# Clean Water Act Methods Update Rule for the Analysis of Effluent > Briefs, arguments, decisions, and more. URL: https://www.frixlaw.com/law-library/documents/fr%3A2017-17271 ## Record - **Collection:** Federal Register - **Document type:** Rule - **Published:** August 28, 2017 - **Citation:** 82 FR 40836 ## Text ENVIRONMENTAL PROTECTION AGENCY 40 CFR Part 136 [EPA-HQ-OW-2014-0797; FRL-9957-24-OW] RIN 2040-AF48 Clean Water Act Methods Update Rule for the Analysis of Effluent AGENCY: Environmental Protection Agency (EPA). ACTION: Final rule. SUMMARY: This rule modifies the testing procedures approved for analysis and sampling under the Clean Water Act. The changes adopted in this final rule fall into the following categories: New and revised EPA methods (including new and/or revised methods published by voluntary consensus standard bodies (VCSB), such as ASTM International and the Standard Methods Committee); updated versions of currently approved methods; methods reviewed under the alternate test procedures (ATP) program; clarifications to the procedures for EPA approval of nationwide and limited use ATPs; and amendments to the procedure for determination of the method detection limit to address laboratory contamination and to better account for intra-laboratory variability. DATES: This regulation is effective on September 27, 2017. The incorporation by reference of certain publications listed in the rule is approved by the Director of the Federal Register as of September 27, 2017. For judicial review purposes, this final rule is promulgated as of 1:00 p.m. (Eastern time) on September 12, 2017 as provided at 40 CFR 23.2 and 23.7. ADDRESSES: EPA has established a docket for this action under Docket ID No. EPA-HQ-OW-2014-0797. All documents in the docket are listed on the www.regulations.gov Web site. Although listed in the index, some information is not publicly available, e.g., confidential business information (CBI) or other information whose disclosure is restricted by statute. Certain other materials, such as copyrighted material are not placed on the Internet and will be publicly available only in hard copy form. Publicly available docket materials are available either electronically through www.regulations.gov or in hard copy at the Water Docket in EPA Docket Center, EPA/DC, EPA West William J. Clinton Building, Room 3334, 1301 Constitution Ave. NW., Washington, DC. The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. The telephone number for the Public Reading Room is 202-566-1744 and the telephone number for the Water Docket is 202-566-2426. FOR FURTHER INFORMATION CONTACT: Adrian Hanley, Engineering and Analysis Division (4303T), Office of Water, Environmental Protection Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460-0001; telephone: 202-564-1564; email: hanley.adrian@epa.gov. SUPPLEMENTARY INFORMATION: A. General Information 1. Does this Action apply to me? EPA proposed the changes in this method update rule for public comment on February 19, 2015 (80 FR 8956). EPA Regions, as well as States, Territories and Tribes authorized to implement the National Pollutant Discharge Elimination System (NPDES) program, issue permits with conditions designed to ensure compliance with the technology-based and water quality-based requirements of the Clean Water Act (CWA). These permits may include restrictions on the quantity of pollutants that may be discharged as well as pollutant measurement and reporting requirements. If EPA has approved a test procedure for analysis of a specific pollutant, the NPDES permittee must use an approved test procedure (or an approved alternate test procedure if specified by the permitting authority) for the specific pollutant when measuring the required waste constituent. Similarly, if EPA has established sampling requirements, measurements taken under an NPDES permit must comply with these requirements. Therefore, entities with NPDES permits will potentially be affected by the actions in this rulemaking. Entities potentially affected by the requirements of this rule 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. 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. B. What process governs judicial review of this rule? Under Section 509(b)(1) of the Clean Water Act (CWA), judicial review of this CWA rule may be obtained by filing a petition for review in a United States Circuit Court of Appeals within 120 days from the date of promulgation of this rule. For judicial review purposes, this final rule is promulgated as of 1 p.m. (Eastern time) on September 12, 2017 as provided at 40 CFR 23.2. Section 509(b)(2) provides that any rule (or requirements of any rule) for which review could have been obtained under Section 509(b)(1) may also not be challenged later in civil or criminal proceedings for enforcement. C. Abbreviations and Acronyms Used in the Preamble and Final Rule Text 4AAP: 4-Aminoantipyrine AA: Atomic Absorption ADMI: American Dye Manufacturers Institute AOAC: AOAC International ASTM: ASTM International ATP: Alternate Test Procedure BOD 5 : 5-day Biochemical Oxygen Demand test CAS: Chemical Abstract Services CATC: Cyanide Amenable to Chlorination CFR: Code of Federal Regulations CIE/UV: Capillary Ion Electrophoresis/Ultraviolet COD: Chemical Oxygen Demand CWA: Clean Water Act DPD: N,N-diethyl- p -phenylenediamine DPD-FAS: N,N-diethyl- p -phenylenediamine with ferrous ammonium sulfate EDTA: Ethylenediamine tetraacetic acid EPA: Environmental Protection Agency FLAA: Flame Atomic Absorption Spectroscopy GC: Gas Chromatograph/Chromatography GC/HSD: Gas chromatography/halogen-specific detector GC/MS: Gas chromatography/mass spectrometry HEM: Hexane extractable material HPLC: High performance liquid chromatography HRGC: High Resolution Gas Chromatography HRMS: High Resolution Mass Spectrometry HSD: Halogen-specific detector ICP: Inductively coupled plasma ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy ICP/MS: Inductively Coupled Plasma-Mass Spectrometry LCS: Laboratory Control Sample MDL: Method Detection Limit MS: Mass Spectrometry MPN: Most Probable Number MS/MSD: Matrix Spike/Matrix Spike Duplicate NARA: National Archives and Records Administration NPDES: National Pollutant Discharge Elimination System NIST: National Institute of Standards and Technology PAH: Polynuclear aromatic hydrocarbons POTW: Publicly Owned Treatment Works QA: Quality Assurance QC: Quality Control RRT: Relative retention time SDDC: Silver diethyldithiocarbamate SGT-HEM: Silica gel treated-hexane extractable material SM: Standard Methods SPADNS: Common name for fluoride dye reagent which is a mixture of chemicals STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption Spectroscopy TKN: Total Kjeldahl Nitrogen TOC: Total Organic Carbon USGS: United States Geological Survey UV: Ultraviolet VCSB: Voluntary Consensus Standards Body WET: Whole Effluent Toxicity Table of Contents I. Statutory Authority II. Summary of Final Rule A. New Versions of Previously Approved EPA Methods in 40 CFR 136.3 and Appendix A B. Methods Incorporated by Reference C. New Standard Methods and New Versions of Approved Standard Methods in 40 CFR 136.3 D. New Versions of Approved ASTM Methods in 40 CFR 136.3 E. New United States Geological Survey (USGS) Methods in 40 CFR 136.3 F. New ATPs in 40 CFR 136.3 G. Changes to 40 CFR Part 136 To Align With 40 CFR Part 122 H. Corrections to 40 CFR Part 136 I. Changes to Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times J. Clarifications/Corrections to ATP Procedures in 40 CFR 136.4, 136.5 and Allowed Modifications in 40 CFR 136.6 K. Changes to Appendix B to 40 CFR Part 136—Definition and Procedure for the Determination of the Method Detection Limit (MDL) III. Changes Between the Proposed Rule and the Final Rule A. Changes to Footnote 30 in Table IA and Footnote 27 in Table IH B. Changes to Table IB C. Changes to Table II D. Change to Method Modifications and Analytical Requirements in § 136.6, Methods Modification Paragraph E. Changes to EPA Method 608.3 F. Change to EPA Method 611 G. Changes to EPA Method 624.1 H. Changes to EPA Method 625.1 I. Changes to Method Detection Limit (MDL) Procedure J. Changes to WET Errata IV. Statutory and Executive Order Reviews A. Executive Order 12866: Regulatory Planning and Review and Review and Executive Order 13563: Improving Regulation and Regulatory Review B. Paperwork Reduction Act C. Regulatory Flexibility Act D. Unfunded Mandates Reform Act E. Executive Order 13132: Federalism F. Executive Order 13175: Consultation and Coordination With Indian Tribal Governments G. Executive Order 13045: Protection of Children From Environmental Health Risks and Safety Risks H. Executive Order 13211: Actions That Significantly Affect Energy Supply, Distribution, or Use I. National Technology Transfer and Advancement Act of 1995 J. Executive Order 12898: Federal Actions to Address Environmental Justice in Minority Populations and Low-Income Populations K. Congressional Review Act I. Statutory Authority EPA is promulgating this rule pursuant to the authority of sections 301(a), 304(h), and 501(a) of the Clean Water Act (“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, a National Pollutant Discharge Elimination System (NPDES) permit issued under section 402 of the CWA. Section 304(h) of the CWA requires the Administrator of the 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). II. Summary of Final Rule The following sections describe the changes EPA is making in this final rule. In addition, further information concerning the rule may be found in a document prepared for this rule providing EPA's responses to comments it received on the proposed rule. That document (“Response to Comments Document for the Methods Update Rule Proposal (80 CFR 8956, February 19, 2015”) is available in the electronic docket listed in the ADDRESSES section at the beginning of this document. The following sections describe changes EPA is making in this final rule. A. New Versions of Previously Approved EPA Methods in 40 CFR 136.3 and Appendix A This rule approves new versions of already approved EPA methods and corrects typographical errors in the methods. The following briefly describes the EPA methods added to part 136. 1. EPA Methods 608.3, 611, 624.1 and 625.1 Method 608.3, Organochlorine Pesticides and PCBs by GC/HSD. This method measures organochorine pesticides and polychlorinated biphenyls (PCBs) in industrial discharges and other environmental samples by gas chromatography (GC) combined with a halogen-specific detector (HSD: e.g., electron capture, electrolytic conductivity), as provided under 40 CFR 136.1. EPA Method 611, Haloethers. This method measures the following haloethers: Bis(2-chloroethyl) ether, bis(2-chloroethoxy) methane, 2, 2′-oxybis (1-chloropropane), 4-bromophenyl phenyl ether, and 4-chlorophenyl phenyl ether in municipal and industrial discharges by gas chromatography (GC) as provided under 40 CFR 136.1. The only change EPA has made is correcting a typographical error in the list of parameters by changing “4-Chlorophenyl phenyl either” to “4-Chlorophenyl phenyl ether” and has corrected an analyte name to 2,2′-oxybis(1-chloropropane), which matches the CAS Number 108-60-1. EPA Method 624.1, Purgeables by GC/MS. This method measures purgeable organic pollutants in industrial discharges and other environmental samples by gas chromatography (GC) combined with mass spectrometry (MS), as provided under 40 CFR 136.1. EPA Method 625.1, Base/Neutrals and Acids by GC/MS. This method measures semivolatile organic pollutants in industrial discharges and other environmental samples by GC/MS, as provided under 40 CFR 136.1. 2. EPA Methods 1600, 1603, 1680, and 1682 This rule implements the following changes for EPA microbiological methods 1600, 1603, 1680, and 1682 that correct typographical or other errors that EPA identified in the methods after publication. This rule revises all of these methods with new EPA document numbers and dates. EPA Method 1600 for Enterococci using membrane filtration: In Table 3 Verification controls, EPA changed the negative control for brain heart infusion broth incubated at 45 °C from Escherichia coli to Enterobacter aerogenes. E. coli is thermotolerant and E. aerogenes is not, so E. coli is not an appropriate negative control when heated. EPA Method 1603 for E. coli using membrane filtration: In section 11.5, EPA changed the number of colonies on a countable plate from 20-60 to 20-80 colonies. Sixty colonies was a typographical error. In addition, the following sentence was inadvertently omitted and EPA included it: Sample volumes of 1-100 mL are normally tested at half-log intervals ( e.g., 100, 30, 10, and 3 mL). EPA Method 1680 for fecal coliforms using multiple tube fermentation: In section 3.1 Definitions, the sentence “The predominant fecal coliform is E. coli.” now reads “The predominant fecal coliform can be E. coli.” EPA Method 1682 for Salmonella by MSRV medium: (1) In section 9.3, Table 2, the lab-prepared spike acceptance criteria now reads: “Detect-254%” and “Detect-287%” and (2) in section 14.5, Table 9, the spiked Salmonella for Example 2, Liquid now reads “3.7 x 10 8 CFU/mL.” 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 the selected method. This rule incorporates by reference revisions to methods from two VCSBs: Standard Methods and ASTM. The VCSB methods in this rule are in compliance, as discussed more fully in Section IV.I below, with the National Technology Transfer Act which directs EPA to use voluntary consensus standards so long as they are consistent with applicable law and not otherwise impractical. The methods are available on their respective VCSB Web sites 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. This rule also includes USGS methods and vendor ATPs that are incorporated by reference. The ATPs and USGS methods are available free of charge on the Web site for that organization. Therefore, EPA concludes that the methods and Alternate Test Procedures (ATPs) incorporated by reference are reasonably available. The individual standards are discussed in greater detail below. C. New Standard Methods and New Versions of Approved Standard Methods in 40 CFR 136.3 This rule approves new versions of currently approved Standard Methods. The new versions of currently approved Standard Methods clarify or improve the instructions in the method, improve the QC requirements, or make editorial corrections. Consistent with the previous method update rule (77 FR 29758, May 18, 2012), EPA generally approves and includes in 40 CFR part 136 only the most recent version of a method published by the Standard Methods Committee by 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 3111 B-2011). The date indicates the latest revision date of the method. This allows use of a specific method in any edition that includes a method with the same method number and year of publication. Most of the revisions included to Standard Methods in this rule do not contain any substantive changes. Each Standard Method entry contains the Standard Methods number and date, the parameter, and a brief description of the analytical technique. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear. The following identifies new versions of previously approved Standard Methods that EPA is including in Table IB at 40 CFR part 136. Where there are substantive changes to the method, these are noted: 1. SM 2120 B-2011, color, platinum cobalt visual comparison method. 2. SM 2120 F-2011, color, ADMI weighted-ordinate spectrophotometer method. EPA previously approved this method as SM 2120 E-1993. It is also similar to the currently approved National Council for Air and Stream Improvement, Inc. method that uses American Dye Manufacturers Institute weighted-ordinate.spectrophotometric parameters. A footnote on the method specifies that the pH should be 7.6 and not 7.0 when used for NPDES monitoring purposes, since the original method was approved with a reference pH of 7.6. Additionally, the currently approved methods for the Color parameter are assigned more specific parameter names. 3. SM 2130 B-2011, turbidity, nephelometric method. 4. SM 2310 B-2011, acidity, titration using electrometric endpoint or phenolphthalein endpoint. 5. SM 2320 B-2011, alkalinity, electrometric or colorimetric titration to pH 4.5. 6. SM 2340 B-2011 and SM 2340 C-2011, hardness, by the calculation method or EDTA titration. 7. SM 2510 B-2011, conductivity, Wheatstone bridge method. 8. SM 2540 B-2011, SM 2540 C-2011, SM 2540 D-2011, SM 2540 E-2011, and SM 2540 F-2011, total, filterable, non-filterable, volatile, and settleable residue (solids, listed in the same order as the method numbers), all by gravimetric methodologies. 9. SM 2550 B-2010, temperature, thermometric. 10. SM 3111 B-2011, SM 3111 C-2011, SM 3111 D-2011, and SM 3111 E-2011, metals, direct aspiration atomic absorption (AA) methods with different gas mixtures. Each method has a different list of metals; these lists were not changed. 11. SM 3112 B-2011, metals, applicable to mercury, cold-vapor atomic absorption spectrometric method. 12. SM 3113 B-2010, metals, electrothermic atomic absorption spectrometric method. The only substantive change is a reduction in the required replicate analyses of each calibration standard from three to two. Similar EPA methods do not require replicates of each calibration standard. 13. SM 3114 B-2011 and SM 3114 C-2011, total arsenic and total selenium, hydride generation/atomic absorption spectrometric methods. Both analyze total arsenic and total selenium. 14. SM 3120 B-2011, metals, inductively coupled plasma (ICP) method; no changes were made to the approved list of metals. 15. SM 3125 B-2011, metals, inductively coupled plasma/mass spectrometry (ICP/MS) method; no changes were made to the approved list of metals. 16. SM 3500-Al B-2011, aluminum, colorimetric method. 17. SM 3500-As B-2011, arsenic, colorimetric method silver diethyldithiocarbamate (SDDC) method. 18. SM 3500-Ca B-2011, calcium, titrimetric method (EDTA). 19. SM 3500-Cr B-2011 and SM 3500-Cr C-2011, chromium. The “B” method uses a colorimetric method (diphenyl-carbazide) and is approved for total or dissolved chromium. The “C” method uses ion chromatography and is only approved for dissolved chromium. 20. SM 3500-Cu B-2011 and SM 3500-Cu C-2011, copper. Both method sections use colorimetric methods. The “B” method uses a neocuproine reagent, and the “C” method uses a bathocuproine reagent. 21. SM 3500-Fe B-2011, iron, colorimetric method (phenanthroline). 22. SM 3500-K B-2011 and SM 3500-K C-2011, potassium. The “B” method is a flame photometric method, and the “C” method is an electrode method. 23. SM 3500-Mn B-2011, manganese, colorimetric method (persulfate). 24. SM 3500-Na B-2011, sodium, flame photometric method. 25. SM 3500-Pb B-2011, lead, colorimetric method (dithizone). 26. SM 3500-V B-2011, vanadium, colorimetric method (gallic acid). 27. SM 3500-Zn B-2011, zinc, colorimetric method (zincon). 28. SM 4110 (B-D)-2011, anions, ion chromatography; no changes were made to the approved analyte list. 29. SM 4140 B-2011, inorganic anions, capillary ion electrophoresis with indirect ultraviolet (UV) detection: No changes were made to the approved analyte list. 30. SM 4500-B B-2011, boron, spectrophotometer or filter photometer (curcumin) 31. SM 4500-Cl − (B-E)-2011, chloride, titrimetric: (Silver nitrate), (mercuric nitrate), automated (ferricyanide), potentiometric titration. 32. SM 4500-Cl (B-G)-2011, chlorine (residual), amperometric direct, amperometric direct (low level), iodometric direct, back titration ether end-point, titrimetric: N,N-diethyl- p -phenylenediamine with ferrous ammonium sulfate (DPD-FAS), spectrophotometric (DPD). 33. SM 4500-CN − (B-G)-2011, cyanide, manual distillation with MgCl 2 followed by: Titrimetric, spectrophotometric, manual, ion selective electrode, cyanide amenable to chlorination (CATC); manual distillation with MgCl 2 , followed by: Titrimetric or spectrophotometric. 34. SM 4500-F − (B-E)-2011, fluoride, manual distillation, followed by any of the following: Electrode, manual, colorimetric, fluoride dye reagent (SPADNS is the common name for the fluoride dye reagent which is a mixture of chemicals), automated complexone. 35. SM 4500-H + B-2011, hydrogen ion (pH), electrometric measurement. 36. SM 4500-NH 3 (B-H)-2011, ammonia (as nitrogen), manual distillation or gas diffusion (pH > 11), followed by any of the following: Titration, electrode, manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods; automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods. 37. SM 4500-NO 2 − B-2011, nitrite (as nitrogen), spectrophotometric: Manual. 38. SM 4500-NO 3 − D-2011, nitrate (as nitrogen), ion selective electrode. 39. SM 4500-NO 3 − (E, F, H)-2011, nitrate-nitrite (as nitrogen), colorimetric: Cadmium reduction-manual and automated, and colorimetric: Automated hydrazine. 40. SM 4500-NO 3 − (E, F)-2011, nitrite (as nitrogen), colorimetric: Cadmium reduction-manual and automated. 41. SM 4500-N org (B-D)-2011, total Kjeldahl nitrogen (as nitrogen, organic), semi-automated block digester colorimetric (distillation not required). 42. SM 4500-O (B-G)-2011, oxygen (dissolved), Winkler (azide modification), electrode. 43. SM 4500-P (B(5), E-H)-2011, phosphorus and ortho-phosphate, persulfate digestion, digestion, followed by any of the following: Manual or automated ascorbic acid reduction. The “B Part 5” method is the persulfate digestion procedure and is required prior to measurement of total phosphorus using SM 4500 P (E-H). The “E” through “G” methods are approved for both total phosphorus and ortho-phosphate. The “H” method is only approved for total phosphorous. 44. SM 4500-S 2− (B-D, F, G)-2011, sulfide, sample pretreatment, titrimetric (iodine) analysis, colorimetric (methylene blue), ion selective electrode. 45. SM 4500-SiO 2 (C, E, F)-2011, silica, 0.45-micron filtration followed by any of the following: Colorimetric, manual or automated (molybdosilicate). 46. SM 4500-SO 3 2− B-2011, sulfite, titrimetric (iodine-iodate). 47. SM 4500-SO 4 2− (C-G)-2011, sulfate, automated colorimetric, gravimetric, and turbidimetric. 48. SM 5210 B-2011, biochemical oxygen demand (BOD5), dissolved oxygen depletion. 49. SM 5220 (B-D)-2011, chemical oxygen demand (COD), titrimetric; spectrophotometric, manual or automatic. 50. SM 5310 (B-D)-2011, total organic carbon (TOC), combustion, heated persulfate or UV persulfate oxidation. 51. SM 5520 (B, F)-2011, oil and grease, hexane extractable material (HEM): n-hexane extraction and gravimetry, silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry. 52. SM 5530 (B, D)-2010, phenols, manual distillation, followed by colorimetric 4-aminoantipyrine (4AAP) manual. 53. SM 5540 C-2011, surfactants, colorimetric (methylene blue). The following identifies new versions of previously approved Standard Methods that EPA is including in Table IC at 40 CFR part 136: 1. SM 6200 (B, C)-2011, volatile organic compounds, purge and trap capillary-column gas chromatographic/mass spectrometric (GC/MS), purge and trap capillary-column gas chromatographic (GC) 2. SM 6440 B-2005, polynuclear aromatic hydrocarbons (PAHs), high performance liquid chromatography (HPLC) The following identifies new versions of previously approved methods that EPA is including in Table ID at 40 CFR part 136: 1. SM 6630 (B, C)-2007, organochlorine pesticides, gas chromatography (GC) 2. SM 6640 B-2006, acidic herbicide compounds, gas chromatography (GC) EPA also revised the approval of certain Standard Methods previously approved in part 136 for which Standard Methods adopted updates that contain substantive changes. The following summarizes these changes for each method, organized by the table at 40 CFR part 136 in which they appear. The following identifies previously approved Standard Methods in Table IA and/or Table IH at 40 CFR part 136 Table IB at 40 CFR part 136 where there are substantive changes to the method: 1. EPA replaced the membrane filtration method SM 9222 B-1997 with SM 9222 B-2006. This method analyzes Coliform (total) in the presence of chlorine. The newer method includes a number of technology updates that do not significantly change the procedure. In addition, the method: a. Modified the procedure to allow for the use of a humidified incubator if loose-lidded plates are used during incubation. b. Added a note that five typical and five atypical colonies per membrane need to be identified during coliform verification. c. Moved the definition of “Coliform” that was Section 4 of SM 9222, and renumbered the rest of the document, such that the “Procedure” is now Section 4, instead of Section 5. This is not a substantive change except that in Table IA, Parameter 4 “Coliform (total), in presence of chlorine, number per 100 mL” the citation for “MF with enrichment” will be changed from “9222 (B+B.5c)-1997” to “9222 (B+B.4c)-2006.” 2. This rule replaces the membrane filtration method SM 9222 D-1997 with SM 9222 D-2006. This method analyzes Coliform (fecal) and Coliform (fecal) in the presence of chlorine. The new method allows use of a dry recirculating incubator as specified in the culture dishes section. In addition, this rule adds the following footnote to Tables IA and IH regarding SM 9222 D-2006 for fecal coliform verification frequency: “The verification frequency is at least five typical and five atypical colonies per sampling site on the day of sample collection & analysis.” SM 9222 D-2006 specifies that the fecal coliform colonies should be verified “at a frequency established by the laboratory,” which can be as low as zero. Colonies need to be verified to prevent misidentification of results as false positive or false negative. 3. This rule replaces the membrane filtration method SM 9222 G-1997 with SM 9222 G-2006 in Table IH. These methods analyze for E. coli and Fecal Coliforms. The newer method includes a number of technology updates that do not significantly change the procedure. In addition, the method now has a modified composition of EC broth to include different quantities of KH 2 PO 4 and 4-methylumbelliferyl-β-D-glucuronide. D. New Versions of Approved ASTM Methods in 40 CFR 136.3 This rule approves new versions of currently approved ASTM methods, for the same reasons outlined in the first paragraph of Section II.B above. Many of the new versions of ASTM Methods approved in 40 CFR part 136 do not contain any substantive changes. Each entry contains (in the following order): Approved ASTM method number and date, the parameter, a brief description of the analytical technique. Where there were substantive changes, they are identified. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear. The following identifies new versions of currently approved ASTM methods that are included in Table IB at 40 CFR part 136: 1. ASTM D 511-09 (A, B), calcium and magnesium, titrimetric ethylenediamine tetraacetic acid (EDTA), AA direct aspiration. 2. ASTM D 516-11, sulfate ion, turbidimetric. 3. ASTM D 858-12 (A-C), manganese, atomic absorption (AA) direct aspiration, AA furnace. 4. ASTM D 859-10, silica, colorimetric, manual. 5. ASTM D 1067-11, acidity or alkalinity, electrometric endpoint or phenolphthalein endpoint; electrometric or colorimetric titration to pH 4.5, manual. 6. ASTM D 1068-10 (A-C), iron, AA direct aspiration; AA furnace; colorimetric (phenanthroline). 7. ASTM D 1126-12, hardness, titrimetric (EDTA). 8. ASTM D 1179-10 (A, B), fluoride ion, electrode, manual; colorimetric, (SPADNS). 9. ASTM D 1246-10, bromide ion, electrode. 10. ASTM D 1687-12 (A-C), chromium (total) and dissolved hexavalent chromium, colorimetric (diphenyl-carbazide); AA direct aspiration; AA furnace. 11. ASTM D 1688-12 (A-C), copper, AA direct aspiration, AA furnace. 12. ASTM D 1691-12 (A, B), zinc, AA direct aspiration. 13. ASTM D 1976-12, dissolved, total-recoverable, or total elements, inductively coupled plasma/atomic emission spectroscopy (ICP/AES). 14. ASTM D 3223-12, total mercury, cold vapor, manual. 15. ASTM D 3373-12, vanadium, AA furnace. 16. ASTM D 3557-12 (A-D), cadmium, AA direct aspiration, AA furnace, voltammetry. 17. ASTM D 3590-11 (A, B), total Kjeldahl nitrogen, manual digestion and distillation or gas diffusion; semi-automated block digester colorimetric (distillation not required). 18. ASTM D 4382-12, barium, AA furnace. 19. ASTM D 4658-09, sulfide ion, ion selective electrode. 20. ASTM D 5257-11, dissolved hexavalent chromium, ion chromatography. 21. ASTM D 5673-10, dissolved elements and total-recoverable elements, ICP/MS. 22. ASTM D 5907-13, filterable matter (total dissolved solids) and nonfilterable matter (total suspended solids), gravimetric, 180 °C gravimetric, 103-105 °C post washing of residue. 23. ASTM D 6508-10, inorganic anions (fluoride, bromide, chloride, nitrite, nitrate, orthophosphate, and sulfate), capillary ion electrophoresis with indirect UV detection. 24. ASTM D 7284-13, total cyanide, manual distillation with MgCl 2 followed by flow injection, gas diffusion amperometry. 25. ASTM D 7511-12, total cyanide, segmented flow injection, in-line ultraviolet digestion, followed by gas diffusion amperometry. EPA has changed Table IC at 40 CFR part 136 as follows: 1. ASTM D 7065-11, nonylphenol, bisphenol A, p-tert -octylphenol, nonylphenol monoethoxylate, nonylphenol diethoxylate, gas chromatography/mass spectrometry (GC/MS). E. New United States Geological Survey (USGS) Methods in 40 CFR 136.3 1. This rule adds USGS Methods I-2547-11 and I-2548-11 titled “Colorimetric Determination of Nitrate Plus Nitrite in Water by Enzymatic Reduction, Automated Discrete Analyzer Methods,” to Table IB for the analytes nitrate, nitrite, and combined nitrate-nitrite. Method I-2548-11 is a low level (analytical range) version of Method I-2547-11. Both methods are included in the same method title. The method can be found in USGS Survey Techniques and Methods, Book 5, Chapter B8. The method is available at no cost from the USGS Web site. This method follows the same procedure as in ATP Case No. N07-0003—Nitrate Elimination Company Inc.'s (NECi) Method N07-0003, Revision 9.0, March 2014, “Method for Nitrate Reductase Nitrate-Nitrogen Analysis,” which EPA approved in this rule. F. New ATPs in 40 CFR 136.3 This rule approves six methods submitted to EPA for review through the alternate test procedures (ATP) program and deemed acceptable based on the evaluation of documented method performance. The following ATP has nationwide approval for wastewater and is incorporated into Table IA: 1. IDEXX Laboratories, Inc., Colilert®-18, “Coliform/ E. coli Enzyme Substrate Test for Fecal Coliforms in Wastewater” (ATP Case No. N09-0004). The method is similar to the already approved E. coli Colilert®-18 method, with the addition of an increased incubation temperature for fecal coliforms, which requires the use of a waterbath incubator. The Colilert®-18 Coliform/ E. coli Enzyme Substrate Test can be obtained from IDEXX Laboratories Inc., One IDEXX Drive, Westbrook, ME 04092. Telephone: 800-321-0207. The following four ATPs have nationwide approval for all matrix types and are incorporated into Table IB: 1. The Nitrate Elimination Company Inc. (NECi) Method N07-0003, “Nitrate Reductase Nitrate-Nitrogen Analysis,” Revision 9.0, dated March 2014 (The Nitrate Elimination Company, Inc., 2014a). The analysis measures nitrate, nitrite, and combined nitrate-nitrite. NECi Method N07-0003 is a “green” alternative to the other approved methods which use cadmium, a known carcinogen for the reduction of nitrate to nitrite prior to analyses. NECi Method N07-0003 can be obtained from The Nitrate Elimination Company, 334 Hecla Street, Lake Linden, Michigan, 49945. Telephone: 888-NITRATE. 2. Timberline Instruments, LLC Method Ammonia-001, “Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis,” dated June 24, 2011 (Timberline Instruments, LLC 2011a). Timberline Instruments, LLC Method Ammonia-001 can be obtained from Timberline Instruments, LLC, 1880 South Flatiron Court, Boulder, Colorado 80301. Telephone: 303-440-8779. 3. Hach Company Method 10242, “Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater,” Revision 1.1, dated January 10, 2013 (Hach Company 2013a). Hach Company Method 10242 is a simplified green chemistry alternative to the other approved methods for measuring TKN. The method uses less toxic reagents ( e.g., eliminating the use of mercuric sulfate). Hach Company Method 10242 can be obtained from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539. Telephone: 970-669-3050. 4. Hach Company Method 10206, “Spectrophotometric Measurement of Nitrate in Water and Wastewater,” Revision 2.1, dated January 10, 2013 (Hach Company 2013b). Hach Company Method 10206 is a “green” alternative to the other approved methods which use cadmium, a known carcinogen for the reduction of nitrate to nitrite prior to analyses. Hach Company Method 10206 can be obtained from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539. Telephone: 970-669-3050. The following ATP has nationwide approval for only pulp, paper and paperboard mill biologically treated effluent and is incorporated into Table IB: 1. National Council for Air and Stream Improvement, Inc. (NCASI) Method TNTP-W10900, “Total (Kjeldahl) Nitrogen (TKN) and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion,” dated June 2011 (National Council for Air and Stream Improvement, Inc. 2011a). NCASI Method TNTP-W10900 can be obtained from The National Council for Air and Stream Improvement, Inc., Publications Coordinator, P.O. Box 13318, Research Triangle Park, NC 27709-3318, Telephone: 919-941-6400. G. Changes to 40 CFR Part 136 To Align With 40 CFR Part 122 This rule amends 40 CFR 136.1 to substitute the term “Director” for the terms “Administrator” and “State having an authorized program.” In addition, the rule amends 40 CFR 136.2(d) to state that the term “Director” by cross-reference to the definition of “Director” in the NPDES regulations at 40 CFR 122.2. EPA eliminated the words “be sufficiently sensitive and” from 40 CFR 136.6(b)(2) to eliminate unnecessary confusion with the term “sufficiently sensitive,” as used in 40 CFR 122. Deleting this term did not change the requirements of 40 CFR 136.6(b)(2). H. Corrections to 40 CFR Part 136 This rule corrected typographical errors, updated methods from VCSBs that went unnoticed during the last update to 40 CFR part 136, and added technology updates to toxicity methods. 1. This rule makes multiple clarifications and corrections to the Whole Effluent Toxicity acute and chronic methods manuals (Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA-821-R-02-012, October 2002; Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA/821/R-02/013, October 2002; and Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA/821/R-02/014, October 2002) listed in Table IA. Clarifications included definition of terms ( e.g., the acronym YCT—yeast, cereal leaves, and trout chow, was not defined), consistency corrections among the three manuals, notation that Cusum figure axes should be log scale, pH and temperature measurements should be done at the beginning of the test (rather than only at the end of the test), etc. Corrections also included deletion of unavailable products, typographical errors, etc. Among the corrections that EPA proposed was a change to the language for Fathead Minnows, Daphnids, and Green Alga in the document Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition, U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA/821/R-02/013, October 2002. For Fathead Minnows and Daphnids, EPA proposed to change “Conductivity, alkalinity, and hardness are measured in each new sample (100% effluent or receiving water) and in the control” to read “Conductivity, alkalinity, and hardness are measured at the beginning of the test for all test concentrations in each new sample and in the control before they are dispersed to the test chambers.” EPA received a number of comments stating that this change would constitute a change to the test rather than a correction or clarification. EPA is in agreement with these comments, and for that reason, will not add the inserted language “at the beginning of the test for all test concentrations.” EPA is retaining its deletion of “(100% effluent or receiving water)” and the insertion of “before they are dispensed to the test chamber” to the end of the sentence. Thus, the sentence will now read “Conductivity, alkalinity, and hardness are measured in each new sample and in the control before they are dispensed to the test chamber.” For Green Alga, the proposed change has been eliminated from the errata because only the increased testing was proposed. 2. This rule changes the Standard Method listed for E. coli most probable number (MPN) in Tables IA and IH. During a previous revision, Standard Methods added sampling as section 9221 B.1. As a result, section 9221 B.1 in previously approved versions has become section 9221 B.2. EPA changed SM 9221 B.1 to 9221 B.2 in Tables IA and IH for E. coli MPN. The related footnotes in Tables IA and IH (12, 14 and 11, 13, respectively) are accurate and EPA did not propose to change them. 3. This rule adds a line for Enterococci that was erroneously deleted in the 2012 Methods Update Rule. The line states “MPN, multiple tube” with Standard Method 9230B-2007. 4. This rule revises a hardness entry in Table IB to state “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.” Previously, this was only allowed for inductively coupled plasma or AA direct aspiration Ca and Mg methods. The rationale behind this change is that if one calcium and magnesium method approved by EPA can be used to calculate hardness, then other EPA approved methods should also be permitted to do so. 5. This rule deletes “p 14” from footnote 24 of Table IB because the method is not on that page. 6. This rule deletes Method 200.5, in Table IB from the cobalt, molybdenum and thallium entries. These analytes have not undergone formal testing by this method, and this method should not have been approved for these analytes. 7. This rule removes the reference to costs in 40 CFR 136.3(b) because costs are not included in the referenced documents. 8. This rule removes the first instance of “are” in 40 CFR 136.3(e) because it is a typographical error. I. Changes to Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times This rule revises Table II at 40 CFR 136.3(e) as follows. 1. The rule adds rows to Table II that specify holding times for total/fecal coliforms, and fecal streptococci in Table IH. Previously the holding times for these bacterial tests were unspecified. Now these methods have the same holding time requirements as the other bacterial tests. 2. This rule changes the sodium thiosulfate concentrations in Table II for bacterial tests from 0.0008% sodium thiosulfate to 0.008%. EPA proposed this change in its last update to 40 CFR part 136 (75 FR 58066-58067), but inadvertently omitted it in the publication of the final rule. 3. The rule re-inserts language that was accidentally deleted from footnote 5 of Table II during the previous update to 40 CFR part 136. Footnote 5 now reads “ASTM D7365-09a specifies treatment options for samples containing oxidants ( e.g., chlorine) for cyanide analysis. Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses dechlorination procedures for microbiological analyses.” Previously, the words: “for microbiological analyses,” were not present, so the footnote did not specify that treatment options for samples containing oxidants is specifically for cyanide analysis, and that the dechlorination procedures are specifically for microbiological analyses. 4. EPA requested public comment on how to approve variances to sample preservation, containers or holding times listed in Table II for specific dischargers. Currently, 40 CFR 136.3(e) grants authority to either the permitting authority in the Region or the Regional ATP Program Coordinator to grant exceptions to Table II for a specific discharger. Of the eight comments received, four commenters thought that the permitting authority should have the sole authority to approve these variance requests. Three commenters thought that the Regional ATP Program Coordinators should have sole authority to approve variance requests, and one commenter thought that the best approach was for the permitting authority and the Regional ATP Program Coordinator to approve Table II variances for specific dischargers collaboratively. Each of these commenters provided sound reasoning for their suggested approach to the review and approval of these types of requests. EPA has chosen to defer any decision on revising the current language and to leave 40 CFR 136.3(e) unchanged in this final rule. J. Clarifications/Corrections to ATP Procedures in 40 CFR 136.4, 136.5 and Allowed Modifications in 136.6 40 CFR 136.4 and 136.5 describe EPA procedures for obtaining approval to use an alternate test procedure either on a national basis, or for limited use by dischargers or facilities specified in the approval. In the 2012 Method Update Rule, EPA made several clarifying changes to the language of these sections. At the same time, however, in many places in 40 CFR 136.4 and 136.5 where the phrase “Regional Alternate Test Procedures Coordinator” or “Regional ATP Coordinator” appears, EPA inadvertently also inserted the phrase “or permitting authority” following the phrase. This error resulted from the use of the “search and replace” function on the computer. The effect of the change was to inadvertently authorize State permitting authorities to approve ATPs for limited use within the State. EPA never intended this result, as is demonstrated by two facts. First, in its proposal for the 2012 Update (75 FR 58024, September 23, 2010), EPA did not propose to authorize State NPDES permitting authorities to approve limited use ATPs. Second, the rule states that the approval may be restricted to specific dischargers or facilities, or to all dischargers or facilities “specified in the approval for the Region.” (emphasis added). This language evidenced EPA's intent that only the Region—not the State—would be authorized to issue any such limited use ATP approval. Finally, as further evidence of EPA's intent, in several places, the text of the rule only makes sense if read to authorize only the Regional ATP Coordinator, not the State permitting authority, to approve limited use ATPs. For example, 40 CFR 136.5(d)(1) provides that after a review of the application by the Alternate Test Procedure Regional ATP Coordinator or permitting authority, the Regional ATP Coordinator or permitting authority notifies the applicant and the appropriate State agency of approval or rejection of the use of the alternate test procedure. As previously written, if the State is acting on a request for approval, the regulation would require the State to inform itself of its own action in approving or rejecting the ATP, a superfluous requirement. This rule deletes all instances of “or permitting authority” from 40 CFR 136.4 and 136.5 to correct this error and revise the rule text to its original intent. Based on this revision, EPA and EPA alone has the authority to approve limited use ATPs. This rule also changes 40 CFR 136.4 and 136.5 to clarify the process for nationwide ATP approvals and the Regional ATP Coordinator's role in limited use ATP approvals. These changes do not significantly change the process; the intent is to make the text simpler and clearer. Finally, this rule adds language to 40 CFR 136.6(b)(1) to clarify that if a method user is uncertain whether or not a modification is allowed under 40 CFR 136.6, the user should contact either their Director or EPA Regional ATP Coordinator. K. Changes to Appendix B to 40 CFR Part 136—Definition and Procedure for the Determination of the Method Detection Limit (MDL) EPA is revising the procedure for determination of the MDL primarily to address laboratory blank contamination and to better account for intra-laboratory variability. The MDL procedure has not been revised since it was originally promulgated in 1983. The suggestion for these revisions came first from The National Environmental Laboratory Accreditation Conference (NELAC) Institute. EPA proposed to adopt these revisions. Following proposal, EPA further evaluated the proposed revision in conjunction with input from the states and commercial laboratories. EPA received extensive comments on the proposed revisions. The revisions address the following issues and add new requirements in the following areas. Background contamination. Under the revisions to appendix B, laboratories are required to evaluate the MDL to account for background levels of contamination. As laboratory methods become more and more sensitive, background levels of contamination are more likely to contribute to the result. These revisions will reduce false positive detects. MDLs that represent multiple instruments. Under the revisions, if a laboratory uses MDL values that represent multiple instruments, then the laboratory is required to calculate the MDL by analyzing MDL samples and method blanks on all of these instruments. ( Note: MDL samples are a reference matrix, such as reagent water, spiked with a known and consistent quantity of the analyte.) Previously, laboratories were known to run all of their prepared MDL samples on the most sensitive instrument, and then use that MDL for other instruments. This modification makes the MDL more representative of the laboratory's actual analytical capability. Deriving an MDL that is representative of multiple instruments is an option, not a requirement; laboratories can determine individual MDL values for individual instruments if they prefer. Under the revisions, laboratories are required to run MDL samples and method blanks every quarter that samples are analyzed using a specific method. Previously, laboratories redetermined the MDL once a year, often under the most ideal circumstances ( e.g., immediately after the instrument has been serviced or after an annual maintenance routine). Quarterly MDL samples and method blanks will determine if the detection limit has significantly drifted over time. Laboratories will be exempt from running the quarterly MDL samples and method blanks for a method during quarters when no samples are analyzed using that method. The ongoing quarterly MDL samples and method blanks are used to calculate the MDL every year, recalculation of the MDL is required once every thirteen months. Thirteen months was selected to give laboratories more flexibility. For example, a laboratory can recalculate an MDL on January 8th one year and then January 17th the next, and still be in compliance. EPA received comments from industries that purchase laboratory services that stated the revised MDL procedure may increase laboratory costs, but not significantly. EPA also received comments from some laboratories stating the revised MDL procedure would impose increased costs to laboratories, while other laboratories stated the opposite. The majority of commenters supported the revised MDL procedure. All of the laboratory associations, who represent the laboratory community, commented in favor of the revised MDL procedure. Comments not in favor of the MDL revision were received from individual laboratories, individuals, one utility, and two state government departments. As a result of the comments, EPA has made minor clarifications to the MDL procedure. Two options were added to the MDL procedure as a result of comments received: (1) A streamlined approach to determine whether a new instrument can be added to a group of instruments with an already established MDL and (2) laboratories have the option to use only the last six months of method blank data or the fifty most recent method blanks, whichever yields the greater number of method blanks to calculate the MDL value derived from method blanks (MDLb). Both of these changes are in line with the goals of the revised MDL procedure, and are responsive to the comments received. Neither of these additions are mandatory; however, they provide the laboratory with more options for calculating the MDL. Commenters also noted that the detection limit definition in § 136.2(f) should undergo a minor revision to match the revisions in the MDL procedure (which the definition references). The words, “distinguishable from the method blank results” has been replaced with “greater than zero” in the definition. III. Changes Between the Proposed Rule and the Final Rule Except as noted below, the content of the final rule is the same as that of the proposed rule. A. Changes to Footnote 30 in Table IA and Footnote 27 in Table IH These footnotes regard SM 9222 D-2006 for fecal coliform verification frequency. EPA proposed a requirement of “at least five typical and five atypical colonies per sampling site on the day of collection and analysis.” A number of commenters identified deficiencies with the proposed changes. After further review, EPA has determined that footnote 30 in Table IA and footnote 27 in Table IH require both modification and clarification and is changing both footnotes to read “On a monthly basis, at least ten blue colonies from the medium 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.” B. Changes to Table IB As pointed out by multiple commenters, and verified by EPA, the color parameter in Table IB contains methodologies and methods that are mislabeled. EPA reorganized the Color methodology descriptions and methods as follows: (1) The ADMI colorimetric procedure SM 2120 F-2011 is now listed on a new “ADMI” methodology row. (2) Footnote 18 is listed on the table row with the methodology “spectrophotometric,” and footnote 18 lists both NCASI Technical Bulletin 253 (1971) and NCASI Technical Bulletin 803 (2000). NCASI Technical Bulletin 803 is an update to NCASI Technical Bulleting 253 for the measurement of color in pulp mill wastewaters. The update adds a stabilizing pH buffer and turbidity reduction approaches. (3) SM 2120 B-2011 and USGS Method I-1250-85 are on a methodology row labeled “platinum cobalt visual comparison” methods. The Capillary Ion Electrophoresis/Ultraviolet (CIE/UV) method, D6508, Rev. 2 has been moved from the ASTM column to the USGS/AOAC/Other column because this method is available from Waters Corporation (see footnote 54 in Table IB). This affects the following parameters: Bromide, mg/L; chloride, mg/L; fluoride—total, mg/L; nitrate (as N), mg/L; nitrite (as N), mg/L; orthophosphate (as P), mg/L; and sulfate (as SO 4 ) mg/L. C. Changes to Table II A time clarification of 15 minutes has been added to the parameter for Temperature. The parameter 2-Chloroethylvinyl ether has been moved from the first row for Table IC organic tests to a separate row. Section 9.7 of the revised EPA Method 624.1 notes that acidification will destroy 2-chlooethylvinyl ether. Thus, adding HCl to pH 2 would not be acceptable for this parameter. D. Change to Method Modifications and Analytical Requirements in § 136.6, Methods Modification Paragraph For clarification purposes, the following two lines have been added to the methods modification paragraph (b): Where the laboratory is using a vendor-supplied method, it is the QC criteria in the reference method, not the vendor's method that must be met to show equivalency. Where a sample preparation step is required ( i.e., digestion, distillation), QC tests are to be run using standards treated in the same way as samples. Also in this paragraph, the paragraph (b)(4)(xvi), “Changes are allowed in purge-and-trap sample volumes or operating conditions,” was incorrectly deleted and is being reinstated. Further, paragraph (b)(4)(xvii), regarding allowable modifcations to Method 625, is being deleted as Method 625 has been replaced in its entirety with an updated version with this rulemaking. E. Changes to EPA Method 608.3 EPA received numerous comments on Method 608.3, ranging from pointing out minor typographical errors to questioning substantive technical aspects of the proposed method. In response, EPA revised the method to address many of those comments. See the Response to Comments document available in the electronic docket listed in the ADDRESSES section at the beginning of this document for a detailed description of the changes. Additionally, based on comments received in response to the proposal, EPA is reverting to the MDL values in the earlier version of Method 608 for those analytes that were included in Table 1 of Method 608.3. The MDLs in the proposed version of 608.3 were chosen for the proposed revision because they were determined with a capillary GC column. However, as noted by commenters, the values are not derived from a multiple laboratory validation study. Therefore, EPA has restored the original Method 608 MDL values. At such time as EPA develops new multi-laboratory MDL and ML values for the method, they will be included in a future revision and rulemaking. Although EPA received comments about updating the QC acceptance criteria in Method 608.3, EPA did not adopt such changes because EPA lacks data from a multi-laboratory validation study from which to develop such criteria. F. Change to EPA Method 611 In Section 1.1, EPA corrected the last parameter in the list of parameters table, that read “4-Chlorophenyl phenyl either,” a typographical error. The word “either” should be “ether.” The correct parameter name is “4-Chlorophenyl phenyl ether.” G. Changes to EPA Method 624.1 EPA received numerous comments on Method 624.1, ranging from pointing out minor typographical errors to questioning substantive technical aspects of the proposed method. In response, EPA revised the method to address many of those comments. See the response to comments document available in the docket listed in the ADDRESSES section at the beginning of this document for a detailed description of the changes. Additionally, section 8.1.2.1.2, subsection e, Sample matrices on which MS/MSD tests must be performed for nationwide use of an allowed modification, has been changed to update the web link for the list of industrial categories with existing effluent guidelines to https://www.epa.gov/cwa-methods/alternate-test-procedure-documents . Although EPA received comments about updating the QC acceptance criteria in Method 624.1, EPA did not adopt such changes because EPA lacks data from a multi-laboratory validation study from which to develop such criteria. H. Changes to EPA Method 625.1 EPA received numerous comments on Method 625.1, ranging from pointing out minor typographical errors to questioning substantive technical aspects of the proposed method. In response, EPA revised the method to address many of those comments. See the response to comments document available in the electronic docket listed in the ADDRESSES section at the beginning of this document for a detailed description of the changes. Additionally, as was the case with EPA Method 624.1, section 8.1.2.1.2, subsection e, Sample matrices on which MS/MSD tests must be performed for nationwide use of an allowed modification, has been changed to update the web link for the list of industrial categories with existing effluent guidelines to https://www.epa.gov/cwa-methods/alternate-test-procedure-documents . Although EPA received comments about updating the QC acceptance criteria in Method 625.1, EPA did not implement such changes because EPA lacks data from a multi-laboratory validation study from which to develop such criteria. I. Changes to Method Detection Limit (MDL) Procedure, Apppendix B No significant revisions were made to the proposed MDL procedure. Some flexibility was added to the procedure, as is discussed in Section II.K above. J. Changes to WET Errata Among the corrections that EPA proposed was a change to the language for Fathead minnows, Daphnids, and Green Alga in the document Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition, U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA/821/R-02/013, October 2002. For Fathead Minnows and Daphnids, EPA proposed to change “Conductivity, alkalinity, and hardness are measured in each new sample (100% effluent or receiving water) and in the control” to read “Conductivity, alkalinity, and hardness are measured at the beginning of the test for all test concentrations in each new sample and in the control before they are dispersed to the test chambers.” EPA agrees with commenters that this change would constitute a change to the test rather than a correction or clarification. For that reason, EPA will not add the inserted language “at the beginning of the test for all test concentrations.” EPA is retaining its deletion of “(100% effluent or receiving water)” and the insertion of “before they are dispensed to the test chamber” to the end of the sentence. Thus, the sentence will now read “Conductivity, alkalinity, and hardness are measured in each new sample and in the control before they are dispensed to the test chamber.” For Green Alga, the proposed change has been eliminated from the errata because only the increased testing was proposed. IV. 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” under the terms of Executive Order (EO) 12866 (58 FR 51735, October 4, 1993) and is therefore not subject to review under EO 12866 and EO 13563. B. Paperwork Reduction Act This action does not impose an information collection burden under the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq. Burden is defined at 5 CFR 1320.3(b). This rule does not impose any information collection, reporting, or recordkeeping requirements. This rule merely adds new and revised versions of testing procedures, and sample preservation requirements. C. Regulatory Flexibility Act The Regulatory Flexibility Act (RFA) generally requires an agency to prepare a regulatory flexibility analysis of any rule subject to notice and comment rulemaking requirements under the Administrative Procedure Act or any other statute unless the agency certifies that the rule will not have a significant economic impact on a substantial number of small entities. Small entities include small businesses, small organizations, and small governmental jurisdictions. For purposes of assessing the impacts of this rule on small entities for methods under the Clean Water Act, small entity is defined as: (1) A small business that meets RFA default definitions (based on SBA size standards) found in 13 CFR 121.201; (2) a small governmental jurisdiction that is a government of a city, county, town, school district or special district with a population less than 50,000; and (3) a small organization that is any not-for-profit enterprise which is independently owned and operated and is not dominant in its field. After considering the economic impacts of this final rule on small entities, I certify that this action will not have a significant economic impact on a substantial number of small entities. This action approves new and revised versions of testing procedures. Generally, these changes will have a positive impact on small entities by increasing method flexibility, thereby allowing entities to reduce costs by choosing more cost-effective methods. D. Unfunded Mandates Reform Act This action contains no Federal mandates under the provisions of Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), 2 U.S.C. 1531-1538 for State, local, or tribal governments, or the private sector. EPA has determined that this final rule contains no regulatory requirements that might significantly or uniquely affect small governments. Generally, this action will have a positive impact by increasing method flexibility, thereby allowing method users to reduce costs by choosing more cost effective methods. In some cases, analytical costs may increase slightly due to changes in methods, but these increases are neither significant, nor unique to small governments. This rule merely approves new and revised versions of testing procedures, and new sample collection, preservation, and holding time requirements. Thus, this rule is not subject to the requirements of Section 203 of UMRA. 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, as specified in Executive Order 13132 (64 FR 43255, Aug. 10, 1999). This rule merely approves new and revised versions of testing procedures, and new sample collection, preservation, and holding time requirements. The costs to State and local governments will be minimal. In fact, governments may see a cost savings because the rule adds flexibility for laboratories and permittees to choose between additional approved test methods and it also provides additional flexibility to modify existing test methods. Thus, laboratories and permittees will not make as many requests for approval of alternative test methods or method modifications, and the rule does not preempt State law. Thus, Executive Order 13132 does not apply to this rule. In the spirit of Executive Order 13132, and consistent with EPA policy to promote communications between EPA and State and local governments, EPA specifically solicited comment on the proposed rule from State and local officials. 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, (65 FR 67249, Nov. 9, 2000). It will not have substantial direct effects on Tribal governments, on the relationship between the federal government and Indian tribes, or on the distribution of power and responsibilities between the federal government and Indian tribes. This rule merely approves new and revised versions of testing procedures, and new sample collection, preservation, and holding time requirements. The costs to tribal governments will be minimal. In fact, tribal governments may see a cost savings because the rule adds flexibility for laboratories and permittees to choose between additional approved test methods and it also provides additional flexibility to modify existing test methods. Thus, laboratories and permittees will not make as many requests for approval of alternative test methods or method modifications. Thus, Executive Order 13175 does not apply to this rule. In the spirit of Executive Order 13175, and consistent with EPA policy to promote communications between EPA and Indian tribes, EPA specifically solicited comment on the proposed rule from tribal officials. EPA did not receive any comments from Indian tribes. G. Executive Order 13045: Protection of Children From Environmental Health Risks and Safety Risks EPA interprets E.O. 13045 (62 FR 19885, April 23, 1997) as applying only to those regulatory actions that concern health or safety risks, such that the analysis required under section 5-501 of the E.O. has the potential to influence the regulation. This action is not subject to E.O. 13045 because it does not establish an environmental standard intended to mitigate health or safety risks. This rule approves new and revised versions of testing procedures, and new sample collection, preservation, and holding time requirements. H. Executive Order 13211: Actions That Significantly Affect Energy Supply, Distribution, or Use This action is not subject to Executive Order 13211, “Actions Concerning Regulations That Significantly Affect Energy Supply, Distribution, or Use” (66 FR 28355 (May 22, 2001)) because it is not a significant regulatory action under Executive Order 12866. I. National Technology Transfer and Advancement Act of 1995 Section 12(d) of the National Technology Transfer and Advancement Act of 1995, (NTTAA), Public Law 104-113, section 12(d) (15 U.S.C. 272 note), directs EPA to use voluntary consensus standards in its regulatory activities unless to do so would be inconsistent with applicable law or otherwise impractical. Voluntary consensus standards are technical standards ( e.g., material specifications, test methods, sampling procedures, and business practices) that are developed or adopted by voluntary consensus standard bodies. The NTTAA directs EPA to provide Congress, through the OMB, explanations when the Agency decides not to use available and applicable voluntary consensus standards. This final rule approves the use of technical standards developed by the Standard Methods Committee, and ASTM International for use in compliance monitoring where the Agency has determined that those standards meet the needs of Clean Water Act programs. EPA did not propose to add one Standard Method because that method had not undergone full inter-laboratory validation as recommended in current Agency guidance (see Section IV.C of the proposal for this rule (80 FR 8956, February 19, 2015)). All proposed voluntary consensus standards are approved in this rule. J. Executive Order 12898: Federal Actions To Address Environmental Justice in Minority Populations and Low-Income Populations Executive Order (E.O.) 12898 (59 FR 7629 (Feb. 16, 1994)) establishes federal executive policy on environmental justice. Its main provision directs federal agencies, to the greatest extent practicable and permitted by law, to make environmental justice part of their mission by identifying and addressing, as appropriate, disproportionately high and adverse human health or environmental effects of their programs, policies, and activities on minority populations and low-income populations in the United States. This final rule provides additional compliance methods for use by any facility or laboratory with no disproportionate impact on minority or low-income populations because it merely approves new and revised versions of testing procedures to measure pollutants in water. K. Congressional Review Act The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the Small Business Regulatory Enforcement Fairness Act of 1996, generally provides that before a rule may take effect, the agency promulgating the rule must submit a rule report, which includes a copy of the rule, to each House of the Congress and to the Comptroller General of the United States. EPA will submit a report containing this rule and other required information to the U.S. Senate, the U.S. House of Representatives, and the Comptroller General of the United States prior to publication of the rule in the Federal Register . This action is not a “major rule” as defined by 5 U.S.C. 804(2). This rule will be effective September 27, 2017. List of Subjects in 40 CFR Part 136 Environmental protection, Incorporation by reference, Reporting and recordkeeping requirements, Test procedures, Water pollution control. Dated: August 7, 2017. E. Scott Pruitt, Administrator. For the reasons set out in the preamble, title 40, chapter I of the Code of Federal Regulations is amended 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. Section 136.1 is amended by revising paragraph (a) to read as follows: § 136.1 Applicability. (a) The procedures prescribed herein shall, except as noted in §§ 136.4, 136.5, and 136.6, be used to perform the measurements indicated whenever the waste constituent specified is required to be measured for: (1) An application submitted to the Director and/or reports required to be submitted under NPDES permits or other requests for quantitative or qualitative effluent data under parts 122 through 125 of this chapter; and (2) Reports required to be submitted by dischargers under the NPDES established by parts 124 and 125 of this chapter; and (3) Certifications issued by States pursuant to section 401 of the Clean Water Act (CWA), as amended. 3. Section 136.2 is amended by revising paragraphs (d) and (f) to read as follows: § 136.2 Definitions. (d) Director means the director as defined in 40 CFR 122.2. (f) Detection limit means the minimum concentration of an analyte (substance) that can be measured and reported with a 99% confidence that the analyte concentration is distinguishable from the method blank results as determined by the procedure set forth at appendix B of this part. 4. In § 136.3: a. Revise paragraph (a) introductory text and tables IA, IB, IC, ID, IF, IG, and IH. b. Revise paragraphs (b) introductory text, (b)(8)(iv), (b)(8)(v), (b)(8)(xiii), (b)(8)(xv), (b)(10)(viii) through (lviii), (b)(10)(lxi) through (lxiii), (b)(10)(lxviii), (b)(15)(v), (b)(15)(viii) through (x), (b)(15)(xii), (b)(15)(xiii), (b)(15)(xv) through (xvii), (b)(15)(xxii) through (xxiv), (b)(15)(xxx), (b)(15)(xxxv), (b)(15)(xxxvii), (b)(15)(xxxix), (b)(15)(xlii), (b)(15)(l), (b)(15)(lii), (b)(15)(lv), (b)(15)(lviii), (b)(15)(lix), (b)(15)(lxi), (b)(15)(lxiv), (b)(15)(lxvi), and (b)(15)(lxviii). c. Redesignate paragraphs (b)(19)(vii) and (viii) as paragraphs (b)(19)(ix) and (x), respectively. d. Add new paragraphs (b)(19)(vii) and (viii). e. Revise paragraphs (b)(20)(i) through (iv). f. Remove paragraph (b)(20)(v). g. Revise paragraph (b)(25)(i). h. Add paragraphs (b)(25)(ii) and (iii). i. Redesignate paragraphs (b)(33) and (34) as paragraphs (b)(35) and (36), respectively, and redesignate paragraphs (b)(26) through (32) as paragraphs (b)(27) through (33), respectively. j. Add new paragraphs (b)(26) and (34). k. Revise newly redesignated paragraph (b)(35). l. Revise paragraph (c) and Table II in paragraph (e). The revisions and additions read as follows: § 136.3 Identification of test procedures. (a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, IF, IG, and IH of this section. The methods listed in Tables IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see paragraph (b) of this section, with the exception of EPA Methods 200.7, 601-613, 624.1, 625.1, 1613, 1624, and 1625. The full texts of Methods 601-613, 624.1, 625.1, 1613, 1624, and 1625 are printed in appendix A of this part, and the full text of Method 200.7 is printed in appendix C of this part. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part. In the event of a conflict between the reporting requirements of 40 CFR parts 122 and 125 and any reporting requirements associated with the methods listed in these tables, the provisions of 40 CFR parts 122 and 125 are controlling and will determine a permittee's reporting requirements. The full texts of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and IH. The year after the method number indicates the latest editorial change of the method. The discharge parameter values for which reports are required must be determined by one of the standard analytical test procedures incorporated by reference and described in Tables IA, IB, IC, ID, IE, IF, IG, and IH or by any alternate test procedure which has been approved by the Administrator under the provisions of paragraph (d) of this section and §§ 136.4 and 136.5. Under certain circumstances (paragraph (c) of this section, in § 136.5(a) through (d) or 40 CFR 401.13) other additional or alternate test procedures may be used. Table IA—List of Approved Biological Methods for Wastewater and Sewage Sludge Parameter and units Method 1 EPA Standard methods AOAC, ASTM, USGS Other Bacteria 1. Coliform (fecal), number per 100 mL or number per gram dry weight Most Probable Number (MPN), 5 tube, 3 dilution, or p. 132, 3 1680, 11 15 1681 11 20 9221 C E-2006 Multiple tube/multiple well, or Colilert-18® 13 8 21 29 . Membrane filter (MF) 2 , single step p. 124 3 9222 D-2006 30 B-0050-85 4 2. Coliform (fecal) in presence of chlorine, number per 100 mL MPN, 5 tube, 3 dilution, or p. 132 3 9221 C E-2006 MF 2 , single step 5 p. 124 3 9222 D-2006 30 3. Coliform (total), number per 100 mL MPN, 5 tube, 3 dilution, or p. 114 3 9221 B-2006 MF 2 , single step or two step p. 108 3 9222 B-2006 B-0025-85 4 4. Coliform (total), in presence of chlorine, number per 100 mL MPN, 5 tube, 3 dilution, or p. 114 3 9221 B-2006 MF 2 with enrichment 5 p. 111 3 9222 B-2006 5. E. coli, number per 100 mL 21 MPN 6 8 16 multiple tube, or 9221B.2-2006/9221F-2006 12 14 multiple tube/multiple well, or 9223 B-2004 13 991.15 10 Colilert® 13 18 . Colilert-18® 13 17 18 MF 2 6 7 8 single step 1603 22 mColiBlue-24® 19 . 6. Fecal streptococci, number per 100 mL MPN, 5 tube, 3 dilution, or p. 139 3 9230 B-2007 MF 2 , or p. 136 3 9230 C-2007 B-0055-85 4 Plate count p. 143 3 7. Enterococci, number per 100 mL 21 MPN, 5 tube, 3 dilution, or p. 139 3 9230 B-2007 MPN 6 8 , multiple tube/multiple well, or 9230 D-2007 D6503-99 9 Enterolert® 13 24 . MF 2 6 7 8 single step or 1600 25 9230 C-2007 Plate count p. 143 3 8. Salmonella number per gram dry weight 11 MPN multiple tube 1682 23 Aquatic Toxicity 9. Toxicity, acute, fresh water organisms, LC 50 , percent effluent Ceriodaphnia dubia acute 2002.0 26 Daphnia puplex and Daphnia magna acute 2021.0 26 Fathead Minnow, Pimephales promelas, and Bannerfin shiner, Cyprinella leedsi, acute 2000.0 26 Rainbow Trout, Oncorhynchus mykiss, and brook trout, Salvelinus fontinalis, acute 2019.0 26 10. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC 50 , percent effluent Mysid, Mysidopsis bahia, acute 2007.0 26 Sheepshead Minnow, Cyprinodon variegatus, acute 2004.0 26 Silverside, Menidia beryllina, Menidia menidia, and Menidia peninsulae, acute 2006.0 26 11. Toxicity, chronic, fresh water organisms, NOEC or IC 25 , percent effluent Fathead minnow, Pimephales promelas, larval survival and growth 1000.0 27 Fathead minnow, Pimephales promelas, embryo-larval survival and teratogenicity 1001.0 27 Daphnia, Ceriodaphnia dubia, survival and reproduction 1002.0 27 Green alga, Selenastrum capricornutum, growth 1003.0 27 12. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC 25 , percent effluent Sheepshead minnow, Cyprinodon variegatus, larval survival and growth 1004.0 28 Sheepshead minnow, Cyprinodon variegatus, embryo-larval survival and teratogenicity 1005.0 28 Inland silverside, Menidia beryllina, larval survival and growth 1006.0 28 Mysid, Mysidopsis bahia, survival, growth, and fecundity 1007.0 28 Sea urchin, Arbacia punctulata, fertilization 1008.0 28 Table IA notes: 1 The method must be specified when results are reported. 2 A 0.45-μm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth. 3 Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. U.S. EPA. 4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS. 5 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies. 6 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample. 7 When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results. 8 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines. 9 Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International. 10 Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International. 11 Approved for enumeration of target organism in sewage sludge. 12 The multiple-tube fermentation test is used in 9221B.2-2006. 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, where, for example, a substrate is used to detect the enzyme β-glucuronidase produced by E. coli. 14 After prior enrichment in a presumptive medium for total coliform using 9221B.2-2006, 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-2006. 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® 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®, and Quanti-Tray® 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 Approved for enumeration of target organism in wastewater effluent. 22 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. 23 Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014. U.S. EPA. 24 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc. 25 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-β-D-Glucoside Agar (mEI), EPA-821-R-14-011. September 2014. U.S. EPA. 26 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. 27 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. 28 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. 29 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. 30 On a monthly basis, at least ten blue colonies from the medium 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. Table IB—List of Approved Inorganic Test Procedures Parameter Methodology 58 EPA 52 Standard methods ASTM USGS/AOAC/other 1. Acidity, as CaCO 3 , mg/L Electrometric endpoint or phenolphthalein endpoint 2310 B-2011 D1067-11 I-1020-85. 2 2. Alkalinity, as CaCO 3 , mg/L Electrometric or Colorimetric titration to pH 4.5, Manual 2320 B-2011 D1067-11 973.43, 3 I-1030-85. 2 Automatic 310.2 (Rev. 1974) 1 I-2030-85. 2 3. Aluminum—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 D-2011 or 3111 E-2011 I-3051-85. 2 AA furnace 3113 B-2010. STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 Direct Current Plasma (DCP) 36 D4190-08 See footnote. 34 Colorimetric (Eriochrome cyanine R) 3500-Al B-2011 4. Ammonia (as N), mg/L Manual distillation 6 or gas diffusion (pH > 11), followed by any of the following: 350.1, Rev. 2.0 (1993) 4500-NH 3 B-2011 973.49. 3 Nesslerization D1426-08 (A) 973.49, 3 I-3520-85. 2 Titration 4500-NH 3 C-2011 Electrode 4500-NH 3 D-2011 or E-2011 D1426-08 (B) Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods 4500-NH 3 F-2011 See footnote. 60 Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods 350.1, 30 Rev. 2.0 (1993) 4500-NH 3 G-2011, 4500-NH 3 H-2011 I-4523-85. 2 Automated electrode See footnote. 7 Ion Chromatography D6919-09 Automated gas diffusion, followed by conductivity cell analysis Timberline Ammonia-001. 74 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 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 6. Arsenic-Total, 4 mg/L Digestion, 4 followed by any of the following: 206.5 (Issued 1978) 1 AA gaseous hydride 3114 B-2011 or 3114 C-2011 D2972-08 (B) I-3062-85. 2 AA furnace 3113 B-2010 D2972-08 (C) I-4063-98. 49 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 Colorimetric (SDDC) 3500-As B-2011 D2972-08 (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 D4382-12 ICP/AES 36 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 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-2011 D3645-08 (A) I-3095-85. 2 AA furnace 3113 B-2010 D3645-08 (B) STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP D4190-08 See footnote. 34 Colorimetric (aluminon) See footnote. 61 9. Biochemical oxygen demand (BOD 5 ), mg/L Dissolved Oxygen Depletion 5210 B-2011 973.44, 3 p. 17, 9 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 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP D4190-08 See footnote. 34 11. Bromide, mg/L Electrode D1246-10 I-1125-85. 2 Ion Chromatography 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997) 4110 B-2011, C-2011, D-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 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-2011 D3557-12 (A or B) 974.27, 3 p. 37, 9 I-3135-85 2 or I-3136-85. 2 AA furnace 3113 B-2010 D3557-12 (D) I-4138-89. 51 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-1472-85 2 or I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP 36 D4190-08 See footnote. 34 Voltametry 11 D3557-12 (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 D511-09(B) I-3152-85. 2 ICP/AES 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP See footnote. 34 Titrimetric (EDTA) 3500-Ca B-2011 D511-09 (A) Ion Chromatography D6919-09 14. Carbonaceous biochemical oxygen demand (CBOD 5 ), mg/L 12 Dissolved Oxygen Depletion with nitrification inhibitor 5210 B-2011 See footnote. 35 63 15. Chemical oxygen demand (COD), mg/L Titrimetric 410.3 (Rev. 1978) 1 5220 B-2011 or C-2011 D1252-06 (A) 973.46, 3 p. 17, 9 I-3560-85. 2 Spectrophotometric, manual or automatic 410.4, Rev. 2.0 (1993) 5220 D-2011 D1252-06 (B) See footnotes. 13 14 , I-3561-85. 2 16. Chloride, mg/L Titrimetric: (silver nitrate) 4500-Cl − B-2011 D512-04 (B) I-1183-85. 2 (Mercuric nitrate) 4500-Cl − C-2011 D512-04 (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 D512-04 (C) Ion Chromatography 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997) 4110 B-2011 or 4110 C-2011 D4327-03 993.30, 3 I-2057-90. 51 CIE/UV 4140 B-2011 D6508-10 D6508, Rev. 2. 54 17. Chlorine-Total residual, mg/L Amperometric direct 4500-Cl D-2011 D1253-08 Amperometric direct (low level) 4500-Cl E-2011 Iodometric direct 4500-Cl B-2011 Back titration ether end-point 15 4500-Cl C-2011 DPD-FAS 4500-Cl F-2011 Spectrophotometric, DPD 4500-Cl G-2011 Electrode See footnote. 16 17A. Chlorine-Free Available, mg/L Amperometric direct 4500-Cl D-2011 D1253-08 Amperometric direct (low level) 4500-Cl E-2011 DPD-FAS 4500-Cl F-2011 Spectrophotometric, DPD 4500-Cl G-2011 18. Chromium VI dissolved, mg/L 0.45-micron filtration followed by any of the following: AA chelation-extraction 3111 C-2011 I-1232-85. 2 Ion Chromatography 218.6, Rev. 3.3 (1994) 3500-Cr C-2011 D5257-11 993.23. 3 Colorimetric (diphenyl-carbazide) 3500-Cr B-2011 D1687-12 (A) I-1230-85. 2 19. Chromium—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 B-2011 D1687-12 (B) 974.27, 3 I-3236-85. 2 AA chelation-extraction 3111 C-2011 AA furnace 3113 B-2010 D1687-12 (C) I-3233-93. 46 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003), 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP 36 D4190-08 See footnote. 34 Colorimetric (diphenyl-carbazide) 3500-Cr B-2011 20. Cobalt—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 3111 B-2011 or 3111 C-2011 D3558-08 (A or B) p. 37, 9 I-3239-85. 2 AA furnace 3113 B-2010 D3558-08 (C) I-4243-89. 51 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP D4190-08 See footnote. 34 21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity Colorimetric (ADMI) 2120 F-2011 78 Platinum cobalt visual comparison 2120 B-2011 I-1250-85. 2 Spectrophotometric See footnote. 18 22. Copper—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 B-2011 or 3111 C-2011 D1688-12 (A or B) 974.27, 3 p. 37, 9 I-3270-85 2 or I-3271-85. 2 AA furnace 3113 B-2010 D1688-12 (C) I-4274-89. 51 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP 36 D4190-08 See footnote. 34 Colorimetric (Neocuproine) 3500-Cu B-2011 Colorimetric (Bathocuproine) 3500-Cu C-2011 See footnote. 19 23. Cyanide—Total, mg/L Automated UV digestion/distillation and Colorimetry Kelada-01. 55 Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometry D7511-12 Manual distillation with MgCl 2 , followed by any of the following: 335.4, Rev. 1.0 (1993) 57 4500-CN − B-2011 and C-2011 D2036-09(A), D7284-13 10-204-00-1-X. 56 Flow Injection, gas diffusion amperometry D2036-09(A) D7284-13 Titrimetric 4500-CN − D-2011 D2036-09(A) p. 22. 9 Spectrophotometric, manual 4500-CN − E-2011 D2036-09(A) I-3300-85. 2 Semi-Automated 20 335.4, Rev. 1.0 (1993) 57 10-204-00-1-X, 56 I-4302-85. 2 Ion Chromatography D2036-09(A) Ion Selective Electrode 4500-CN − F-2011 D2036-09(A) 24. Cyanide—Available, mg/L Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl 2 , followed by Titrimetric or Spectrophotometric 4500-CN − G-2011 D2036-09(B) Flow injection and ligand exchange, followed by gas diffusion amperometry 59 D6888-09 OIA-1677-09. 44 Automated Distillation and Colorimetry (no UV digestion) Kelada-01. 55 24.A Cyanide—Free, mg/L Flow Injection, followed by gas diffusion amperometry D7237-10 OIA-1677-09. 44 Manual micro-diffusion and colorimetry D4282-02 25. Fluoride—Total, mg/L Manual distillation, 6 followed by any of the following: 4500-F − B-2011 Electrode, manual 4500-F − C-2011 D1179-10 (B) Electrode, automated I-4327-85. 2 Colorimetric, (SPADNS) 4500-F − D-2011 D1179-10 (A) Automated complexone 4500-F − E-2011 Ion Chromatography 300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 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) 1 3113 B-2010 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP See footnote. 34 27. Hardness—Total, as CaCO 3 , mg/L Automated colorimetric 130.1 (Issued 1971) 1 Titrimetric (EDTA) 2340 C-2011 D1126-12 973.52B, 3 I-1338-85. 2 Ca plus Mg as their carbonates, by any approved method for Ca and Mg (See Parameters 13 and 33), provided that the sum of the lowest point of quantitation for Ca and Mg is below the NPDES permit requirement for Hardness. 2340 B-2011 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 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 or 3111 C-2011 D1068-10 (A) 974.27, 3 I-3381-85. 2 AA furnace 3113 B-2010 D1068-10 (B) STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP 36 D4190-08 See footnote. 34 Colorimetric (Phenanthroline) 3500-Fe B-2011 D1068-10 (C) See footnote. 22 31. Kjeldahl Nitrogen 5 —Total, (as N), mg/L Manual digestion 20 and distillation or gas diffusion, followed by any of the following: 4500-N org B-2011 or C-2011 and 4500-NH 3 B-2011 D3590-11 (A) I-4515-91. 45 Titration 4500-NH 3 C-2011 973.48. 3 Nesslerization D1426-08 (A) Electrode 4500-NH 3 D-2011 or E-2011 D1426-08 (B) Semi-automated phenate 350.1, Rev. 2.0 (1993) 4500-NH 3 G-2011 4500-NH 3 H-2011 Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods 4500-NH 3 F-2011 See footnote. 60 Automated gas diffusion, followed by conductivity cell analysis Timberline Ammonia-001. 74 Automated Methods for TKN that do not require manual distillation. Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation) 351.1 (Rev. 1978) 1 I-4551-78. 8 Semi-automated block digestor colorimetric (distillation not required) 351.2, Rev. 2.0 (1993) 4500-N org D-2011 D3590-11 (B) I-4515-91. 45 Block digester, followed by Auto distillation and Titration See footnote. 39 Block digester, followed by Auto distillation and Nesslerization See footnote. 40 Block Digester, followed by Flow injection gas diffusion (distillation not required) See footnote. 41 Digestion with peroxdisulfate, followed by Spectrophotometric (2,6-dimethyl phenol) Hach 10242. 76 Digestion with persulfate, followed by Colorimetric NCASI TNTP W10900. 77 32. Lead—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 B-2011 or 3111 C-2011 D3559-08 (A or B) 974.27, 3 I-3399-85. 2 AA furnace 3113 B-2010 D3559-08 (D) I-4403-89. 51 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP 36 D4190-08 See footnote. 34 Voltametry 11 D3559-08 (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 D511-09 (B) 974.27, 3 I-3447-85. 2 ICP/AES 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP See footnote. 34 Ion Chromatography D6919-09 34. Manganese—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 B-2011 D858-12 (A or B) 974.27, 3 I-3454-85. 2 AA furnace 3113 B-2010 D858-12 (C) STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP 36 D4190-08 See footnote. 34 Colorimetric (Persulfate) 3500-Mn B-2011 920.203. 3 Colorimetric (Periodate) See footnote. 23 35. Mercury—Total, 4 mg/L Cold vapor, Manual 245.1, Rev. 3.0 (1994) 3112 B-2011 D3223-12 977.22, 3 I-3462-85. 2 Cold vapor, Automated 245.2 (Issued 1974) 1 Cold vapor atomic fluorescence spectrometry (CVAFS) 245.7 Rev. 2.0 (2005) 17 I-4464-01. 71 Purge and Trap CVAFS 1631E 43 36. Molybdenum—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 3111 D-2011 I-3490-85. 2 AA furnace 3113 B-2010 I-3492-96. 47 ICP/AES 36 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 DCP See footnote. 34 37. Nickel—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 36 3111 B-2011 or 3111 C-2011 D1886-08 (A or B) I-3499-85. 2 AA furnace 3113 B-2010 D1886-08 (C) I-4503-89. 51 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP 36 D4190-08 See footnote. 34 38. Nitrate (as N), mg/L Ion Chromatography 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 D6508, Rev. 2. 54 Ion Selective Electrode 4500-NO 3 − D-2011 Colorimetric (Brucine sulfate) 352.1 (Issued 1971) 1 973.50, 3 419D1, 7 p. 28. 9 Spectrophotometric (2,6-dimethylphenol) Hach 10206. 75 Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40) 39. Nitrate-nitrite (as N), mg/L Cadmium reduction, Manual 4500-NO 3 − E-2011 D3867-04 (B) Cadmium reduction, Automated 353.2, Rev. 2.0 (1993) 4500-NO 3 − F-2011 D3867-04 (A) I-2545-90. 51 Automated hydrazine 4500-NO 3 − H-2011 Reduction/Colorimetric See footnote. 62 Ion Chromatography 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 D6508, Rev. 2. 54 Enzymatic reduction, followed by automated colorimetric determination I-2547-11, 72 I-2548-11, 72 N07-0003. 73 Spectrophotometric (2,6-dimethylphenol) Hach 10206. 75 40. Nitrite (as N), mg/L Spectrophotometric: Manual 4500-NO 2 − B-2011 See footnote. 25 Automated (Diazotization) I-4540-85, 2 See footnote. 62 Automated (*bypass cadmium reduction) 353.2, Rev. 2.0 (1993) 4500-NO 3 − F-2011 D3867-04 (A) I-4545-85. 2 Manual (*bypass cadmium reduction) 4500-NO 3 − E-2011 D3867-04 (B) Ion Chromatography 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 D6508, Rev. 2. 54 Automated (*bypass Enzymatic reduction) I-2547-11, 72 I-2548-11, 72 N07-0003. 73 41. Oil and grease—Total recoverable, mg/L Hexane extractable material (HEM): n-Hexane extraction and gravimetry 1664 Rev. A; 1664 Rev. B 42 5520 B-2011 38 Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry 1664 Rev. A; 1664 Rev. B 42 5520 B-2011 38 and 5520 F-2011 38 42. Organic carbon—Total (TOC), mg/L Combustion 5310 B-2011 D7573-09 973.47, 3 p. 14. 24 Heated persulfate or UV persulfate oxidation 5310 C-2011, 5310 D-2011 D4839-03 973.47, 3 p. 14. 24 43. Organic nitrogen (as N), mg/L Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4). 44. Ortho-phosphate (as P), mg/L Ascorbic acid method: Automated 365.1, Rev. 2.0 (1993) 4500-P F-2011 or G-2011 973.56, 3 I-4601-85. 2 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 (1993) and 300.1, Rev. 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30. 3 CIE/UV 4140 B-2011 D6508-10 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 modification) 4500-O (B-F)-2011 D888-09 (A) 973.45B, 3 I-1575-78. 8 Electrode 4500-O G-2011 D888-09 (B) I-1576-78. 8 Luminescence Based Sensor D888-09 (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 followed by any of the following: 420.1 (Rev. 1978) 1 5530 B-2010 D1783-01 Colorimetric (4AAP) manual 420.1 (Rev. 1978) 1 5530 D-2010 27 D1783-01 (A or B) Automated colorimetric (4AAP) 420.4 Rev. 1.0 (1993) 49. Phosphorus (elemental), mg/L Gas-liquid chromatography See footnote. 28 50. Phosphorus—Total, mg/L Digestion, 20 followed by any of the following: 4500-P B(5)-2011 973.55. 3 Manual 365.3 (Issued 1978) 1 4500-P E-2011 D515-88 (A) Automated ascorbic acid reduction 365.1 Rev. 2.0 (1993) 4500-P (F-H)-2011 973.56, 3 I-4600-85. 2 ICP/AES 4 36 200.7, Rev. 4.4 (1994) 3120 B-2011 I-4471-97. 50 Semi-automated block digestor (TKP digestion) 365.4 (Issued 1974) 1 D515-88 (B) I-4610-91. 48 Digestion with persulfate, followed by Colorimetric NCASI TNTP W10900. 77 51. Platinum—Total 4 , mg/L Digestion, 4 followed by any of the following: AA direct aspiration 3111 B-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 (1994) 3120 B-2011 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 Flame photometric 3500-K B-2011 Electrode 3500-K C-2011 Ion Chromatography D6919-09 53. Residue—Total, mg/L Gravimetric, 103-105° 2540 B-2011 I-3750-85. 2 54. Residue—filterable, mg/L Gravimetric, 180° 2540 C-2011 D5907-13 I-1750-85. 2 55. Residue—non-filterable (TSS), mg/L Gravimetric, 103-105° post washing of residue 2540 D-2011 D5907-13 I-3765-85. 2 56. Residue—settleable, mg/L Volumetric, (Imhoff cone), or gravimetric 2540 F-2011 57. Residue—Volatile, mg/L Gravimetric, 550° 160.4 (Issued 1971) 1 2540-E-2011 I-3753-85. 2 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 D3859-08 (B) I-4668-98. 49 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 36 200.5, Rev 4.2 (2003) 68 ; 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 AA gaseous hydride 3114 B-2011, or 3114 C-2011 D3859-08 (A) I-3667-85. 2 61. Silica—Dissolved, 37 mg/L 0.45-micron filtration followed by any of the following: Colorimetric, Manual 4500-SiO 2 C-2011 D859-10 I-1700-85. 2 Automated (Molybdosilicate) 4500-SiO 2 E-2011 or F-2011 I-2700-85. 2 ICP/AES 200.5, Rev. 4.2 (2003) 68 ; 200.7, Rev. 4.4 (1994) 3120 B-2011 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 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-2011 974.27, 3 p. 37, 9 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 (2003) 68 ; 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 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 (2003) 68 ; 200.7, Rev. 4.4 (1994) 3120 B-2011 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP See footnote. 34 Flame photometric 3500-Na B-2011 Ion Chromatography D6919-09 64. Specific conductance, micromhos/cm at 25 °C Wheatstone bridge 120.1 (Rev. 1982) 1 2510 B-2011 D1125-95(99) (A) 973.40, 3 I-2781-85. 2 65. Sulfate (as SO 4 ), mg/L Automated colorimetric 375.2, Rev. 2.0 (1993) 4500-SO 4 2 − F-2011 or G-2011 Gravimetric 4500-SO 4 2 − C-2011 or D-2011 925.54. 3 Turbidimetric 4500-SO 4 2 − E-2011 D516-11 Ion Chromatography 300.0, Rev. 2.1 (1993) and 300.1, Rev. 1.0 (1997) 4110 B-2011 or C-2011 D4327-03 993.30, 3 I-4020-05. 70 CIE/UV 4140 B-2011 D6508-1010 D6508, Rev. 2. 54 66. Sulfide (as S), mg/L Sample Pretreatment 4500-S 2 − B, C-2011 Titrimetric (iodine) 4500-S 2 − F-2011 I-3840-85. 2 Colorimetric (methylene blue) 4500-S 2 − D-2011 Ion Selective Electrode 4500-S 2 − G-2011 D4658-09 67. Sulfite (as SO 3 ), mg/L Titrimetric (iodine-iodate) 4500-SO 3 2 − B-2011 68. Surfactants, mg/L Colorimetric (methylene blue) 5540 C-2011 D2330-02 69. Temperature, °C Thermometric 2550 B-2010 See footnote. 32 70. Thallium—Total, 4 mg/L Digestion, 4 followed by any of the following: AA direct aspiration 3111 B-2011 AA furnace 279.2 (Issued 1978) 1 3113 B-2010 STGFAA 200.9, Rev. 2.2 (1994) ICP/AES 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4471-97. 50 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 (1994) 3125 B-2011 D5673-10 993.14. 3 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 (1994) 3125 B-2011 D5673-10 993.14. 3 DCP See footnote. 34 73. Turbidity, NTU 53 Nephelometric 180.1, Rev. 2.0 (1993) 2130 B-2011 D1889-00 I-3860-85. 2 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 D3373-12 ICP/AES 200.5, Rev. 4.2 (2003); 68 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP D4190-08 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-2011 D1691-12 (A or B) 974.27, 3 p. 37, 9 I-3900-85. 2 AA furnace 289.2 (Issued 1978) 1 ICP/AES 36 200.5, Rev. 4.2 (2003) 68 ; 200.7, Rev. 4.4 (1994) 3120 B-2011 D1976-12 I-4471-97. 50 ICP/MS 200.8, Rev. 5.4 (1994) 3125 B-2011 D5673-10 993.14, 3 I-4020-05. 70 DCP 36 D4190-08 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 the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of “Methods for the Determination of Metals in Environmental Samples” EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure ( e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as “total” metals. 5 Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate. 6 Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: However, manual distillation will be required to resolve any controversies. In general, the analytical method should be consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is defined as 7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH 4 OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water. 32 “Water Temperature-Influential Factors, Field Measurement and Data Presentation,” Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1. 1975. USGS. 33 Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company. 34 Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised 1991. Thermo Jarrell Ash Corporation. 35 In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated. 36 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. CEM Corporation. 37 When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. 38 Only use n-hexane (n-Hexane—85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of other extraction solvents is prohibited. 39 Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical. 40 Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical. 41 Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical. 42 Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001. 43 Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August 2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations. 44 Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical. 45 Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS. 46 Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS. 47 Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS. 48 Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS. 49 Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS. 50 Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS. 51 Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS. 52 Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in U.S. EPA. May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography. 53 Styrene divinyl benzene beads ( e.g., [Text truncated at 120,000 characters. The full text is on the page linked above.] --- Source: Frix Law Library, https://www.frixlaw.com/law-library/documents/fr%3A2017-17271. Public record. Not legal advice.