Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; National Primary Drinking Water Regulations; and National Secondary Drinking Water Regulations; Analysis and Sampling Procedures

Federal RegisterMar 12, 2007

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 122, 136, 141, 143, 430, 455, and 465

[EPA-HQ-OW-2003-0070; FRL-8203-8]

RIN 2040-AD71

Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; National Primary Drinking Water Regulations; and National Secondary Drinking Water Regulations; Analysis and Sampling Procedures

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 and Safe Drinking Water Act. EPA proposed these changes for public comment on August 18, 2003 and April 6, 2004. The Clean Water Act changes adopted in this final rule fall into the following categories: new vendor-developed methods as well as EPA and voluntary consensus standard bodies (VCSB) methods, updated versions of currently approved methods, revisions to method modification and analytical requirements, withdrawal of certain outdated methods, and changes to sample collection, preservation, and holding time requirements. This rule also changes regulations under the Safe Drinking Water Act that establish drinking water sampling and analysis procedures. The changes include approval of vendor-developed methods, new EPA and VCSB methods, updated VCSB methods, and approval of a modification to the test kit used with Syngenta Method AG-625 that restricts its use in certain circumstances. The addition of new and updated methods to the wastewater and drinking water regulations provides increased flexibility to the regulated community and laboratories in the selection of analytical methods.

ADDRESSES:

EPA has established a docket for this action under Docket ID No. EPA-OW-2003-0070. All documents in the docket are listed on the

http://www.regulations.gov

web site. Although listed in the index, some information is not publicly available, e.g., CBI or other information whose disclosure is restricted by statute. Certain other material, such as copyrighted material, is not placed on the Internet and will be publicly available only in hard copy form. Publicly available docket materials are available either electronically through

http://www.regulations.gov

or in hard copy at the HQ Water Docket Center, EPA/DC, EPA West, 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 is (202) 566-2426 for the HQ Water Docket Center.

DATES:

This regulation is effective April 11, 2007. The incorporation by reference of these methods is approved by the Director of the Federal Register on April 11, 2007. For judicial review purposes, this final rule is promulgated as of 1:00 p.m. (Eastern time) on March 26, 2007 as provided at 40 CFR 23.2 and 23.7.

FOR FURTHER INFORMATION CONTACT:

For information regarding the changes to wastewater regulations, contact Meghan Hessenauer, Engineering and Analysis Division (4303T), USEPA Office of Science and Technology, 1200 Pennsylvania Ave., NW., Washington, DC 20460, 202-566-1040 (e-mail:

hessenauer.meghan@epa.gov

). For information regarding the changes to drinking water regulations, contact Patricia Snyder Fair, Technical Support Center (MS 140), USEPA, Office of Ground Water and Drinking Water, 26 West Martin Luther King Drive, Cincinnati, OH 45268, 513-569-7937 (e-mail:

fair.pat@epa.gov

SUPPLEMENTARY INFORMATION:

A. Potentially Regulated Entities

1. Clean Water Act

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 test procedures for analysis of a specific pollutant, the NPDES permittee must use an approved test procedure (or an approved alternate test procedure) 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 regulated by the actions in this rulemaking. Categories and entities that may potentially be subject to the requirements of today's rule include:

Category

Examples of potentially regulated entities

NAICS

State, Local, & Tribal Governments

States, local and tribal governments that analyze water samples on behalf of public water systems required to conduct such analysis; States, local and tribal governments that themselves operate community and non-transient non-community water systems required to monitor

924110

Industry

Private operators of community and non-transient non-community water systems required to monitor

221310

Municipalities

Municipal operators of community and non-transient non-community water systems required to monitor

924110

North American Industry Classification System.

This table is not intended to be exhaustive, but rather provides a guide for readers regarding entities likely to be regulated by this action. The table lists types of entities that EPA is now aware could potentially be regulated by this action. Other types of entities not listed in the table could also be regulated. To determine whether your facility is regulated by this action, you should carefully examine the applicability language at 40 CFR 141.2 (definition of public water system). 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 today's CWA rule may be obtained by filing a petition for review in the 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 March 26, 2007 as provided at 40 CFR 23.2. Under section 1448 (a) of the Safe Drinking Water Act (SDWA), judicial review of today's SDWA rule may be obtained by filing a petition for review only in the United States Court of Appeal for the District of Columbia Circuit within 45 days from the date of promulgation of this rule. For SDWA judicial review purposes, this final rule is promulgated as of 1 p.m. (Eastern time) on March 26, 2007 as provide at 40 CFR 23.7. The requirements of this regulation may also not be challenged later in civil or criminal proceedings brought by EPA.

C. Abbreviations and Acronyms Used in the Preamble and Final Rule

AOAC: AOAC-International

ASTM: ASTM International

ATP: Alternate Test Procedure

CWA: Clean Water Act

EPA: Environmental Protection Agency

FLAA: Flame Atomic Absorption Spectroscopy

ICP-AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy

ICP-MS: Inductively Coupled Plasma-Mass Spectroscopy

NPDES: National Pollutant Discharge Elimination System

NPDWR: National Primary Drinking Water Regulations

NSDWR: National Secondary Drinking Water Regulations

QC: Quality Control

SDWA: Safe Drinking Water Act

STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption Spectroscopy

USGS: United States Geological Survey

VCSB: Voluntary Consensus Standard Body

D. Table of Contents

I. Statutory Authority

A. Clean Water Act

B. Safe Drinking Water Act

II. Summary of Final Rule

A. 40 CFR Part 122

B. 40 CFR Part 136

C. 40 CFR Parts 141 and 143

D. 40 CFR Part 430

E. 40 CFR Part 455

F. 40 CFR Part 465

III. Changes Between the Proposed Rule and the Final Rule

A. Silver Determinations

B. ASTM Method D5673-02 “Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry”

C. Ammonia Determinations

D. Available Cyanide Determinations

E. Kelada-01 Method for Determination of Available Cyanide and Total Cyanide

F. Mandatory Replacement of Mercuric Sulfate with Copper Sulfate in Methods for Determination of Total Kjeldahl Nitrogen

G. Approval of Additional Standards for Turbidity Determinations

H. Allowed Use of Capillary Columns in EPA Methods 601-613, 624, 625, and 1624B

I. Changes to Sampling Requirements at 40 CFR Parts 122, 136, and 403

J. Approval Status of Total Elements Digestion

K. EPA Method 245.7 for Determination of Mercury

L. Clarification of Reporting Requirements

M. Corrections to 40 CFR Part 136, Tables IA, IB, IC, ID, IE and Footnotes

N. Revisions to 40 CFR Part 136, Table II

O. Corrections to Tables 40 CFR 141.23, 141.24, 141.25, and 141.74 and Footnotes

P. Retention of Syngenta Method AG-625 for Determination of Atrazine

Q. EPA Method 327.0 for Determination of Chlorine Dioxide

R. Deferral of Action on Microtox® 1010

IV. Response to Comments

A. Use of Syngenta Method AG-625 for Determination of Atrazine

B. Results From Use of Revised Methods, “The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors.” (Revision 1.2, December 2004)

V. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and 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

J. Congressional Review Act

I. Statutory Authority

A. Clean Water Act

EPA is promulgating today's rule pursuant to the authority of sections 301(a), 304(h), and 501(a) of the Clean Water Act (“CWA” or the “Act”), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of the Act prohibits the discharge of any pollutant into navigable waters unless the discharge complies with a National Pollutant Discharge Elimination System (NPDES) permit issued under section 402 of the Act. Section 304(h) of the Act 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 this Act] or permit application pursuant to [section 402 of this Act].” Section 501(a) of the Act authorizes the Administrator to “* * * prescribe such regulations as are necessary to carry out this function under [the Act].” 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).

B. Safe Drinking Water Act

The Safe Drinking Water Act (SDWA), as amended in 1996, requires EPA to promulgate national primary drinking water regulations (NPDWRs) that specify maximum contaminant levels (MCLs) or treatment techniques for drinking water contaminants (SDWA section 1412 (42 U.S.C. 300g-1)). NPDWRs apply to public water systems pursuant to SDWA sections 1401(1)(A) (42 U.S.C. 300f(1)(A)). According to SDWA section 1401(1)(D), NPDWRs include “* * * criteria and procedures to assure a supply of drinking water which dependably complies with such maximum contaminant levels; including accepted methods for quality control and testing procedures * * *” (42 U.S.C. 300f(1)(D)). In addition, SDWA section 1445(a) authorizes the Administrator to establish regulations for monitoring to help determine whether persons are acting in compliance with the requirements of the SDWA (42 U.S.C. 300j-4). EPA's promulgation of analytical methods for NPDWRs is authorized under these sections of the SDWA as well as the general rulemaking authority in SDWA section 1450(a) (42 U.S.C. 300j-9(a)).

The SDWA also authorizes EPA to promulgate national secondary drinking water regulations (NSDWRs) for contaminants in drinking water that primarily affect the aesthetic qualities relating to the public acceptance of drinking water (SDWA section 1412 (42 U.S.C. 300g-1)). These regulations are not Federally enforceable but are guidelines for the States (40 CFR 143.1). The NSDWRs also include analytical techniques for determining compliance with the regulations (40 CFR 143.4). EPA's promulgation of analytical methods for NSDWRs is authorized under general rulemaking authority in SDWA section 1450(a) (42 U.S.C. 300j-9(a)).

II. Summary of Final Rule

The following sections describe the changes EPA is making in today's final rule.

A. 40 CFR Part 122

1. Some EPA Effluent Guideline regulations, as well as EPA's Sewage Sludge Use and Disposal Regulations, require the use of analytical methods specifically prescribed by the Guideline (see e.g. 40 CFR Part 420.21(c)). This rule amends the National Pollutant Discharge Elimination System (NPDES) regulations at 40 CFR Part 122 to clarify when an NPDES permittee must use for its monitoring and reporting the analytical methods specifically required in Title 40 of the CFR, Chapter I, Subchapters N and O (effluent guidelines and sewage sludge, respectively) rather than the methods in 40 CFR Part 136. The regulatory language has been amended to explicitly require either use of methods at 40 CFR Part 136, or other methods that are specifically prescribed for the particular wastestream or for sewage sludge monitoring requirements.

2. The rule also corrects inconsistencies in sampling requirements by referencing back to 40 CFR Part 136 to explicitly require use of procedures at 40 CFR Part 136.

3. Sections 122.21(g)(7), 122.21(h)(4)(i), and 122.21(j)(4)(viii) require an NPDES permit applicant to report quantitative data for certain pollutants. The rule adds

E. coli

and Enterococci to the list of parameters at 40 CFR 122.21(g)(7) and 122.21(h)(4)(i), and adds

E. coli

to the list of parameters at 40 CFR 122.21(j)(4)(viii).

B. 40 CFR Part 136

This rule approves new and revised methods for inclusion in 40 CFR Part 136. Many of those methods are from the voluntary consensus standards body (VCSB) that publishes Standard Methods for the Examination of Water and Wastewater. Those “Standard Methods” are now available in both hard copy and electronic formats. The publisher identifies Standard Methods in two ways, depending on the medium of publication. Hard copy methods are identified by the method number (e.g., SM 4500-Cl E) and the edition of the manual in which they appear (e.g., 18th, 19th, 20th Editions), while the electronic versions available on-line are identified by the same method number and the year the method was approved for release (e.g., 4500-Cl E-00).

The following discussion briefly describes the changes to Part 136 methods approved today.

1. This rule amends the regulations at 40 CFR Part 136 to approve three new methods submitted as alternate test procedures for monitoring chemical pollutants. These methods are “Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte” (D6508, Rev. 2) by Waters Corporation, “Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis” (QuikChem Method 10-204-00-1-X) by Lachat Instruments, and “Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate” (Kelada-01) by Dr. Nabih Kelada.

2. The rule approves a broad purpose digestion procedure for total recoverable elements digestion. EPA is approving EPA Method 200.2 (Revision 2.8, 1994) for use with Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS), Stabilized Temperature Graphite Furnace Atomic Absorption (STGFAA), and Flame Atomic Absorption Spectroscopy (FLAA) methods.

3. The rule approves three new multi-element test procedures. The approved methods are EPA Method 200.8 (Revision 5.4, 1994), AOAC Method 993.14 [16th Edition], and ASTM D5673-03 for determination of elements by ICP-MS.

4. EPA is also approving a new multi-element test procedure, EPA Method 200.9 (Revision 2.2, 1994), for determination of elements by STGFAA.

5. The rule approves four new methods for determination of hexavalent chromium by ion chromatography. The methods are EPA Method 218.6, AOAC Method 993.23 [16th Edition], and ASTM D5257-97—SM 3500-Cr C [20th Edition] and SM 3500-Cr E [18th, 19th Editions].

6. The rule approves five new methods for determination of anions by ion chromatography. The methods are EPA Method 300.0 (Revision 2.1, 1993), EPA Method 300.1 (Revision 1.0, 1997), AOAC Method 993.30 [16th Edition], ASTM D4327, and SM 4110 B [18th, 19th, and 20th Editions].

7. The rule approves the use of six automated cadmium reduction methods to determine nitrate and nitrite individually, as well as in combination. The methods are EPA Method 353.2 (Revision 2.0, 1993), ASTM D3867-99 (A) and (B), SM 4500-NO

E and F [18th, 19th, 20th Editions] and 4500-NO

E and F (2000), and USGS Method I-4545-85.

8. The rule approves a new method for determination of chlorine by low level amperometry—SM 4500-Cl E [18th, 19th, 20th Editions] and SM 4500-Cl E (2000).

9. The rule replaces EPA Method 180.1 (1978) for determination of turbidity with EPA Method 180.1 (Revision 2.0, 1993).

10. The rule replaces EPA Method 200.7 (1990) for determination of elements by ICP-AES with EPA Method 200.7 (Revision 4.4, 1994).

11. The rule replaces EPA Method 245.1 (1974) for determination of mercury with EPA Method 245.1 (Revision 3.0, 1994).

12. The rule replaces EPA Method 335.3 (1978) for determination of total cyanide with EPA Method 335.4 (Revision 1.0, 1993) with a footnote to clarify the proper procedure for removing sulfide interferences.

13. The rule replaces EPA Method 350.1 (1978) for determination of ammonia with EPA Method 350.1 (Revision 2.0, 1993).

14. The rule replaces EPA Method 351.2 (1978) for determination of total Kjeldahl nitrogen (TKN) with EPA Method 351.2 (Revision 2.0 1993).

15. The rule replaces EPA Method 353.2 (1978) for determination of nitrate-nitrite with EPA Method 353.2 (Revision 2.0, 1993).

16. The rule replaces EPA Method 365.1 (1978) for determination of phosphorus (all forms) with EPA Method 365.1 (Revision 2.0, 1993).

17. The rule replaces EPA Method 375.2 (1978) for determination of sulfate with EPA Method 375.2 (Revision 2.0, 1993).

18. The rule replaces EPA Method 410.4 (1978) for determination of chemical oxygen demand (COD) with EPA Method 410.4 (Revision 2.0, 1993).

19. The rule replaces EPA Method 420.2 (1974) for determination of total phenols with EPA Method 420.4 (Revision 1.0, 1993).

20. The rule approves a new method for the determination of mercury, EPA Method 245.7 “Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry'' [Revision 2.0, 2005] (EPA-821-R-05-001).

21. The rule approves a new method for determination of available cyanide by ligand exchange followed by flow injection analysis, ASTM D6888-04.

22. The rule approves a new method for determination of cations by ion chromatography, ASTM D6919-03.

23. The rule approves a new method for determination of chloride by potentiometry, SM 4500-Cl

D [18th, 19th, 20th Editions] and SM 4500-Cl

D (2000).

24. The rule approves a new method for determination of chloride by ion selective electrode, ASTM D512-89 (1999).

25. The rule approves two new methods for determination of total cyanide by ion selective electrode, SM 4500-CN

F [18th, 19th, 20th Editions] and SM 4500-CN

F (2000), and ASTM D2036-98 A.

26. The rule approves two new methods for determination of sulfide by ion selective electrode, SM 4500-S

G [18th, 19th, 20th Editions] and ASTM D4658-03 (1996).

27. The rule approves a new method for determination of nitrate by ion selective electrode, SM 4500-NO

[18th, 19th, 20th Editions] and SM 4500-NO

(2000).

28. The rule approves an errata sheet to correct typographical errors in the following methods manuals, “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 (the “freshwater chronic manual”), and “Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms,” Fifth Edition, U.S. Environmental Protection Agency, Office of Water, Washington DC, EPA/821/R-02/012 (the “freshwater acute manual'').

29. The rule approves the use of newer versions of 74 methods published by ASTM International. The new versions are published in the 1994, 1996, and 1999 Annual Book of ASTM Standards Vols. 11.01 and 11.02, in the 2000 Annual Book of ASTM Standards, Vol. 11.02 and in individual standards published after 2000.

30. The rule approves the use of newer versions of 88 methods published by the Standard Methods Committee and adopts a new numbering system to track the approved versions of Standard Methods. The new versions are published in Standard Methods Online (APHA 2003).

31. The rule approves the use of newer versions of 19 methods published by AOAC-International. The new versions of these methods are published in Official Methods of Analysis of AOAC-International, 16th Edition, 1995.

32. The rule approves the replacement of the mercuric sulfate catalyst with copper sulfate in methods approved for the determination of total Kjeldahl nitrogen (TKN).

33. The rule approves the use of styrene divinyl benzene beads and stabilized formazin as alternatives to the presently approved formazin standard for determination of turbidity.

34. As described in the preamble to the April 2004 proposed rule (69 FR 18213), EPA is adopting a new § 136.6 to introduce greater flexibility in the use of approved methods. The section describes the circumstances in which approved methods may be modified and the requirements that analysts must meet to use these modified methods in required measurements without prior EPA approval. The rule also includes language at § 136.6(c) to clarify that analysts need only meet method performance requirements for target analytes (those analytes being measured for NPDES reporting) when using multi-analyte methods for compliance monitoring purposes. The rule also includes the language at § 136.6(d) to allow explicitly the use of capillary (open tubular) GC columns with EPA Methods 601-613, 624, 625, and 1624B as alternatives to the packed GC columns specified in those methods, provided that analysts generate new retention time tables with capillary columns to be kept on file with other information for review by auditors.

35. The rule withdraws 109 methods contained in EPA's “Methods for the Chemical Analysis of Water and Wastes” for which approved alternatives published by voluntary consensus standards bodies (

e.g.

, ASTM and Standard Methods) are available.

36. The rule withdraws liquid-liquid extraction (LLE) methods, including EPA Methods 612 and 625, as approved procedures for determination of 1,2-dichlorobenzene, 1,3-dichlorobenzene, and 1,4-dichlorobenzene.

37. The rule withdraws approval of all oil and grease methods that use chlorofluorocarbon-113 (CFC-113; Freon-113) as an extraction solvent.

38. The rule revises Table II (Required Containers, Preservation Techniques, and Holding Times) and the footnotes to the table at 40 CFR 136.3(e). The table and footnotes specify approved sampling, preservation, and holding time requirements for the methods approved for compliance monitoring to reduce confusion, resolve any conflicts with instructions in the underlying compliance monitoring method, and reflect current understanding of sample preservation requirements. The most significant of the changes are those made to Footnote 6, which addresses the preservation of samples to be analyzed for cyanide. Based on information gathered during the development of new cyanide methods approved in this rulemaking, and information collated from various commenters and experts in cyanide analyses, EPA revised footnote 6 to Table II by adding text that describes procedures that are recommended for removal or suppression of cyanide interferences, including interferences

from sulfur, sulfide, sulfite, thiocyanate, and aldehydes. The recommended procedures may differ from those described in the older approved methods.

39. EPA is changing “Director of the Environmental Monitoring Systems Laboratory” and “Director, Analytical Methods Staff” to “Alternate Test Procedure Program Coordinator, Washington, DC'' every place the phrases appear in the regulations. This reflects the current organizational structure and title for the head of EPA's Alternate Test Procedure (ATP) Program management. In addition, addresses for submission of ATPs are being updated to reflect the current location of the Alternate Test Procedure Program Coordinator.

40. The rule makes other minor editorial revisions to clarify existing regulations.

C. 40 CFR Parts 141 and 143

1. This rule amends the regulations at 40 CFR Part 141 and Part 143 to allow the use of 66 methods in ”Standard Methods Online” (APHA 2003) (40 CFR 141.21, 141.23, 141.74, and 143.4).

2. This rule allows the use of 28 newer versions of methods published by ASTM International. The new versions are published in the 1999 “Annual Book of ASTM Standards,”' Vols.11.01 and 11.02, in the 2000 “Annual Book of ASTM Standards,” Vol. 11.02 and in individual standards published after 2000 (40 CFR 141.23).

3. This rule approves a new method submitted as an alternate test procedure for the determination of common anions—chloride, fluoride, nitrate, nitrite, orthophosphate, and sulfate, “Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte” (D6508, Rev. 2) by Waters Corporation (40 CFR 141.23 and 143.4).

4. This rule approves two new methods for determination of available cyanide, “Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,” Method OIA-1677, DW (January 2004), and ASTM D6888-04 (40 CFR 141.23).

5. This rule approves the use of EPA Method 300.1 (Revision 1.0, 1997) for compliance determinations of chloride, fluoride, nitrate, nitrite, orthophosphate, and sulfate (40 CFR 141.23 and § 143.4).

6. This rule approves the use of EPA Method 552.3 (Revision 1.0, 2003) for compliance determinations of dalapon (40 CFR 141.24).

7. This rule amends 40 CFR 141.25 to add a new method for determination of radium-226 and radium-228. This method, “The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors” (Revision 1.2, December 2004), was developed by the Environmental Resources Center at the Georgia Institute of Technology, and was originally submitted to EPA as an alternate test procedure to the currently approved methods for determination of radium-226 and radium-228.

8. This rule allows States the option of approving ITS Free chlorine test strips as a test kit for the measurement of free chlorine using “Free Chlorine Species” (HOCl- and OCl-) by Test Strip,'' ITS Method D99-003 (Revision 3.0, November 21, 2003) by Industrial Test Systems, Inc. (40 CFR 141.74).

9. This rule approves EPA Method 327.0 (Revision 1.1, 2005) for measurement of chlorine dioxide residuals (40 CFR 141.74).

10. This rule approves the use of styrene divinyl benzene beads and stabilized formazin as alternatives to the presently approved formazin standard for determination of turbidity (40 CFR 141.74).

11. This rule revises footnote 17 to the table at 40 CFR 141.23 to allow the use of a 450-W UV lamp in the Kelada Method-01 for determination of cyanide.

12. This rule allows the use of Syngenta Method AG-625, with the modified immunoassay testing product manufactured by Beacon Analytical Systems, for the measurement of atrazine under certain conditions. It may only be used by those systems that do not use chlorine dioxide for drinking water treatment. In addition, the results of the analysis of samples with concentrations of atrazine more than one-half the atrazine MCL (

i.e.

, more than 1.5 μg/L) must be confirmed using another approved method (40 CFR 141.24).

13. This rules also revises footnote 8 to the table in paragraph (a)(1) to correct a long-standing discrepancy between the footnote and the specifications in Standard Method 9221 E. The table in question lists Standard Method 9221 E as one of two procedures that may be used for monitoring fecal coliforms. Footnote 8 simply notes the holding time for the A-1 broth used in this procedure. Today's action corrects the holding time specified in the footnote 8 to match the 7-day holding time that is specified in Standard Method 9221 E (40 CFR 141.74)

D. 40 CFR Part 430

This rule amends the Effluent Limitations Guidelines for the pulp, paper, and paperboard point source category at 40 CFR Part 430 to approve a new method for determination of chlorinated phenolics in wastewaters generated by these industries. The rule adds a new section, 430.02(g), to allow the use of “Chlorinated Phenolics in Water by In situ Acetylation and GC/MS Determination” (Method CP-86.07) developed by the National Council for Air and Stream Improvement (NCASI) as an alternative to otherwise required Method 1653 in Part 430, Appendix A.

E. 40 CFR Part 455

This rule amends the regulations at 40 CFR Part 455 by moving Table 7 from 40 CFR Part 455 to 40 CFR Part 136.3(a) as new Table IG.

F. 40 CFR Part 465

This rule amends the Effluent Limitations Guidelines for the coil coating point source category at 40 CFR Part 465 to replace the method listed at section 465.03(c) for determination of oil and grease in wastewater samples from all subcategories of coil coating with EPA Method 1664A for determination of non-polar materials (NPM), which is generally equivalent to total petroleum hydrocarbons.

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. In some instances, EPA revised for clarity the language of the final rule from that in the proposed rule.

A. Silver Determinations

EPA received comments on the Agency's proposed withdrawal of EPA Method 272.1 which included information on how to keep silver in solution in samples with known or suspected high levels of silver by adding a solution containing cyanogen chloride. As a result, EPA has added a footnote to Table IB at § 136.3 to include procedures for preparation and addition of this reagent to digested samples of this type to keep the silver in solution for analysis by any of the approved methods. The Agency is withdrawing EPA Method 272.1, as proposed in April 2004 (69 FR 18183 April 6, 2004).

B. ASTM Method D5673-02 “Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry”

Based on comment received on the Agency's proposed approval of ASTM Method D5673-02, EPA is approving an updated version of this method ASTM D5673-03. EPA included the updated version of this method in a notice of data availability (70 FR 7909, February 16, 2005) and requested public

comment on whether it should be approved. EPA received no adverse comments.

C. Ammonia Determinations

EPA received comment on the Agency's proposed approval of an updated version of EPA Method 350.1. The commenter stated that mandating the use of ethylene-diamine-tetra-acetate (EDTA) in the method could adversely affect method performance when using an automated analyzer and submitted data to support this claim. Based on EPA's review of the data, the Agency is adding a footnote to Table IB at § 136.3 allowing analysts to omit EDTA from EPA Method 350.1, provided that all of the quality control (QC) acceptance criteria in the method are met.

D. Available Cyanide Determinations

The Agency solicited comment regarding problems encountered with the use of ligand exchange-amperometric detection methods for determination of available cyanide in samples that contain significant amounts of solids and solicited potential solutions to these problems. Based on public comment, EPA is adding a footnote to Table IB at § 136.3 that includes suggestions for sample filtration and for limiting the time between addition of ligand exchange reagents and analysis to solve these problems when necessary. The Agency proposed ASTM Method D6888-03 for determining available cyanide. Since publication of the proposal, EPA has received a revised version of this method. EPA included this revised version in a Notice of Data Availability (NODA) and requested public comment on the approval of this revised version of the method (70 FR 7909, February 16, 2005). D6888-04 contains a new online sulfide removal procedure and represents a refinement to the proposed version. EPA received no adverse comments on this revised version of the method and is approving ASTM Method D6888-04 in today's rule.

E. Kelada-01 Method for Determination of Available Cyanide and Total Cyanide

Based on a comment and data received on the Agency's proposed approval of the Kelada-01 method for determination of available cyanide and total cyanide for use in NPDES compliance monitoring, a note has been added at 40 CFR 136.3, Table IB, Footnote 55 to allow the use of 450-W UV lamp instead of the 550-W lamp specified in the method if it provides performance within the quality control acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met. The Agency also is adding the note at 40 CFR 141.23, Footnote 17, as this method was previously approved for use in drinking water compliance monitoring.

F. Mandatory Replacement of Mercuric Sulfate With Copper Sulfate in Methods for Determination of Total Kjeldahl Nitrogen

The Agency proposed the mandatory replacement of mercury sulfate with copper sulfate in total Kjeldahl nitrogen (TKN) digestion. Comments expressed concern that copper sulfate will provide inferior performance in some samples, and suggested that EPA allow the continued use of mercury sulfate in analyses, offering copper sulfate as an option. Based on EPA's evaluation of these comments, the Agency has decided that it will continue to allow the use of mercury sulfate in TKN analyses.

G. Approval of Additional Standards for Turbidity Determinations

Based on comments received on the proposed approval of additional standards for use in methods to determine turbidity, the Agency is replacing turbidity standard trade names with more generic listings in the footnote to Table IB at § 136.3. An example formulation for each generic listing is also included in order to provide a reference to at least one source of the generic standard material. The Agency also is adding a similar footnote to the table in 40 CFR 141.74 where the approved methods for the determination of turbidity in drinking water are listed.

H. Allowed Use of Capillary Columns in EPA Methods 601-613, 624, 625, and 1624B

The Agency proposed new language that explicitly allows the use of capillary columns in place of packed columns with EPA Methods 601-613, 624, 625, and 1624B, provided that all QC tests in these methods are performed and all QC acceptance criteria are met. Based on comments received on this proposal, EPA is clarifying the regulations at § 136.6 to state that retention times will change with the switch from packed to capillary columns, so analysts are not required to meet the retention times specified in the method when the switch is made. Instead, analysts must generate new retention time tables with capillary columns to be kept on file with other information for review by auditors.

I. Changes to Sampling Requirements at 40 CFR Parts 122, 136, and 403

The Agency proposed changes to the sampling requirements specified at 40 CFR Parts 122, 136 and 403. Based on comments received on these proposed updates, the sampling requirements have been modified to include clarifying language with respect to grab and composite sampling requirements, and to add

E. coli

and Enterococci to the parameters listed at Part 122.21 for which an NPDES applicant must provide analytical information. In addition, on October 14, 2005, EPA published in the

Federal Register

final changes to its General Pretreatment Regulations (70 FR 60134). In these regulations, EPA consolidated monitoring requirements for indirect dischargers into 40 CFR 403.12(g). In the proposal for the current rule, EPA proposed to modify 40 CFR 403.12 (b). Based on changes made to 40 CFR Part 403 on October 14, 2005, however, the proposed modifications to CFR 403.12 (b) are no longer required.

J. Approval Status of Total Elements Digestion

The Agency proposed to approve a “total recoverable” elements digestion procedure, and also to retain “total” elements digestion for graphite furnace atomic absorption (GFAA) analyses. Based on comments received on this proposal, EPA is clarifying the language in Table IB at § 136.3 to specify Section 4.1.3 of Methods for Chemical Analysis of Water and Wastes (MCAWW) as the approved digestion procedure for use with non-platform graphite furnace atomic absorption determinations.

K. EPA Method 245.7 for Determination of Mercury

The Agency proposed approval of EPA Method 245.7 (December 2003) as an additional method for determination of mercury. Based on comments received on this proposal, EPA has revised the method and is approving EPA Method 245.7 (Revision 2.0, 2005) in this rule. Specifically, EPA has approved the method with the following changes: includes a discussion of the gas-liquid separator in Section 2.6, reduces the amount of hydrochloric acid used during sample digestion, includes the addition of hydrochloric acid (HCl) to standard solutions, clarifies that additional procedures for handling difficult matrices may be used provided that laboratories meet the method performance criteria, and revises procedures for preparing reagent blanks to remove the addition of stannous chloride (SnCl

) and include addition of

HCl. EPA also has corrected section numbering and references throughout Sections 4 and 7 of the method.

L. Clarification of Reporting Requirements

The Agency proposed to add a new § 136.7 that would clarify that a quality control (QC) failure does not relieve a permittee of the duty to report results and that results are to be reported to the level specified in the method or required in the permit, whichever is lower. EPA agrees with public comment that the proposed revision was unclear. In this rule, EPA is revising this action to clarify our intent in text at § 136.3, rather than take final action on the proposed text at § 136.7.

EPA proposed a new § 136.7 amendment to resolve conflicts between current reporting requirements at 40 CFR Parts 122 and 125 and preservation requirements at 40 CFR 136.3(e) and instructions in compliance monitoring methods specified in the tables at 40 CFR 136.3(a). For example, some methods provide “reject tests” (e.g. Method 5210 B 5-day BOD, section 6a, Standard Methods, 20th edition) or state that a “result may not be reported for regulatory compliance purposes” (e.g. Method OIA 1677: Available Cyanide, section 9.3.4, OI Analytical) if an analytical quality control measure is outside its control limit range (acceptance criteria). However, it may be necessary to report such results if resampling, reanalysis or other corrective action is not possible. Not reporting these results may cause a permittee to be in violation of Part 122 or 125 reporting requirements. Reporting such available data is recommended as a good laboratory practice (D3856-95 Standard Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water,

Annual Book of ASTM Standards,

Water and Environmental Technology, Vol 11.01 Water (I), p. 353, 2003).

For clarification, in this rule, EPA is adding a statement to the text preceding Tables IA to IG at § 136.3(a), and Table II at § 136.3(e) to state that reporting requirements of Parts 122 or 125 may take precedence over the otherwise applicable reporting or preservation requirements of a particular analytical method.

M. Corrections to 40 CFR Part 136, Tables IA, IB, IC, ID, IE and Footnotes

The Agency is correcting errors that were published in the proposed Table IA (List of Approved Biological Methods), Table IB (List of Approved Inorganic Test Procedures), Table IC (List of Approved Test Procedures for Non-Pesticide Organic Compounds), Table ID (List of Approved Test Procedures for Pesticides), and Table IE (List of Approved Radiologic Test Procedures) and the footnotes to those tables.

N. Revisions to 40 CFR Part 136, Table II

The rule revises Table II (Required Containers, Preservation Techniques, and Holding Times), and the footnotes to Table II at 40 CFR 136.3(e). The action of updating Table II at § 136.3(e) reflects EPA's evaluation of comments received on the April 6, 2004 proposal. EPA revised footnote 1 to more clearly distinguish between polyethylene (P), fluoropolymer (FP), glass (G), and low-density polyethylene (LDPE) and has made it explicit that a sample to be used to determine fluoride is to be collected in a polyethylene bottle. EPA revised footnotes 2 and 7 to add language to make more clear that preservation must be within 15 minutes after collection of a grab sample, a composite sample, or an aliquot split from a composite sample collected automatically over time.

EPA modified footnote 4 to clarify the start of holding times for the different types of sample collection (grab samples, composite samples collected automatically, and a set of grab samples that is composited in the laboratory). The revisions remove the requirement for collection of samples to determine cyanide in amber glass bottles with PTFE-lined caps from footnote 6. Footnotes 5 and 6 describe procedures recommended for removal or suppression of cyanide interferences, including interferences from oxidants, sulfide, sulfite, thiocyanate, and aldehydes. In addition, the footnote also provides that other procedures for removal or suppression of cyanide interferences may be employed, provided the analyst demonstrates that such other procedures more accurately measure cyanide.

EPA clarified requirements in footnote 17 specific to sampling for trace mercury, added EPA Method 245.7 to footnote 17, and removed footnote 17 from the “Preservation” and “Maximum Holding Time” headers. EPA has clarified footnote 18 to indicate that the number of significant figures is intended to establish an absolute upper limit on sample temperature and preclude meeting the specification through rounding of numbers and added an exception to footnote 18 for a sample analyzed immediately (in less than 15 minutes from collection). EPA deleted footnote 19 because the information is now in footnote 5. Deletion of this footnote resulted in renumbering all of the subsequent footnotes to Table II.

EPA has also clarified that preservation is not required for soil and sediment samples. EPA also has revised preservation requirements for acrolein, acrylonitrile, and purgeable aromatics to remove inconsistences, revised requirements for collection of samples to be tested for Cryptosporidium and Giardia, and established 0-8 °C as the holding temperature for samples to be tested for Cryptosporidium. In addition, the Agency is correcting minor formatting and typographical errors that were published in the proposed Table II.

EPA recognizes that the requirements at § 136.3 may differ from those described in some older approved methods and today's action clarifies that this section supersedes instructions in a compliance method. Where there are conflicts with existing methods published by EPA, VCSBs, or other entities, we expect that the next revisions of these methods will conform to the requirements at § 136.3(e).

O. Corrections to Tables 40 CFR Parts 141.23, 141.24, 141.25, and 141.74 and Footnotes

The final rule corrects a number of errors in the proposed tables at § 141.23 (Inorganic Chemical Sampling and Analytical Requirements), 141.24 (Organic Chemicals, Sampling and Analytical Requirements), 141.25 (Analytical Methods for Radioactivity) and 141.74 (Analytical and Monitoring Requirements) and the footnotes to those tables. The Agency also revised the wording of several entries for the cyanide methods in the tables at 40 CFR 141.23 to more clearly distinguish among the various methodologies listed in those tables.

P. Retention of Syngenta Method AG-625 for Determination of Atrazine

The Agency proposed to withdraw approval of Syngenta Method AG-625 for the determination of atrazine in drinking water. Based on comments received regarding the April 6, 2004 proposal and comments received regarding additional data submitted in response to the Notice of Data Availability (70 FR 7909, February 16, 2005), EPA has decided to retain Syngenta Method AG-625 with some restrictions on its use. The revised approval requires confirmation of any compliance monitoring results for atrazine that are greater than one half of the MCL for atrazine, using an alternate approved method. EPA based its approval on the use of the modified immunoassay testing product produced

by Beacon Analytical Systems, the only version of the product that is currently offered for sale. However, use is not authorized for public water systems which use chlorine dioxide for drinking water treatment.

Q. EPA Method 327.0 for Determination of Chlorine Dioxide

The Agency proposed to approve EPA Method 327.0 (Revision 1.0, 2003) for the determination of chlorine dioxide (40 CFR 141.74). In the final rule, the Agency has approved EPA Method 327.0 (Revision 1.1, 2005) and corrected three typographical errors in the proposed method.

R. Deferral of Action on Microtox® 1010

Because EPA is continuing to evaluate public comment about use of the Microtox® 1010 test procedure for determinations of acute whole effluent toxicity, and the data supporting use of this test procedure, EPA is not taking final action on the proposal to approve Microtox® 1010 for compliance monitoring.

IV. Response to Comments

EPA received two comments regarding methods included in this final rule from the August 18, 2003 proposal (68 FR 49548), 115 comments on the April 6, 2004 proposal (69 FR 18166), and nine comments on the February 16, 2005 Notice of Data Availability (NODA) (70 FR 7909). Commenters represented a number of different interests, including analytical laboratories, water utilities, instrument manufacturers, State and local governments, trade associations, scientists, and private citizens. A summary of major public comments on the proposed rules and the NODA and the Agency's responses is presented in this section, and section III of this preamble. The public docket for this rule includes the Agency's response to all comments.

A. Use of Syngenta Method AG-625 for Determination of Atrazine

EPA proposed withdrawing approval of Syngenta Method AG-625 (Syngenta Crop Protection Inc.) for the determination of atrazine. Based on comments and additional data submitted in response to the NODA, EPA has decided to retain Syngenta Method AG-625 as an approved method for atrazine, subject to certain conditions. Today's amended rule will require the use of an alternate approved method for atrazine to confirm any results from the Syngenta method that are greater than one half of the MCL for atrazine. EPA's decision to retain the approval of Method AG-625 is based on using the modified immunoassay testing product manufactured by Beacon Analytical Systems (Atrazine Plate Kit-Cat# CPP-004), the only version of the product currently offered for sale. However, based on data submitted in response to the NODA, EPA is not approving Method AG-625 for use when chlorine dioxide is used for drinking water treatment.

One commenter supported the withdrawal of Syngenta Method AG-625, citing EPA's Environmental Technology Verification (ETV) study, and suggested that the method had not been validated adequately prior to EPA's earlier approval. The commenter also suggested that approval of a modified version of AG-625 may be preferable, but was concerned that the method using the original testing product could lead to reports of non-compliance and/or increased treatment cost based on erroneous atrazine measurements in the interim.

Other comments questioned the validity of data submitted by the American Water Works Association (AWWA) that demonstrated method deficiencies and requested that the data not be considered by EPA. The commenters noted that data were not accompanied by suitable quality control checks and that some tests (

i.e.

, testing the effect of humic acid) were not reproducible in later studies by the same investigator. The commenters also suggested that data generated by AWWA was not generated according to Method AG-625, but rather by simply using the commercial testing product without reference to the method.

As reported by Adams (Adams

et al.

, JAWWA, 2004, pp. 126-139), the original immunoassay test kit used with Method AG-625 was subject to a positive bias in the measurement of atrazine in the presence of disinfectants used in drinking water treatment, such as chlorine, monochloroamine, chloramine T, chlorine dioxide and other substances. Additionally, data reported by Adams using the modified Beacon test kit, data from the Environmental Technology Verification (ETV) Program, and, in fact, data in the December 2004 Syngenta study (Atrazine: Final Report, Syngenta Number T006141-04, 12/10/2004), demonstrate that test kits marketed by Beacon, Abraxis, and SDI show a modest positive bias in raw and finished drinking water for most samples (

i.e.

, the measured concentrations in most samples were higher than the expected values). For a distinct minority of samples in these two studies, no bias or a negative bias was shown (

i.e.

, the measured concentrations were equal to or lower than the expected concentrations in a few samples). The December 2004 Syngenta study submitted to EPA demonstrated that the modified Beacon immunoassay test kit performed suitably in the presence of chlorine, monochloroamine, chloramine T, chloroform, and humic acid. However the data show that an interference occurred in the presence of chlorine dioxide unless samples were analyzed within one day of collection.

EPA agrees that data from both Syngenta and AWWA (Adams) indicate that, except for cases involving chlorine dioxide, the modified testing product performed substantially better with regard to the positive bias and interferences than did the original product in the presence of disinfectants and other interferences. EPA also agrees that, in general, the immunoassay products examined in these studies exhibit some positive bias for atrazine. Low results were only obtained from analyses of a few samples.

EPA recognizes that a potential positive bias is a concern for water utilities, particularly those located in areas such as the Midwest, where atrazine is used extensively to control weeds in corn and sorghum crops. However, in many other areas, where it is not used, atrazine is not likely to be found in drinking water samples at all. Because accurate information on the occurrence of contaminants at concentrations close to the MCL is necessary for EPA to meet its obligation to review MCLs every six years, EPA has retained approval of Syngenta Method AG-625 for atrazine with the conditions on its use described below. The following conditions have been added as Footnote 5 to the table at 40 CFR 141.24(e)(1).

“This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for drinking water treatment. In samples from all other systems, any result for atrazine generated by Method AG-625 that is greater than one-half the maximum contaminant level (MCL) (i.e., greater than 0.0015 mg/L or 1.5 μg/L) must be confirmed using another approved method for this contaminant and should use additional volume of the original sample collected for compliance monitoring. In instances where a result from Method AG-625 triggers such confirmatory testing, the confirmatory result is to be used to determine compliance.''

The MCL for atrazine is 0.003 mg/L (3 μg/L). Thus, any results from Method AG-625 greater than 0.0015 mg/L (1.5 μg/L) must be confirmed through the use of another approved method for atrazine. In such instances, the

confirmatory result is used to determine compliance, because the methods used for confirmatory testing are considered more accurate.

EPA acknowledges that this requirement for confirmation may cause some utilities to choose not to employ Method AG-625. However, the approval of a method at 40 CFR Part 141 does not constitute a requirement for its use when other approved methods are available. Furthermore, EPA has concluded that, given the distribution of atrazine use nationwide, the majority of water utilities will not be negatively affected by the confirmation requirement and can take advantage of the potential cost savings afforded by Method AG-625 relative to other approved methods for atrazine. EPA notes that if utilities are monitoring for a broad range of contaminants using approved methods that cover multiple analytes (e.g., Method 525.2), then the use of a test kit may not offer a cost advantage because of the ability to include atrazine in a broad spectrum method.

Based on the data provided in response to the proposed rule and NODA, EPA agrees that the presence of chlorine dioxide has substantial potential to interfere with Method AG-625. Therefore, EPA has not approved the method for use in water systems where chlorine dioxide is used for drinking water treatment. While the data from one study suggest that the atrazine results are not affected if samples are analyzed within 24 hours after sample collection, the circumstances surrounding this observation in the study have not been fully characterized. At a future date, EPA may reconsider the use of Method AG-625 by water systems using chlorine dioxide, if more information is available characterizing the performance of the method.

B. Results From Use of Revised Methods, “The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors.” (Revision 1.2, December 2004)

The final rule establishing radionuclide drinking water standards published on December 7, 2000 (65 FR 76708) required drinking water systems to sample and report on radionuclides in their drinking water supplies during the period from December 8, 2003 to December 31, 2007, including the combined result for radium-226 and radium-228. Prior to today's rule, separate methods were required for the measurement of radium-226 and radium-228. The separate results of the two isotopes are summed to provide the “combined” result that is compared to the MCL. One commenter supported the approval of the method from the Georgia Institute of Technology because one method can be used to measure both radium isotopes and would make for a faster result. The commenter also noted that there are approximately 150,000 Public Water Supply source water taps across the country that would have to be sampled. Given these monitoring requirements, the commenter was concerned about sufficient laboratory capacity to meet the monitoring requirements of the December 2000 rule because approval of the Georgia Institute of Technology method would not become effective until promulgation of today's rule.

In response to this comment, EPA is allowing community water systems to use samples collected after January 1, 2005 and analyzed using the analytical method approved in this rule to satisfy the radium-226 and radium-228 monitoring requirements for the 2005-2007 compliance period. (Minor corrections to the method were made in December 2004 and are reflected in the version approved in this rule, so it was not available for analyzing samples collected prior to 2005.) Allowing this early use of the method should alleviate some of the laboratory capacity concerns. EPA has included a footnote in the revised table of analytical methods for radioactivity at § 141.25 to indicate that samples analyzed using the newly approved method are acceptable. Such “grandfathered” data must be based on results from the analytical method approved for use by this final rule. The term “grandfathered data” used in this rule does not apply to data collected to meet other grandfathering provisions specified in the radionuclide final rule that was published on December 7, 2000 (65 FR 76708).

V. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review

Under Executive Order 12866 (58 FR 51735, October 4, 1993), the Agency must determine whether the regulatory action is “significant” and therefore subject to OMB review and the requirements of the Executive Order. The Executive Order defines “significant regulatory action” as one that is likely to result in a rule that may:

(1) Have an annual effect on the economy of $100 million or more, or adversely affect in a material way the economy, a sector of the economy, productivity, competition, jobs, the environment, public health or safety, or State, local, or Tribal governments or communities;

(2) Create a serious inconsistency or otherwise interfere with an action taken or planned by another agency;

(3) Materially alter the budgetary impact of entitlements, grants, user fees, or loan programs or the rights and obligations of recipients thereof; or

(4) Raise novel legal or policy issues arising out of legal mandates, the President's priorities, or the principles set forth in the Executive Order.

It has been determined that this rule is not a “significant regulatory action” under the terms of Executive Order 12866 and is therefore not subject to OMB review.

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.

This rule does not impose any information collection, reporting, or recordkeeping requirements. This rule merely adds new and updated versions of testing procedures, withdraws some older testing procedures, and establishes new sample collection, preservation, and holding time requirements.

Burden means the total time, effort, or financial resources expended by persons to generate, maintain, retain, or disclose or provide information to or for a Federal agency. This includes the time needed to review instructions; develop, acquire, install, and utilize technology and systems for the purpose of collecting, validating, and verifying information, processing and maintaining information, and disclosing and providing information; adjust the existing ways to comply with any previously applicable instructions and requirements; train personnel to be able to respond to a collection of information; search data sources; complete and review the collection of information; and transmit or otherwise disclose the information.

An Agency may not conduct or sponsor, and a person is not required to respond to a collection of information unless it displays a currently valid OMB control number. The OMB control numbers for EPA's regulations in 40 CFR are listed in 40 CFR Part 9.

C. Regulatory Flexibility Act

The 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 as defined by the Small Business Administration's (SBA) regulations at 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. The RFA provides default definitions for each type of small entity. It also authorizes an agency to use alternative definitions for each category of small entity, “which are appropriate to the activities of the agency” after proposing the alternative definition(s) in the

Federal Register

and taking comment (5 U.S.C. 601(3)-(5)). In addition to the above, to establish an alternative small business definition, agencies must consult with SBA's Chief Counsel for Advocacy.

For purposes of assessing the impacts of this rule on small entities for methods under the Safe Drinking Water Act, EPA considered small entities to be public water systems serving 10,000 or fewer persons. This is the cut-off level specified by Congress in the 1996 Amendments to the Safe Drinking Water Act for small system flexibility provisions. In accordance with the RFA requirements, EPA proposed using this alternative definition in the

Federal Register

(63 FR 7620, February 13, 1998), requested public comment, consulted with the Small Business Administration, and expressed its intention to use the alternative definition for all future drinking water regulations in the Consumer Confidence Reports regulation (63 FR 44511, August 19, 1998). As stated in that final rule, the alternative definition would be applied to this regulation as well.

After considering the economic impacts of today's 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 updated versions of testing procedures, withdraws some older testing procedures, and approves new sample collection, preservation, and holding time requirements. 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. In some cases, analytical costs may increase slightly due to the additional QC requirements included in the methods that are being approved to replace older EPA methods. However, most laboratories that analyze samples for EPA compliance monitoring have already instituted QC requirements as part of their laboratory practices. We have determined that a small number of small entities that are still using the CFC-113 based oil and grease methods may need to devote resources to analyst training when they switch to hexane-based methods. However, due to the decreased availability of CFC-113 in the marketplace, we anticipate that the cost differential, if any, will soon favor the use of the hexane-based methods. The phaseout of CFC-113 based methods is required to comply with the Montreal Protocol which prohibits the use of CFC-113 based methods after December 31, 2005.

Although this final rule will not have a significant economic impact on a substantial number of small entities, EPA nonetheless has tried to reduce the impact of this rule on small entities. Anticipating the prohibition of CFC-113 based methods, EPA promulgated hexane-based methods in May 1999. EPA has determined that most laboratories have now switched to hexane-based oil and grease methods, making the analysis costs competitive with the CFC-113 based methods.

D. Unfunded Mandates Reform Act

Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Public Law 104-4, establishes requirements for Federal agencies to assess the effects of their regulatory actions on State, Tribal, and local governments and the private sector. Under section 202 of the UMRA, EPA generally must prepare a written statement, including a cost-benefit analysis, for proposed and final rules with “Federal mandates” that may result in expenditures to State, local, and Tribal governments, in the aggregate, or to the private sector, of $100 million or more in any one year. Before promulgating an EPA rule for which a written statement is needed, section 205 of the UMRA generally requires EPA to identify and consider a reasonable number of regulatory alternatives and adopt the least costly, most cost-effective or least burdensome alternative that achieves the objectives of the rule. The provisions of section 205 do not apply when they are inconsistent with applicable law. Moreover, section 205 allows EPA to adopt an alternative other than the least costly, most cost-effective or least burdensome alternative if the Administrator publishes with the final rule an explanation of why that alternative was not adopted.

Before EPA establishes any regulatory requirements that may significantly or uniquely affect small governments, including Tribal governments, it must have developed under section 203 of the UMRA a small government agency plan. The plan must provide for the notification of potentially affected small governments, enabling officials of affected small governments to have meaningful and timely input in the development of EPA regulatory proposals with significant Federal intergovernmental mandates, and informing, educating, and advising small governments on compliance with the regulatory requirements.

This rule contains no Federal mandates (under the regulatory provisions of Title II of UMRA) for State, local, or Tribal governments or the private sector. The rule imposes no enforceable duty on any State, local, or Tribal governments or the private sector. In fact, this rule should (on the whole) save money for governments and the private sector by increasing method flexibility, and allowing these entities to reduce monitoring costs by taking advantage of innovations. Thus, today's rule is not subject to the requirements of Sections 202 and 205 of the UMRA.

EPA has determined that this 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 updated versions of testing procedures, withdraws some older testing procedures, and approves new sample collection, preservation, and holding time requirements. Thus, today's rule is not subject to the requirements of Section 203 of UMRA.

E. Executive Order 13132: Federalism

Executive Order 13132, entitled “Federalism” (64 FR 43255, August 10, 1999), requires EPA to develop an accountable process to ensure “meaningful and timely input by State and local officials in the development of regulatory policies that have federalism implications.” “Policies that have federalism implications” is defined in the Executive Order to include

regulations that 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.”

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. This rule merely approves new and updated versions of testing procedures, withdraws some older testing procedures, and approves 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), 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

Executive Order 13175, entitled “Consultation and Coordination with Indian Tribal Governments” (65 FR 67249, November 9, 2000), requires EPA to develop an accountable process to ensure “meaningful and timely input by tribal officials in the development of regulatory policies that have tribal implications.”

This final rule does not have tribal implications, as specified in Executive Order 13175. 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 updated versions of testing procedures, withdraws some older testing procedures, and approves new sample collection, preservation, and holding time requirements. The costs to Tribal governments will be minimal (in fact, governments may see a cost savings), and the rule does not preempt State law. Thus, Executive Order 13175 does not apply to this rule.

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

Executive Order 13045: “Protection of Children from Environmental Health Risks and Safety Risks” (62 FR 19885, April 23, 1997) applies to any rule that: (1) Is determined to be “economically significant” as defined under Executive Order 12866, and (2) concerns an environmental health or safety risk that EPA has reason to believe may have a disproportionate effect on children. If the regulatory action meets both criteria, the Agency must evaluate the environmental health or safety effects of the planned rule on children, and explain why the planned regulation is preferable to other potentially effective and reasonably feasible alternatives considered by the Agency. This final rule is not subject to the Executive Order 13045 because it is not economically significant as defined in Executive Order 12866. Further it does not concern an environmental health or safety risk that EPA has reason to believe may have a disproportionate effect on children. This action approves new and updated versions of testing procedures, withdraws some older testing procedures, and approves new sample collection, preservation, and holding time requirements.

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

This rule 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

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 over 150 standards developed by Standard Methods and ASTM International for use in compliance monitoring.

J. Congressional Review Act

The Congressional Review Act, 5 U.S.C. Section 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

. A major rule cannot take effect until 60 days after it is published in the

Federal Register

. This action is not a “major rule” as defined by 5 U.S. C Section 804(2). This rule will be effective April 11, 2007.

List of Subjects

40 CFR Part 122

Administrative practice and procedure, Confidential business information, Environmental protection, Hazardous substances, Reporting and recordkeeping requirements, Water pollution control.

40 CFR Part 136

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

40 CFR Part 141

Chemicals, Environmental protection, Incorporation by reference, Indians-lands, Intergovernmental relations, Radiation Protection, Reporting and recordkeeping requirements, Water supply.

40 CFR Part 143

Chemicals, Environmental protection, Incorporation by reference, Indians-lands, Water supply.

40 CFR Part 430

Environmental protection, Paper and paper products industry, Reporting and recordkeeping requirements, Waste treatment and disposal, Water pollution control.

40 CFR Part 455

Chemicals, Environmental protection, Packaging and containers, Pesticides and pests, Waste treatment and disposal, Water pollution control.

40 CFR Part 465

Coil coating industry, Environmental protection, Reporting and recordkeeping requirements, Waste treatment and disposal, Water pollution control.

Dated: July 21, 2006.

Stephen L. Johnson,

Administrator.

For the reasons set out in the preamble, title 40, chapter I of the Code of Federal Regulations, is amended as follows:

PART 122—EPA ADMINISTERED PERMIT PROGRAMS: THE NATIONAL POLLUTANT DISCHARGE ELIMINATION SYSTEM

1. The authority citation for Part 122 continues to read as follows:

Authority:

The Clean Water Act, 33 U.S.C. 1251

et seq.

2. Section 122.1 is amended by revising paragraph (a)(4) to read as follows:

§ 122.1

Purpose and Scope.

(a) * * *

(4) Regulatory provisions in Parts 125, 129, 133, 136 of this chapter and 40 CFR subchapter N and subchapter O of this chapter also implement the NPDES permit program.

3. Section 122.21 is amended as follows:

a. By revising paragraph (g)(7)(i).

b. By revising introductory text in paragraph (h)(4)(i).

c. By revising paragraph (j)(4)(viii).

§ 122.21

Application for a permit (applicable to State programs, see § 123.25)

(g) * * *

(7)

Effluent characteristics.

(i) Information on the discharge of pollutants specified in this paragraph (g)(7) (except information on storm water discharges which is to be provided as specified in § 122.26). When “quantitative data” for a pollutant are required, the applicant must collect a sample of effluent and analyze it for the pollutant in accordance with analytical methods approved under Part 136 of this chapter unless use of another method is required for the pollutant under 40 CFR subchapters N or O. When no analytical method is approved under Part 136 or required under subchapters N or O, the applicant may use any suitable method but must provide a description of the method. When an applicant has two or more outfalls with substantially identical effluents, the Director may allow the applicant to test only one outfall and report that quantitative data as applying to the substantially identical outfall. The requirements in paragraphs (g)(7)(vi) and (vii) of this section state that an applicant must provide quantitative data for certain pollutants known or believed to be present do not apply to pollutants present in a discharge solely as the result of their presence in intake water; however, an applicant must report such pollutants as present. When paragraph (g)(7) of this section requires analysis of pH, temperature, cyanide, total phenols, residual chlorine, oil and grease, fecal coliform (including

E. coli

), and Enterococci (previously known as fecal streptococcus at § 122.26 (d)(2)(iii)(A)(3)), or volatile organics, grab samples must be collected for those pollutants. For all other pollutants, a 24-hour composite sample, using a minimum of four (4) grab samples, must be used unless specified otherwise at 40 CFR Part 136. However, a minimum of one grab sample may be taken for effluents from holding ponds or other impoundments with a retention period greater than 24 hours. In addition, for discharges other than storm water discharges, the Director may waive composite sampling for any outfall for which the applicant demonstrates that the use of an automatic sampler is infeasible and that the minimum of four (4) grab samples will be a representative sample of the effluent being discharged. Results of analyses of individual grab samples for any parameter may be averaged to obtain the daily average. Grab samples that are not required to be analyzed immediately (see Table II at 40 CFR 136.3 (e)) may be composited in the laboratory, provided that container, preservation, and holding time requirements are met (see Table II at 40 CFR 136.3 (e)) and that sample integrity is not compromised by compositing.

(h) * * *

(4) * * *

(i) Quantitative data for the pollutants or parameters listed below, unless testing is waived by the Director. The quantitative data may be data collected over the past 365 days, if they remain representative of current operations, and must include maximum daily value, average daily value, and number of measurements taken. The applicant must collect and analyze samples in accordance with 40 CFR Part 136. When analysis of pH, temperature, residual chlorine, oil and grease, or fecal coliform (including

E. coli

), and Enterococci (previously known as fecal streptococcus) and volatile organics is required in paragraphs (h)(4)(i)(A) through (K) of this section, grab samples must be collected for those pollutants. For all other pollutants, a 24-hour composite sample, using a minimum of four (4) grab samples, must be used unless specified otherwise at 40 CFR Part 136. For a composite sample, only one analysis of the composite of aliquots is required. New dischargers must include estimates for the pollutants or parameters listed below instead of actual sampling data, along with the source of each estimate. All levels must be reported or estimated as concentration and as total mass, except for flow, pH, and temperature.

(j) * * *

(4) * * *

(viii) Applicants must collect samples of effluent and analyze such samples for pollutants in accordance with analytical methods approved under 40 CFR Part 136 unless an alternative is specified in the existing NPDES permit. When analysis of pH, temperature, cyanide, total phenols, residual chlorine, oil and grease, fecal coliform (including

E. coli

), or volatile organics is required in paragraphs (j)(4)(ii) through (iv) of this section, grab samples must be collected for those pollutants. For all other pollutants, 24-hour composite samples must be used. For a composite sample, only one analysis of the composite of aliquots is required.

4. Section 122.41 is amended by revising paragraphs (j)(4) and (l)(4)(ii) to read as follows:

§ 122.41

Conditions applicable to all permits (applicable to State programs, see § 123.25).

(j) * * *

(4) Monitoring must be conducted according to test procedures approved under 40 CFR Part 136 unless another method is required under 40 CFR subchapters N or O.

(l) * * *

(4) * * *

(ii) If the permittee monitors any pollutant more frequently than required by the permit using test procedures approved under 40 CFR Part 136, or another method required for an industry-specific waste stream under 40 CFR subchapters N or O, the results of such monitoring shall be included in the calculation and reporting of the data submitted in the DMR or sludge reporting form specified by the Director.

5. Section 122.44 is amended by revising paragraph (i)(1)(iv) to read as follows:

§ 122.44

Establishing limitations, standards, and other permit conditions (applicable to State NPDES programs; see § 123.25).

(i) * * *

(1) * * *

(iv) According to test procedures approved under 40 CFR Part 136 for the analyses of pollutants or another method is required under 40 CFR subchapters N or O. In the case of pollutants for which there are no approved methods under 40 CFR Part 136 or otherwise required under 40 CFR subchapters N or O, monitoring must be conducted according to a test procedure specified in the permit for such pollutants.

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

6. 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.)

7. Section 136.3 is amended as follows:

a. In paragraph (a) by revising the introductory text and Tables IA, IB, IC, ID, and IE.

b. In paragraph (a) by adding Table IG after the notes of Table IF.

c. In paragraph (b) by revising references 6, 10, and 17, and adding references 63 through 69.

d. By revising paragraphs (c), (d), and (e).

§ 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, and IG. 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 text of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, IF, and IG. The incorporation by reference of these documents, as specified in paragraph (b) of this section, was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed in paragraph (b) of this section. You can get information about obtaining these documents from the EPA Office of Water Engineering and Analysis Division at 202-566-1000. Documents may be inspected at EPA’s Water Docket, EPA West, 1301 Constitution Avenue, NW., Washington, DC (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to:

http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html

These test procedures are incorporated as they exist on the day of approval and a notice of any change in these test procedures will be published in the

Federal Register

. 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, IE, IF, and IG 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 (b) or (c) of this section or 40 CFR 401.13) other test procedures may be used if such other test procedures have been previously approved by the Regional Administrator of the Region in which the discharge will occur, and the Director of the State in which such discharge will occur does not object to the use of an additional or alternate test procedure.

Table IA.—List of Approved Biological Methods

Parameter and units

Method

EPA

Standard

methods 18th, 19th, 20th Ed.

Standard

methods online

AOAC, ASTM, USGS

Other

Bacteria:

1. Coliform (fecal), number per 100 mL

Most Probable Number (MPN), 5 tube 3 dilution, or

p. 132

9221C or E

9221C or E-99

Membrane filter (MF)

, single step

p. 124

9222D

9222D-97

B-0050-85

2. Coliform (fecal) in presence of chlorine, number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 132

9221C or E

9221C or E-99

MF, single step

p. 124

9222D

9222D-97

3. Coliform (total), number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 114

9221B

9221B-99

, single step or two step

p. 108

9222B

9222B-97

B-0025-85

4. Coliform (total), in presence of chlorine, number per 100 mL

MPN, 5 tube, 3 dilution, or

p. 114

9221B

9221B-99

with enrichment

p. 111

9222 (B+B.5c)

9222 (B+B.5c)-97

5. E. coli, number per 100 mL

MPN

, multiple tube,

9221B.1/9221F

9221B.1-99/9221F

multiple tube/multiple well,

9223B

9223B-97

991.15

Colilert®

13,

Colilert-18®

13,

16,

MF two step, or

1103.1

9222B/9222G

, 9213D

9222B-97/9222G

D5392-93

single step

1603

, 1604

mColiBlue-24®

6. Fecal streptococci, number per 100 mL

MPN, 5 tube, 3 dilution,

p. 139

9230B

9230B-93

, or

p. 136

9230C

9230C-93

B-0055-85

Plate count

p. 143

7. Enterococci, number per 100 mL

MPN

multiple tube,

9230B

9230B-93

multiple tube/multiple well

D6503-99

Entero-lert®

13,

, two step

single step, or

Plate count

1106.1

1600

p. 143

9230C

9230C-93

D5259-92

Protozoa:

Crypto-sporidium

Filtration/IMS/FA

1622

, 1623

Giardia

Filtration/IMS/FA

1623

Aquatic Toxicity:

10. Toxicity, acute, fresh water organisms, LC

, percent effluent

Ceriodaphnia dubia

acute

2002.0

Daphnia puplex

and

Daphnia magna

acute

2021.0

Fathead Minnow,

Pimephales promelas,

and Bannerfin shiner,

Cyprinella leedsi,

acute

2000.0

Rainbow Trout,

Oncorhynchus mykiss,

and brook trout,

Salvelinus fontinalis,

acute

2019.0

11. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC

, percent effluent

Mysid,

Mysidopsis bahia,

acute

2007.0

Sheepshead Minnow,

Cyprinodon variegatus,

acute

2004.0

Silverside,

Menidia beryllina, Menidia menidia,

and

Menidia peninsulae,

acute

2006.0

12. Toxicity, chronic, fresh water organisms, NOEC or IC

, percent effluent

Fathead minnow,

Pimephales promelas,

larval survival and growth

1000.0

Fathead minnow,

Pimephales promelas,

embryo-larval survival and teratogenicity

1001.0

Daphnia,

Ceriodaphnia dubia,

survival and reproduction

1002.0

Green alga,

Selenastrum capricornutum,

growth

1003.0

13. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC

, percent effluent

Sheepshead minnow,

Cyprinodon variegatus,

larval survival and growth

1004.0

Sheepshead minnow,

Cyprinodon variegatus,

embryo-larval survival and teratogenicity

1005.0

Inland silverside,

Menidia beryllina,

larval survival and growth

1006.0

Mysid,

Mysidopsis bahia,

survival, growth, and fecundity

1007.0

Sea urchin,

Arbacia punctulata,

fertilization

1008.0

The method must be specified when results are reported.

A 0.45-μ 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.

USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.

[Reserved]

USGS. 1989. 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, U.S. Geological Survey, U.S. Department of Interior, Reston, VA.

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.

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.

When the MF method has not been used previously to test ambient waters with high turbidity, large number 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.

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.

ASTM. 2000, 1999, 1996.

Annual Book of ASTM Standards—Water and Environmental Technology.

Section 11.02. ASTM International. 100 Barr Harbor Drive, West Conshohocken, PA 19428.

AOAC. 1995.

Official Methods of Analysis of AOAC International,

16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.

The multiple-tube fermentation test is used in 9221B.1. 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.

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.

After prior enrichment in a presumptive medium for total coliform using 9221B.1, 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. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 μg/mL of MUG may be used.

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

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.

Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.

A description of the mColiBlue24® test, Total Coliforms and

E. coli,

is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.

Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA MUG media.

USEPA. 2002. Method 1103.1:

Escherichia coli

(

E. coli

) In Water By Membrane Filtration Using membrane-Thermotolerant

Escherichia coli

Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-020.

USEPA. 2002. Method 1603:

Escherichia coli

(

E. coli

) In Water By Membrane Filtration Using Modified membrane-Thermotolerant

Escherichia coli

Agar ( modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-023.

Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner

et al.

1993. “New Medium for the Simultaneous Detection of Total Coliform and

Escherichia coli

in Water.” Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604: Total Coliforms and

Escherichia coli

(

E. coli

) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA 821-R-02-024.

A description of the Enterolert® test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.

USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-021.

USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-β-D-Glucoside Agar (mEI). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-022.

Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of

Cryptosporidium.

USEPA. 2001. Method 1622:

Cryptosporidium

in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-01-026.

Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of

Cryptosporidium

and

Giardia

oocysts and cysts. USEPA. 2001. Method 1623.

Cryptosporidium

and

Giardia

in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-01-025.

Recommended for enumeration of target organism in ambient water only.

USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/012.

USEPA. October 2002. 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.

USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/014.

Table IB.—List of Approved Inorganic Test Procedures

Parameter

Methodology

Reference (method number or page)

EPA

35,

Standard methods

(18th, 19th)

Standard methods

(20th)

Standard methods

online

ASTM

USGS/AOAC/other

1. Acidity, as CaCO

, mg/L

Electrometric endpoint or phenolphthalein endpoint

2310 B(4a)

2310 B(4a)-97

D1067-92, 02

I-1020-85

2. Alkalinity, as CaCO

, mg/L

Electrometric or Colorimetric titration to pH 4.5, manual, or

2320 B

2320 B-97

D1067-92, 02

973.43

, I-1030-85

automatic

310.2 (Rev. 1974)

I-2030-85

3. Aluminum—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

I-3051-85

AA furnace

3113 B

3113 B-99

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-9750

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

Direct Current Plasma (DCP)

D4190-94, 99

See footnote

Colorimetric (Eriochrome cyanine R)

3500-Al D

3500-Al B

3500-Al B-01

4. Ammonia (as N), mg/L

Manual, distillation (at pH 9.5)

followed by:

350.1, Rev. 2.0 (1993)

4500-NH B

4500-NH

B-97

973.49

Nesslerization

4500-NH

C (18th only)

D1426-98, 03 (A)

973.49

, I-3520-85

Titration

4500-NH

C (19th) and 4500-NH

E (18th)

4500-NH

C-97

Electrode

4500-NH

D or E (19th) and 4500-NH

F or G (18th)

4500-NH

D or E

4500-NH

D or E-97

D1426-98, 03 (B)

Automated phenate, or

350.1

, Rev. 2.0 (1993)

4500-NH

G (19th) and 4500-NH

H (18th)

4500-NH

G-97

I-4523-85

Automated electrode

See footnote 7

Ion Chromatography

D6919-03

5. Antimony—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

AA furnace

3113 B

3113 B-99

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

6. Arsenic—Total,

mg/L

Digestion

followed by

206.5 (Issued 1978)

AA gaseous hydride

3114 B 4.d

3114 B 4.d-97

D2972-97, 03 (B)

I-3062-85

AA furnace

3113 B

3113 B-99

D2972-97, 03 (C)

I-4063-98

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

Colorimetric (SDDC)

3500-As C

3500-As B

3500-As B-97

D2972-97, 03 (A)

I-3060-85

7. Barium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

I-3084-85

AA furnace

3113 B

3113 B-99

D4382-95, 02

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

See footnote

8. Beryllium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

D3645-93 (88), 03 (A)

I-3095-85

AA furnace

3113 B

3113 B-99

D3645-93 (88), 03 (B)

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP, or

D4190-94, 99

See footnote

Colorimetric (aluminon)

3500-Be D

9. Biochemical oxygen demand (BOD

), mg/L

Dissolved Oxygen Depletion

5210 B

5210 B-01

973.44,

p. 17.

, I-1578-78

10. Boron—Total,

mg/L

Colorimetric (curcumin)

4500-B B

4500-B B-00

I-3112-85

ICP/AES, or

200.7, Rev. 4.4 (1994)

3120 B

3120 B 99

I-4471-97

DCP

D4190-94, 99

See footnote 34

11. Bromide, mg/L

Titrimetric

D1246-95, 99 (C)

p. S44.

I-1125-85

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev. 2

12. Cadmium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D3557-95, 02 (A or B)

974.27,

p. 37.

, I-3135-85

or I-3136-85

AA furnace

3113 B

3113 B-99

D3557-95, 02 (D)

I-4138-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-1472-85

or I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

D4190-94, 99

See footnote

Voltametry

, or

D3557-95, 02 (C)

Colorimetric (Dithizone)

3500-Cd D

13. Calcium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

D511-93, 03(B)

I-3152-85

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

DCP, or

See footnote

Titrimetric (EDTA)

3500-Ca D

3500-Ca B

3500-Ca B-97

D511-93, 03(A)

Ion Chromatography

D6919-03

14. Carbonaceous biochemical oxygen demand (CBOD

), mg/L

Dissolved Oxygen Depletion with nitrification inhibitor

5210 B

5210 B-01

15. Chemical oxygen demand (COD), mg/L

Titrimetric

410.3 (Rev. 1978)

5220 C

5220 C-97

D1252-95, 00 (A)

973.46

, p. 17

I-3560-85

Spectrophotometric, manual or automatic

410.4, Rev. 2.0 (1993)

5220 D

5220 D-97

D1252-95, 00 (B)

See footnotes

13, 14

. I-3561-85

16. Chloride, mg/L

Titrimetric: (silver nitrate) or

4500-Cl-B

4500-Cl-B-97

D512-89(99) (B)

I-1183-85

(Mercuric nitrate)

4500-Cl-C

4500-Cl-C-97

D512-89 (99) (A)

973.51

, I-1184-85

Colorimetric: manual or

I-1187-85

Automated (Ferricyanide)

4500-Cl-E

4500-Cl-E-97

I-2187-85

Potentiometric Titration

4500-Cl-D

4500-Cl-D-97

Ion Selective Electrode

D512-89(99)(C)

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev. 2

17. Chlorine—Total residual, mg/L; Titrimetric

Amperometric direct, or

4500-Cl D

4500-Cl D-00

D1253-86 (96), 03

Amperometric direct (low level)

4500-Cl E

4500-Cl E-00

Iodometric direct

4500-Cl B

4500-Cl B-00

Back titration ether end-point

4500-Cl C

4500-Cl C-00

DPD-FAS

4500-Cl F

4500-Cl F-00

Spectrophotometric, DPD or

4500-Cl G

4500-Cl G-00

Electrode

See footnote

18. Chromium VI dissolved, mg/L

0.45-micron Filtration followed by:

AA chelation-extraction or

3111 C

3111 C-99

I-1232-85

Ion Chromatography

218.6, Rev. 3.3 (1994)

3500-Cr E

3500-Cr C

3500-Cr C-01

D5257-97

993.23

Colorimetric (Diphenyl-carbazide)

3500-Cr D

3500-Cr B

3500-Cr B-01

D1687-92, 02 (A)

I-1230-85

19. Chromium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

D1687-92, 02 (B)

974.27

, I-3236-85

AA chelation-extraction

3111 C

3111 C-99

AA furnace

3113 B

3113 B-99

D1687-92, 02 (C)

I-3233-93

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP,

D4190-94, 99

See footnote

Colorimetric (Diphenyl-carbazide)

3500-Cr D

3500-Cr B

3500-Cr B-01

20. Cobalt—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D3558-94, 03 (A or B)

p. 37

, I-3239-85

AA furnace

3113 B

3113 B-99

D3558-94, 03 (C)

I-4243-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

D4190-94, 99

See footnote

21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity

Colorimetric (ADMI), or

2120 E

See footnote

(Platinum cobalt), or

2120 B

2120 B-01

I-1250-85

Spectrophotometric

2120 C

22. Copper—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D1688-95, 02 (A or B)

974.27

p. 37

I-3270-85

or I-3271-85

AA furnace

3113 B

3113 B-99

D1688-95, 02 (C)

I-4274-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

D4190-94, 99

See footnote

Colorimetric (Neocuproine) or

3500-Cu D

3500-Cu B

3500-Cu B-99

(Bicinchoninate)

3500-Cu E

3500-Cu C

3500-Cu C-99

See footnote

23. Cyanide—Total, mg/L

Automated Distillation and Colorimetry, or

Kelada-01

Manual distillation with MgCl

followed by:

335.4, Rev. 1.0 (1993)

4500-CN

D2036-98(A)

10-204-00-1-X

Titrimetric or

4500-CN

D-99

p. 22

Spectrophotometric, manual or

4500-CN

E-99

D2036-98(A)

I-3300-85

Automated

335.4, Rev. 1.0 (1993)

10-204-00-1-X

, I-4302-85

Ion Selective Electrode

4500-CN

F-99

D2036-98(A)

24. Available Cyanide, mg/L

Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl

followed by Titrimetric or Spectrophotometric

4500-CN

G-99

D2036-98(B)

Flow injection and ligand exchange, followed by amperometry

D6888-04

OIA-1677

Automated Distillation and Colorimetry

Kelada-01

25. Fluoride—Total, mg/L

Manual distillation

followed by:

4500-F

B-97

Electrode, manual or

4500-F

C-97

D1179-93, 99 (B)

Automated

I-4327-85

Colorimetric, (SPADNS) or

4500-F

D-97

D1179-93, 99 (A)

Automated complexone

4500-F

E-97

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97,03

993.30

CIE/UV

D6508, Rev. 2

26. Gold—Total,

mg/L

Digestion

followed by:

AA direct aspiration, or

3111 B

3111 B-99

AA furnace, or

231.2 (Rev. 1978)

DCP

See footnote

27. Hardness—Total, as CaCO

, mg/L

Automated colorimetric,

130.1 (Issued 1971)

Titrimetric (EDTA) or

2340 B or C

2340 B or C-97

D1126-86(92), 02

973.5 2B

, I-1338-85

Ca plus Mg as their carbonates, by inductively coupled plasma or AA direct aspiration. (See Parameters 13 and 33).

28. Hydrogen ion (pH), pH units

Electrometric measurement or

4500-H

B-00

D1293-84 (90), 99 (A or B)

973.41.

, I-1586-85

Automated electrode

150.2 (Dec. 1982)

See footnote

, I-2587-85

29. Iridium—Total,

mg/L

Digestion

followed by:

AA direct aspiration or

3111 B

3111 B-99

AA furnace

235.2 (Issued 1978)

30. Iron—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D1068-96, 03 (A or B)

974.27

, I-3381-85

AA furnace

3113 B

3113 B-99

D1068-96, 03 (C)

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

DCP

D4190-94, 99

See footnote

Colorimetric (Phenanthroline)

3500-Fe D

3500-Fe B

3500-Fe B-97

D1068-96, 03 (D)

See footnote

31. Kjeldahl Nitrogen

—Total, (as N), mg/L

Digestion and distillation followed by:

4500-N

org

B or C and 4500-NH

4500-N

org

B or C and 4500-NH

4500-N

org

B or C-97 and 4500-NH

B-97

D3590-89, 02 (A)

Titration or

4500-NH

C (19th) and 4500-NH

E (18th)

4500-NH

C-97

D3590-89, 02 (A)

973.48

Nesslerization or

4500-NH

C (18th Only)

D3590-89, 02 (A)

Electrode

4500-NH

F or G (18th) and 4500-NH

D or E (19th)

4500-NH

D or E

4500-NH

D or E-97

Automated phenate colorimetric

351.1 (Rev. 1978)

I-4551-78

Semi-automated block digestor colorimetric

351.2, Rev. 2.0 (1993)

D3590-89, 02 (B)

I-4515-91

Manual or block digestor potentiometric

D3590-89, 02 (A)

Block digester, followed by Auto distillation and Titration, or

See footnote

Nesslerization, or

See footnote

Flow injection gas diffusion

See footnote

32. Lead—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D3559-96, 03 (A or B)

974.27

, I-3399-85

AA furnace

3113 B

3113 B-99

D3559-96, 03 (D)

I-4403-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

D4190-94, 99

See footnote

Voltametry

D3559-96, 03 (C)

Colorimetric (Dithizone)

3500-Pb D

3500-Pb B

3500-Pb B-97

33. Magnesium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

D511-93, 03(B)

974.27

, I-3447-85

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

DCP or

See footnote

Gravimetric

3500-Mg D

Ion Chromatography

D6919-03

34. Manganese—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

D858-95, 02 (A or B)

974.27

, I-3454-85

AA furnace

3113 B

3113 B-99

D858-95, 02 (C)

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP36, or

D4190-94, 99

See footnote

Colorimetric (Persulfate), or

3500--Mn D

3500-Mn B

3500-Mn B-99

920.203

(Periodate)

See footnote

35. Mercury—Total

, mg/L

Cold vapor, manual or

245.1, Rev. 3.0 (1994)

3112 B

3112 B-99

D3223-97, 02

977.22

, I-3462-85

Automated

245.2 (Issued 1974)

Cold vapor atomic fluorescence spectrometry (CVAFS)

245.7 Rev. 2.0 (2005)

Purge and Trap CVAFS

1631E

36. Molybdenum—Total

, mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

I-3490-85

AA furnace

3113 B

3113 B-99

I-3492-96

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

See footnote

37. Nickel—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D1886-90, 94 (98) (A or B)

I-3499-85

AA furnace

3113 B

3113 B-99

D1886-90, 94 (98) (C)

I-4503-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

, or

D4190-94, 99

See footnote

Colorimetric (heptoxime)

3500-Ni D (17th Edition)

38. Nitrate (as N), mg/L

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev. 2

Ion Selective Electrode

4500-NO

D-00

Colorimetric (Brucine sulfate), or

352.1

973.50

, 419D

, p. 28

Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40).

39. Nitrate-nitrite (as N), mg/L

Cadmium reduction, manual or

4500-NO

4500-NO3

E-00

D3867-99(B)

Automated, or

353.2, Rev. 2.0 (1993)

4500-NO

F-00

D3867-99(A)

I-4545-85

Automated hydrazine

4500-NO

H-00

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97

993.30

CIE/UV

D6508, Rev. 2

40. Nitrite (as N), mg/L

Spectrophotometric: Manual or

4500-NO

B-00

See footnote

Automated (Diazotization)

I-4540-85

Automated (*bypass cadmium reduction)

353.2, Rev. 2.0 (1993)

4500-NO

F-00

D3867-99(A)

I-4545-85

Manual (*bypass cadmium reduction)

4500-NO

E-00

D3867-99(B)

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev.2

41. Oil and grease—Total recoverable, mg/L

Hexane extractable material (HEM): n-Hexane extraction and gravimetry

1664A

5520 B

5520 B-01

Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry.

1664A

42. Organic carbon—Total (TOC), mg/L

Combustion or oxidation

5310 B, C, or D

5310 B, C, or D-00

D2579-93 (A or B)

973.47,

p. 14

43. Organic nitrogen (as N), mg/L

Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4)

44. Orthophosphate (as P), mg/L

Ascorbic acid method:

Automated, or

365.1, Rev. 2.0 (1993)

4500-P F

973.56

, I-4601-85

Manual single reagent

4500-P E

D515-88(A)

973.55

Manual two reagent

365.3 (Issued 1978)

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev. 2

45. Osmium—Total

, mg/L

Digestion

followed by:

AA direct aspiration, or

3111 D

3111 D-99

AA furnace

252.2 (Issued 1978)

46. Oxygen, dissolved, mg/L

Winkler (Azide modification), or

4500-O C

4500-O C-01

D888-92, 03 (A)

973.4 5B

, I-1575-78

Electrode

4500-O G

4500-O G-01

D888-92, 03 (B)

I-1576-78

47. Palladium—Total,

mg/L

Digestion

followed by:

AA direct aspiration, or

3111 B

3111 B-99

p. S27

AA furnace

253.2

(Issued 1978)

p. S28

DCP

See footnote

48. Phenols, mg/L

Manual distillation

Followed by:

420.1

(Rev. 1978)

See footnote

Colorimetric (4AAP) manual, or

420.1

(Rev. 1978)

See footnote

Automated

420.4 Rev. 1.0 (1993)

49. Phosphorus (elemental), mg/L

Gas-liquid chromatography

See footnote

50. Phosphorus—Total, mg/L

Persulfate digestion followed by:

4500-P B.5

973.55

Manual or

365.3

(Issued 1978)

4500-P E

D515-88(A)

Automated ascorbic acid reduction

365.1 Rev. 2.0 (1993)

4500-P F

973.56

, I-4600-85

Semi-automated block digestor

365.4

(Issued 1974)

D515-88(B)

I-4610-91

51. Platinum—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

AA furnace

255.2

DCP

See footnote

52. Potassium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

973.53

, I-3630-85

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

Flame photometric, or

3500-K D

3500-K B

3500-K B-97

Colorimetric

317 B

Ion Chromatography

D6919-03

53. Residue—Total, mg/L

Gravimetric, 103-105°

2540 B

2540 B-97

I-3750-85

54. Residue—filterable, mg/L

Gravimetric, 180°

2540 C

2540 C-97

I-1750-85

55. Residue—non-filterable (TSS), mg/L

Gravimetric, 103-105 °C post washing of residue

2540 D

2540 D-97

I-3765-85

56. Residue—settleable, mg/L

Volumetric, (Imhoff cone), or gravimetric

2540 F

2540 F-97

57. Residue—Volatile, mg/L

Gravimetric, 550 °C

160.4

I-3753-85

58. Rhodium—Total,

mg/L

Digestion

followed by:

AA direct aspiration, or

3111 B

3111 B-99

AA furnace

265.2

59. Ruthenium—Total,

mg/L

Digestion

followed by:

AA direct aspiration, or

3111 B

3111 B-99

AA furnace

267.2

60. Selenium—Total,

mg/L

Digestion

followed by:

AA furnace

3113 B

3113 B-99

D3859-98, 03 (B)

I-4668-98

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

AA gaseous hydride

3114 B

3114 B-97

D3859-98, 03 (A)

I-3667-85

61. Silica—Dissolved,

mg/L

0.45 micron filtration followed by:

Colorimetric, Manual or

4500-Si D

4500-SiO

C-97

D859-94, 00

I-1700-85

Automated (Molybdosilicate), or

I-2700-85

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

62. Silver—Total,

4, 31

mg/L

Digestion

4, 29

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

974.27

, p. 37

, I-3720-85

AA furnace

3113 B

3113 B-99

I-4724-89

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP

See footnote

63. Sodium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

973.54

, I-3735-85

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

DCP, or

See footnote

Flame photometric

3500-Na D

3500-Na B

3500-Na B-97

Ion Chromatography

D 6919-03

64. Specific conductance, micromhos/cm at 25°C

Wheatstone bridge

120.1

(Rev. 1982)

2510 B

2510 B-97

D1125-95 (99) (A)

973.40

, I-2781-85

65. Sulfate (as SO

), mg/L

Automated colorimetric

375.2, Rev. 2.0 (1993)

Gravimetric

4500-SO

C or D

4500-SO

C or D

925.54

Turbidimetric

D516-90, 02

426C

Ion Chromatography

300.0, Rev 2.1 (1993) and 300.1, Rev 1.0 (1997)

4110 B

4110 B-00

D4327-97, 03

993.30

CIE/UV

D6508, Rev. 2

66. Sulfide (as S), mg/L

Titrimetric (iodine), or

4500-S

F (19th) 4500-S

E (18th)

4500-S

F-00

I-3840-85

Colorimetric (methylene blue)

4500-S

D-00

Ion Selective Electrode

4500-S

G-00

D4658-03

67. Sulfite (as SO

), mg/L

Titrimetric (iodine-iodate)

4500-SO

B-00

68. Surfactants, mg/L

Colorimetric (methylene blue)

5540 C

5540 C-00

D2330-88, 02

69. Temperature, °C

Thermometric

2550 B

2550 B-00

See footnote

70. Thallium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

AA furnace

279.2

(Issued 1978)

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

71. Tin—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 B

3111 B-99

I-3850-78

AA furnace, or

3113 B

3113 B-99

STGFAA

200.9, Rev. 2.2 (1994)

ICP/AES

200.7, Rev. 4.4 (1994)

72. Titanium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

AA furnace

283.2

(Issued 1978)

DCP

See footnote

73. Turbidity, NTU

Nephelometric

180.1, Rev. 2.0 (1993)

2130 B

2130 B-01

D1889-94, 00

I-3860-85

74. Vanadium—Total,

mg/L

Digestion

followed by:

AA direct aspiration

3111 D

3111 D-99

AA furnace

D3373-93, 03

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP, or

D4190-94, 99

See footnote

Colorimetric (Gallic Acid)

3500-V D

3500-V B

3500-V B-97

75. Zinc -Total

, mg/L

Digestion

followed by:

AA direct aspiration

3111 B or C

3111 B or C-99

D1691-95, 02 (A or B)

974.27

, p. 37

, I-3900-85

AA furnace

289.2

(Issued 1978)

ICP/AES

200.7, Rev. 4.4 (1994)

3120 B

3120 B-99

I-4471-97

ICP/MS

200.8, Rev. 5.4 (1994)

D5673-03

993.14

DCP,

D4190-94, 99

See footnote

Colorimetric (Dithizone) or

3500-Zn E

(Zincon)

3500-Zn F

3500-Zn B

3500-Zn B-97

See footnote

Table 1B Notes:

“Methods for Chemical Analysis of Water and Wastes,” Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI), EPA-600/4-79-020 (NTIS PB 84-128677), Revised March 1983 and 1979 where applicable.

Fishman, M. J.,

et al.

“Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,” U.S. Department of the Interior, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.

“Official Methods of Analysis of the Association of Official Analytical Chemists,” Methods Manual, Sixteenth Edition, 4th Revision, 1998.

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 the 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.

Copper sulfate may be used in place of mercuric sulfate.

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.

Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.

The approved method is that cited in “Methods for Determination of Inorganic Substances in Water and Fluvial Sediments”, USGS TWRI, Book 5, Chapter A1 (1979).

American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd st., New York, NY 10036.

“Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,” Supplement to the Fifteenth Edition of

Standard Methods for the Examination of Water and Wastewater

(1981).

The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.

Carbonaceous biochemical oxygen demand (CBOD

) must not be confused with the traditional BOD

test method which measures “total BOD.” The addition of the nitrification inhibitor is not a procedural option, but must be included to report the CBOD

parameter. A discharger whose permit requires reporting the traditional BOD

may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's permit specifically states CBOD

is required can the permittee report data using a nitrification inhibitor.

OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.

Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.

The back titration method will be used to resolve controversy.

Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.

The approved method is that cited in

Standard Methods for the Examination of Water and Wastewater,

14th Edition, 1976.

National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971.

Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.

When using a method with block digestion, this treatment is not required.

Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.

Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.

Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.

Wershaw, R. L.,

et al.

, “Methods for Analysis of Organic Substances in Water,” Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14.

Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.

Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.

The approved method is cited in

Standard Methods for the Examination of Water and Wastewater,

14th Edition. The colorimetric reaction is conducted at a pH of 10.0±0.2. The approved methods are given on pp 576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 510C for the manual spectrometric procedure.

R.F. Addison and R. G. Ackman, “Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,”

Journal of Chromatography,

Vol. 47, No.3, pp. 421-426, 1970.

Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M Na

and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.

The approved method is that cited in

Standard Methods for the Examination of Water and Wastewater,

15th Edition.

For samples known or suspected to contain high levels of silver (

e.g.

, in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH

OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I

to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH

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.

Stevens, H.H., Ficke, J. F., and Smoot, G. F., “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.

Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.

“Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,” 1986—Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin, MA 02038

Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC method for arsenic are provided in Appendix D of this part titled, “Precision and Recovery Statements for Methods for Measuring Metals.”

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”, CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation.

When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.

Only use n-hexane extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664A). Use of other extraction solvents (

e.g.,

those in the 18th and 19th editions) is prohibited.

Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.

Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.

Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.

Method 1664, Revision A “

-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated

-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry” EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161.

USEPA. 2001. Method 1631, Revision E, “Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry” September 2002, Office of Water, U.S. Environmental Protection Agency (EPA-821-R-02-024). The application of clean techniques described in EPA's draft 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.

Available Cyanide, Method OIA-1677, “Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,” ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842-9010.

“Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method,” Open File Report (OFR) 00-170.

“Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry,” Open File Report (OFR) 93-449.

“Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry,” Open File Report (OFR) 97-198.

“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” Open File Report (OFR) 92-146.

“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” Open File Report (OFR) 98-639.

“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,” Open File Report (OFR) 98-165.

“Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment,” Open File Report (OFR) 93-125.

All EPA methods, excluding EPA Method 300.1, are published in “Methods for the Determination of Metals in Environmental Samples,” Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/R-94/111, May 1994; and “Methods for the Determination of Inorganic Substances in Environmental Samples,” NERL-CI, EPA/600/R-93/100, August, 1993. EPA Method 300.1 is available from

http://www.epa.gov/safewater/methods/pdfs/met300.pdf.

Styrene divinyl benzene beads (

e.g.

AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCal

or equivalent) are acceptable substitutes for formazin.

Method D6508, Rev. 2, “Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,” available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.

Kelada-01, “Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,” EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. The toll free telephone number is: 800-553-6847. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.

QuikChem Method 10-204-00-1-X, “Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis” is available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414-358-4200.

When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to distillation.

Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation “followed by” analysis with a method, approved digestion and/or distillation are required prior to analysis.

Method 245.7, Rev. 2.0, “Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,” February 2005, EPA-821-R-05-001, available from the U.S. EPA Sample Control Center (operated by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100, Fax: 703-461-8056.

The use of EDTA may decrease method sensitivity in some samples. Analysts may omit EDTA provided that all method specified quality control acceptance criteria are met.

Samples analyzed for available cyanide using Methods OIA-1677 or D6888-04 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples.

Table IC.—List of Approved Test Procedures for Non-Pesticide Organic Compounds

Parameter

EPA method number

GC/MS

HPLC

Other approved methods

Standard Methods

[Edition(s)]

Standard Methods

Online

ASTM

Other

1. Acenaphthene

610

625, 1625B

610

6440 B [18th, 19th, 20th]

D4657-92 (99)

See footnote

, p. 27

2. Acenaphthylene

610

625, 1625B

610

6410 B, 6440 B, [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

3. Acrolein

603

624

, 1624B

4. Acrylonitrile

603

624

, 1624B

5. Anthracene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

6. Benzene

602

624, 1624B

6200 B [20th] and 6210 B [18th,19th], 6200 C [20th] and 6220 B [18th,19th]

6200 B and C-97

7. Benzidine

625

, 1625B

605

See footnote

, p.1

8. Benzo(a)anthracene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

9. Benzo(a)pyrene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

10. Benzo(b)fluoranthene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

11. Benzo(g,h,i) perylene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

12. Benzo(k) fluoranthene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

13. Benzyl chloride

See footnote

, p. 130: See footnote

, p. S102

14. Benzyl butyl phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

15. Bis(2-chloroethoxy) methane

611

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

16. Bis(2-chloroethyl) ether

611

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

17. Bis(2-ethylhexyl) phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

18. Bromodichloro-methane

601

624, 1624B

6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th]

6200 B and C-97

19. Bromoform

601

624, 1624B

6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th]

6200 B and C-97

20. Bromomethane

601

624, 1624B

6200 C [20th] and 6230 B [18th, 19th], 6200 B [20th] and 6210 B [18th, 19th]

6200 B and C-97

21. 4-Bromophenyl phenyl ether

611

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

22. Carbon tetrachloride

601

624, 1624B

6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

See footnote

, p. 130

23. 4-Chloro-3-methyl phenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

24. Chlorobenzene

601, 602

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

See footnote

, p. 130

25. Chloroethane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

26. 2-Chloroethylvinyl ether

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

27. Chloroform

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

See footnote

, p. 130

28. Chloromethane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th] 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

29. 2-Chloronaph-thalene

612

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

30. 2-Chlorophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B(00, 6420 B-00

See footnote

, p. 27

31. 4-Chlorophenyl phenyl ether

611

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

32. Chrysene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

33. Dibenzo(a,h)an-thracene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

34. Dibromochloro-methane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th] 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

35. 1,2-Dichloro-benzene

601, 602

624, 1625B

6200 C [20th] and 6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

See footnote

, p. 27

36. 1,3-Dichloro-benzene

601, 602

624, 1625B

6200 C [20th] and 6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

See footnote

, p. 27

37. 1,4-Dichloro-benzene

601, 602

624, 1625B

6200 C [20th] and 6220 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

See footnote

, p. 27

38. 3,3-Dichloro-benzidine

625, 1625B

605

6410 B [18th, 19th, 20th]

6410 B-00

39. Dichlorodifluoro-methane

601

6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

40. 1,1-Dichloroethane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

41. 1,2-Dichloroethane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

42. 1,1-Dichloroethene

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

43. trans-1,2-Dichloro-ethene

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

44. 2,4-Dichlorophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

45. 1,2-Dichloro-propane

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

46. cis-1,3-Dichloro-propene

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

47. trans-1,3-Dichloro-propene

601

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6230 B [18th, 19th]

6200 B and C-97

48. Diethyl phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

49. 2,4-Dimethylphenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

50. Dimethyl phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

51. Di-n-butyl phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

52. Di-n-octyl phthalate

606

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

53. 2,3-Dinitrophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

54. 2,4-Dinitrotoluene

609

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

55. 2,6-Dinitrotoluene

609

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

56. Epichlorohydrin

See footnote

, p. 130; See footnote

, p. S102

57. Ethylbenzene

602

624, 1624B

6200 B [20th] and 6210 B [18th, 19th], 6200 C [20th] and 6220 B [18th, 19th]

6200 B and C-97

58. Fluoranthene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

59. Fluorene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

60. 1,2,3,4,6,7,8-Heptachloro-dibenzofuran

1613B

61. 1,2,3,4,7,8,9-Heptachloro-dibenzofuran

1613B

62. 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin

1613B

63. Hexachlorobenzene

612

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

64. Hexachloro-butadiene

612

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

65. Hexachlorocyclo-pentadiene

612

625

, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

66. 1,2,3,4,7,8-Hexachlorodibenzofuran

1613B

67. 1,2,3,6,7,8-Hexachlorodibenzofuran

1613B

68. 1,2,3,7,8,9-Hexachlorodibenzofuran

1613B

69. 2,3,4,6,7,8-Hexachlorodibenzofuran

1613B

70. 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin

1613B

71. 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin

1613B

72. 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin 1613B

1613B

73. Hexachloroethane

612

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

74. Ideno(1,2,3-cd) pyrene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

75. Isophorone

609

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

76. Methylene chloride

601

624, 1624B

6200 C [20th] and 6230 B [18th, 19th]

6200 C-97

See footnote

, p. 130

77. 2-Methyl-4,6-dinitrophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

78. Naphthalene

610

625, 1625B

610

6410 B, 6440 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

79. Nitrobenzene

609

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

D4657-92 (99)

See footnote

, p. 27

80. 2-Nitrophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

81. 4-Nitrophenol

604

625, 1625B

6410 B, 6420 B [18th, 19th, 20th]

6410 B-00, 6420 B-00

See footnote

, p. 27

82. N-Nitrosodimethylamine

607

6255, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

83. N-Nitrosodi-n-propylamine

607

6255, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

84. N-Nitrosodiphenylamine

607

6255, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 27

85. Octachlorodibenzofuran

1613B

86. Octachlorodibenzo-p-dioxin

1613B

87. 2,2'-Oxybis(2-chloropropane) [also known as bis(2-chloroisopropyl) ether]

611

625, 1625B

6410 B [18th, 19th, 20th]

6410 B-00

88. PCB-1016

608

625

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 43; See footnote

89. PCB-1221

608

625

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 43; See footnote

90. PCB-1232

608

625

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 43; See footnote

91. PCB-1242

608

625

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 43; See footnote

92. PCB-1248

608

625

93. PCB-1254

608

625

6410 B [18th, 19th, 20th]

6410 B-00

See footnote

, p. 43; See footnote

94. PCB-1260

608

625

6410 B, 6630 B [18th, 19th, 20th]

6410 B-00

See footnote 3, p. 43; See footnote 8

95. 1,2,3,7,8-Pentachloro-dibenzofuran

1613B

96. 2,3,4,7,8-Pentachloro-dibenzofuran

1613B

97. 1,2,3,7,8,-Pentachlorodibenzo-

-dioxin

1613B

98. Pentachlo

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