: 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]
* * * * *
    (38) * * *
    (ii) Determination of Heat Purgeable and Ambient Purgeable Volatile 
Organic Compounds in Water by Gas Chromatography/Mass Spectrometry. 
Chapter 12 of Section B, Methods of the National Water Quality 
Laboratory, of Book 5, Laboratory Analysis. 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, 
Note 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. 1999. 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.
* * * * *
    (e) * * *

[[Page 27257]]



                    Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
                                                                                          Maximum holding time 4
        Parameter number/name                Container 1            Preservation 2 3
----------------------------------------------------------------------------------------------------------------
                                            Table IA--Bacterial Tests
----------------------------------------------------------------------------------------------------------------
1-4. Coliform, total, fecal, and E.    PA, G..................  Cool, <10 [deg]C,        8 hours.22 23
 coli.                                                           0.008% Na2S2O3 5.
5. Fecal streptococci................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
6. Enterococci.......................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
7. Salmonella........................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
----------------------------------------------------------------------------------------------------------------
                                        Table IA--Aquatic Toxicity Tests
----------------------------------------------------------------------------------------------------------------
8-11. Toxicity, acute and chronic....  P, FP, G...............  Cool, <=6 [deg]C 16....  36 hours.
----------------------------------------------------------------------------------------------------------------
                                            Table IB--Inorganic Tests
----------------------------------------------------------------------------------------------------------------
1. Acidity...........................  P, FP, G...............  Cool, <=6 [deg]C 18....  14 days.
2. Alkalinity........................  P, FP, G...............  Cool, <=6 [deg]C 18....  14 days.
4. Ammonia...........................  P, FP, G...............  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
9. Biochemical oxygen demand.........  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
10. Boron............................  P, FP, or Quartz.......  HNO3 to pH <2..........  6 months.
11. Bromide..........................  P, FP, G...............  None required..........  28 days.
14. Biochemical oxygen demand,         P, FP G................  Cool, <=6 [deg]C 18....  48 hours.
 carbonaceous.
15. Chemical oxygen demand...........  P, FP, G...............  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
16. Chloride.........................  P, FP, G...............  None required..........  28 days.
17. Chlorine, total residual.........  P, G...................  None required..........  Analyze within 15
                                                                                          minutes.
21. Color............................  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
23-24. Cyanide, total or available     P, FP, G...............  Cool, <=6 [deg]C 18,     14 days.
 (or CATC) and free.                                             NaOH to pH >10 5 6,
                                                                 reducing agent if
                                                                 oxidizer present.
25. Fluoride.........................  P......................  None required..........  28 days.
27. Hardness.........................  P, FP, G...............  HNO3 or H2SO4 to pH <2.  6 months.
28. Hydrogen ion (pH)................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
31, 43. Kjeldahl and organic N.......  P, FP, G...............  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
----------------------------------------------------------------------------------------------------------------
                                               Table IB--Metals 7
----------------------------------------------------------------------------------------------------------------
18. Chromium VI......................  P, FP, G...............  Cool, <=6 [deg]C 18, pH  28 days.
                                                                 = 9.3-9.7 20.
35. Mercury (CVAA)...................  P, FP, G...............  HNO3 to pH <2..........  28 days.
35. Mercury (CVAFS)..................  FP, G; and FP-lined cap  5 mL/L 12N HCl or 5 mL/  90 days.17
                                        17.                      L BrCl 17.
3, 5-8, 12, 13, 19, 20, 22, 26, 29,    P, FP, G...............  HNO3 to pH <2, or at     6 months.
 30, 32-34, 36, 37, 45, 47, 51, 52,                              least 24 hours prior
 58-60, 62, 63, 70-72, 74, 75.                                   to analysis 19.
 Metals, except boron, chromium VI,
 and mercury.
38. Nitrate..........................  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
39. Nitrate-nitrite..................  P, FP, G...............  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
40. Nitrite..........................  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
41. Oil and grease...................  G......................  Cool to <=6 [deg]C 18,   28 days.
                                                                 HCl or H2SO4 to pH <2.
42. Organic Carbon...................  P, FP, G...............  Cool to <=6 [deg]C 18,   28 days.
                                                                 HCl, H2SO4, or H3PO4
                                                                 to pH <2.
44. Orthophosphate...................  P, FP, G...............  Cool, to <=6 [deg]C 18   Filter within 15
                                                                 24.                      minutes; Analyze
                                                                                          within 48 hours.
46. Oxygen, Dissolved Probe..........  G, Bottle and top......  None required..........  Analyze within 15
                                                                                          minutes.
47. Winkler..........................  G, Bottle and top......  Fix on site and store    8 hours.
                                                                 in dark.
48. Phenols..........................  G......................  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
49. Phosphorus (elemental)...........  G......................  Cool, <=6 [deg]C 18....  48 hours.
50. Phosphorus, total................  P, FP, G...............  Cool, <=6 [deg]C 18,     28 days.
                                                                 H2SO4 to pH <2.
53. Residue, total...................  P, FP, G...............  Cool, <=6 [deg]C 18....  7 days.
54. Residue, Filterable (TDS)........  P, FP, G...............  Cool, <=6 [deg]C 18....  7 days.
55. Residue, Nonfilterable (TSS).....  P, FP, G...............  Cool, <=6 [deg]C 18....  7 days.
56. Residue, Settleable..............  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
57. Residue, Volatile................  P, FP, G...............  Cool, <=6 [deg]C 18....  7 days.
61. Silica...........................  P or Quartz............  Cool, <=6 [deg]C 18....  28 days.
64. Specific conductance.............  P, FP, G...............  Cool, <=6 [deg]C 18....  28 days.
65. Sulfate..........................  P, FP, G...............  Cool, <=6 [deg]C 18....  28 days.
66. Sulfide..........................  P, FP, G...............  Cool, <=6 [deg]C 18,     7 days.
                                                                 add zinc acetate plus
                                                                 sodium hydroxide to pH
                                                                 >9.
67. Sulfite..........................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
68. Surfactants......................  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
69. Temperature......................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
73. Turbidity........................  P, FP, G...............  Cool, <=6 [deg]C 18....  48 hours.
----------------------------------------------------------------------------------------------------------------

[[Page 27258]]

 
                                            Table IC--Organic Tests 8
----------------------------------------------------------------------------------------------------------------
13, 18-20, 22, 24, 25, 27, 28, 34-37,  G, FP-lined septum.....  Cool, <=6 [deg]C 18,     14 days.9
 39-43, 45-47, 56, 76, 104, 105, 108-                            0.008% Na2S2O3 5, HCl
 111, 113. Purgeable Halocarbons.                                to pH 2 9.
26. 2-Chloroethylvinyl ether.........  G, FP-lined septum.....  Cool, <=6 [deg]C 18,     14 days.
                                                                 0.008% Na2S2O3 5.
6, 57, 106. Purgeable aromatic         G, FP-lined septum.....  Cool, <=6 [deg]C 18,     14 days.9
 hydrocarbons.                                                   0.008% Na2S2O3 5, HCl
                                                                 to pH 2 9.
3, 4. Acrolein and acrylonitrile.....  G, FP-lined septum.....  Cool, <=6 [deg]C 18,     14 days.10
                                                                 0.008% Na2S2O3, pH to
                                                                 4-5 10.
23, 30, 44, 49, 53, 77, 80, 81, 98,    G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
 100, 112. Phenols 11.                                           0.008% Na2S2O3.          extraction, 40 days
                                                                                          after extraction.
7, 38. Benzidines 11 12..............  G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
                                                                 0.008% Na2S2O3 5.        extraction.13
14, 17, 48, 50-52. Phthalate esters    G, FP-lined cap........  Cool, <=6 [deg]C 18....  7 days until
 11.                                                                                      extraction, 40 days
                                                                                          after extraction.
82-84. Nitrosamines 11 14............  G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
                                                                 store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3 5.               after extraction.
88-94. PCBs 11.......................  G, FP-lined cap........  Cool, <=6 [deg]C 18....  1 year until
                                                                                          extraction, 1 year
                                                                                          after extraction.
54, 55, 75, 79. Nitroaromatics and     G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
 isophorone 11.                                                  store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3 5.               after extraction.
1, 2, 5, 8-12, 32, 33, 58, 59, 74,     G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
 78, 99, 101. Polynuclear aromatic                               store in dark, 0.008%    extraction, 40 days
 hydrocarbons 11.                                                Na2S2O3 5.               after extraction.
15, 16, 21, 31, 87. Haloethers 11....  G, FP-lined cap........  Cool, <=6 [deg]C 18,     7 days until
                                                                 0.008% Na2S2O3 5.        extraction, 40 days
                                                                                          after extraction.
29, 35-37, 63-65, 73, 107.             G, FP-lined cap........  Cool, <=6 [deg]C 18....  7 days until
 Chlorinated hydrocarbons 11.                                                             extraction, 40 days
                                                                                          after extraction.
60-62, 66-72, 85, 86, 95-97, 102,      G......................  See footnote 11........  See footnote 11.
 103. CDDs/CDFs 11.
----------------------------------------------------------------------------------------------------------------
    Aqueous Samples: Field and Lab     G......................  Cool, <=6 [deg]C 18,     1 year.
     Preservation.                                               0.008% Na2S2O3 5, pH
                                                                 <9.
    Solids and Mixed-Phase Samples:    G......................  Cool, <=6 [deg]C 18....  7 days.
     Field Preservation.
    Tissue Samples: Field              G......................  Cool, <=6 [deg]C 18....  24 hours.
     Preservation.
    Solids, Mixed-Phase, and Tissue    G......................  Freeze, <=-10 [deg]C...  1 year.
     Samples: Lab Preservation.
114-118. Alkylated phenols...........  G......................  Cool, <6 [deg]C, H2SO4   28 days until
                                                                 to pH <2.                extraction, 40 days
                                                                                          after extraction.
119. Adsorbable Organic Halides (AOX)  G......................  Cool, <6 [deg]C, 0.008%  Hold at least 3 days,
                                                                 Na2S2O3, HNO3 to pH <2.  but not more than 6
                                                                                          months.
120. Chlorinated Phenolics...........  G, FP-lined cap........  Cool, <6 [deg]C, 0.008%  30 days until
                                                                 Na2S2O3, H2SO4 to pH     acetylation, 30 days
                                                                 <2.                      after acetylation.
----------------------------------------------------------------------------------------------------------------
                                           Table ID--Pesticides Tests
----------------------------------------------------------------------------------------------------------------
1-70. Pesticides 11..................  G, FP-lined cap........  Cool, <=6 [deg]C 18, pH  7 days until
                                                                 5-9 15.                  extraction, 40 days
                                                                                          after extraction.
----------------------------------------------------------------------------------------------------------------
                                          Table IE--Radiological Tests
----------------------------------------------------------------------------------------------------------------
1-5. Alpha, beta, and radium.........  P, FP, G...............  HNO3 to pH <2..........  6 months.
----------------------------------------------------------------------------------------------------------------
                                            Table IH--Bacterial Tests
----------------------------------------------------------------------------------------------------------------
1, 2. Coliform, total, fecal.........  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
3.E. coli............................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
4. Fecal streptococci................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
5. Enterococci.......................  PA, G..................  Cool, <10 [deg]C,        8 hours.22
                                                                 0.008% Na2S2O3 5.
----------------------------------------------------------------------------------------------------------------
                                            Table IH--Protozoan Tests
----------------------------------------------------------------------------------------------------------------
6. Cryptosporidium...................  LDPE; field filtration.  1-10 [deg]C............  96 hours.21
7. Giardia...........................  LDPE; field filtration.  1-10 [deg]C............  96 hours.21
----------------------------------------------------------------------------------------------------------------
1 ''P'' is for polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene [PTFE]; Teflon[supreg]), 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.

[[Page 27259]]

 
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
  [deg]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 [deg]C,
  unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
  is completed. Add the preservative to the sample container prior to sample collection when the preservative
  will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite
  sample within 15 minutes of collection. If a composite measurement is required but a composite sample would
  compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4
  samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the
  concentrations averaged. Alternatively, grab samples may be collected in the field and composited in the
  laboratory if the compositing procedure produces results equivalent to results produced by arithmetic
  averaging of results of analysis of individual grab samples. For examples of laboratory compositing
  procedures, see EPA Method 1664 Rev. A (oil and grease) and the procedures at 40 CFR 141.24(f)(14)(iv) and (v)
  (volatile organics).
3 When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
  the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering such
  material for transportation is responsible for ensuring such compliance. For the preservation requirement of
  Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
  determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
  (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater; Nitric acid
  (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
  acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
  Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
  less).
4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
  samples may be held before the start of analysis and still be considered valid. Samples may be held for longer
  periods only if the permittee or monitoring laboratory have data on file to show that, for the specific types
  of samples under study, the analytes are stable for the longer time, and has received a variance from the
  Regional ATP Coordinator under Sec.   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 Sec.   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 [deg]C, with minimum head space.
5 ASTM D7365-09a 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 [deg]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 [deg]C.
14 For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
  of sampling.
15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
  extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
16 Place sufficient ice with the samples in the shipping container to ensure that ice is still present when the
  samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately measure
  the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In
  the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can
  be given the option of on-site testing or can request a variance. The request for a variance should include
  supportive data which show that the toxicity of the effluent samples is not reduced because of the increased
  holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection
  do not need to be cooled to 0 to 6 [deg]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 [deg]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 ``<= [deg]C'' is used in
  place of the ``4 [deg]C'' and ``<4 [deg]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 [deg]C may not be used to meet the <=6 [deg]C
  requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than
  15 minutes).

[[Page 27260]]

 
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).


0
3. Amend Sec.  136.6 by adding paragraph (b)(4)(xxiii) to read as 
follows:


Sec.  136.6   Method modifications and analytical requirements.

* * * * *
    (b) * * *
    (4) * * *
    (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.
* * * * *
[FR Doc. 2021-09596 Filed 5-18-21; 8:45 am]
BILLING CODE 6560-50-P

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