Analysis and Sampling Procedures:

Federal Register: September 23, 2010 (Volume 75, Number 184)

Proposed Rules

Page 58023-58076

From the Federal Register Online via GPO Access [wais.access.gpo.gov]

DOCID:fr23se10-18

Page 58023

Part II

Environmental Protection Agency

40 CFR Parts 136, 260, 423, et al.

Guidelines Establishing Test Procedures for the Analysis of Pollutants

Under the Clean Water Act; Analysis and Sampling Procedures; Proposed

Rule

Page 58024

ENVIRONMENTAL PROTECTION AGENCY 40 CFR Parts 136, 260, 423, 430, and 435

EPA-HQ-OW-2010-0192; FRL-9189-4

RIN 2040-AF09

Guidelines Establishing Test Procedures for the Analysis of

Pollutants Under the Clean Water Act; Analysis and Sampling Procedures

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

SUMMARY: EPA is proposing changes to analysis and sampling test procedures in wastewater regulations. These changes will provide increased flexibility to the regulated community and laboratories in their selection of analytical methods (test procedures) for use in

Clean Water Act programs. The changes include proposal of EPA methods and methods published by voluntary consensus standard bodies, such as

ASTM International and the Standard Methods Committee and updated versions of currently approved methods. EPA is also proposing to add certain methods reviewed under the alternate test procedures program.

Further, EPA is proposing changes to the current regulations to clarify the process for EPA approval for use of alternate procedures for nationwide and Regional use. In addition, EPA is proposing minimum quality control requirements to improve consistency across method versions; corrections to previously approved methods; and changes to sample collection, preservation, and holding time requirements.

Finally, EPA is proposing changes to how EPA cites methods in three effluent guideline regulations.

DATES: EPA must receive your comments on this proposal on or before

November 22, 2010.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-OW- 2010-0192, by one of the following methods: http://www.regulations.gov: Follow the on-line instructions for submitting comments.

E-mail: OW-Docket@epa.gov, Attention Docket ID No. EPA-HQ-

OW-2010-0192.

Mail: Water Docket, U.S. Environmental Protection Agency,

Mailcode: 2822T, 1200 Pennsylvania Ave., NW., Washington, DC 20460.

Attention Docket ID No. EPA-HQ-OW-2010-0192. Please include a total of 3 copies.

Hand Delivery: Water Docket, EPA Docket Center, EPA West

Building Room 3334, 1301 Constitution Ave., NW., Washington, DC,

Attention Docket ID No. EPA-HQ-OW-2010-0192. Such deliveries are only accepted during the Docket's normal hours of operation, and special arrangements should be made for deliveries of boxed information by calling 202-566-2426.

Instructions: Direct your comments to Docket ID No. EPA-HQ-OW-2010- 0192. EPA's policy is that all comments received will be included in the public docket without change and may be made available online at http://www.regulations.gov, including any personal information provided, unless the comment includes information claimed to be

Confidential Business Information (CBI) or other information whose disclosure is restricted by statute. Do not submit information that you consider to be CBI or otherwise protected through http:// www.regulations.gov or e-mail. The http://www.regulations.gov Web site is an ``anonymous access'' system, which means EPA will not know your identity or contact information unless you provide it in the body of your comment. If you send an e-mail comment directly to EPA without going through http://www.regulations.gov your e-mail address will be automatically captured and included as part of the comment that is placed in the public docket and made available on the Internet. If you submit an electronic comment, EPA recommends that you include your name and other contact information in the body of your comment and with any disk or CD-ROM you submit. If EPA cannot read your comment due to technical difficulties and cannot contact you for clarification, EPA may not be able to consider your comment. Electronic files should avoid the use of special characters, any form of encryption, and be free of any defects or viruses.

Docket: All documents in the docket are listed in the http:// www.regulations.gov index. 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, will be publicly available only in hard copy.

Publicly available docket materials are available either electronically in http://www.regulations.gov or in hard copy at the Water Docket in the EPA 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 for the Water Docket is 202-566-2426.

FOR FURTHER INFORMATION CONTACT: Lemuel Walker, Engineering and

Analysis Division (4303T), USEPA Office of Science and Technology, 1200

Pennsylvania Ave., NW., Washington, DC 20460, 202-566-1077, (e-mail: walker.lemuel@epa.gov), or 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).

SUPPLEMENTARY INFORMATION:

  1. General Information 1. Does this action apply to me?

    This proposed rule could affect a number of different entities.

    Potential regulators may include EPA Regions, as well as States,

    Territories and Tribes authorized to implement the National Pollutant

    Discharge Elimination System (NPDES) program, and issue permits with conditions designed to ensure compliance with the technology-based and water quality-based requirements of the Clean Water Act (CWA). These permits may include restrictions on the quantity of pollutants that may be discharged as well as pollutant measurement and reporting requirements. If EPA has approved a test procedure for analysis of a specific pollutant, the NPDES permitee 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:

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    Examples of potentially regulated

    Category

    entities

    State, Territorial, and

    States, Territories, and Tribes

    Indian Tribal Governments.

    authorized to administer the NPDES permitting program; States, Territories, and Tribes providing certification under

    Clean Water Act section 401.

    Industry..................... Facilities that must conduct monitoring to comply with NPDES permits.

    Municipalities............... POTWs that must conduct monitoring to comply with NPDES permits.

    This table is not intended to be exhaustive, but rather provides a guide for readers regarding entities likely to be regulated by this action. This table lists types of entities that EPA is now aware that 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 136.1 (NPDES permits and CWA) and 40 CFR 403.1 (Pretreatment standards purpose and applicability). If you have questions regarding the applicability of this action to a particular entity, consult the appropriate person listed in the preceding FOR FURTHER INFORMATION CONTACT section.

  2. What should I consider as I prepare my comments for EPA? 1. Submitting Confidential Business Information (CBI). Do not submit this information to EPA through http://www.regulations.gov or e- mail. Clearly mark the part or all of the information that you claim to be CBI. For CBI information in a disk or CD-ROM that you mail to EPA, mark the outside of the disk or CD-ROM as CBI and then identify electronically within the disk or CD-ROM the specific information that is claimed as CBI. In addition to one complete version of the comment that includes information claimed as CBI, a copy of the comment that does not contain the information claimed as CBI must be submitted for inclusion in the public docket. Information so marked will not be disclosed except in accordance with procedures set forth in 40 CFR part 2. 2. Tips for Preparing Your Comments. When submitting comments, remember to:

    Identify the rulemaking by docket number and other identifying information (subject heading, Federal Register date and page number).

    Follow directions--The agency may ask you to respond to specific questions or organize comments by referencing a Code of

    Federal Regulations (CFR) part or section number.

    Explain why you agree or disagree, suggest alternatives, and substitute language for your requested changes.

    Describe any assumptions and provide any technical information and/or data that you used.

    If you estimate potential costs or burdens, explain how you arrived at your estimate in sufficient detail to allow for it to be reproduced.

    Provide specific examples to illustrate your concerns, and suggest alternatives.

    Explain your views as clearly as possible, avoiding the use of profanity or personal threats.

    Make sure to submit your comments by the comment period deadline identified.

  3. Abbreviations and Acronyms Used in the Preamble and Proposed Rule

    Text

    ASTM: ASTM International

    ATP: Alternate Test Procedure

    CFR: Code of Federal Regulations

    CWA: Clean Water Act

    EPA: Environmental Protection Agency

    FLAA: Flame Atomic Absorption Spectroscopy

    HRGC: High Resolution Gas Chromatography

    HRMS: High Resolution Mass Spectrometry

    ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy

    ICP/MS: Inductively Coupled Plasma-Mass Spectrometry

    MS: Mass Spectrometry

    NPDES: National Pollutant Discharge Elimination System

    QA: Quality Assurance

    QC: Quality Control

    SDWA: Safe Drinking Water Act

    SM: Standard Methods

    STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption

    Spectroscopy

    USGS: United States Geological Survey

    VCSB: Voluntary Consensus Standards Body

    WET: Whole Effluent Toxicity

    Table of Contents

    I. Statutory Authority

    II. Summary of Proposed Rule

  4. Changes to 40 CFR 136.3 To Include New EPA Methods and New

    Versions of Previously Approved EPA Methods

  5. Changes to 40 CFR 136.3 To Include New Standard Methods and

    New Versions of Approved Standard Methods

  6. Changes to 40 CFR 136.3 To Include New ASTM Methods or New

    Versions of Previously Approved ASTM Methods

  7. Changes to 40 CFR 136.3 To Include Alternate Test Procedures

  8. Clarifications and Corrections to Previously Approved Methods in 40 CFR 136.3

  9. Proposed Revisions in Table II at 40 CFR 136.3(e) to Required

    Containers, Preservation Techniques, and Holding Times

  10. Proposed Revisions to 40 CFR 136.4 and 136.5

  11. Proposed Revisions to Method Modification Provisions at 40

    CFR 136.6

    I. Proposed New Quality Assurance and Quality Control Language at 40 CFR 136.7

  12. Proposed Withdrawal of Appendices at 40 CFR 136

  13. Proposed Revisions to 40 CFR 423

    L. Proposed Revisions to 40 CFR 430

  14. Proposed Revisions to 40 CFR 435

    III. Statutory and Executive Order Reviews

  15. Executive Order 12866: Regulatory Planning and Review

  16. Paperwork Reduction Act

  17. Regulatory Flexibility Act

  18. Unfunded Mandates Reform Act

  19. Executive Order 13132: Federalism

  20. Executive Order 13175: Consultation and Coordination With

    Indian Tribal Governments

  21. Executive Order 13045: Protection of Children From

    Environmental Health Risks and Safety Risks

  22. Executive Order 13211: Actions That Significantly Affect

    Energy Supply, Distribution, or Use

    I. National Technology Transfer and Advancement Act of 1995

  23. Executive Order 12898: Federal Actions To Address

    Environmental Justice in Minority Populations and Low-Income

    Populations

    IV. References

    I. Statutory Authority

    EPA is proposing 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

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    requirements) for CWA programs at 40 CFR part 136, though some requirements are codified in other Parts (e.g., 40 CFR chapter I, subchapters N and O).

    II. Summary of Proposed Rule

    EPA's regulations at 40 CFR part 136 identify test procedures that must be used for the analysis of pollutants in all applications and report under the CWA NPDES program as well as State certifications pursuant to section 401 of the CWA. Included among the approved test procedures are analytical methods developed by EPA as well as methods developed by voluntary standards development organizations such as ASTM

    International and by the joint efforts of the Standard Methods

    Committee which is comprised of three technical societies (American

    Public Health Association, American Water Works Association and the

    Water Environment Federation) and produce Standard Methods for the

    Examination of Water and Wastewater. EPA approves analytical methods

    (test procedures) for measuring regulated pollutants in wastewater.

    Regulated and regulatory entities use these approved methods for determining compliance with NPDES permits or other monitoring requirements. Often, these entities have a choice in deciding which approved method they will use because EPA has approved the use of more than one method. This rule proposes to add to this list of approved methods. Associated with the proposed approved methods are their regulated analytes (parameters) within the method. Some of these proposed methods introduce new technologies to the NPDES program, while others are updated versions of previously approved methods. These additions will improve data quality and provide the regulated community with greater flexibility. Further, EPA is aware that organizations sometimes republish methods to correct errors or revise the description. These changes do not affect the performance of the method.

    Therefore, if there are changes for methods in this proposed rule before publication of a final rule, EPA will include the updated versions. In the tables at Section 136.3, EPA lists the parameters in alphabetical order. To better identify new parameters proposed in this rule EPA added some of these parameters, such as bisphenol A and nonylphenol, at the end of these lists. In the final rule, EPA may choose to reorder the listings to arrange all parameters alphabetically.

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

    EPA is proposing to add new EPA methods that require new technologies to its Part 136 test procedures. EPA also is proposing new versions of already approved EPA methods with technologies that have been in use for many years. The new EPA methods and new versions of EPA approved methods are described in the following paragraphs. 1. EPA is proposing a new version of EPA Method 1664, 1664B: N-

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

    Treated N-Hexane Extractable Material (SGT-HEM; Non-polar Material) by

    Extraction and Gravimetry for use in CWA programs. In addition, EPA is proposing to amend the RCRA regulations at 40 CFR 260.11, which currently specify use of method 1664A, to additionally specify the revised version, 1664B.

    Currently, Method 1664A is used as a required testing method to determine eligibility of materials for certain conditional exclusions from RCRA regulations under 40 CFR 260.20 and 260.22. These exclusions are known as ``delistings.'' These delistings provide that certain wastes generated at particular facilities are no longer classified as hazardous wastes under RCRA. When delistings are granted by EPA, the

    Agency describes them, along with applicable conditions, in appendix IX to 40 CFR part 261.

    A number of delistings specify, among other things, the following test method: ``Method 9070A (uses EPA Method 1664, Rev. A).'' This testing method must be used by waste generators to determine if their wastes are an oily waste for delisting purposes. The language used in

    Appendix IX reads this way because Method 9070A in SW-846 (including on the SW-846 Web site, http://www.epa.gov/epawaste/hazard/testmethods/ sw846/pdfs/9070a.pdf ) simply reads that Method 1664A is to be used.

    Thus, although Method 9070A is cited, it is actually Method 1664A.

    Method 9070A does not exist independently of Method 1664A.

    Once this rule becomes final, we would encourage future delistings, if applicable, to cite the test method as ``Method 9070A (uses Method

    EPA 1664, Rev. B).'' EPA is not proposing to amend delistings granted in previous years that reference Method 1664A at this time, since it would require additional review to assess the need for such a change and an analysis of each delisting.

    Oil and Grease is a method-defined parameter that measures hexane extractable material (HEM) using n-hexane (85% minimum purity, 99.0% minimum saturated C6 isomer, residue 2[middot]6H2O). In

    Methods 1106.1 and 1600, in Tables 6 and 7, respectively, the true spiked Enterococci ``T (CFU/100 mL)'' in the spiked sample based on the lot mean valued provided by the manufacturer should be 32 instead of 11.2. In Method 1680, the lactose for Lauryl Tryptose Broth (LTB) should be 5.0 g, not 25.0 g (section 7.6.1), and the dipotassium hydrogen phosphate for EC medium should be 4.0 g, not 44.0 g (section 7.7.1). 8. EPA is proposing to add Method 1627, ``Kinetic Test Method for the Prediction of Mine Drainage Quality.'' The method is a standardized simulated weathering test that provides information to predict the quality of mine drainage from coal mining operations or weathering. The method also can be a tool with which to generate data in the design and implementation of best management practices and treatment processes needed by mining operations to meet U.S. EPA discharge requirements at 40 CFR part 434. Other publications have referred to this method generically as the ADTI Weathering Procedure 2 (ADTI-WP2). EPA lists

    Method 1627 in Table IB as ``Acid Mine Drainage.'' The method is suitable for determinations of probable hydrologic consequences and to develop cumulative hydrologic impact assessment data to support Surface

    Mining Control and Reclamation Act (SMCRA) permit application requirements. Although this method is directed toward the coal mining industry and regulatory agencies, the method may be applicable to highway and other construction involving cut and fill of potentially acid-producing rock. This method may be used to predict the water quality characteristics (e.g., pH, acidity, metals) of mine site discharges using observations from sample behavior under simulated and controlled weathering conditions. The method was developed and evaluated in single, multiple and interlaboratory method validation studies in laboratories representing the mining industry, private sector, federal agencies, and academia. 9. EPA proposes to approve EPA Method 624, ``Purgeables,'' for definitive measurements of acrolein and acrylonitrile in wastewater.

    Currently this method is approved only to screen samples for the presence of acrolein and acrylonitrile. Footnote 4 to Table IC requires that the analyst confirm occurrences with either EPA Method 603 or 1624 because, when EPA promulgated this method, EPA believed the confirmatory step was necessary. Commenters on a previous proposed rule to amend part 136 (69 FR 18166, April 6, 2004) requested that EPA allow use of Method 624 for definitive determination of acrolein and acrylonitrile in wastewater without a confirmatory step and provided

    EPA with data. EPA has considered this comment and after reviewing additional data (Test America 1, 2) is proposing to revise the listing of Method 624 in Table IC to remove footnote 4 that requires a confirmatory analysis.

  25. Changes to 40 CFR 136.3 To Include New Standard Methods and New

    Versions of Approved Standard Methods

    EPA is proposing to revise how we identify approved methods that are published by the Standard Methods Committee. Currently in the tables at 136.3(a), EPA lists these methods in one or more columns as being in the 18th, 19th, 20th printed compendiums, or in the On-line editions published by the Standard Methods Committee. EPA identifies which versions are approved by the printed edition in which the

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    method is published or, in the case of the electronic version of the method, by the last two digits of the year in which the method was published by the Standard Methods Committee (e.g., Standard Method 2320

    B-97). In some cases, EPA has approved more than one version of a

    Standard Method. Approval of several versions of the same Standard

    Method has led to inconsistencies in how laboratories conduct these analyses especially in quality assurance/quality control (QA/QC) practices. For this reason, EPA is proposing to approve only the most recent version of a method published by the Standard Methods Committee with as few exceptions as possible by listing only one version of the method with the year of publication designated by the last four digits in the method number (e.g., Standard Method 2320 B-1997). This change allows use of a specific method in any edition that includes a method with the same method number and year of publication. Previously, a laboratory only could use the method that was published in the edition of Standard Methods listed in the tables at 136.3(a). In some cases,

    EPA used footnotes to designate approved Standard Methods that are no longer published in Standard Methods.

    In addition, EPA is proposing to approve new Standard Methods, SM, new versions of currently approved SM, and the use of an already approved SM for a chemical that is not currently listed in Table IB.

    The new versions of currently approved SM have been revised to clarify or improve the instructions in the method, improve the quality control

    (QC) instructions, or make editorial corrections. The proposed new SM and new versions of SM are described in the following paragraphs. 1. EPA is proposing to add SM 5520 B-2001 and SM 5520 F-2001 for

    Oil and Grease determinations. These methods measure hexane extractable material (HEM). EPA is proposing these methods because they use n- hexane as the extraction solvent. EPA is not proposing SM 5520 G-2001 because it allows use of a co-solvent, such as acetone. In the preceding description of EPA's proposed Method 1664B, EPA explained that oil and grease is a measurement defined by the solvent, in this case n-hexane, used to extract oil and grease from the sample. Thus, use of any other solvent system, such as a co-solvent is precluded. 2. EPA is proposing to add SM 4500-NH3G-1997, Ammonia

    (as N) and TKN, Phenate Method, which is an automated version of the previous version of a previously approved SM 4500-NH3F- 1997. 3. EPA is proposing to add SM 4500-B B-2000, Boron, Curcumin

    Method, which uses the same chemistry and instruments as Method I-3112- 85. 4. EPA is proposing to add SM 4140-1997, Inorganic Ions (Bromide,

    Chloride, Fluoride, Orthophosphate, and Sulfate), Capillary Ion

    Electrophoresis with Indirect UV Detection, which uses the same technology as the EPA approved ASTM Method D6508-00. 5. EPA is proposing to add SM 3114 C-2009, Arsenic and Selenium by

    Continuous Hydride Generation/Atomic Absorption Spectrometry, which is an automated version of the approved manual method, and uses the same technology as Method I-2062-85. 6. EPA is proposing to add SM 3111 E-1999 for determinations of aluminum and beryllium. The method uses the same instrumental techniques as SM 3111D with an additional chelation concentration step for increased sensitivity. 7. EPA is proposing to add SM 5220 B-1997 for Chemical Oxygen

    Demand which is similar to EPA Method 410.3. 8. EPA is proposing to add SM 4500 NORGD-1997 for determinations of Kjeldahl Nitrogen--Total, which has a similar chemical and instrument setup as in EPA Method 351.2 in Table IB. The same chemical reaction is measured in both of these methods. 9. EPA is proposing to add SM 4500 P G-1999 and SM 4500 P H-1999,

    Phosphorus. Both of these methods use separate flow injection instrumentation that is the same as EPA Method 365.1. 10. EPA is proposing to add SM 4500 P E-1999 and SM 4500 P F-1999,

    Phosphorus. These methods, 4500 P E-1999 Manual Single Reagent and F- 1999 Automated Ascorbic Acid, have been approved for drinking water analyses (73 FR 31616, June 3, 2008). 11. EPA is proposing to add SM 4500 O B, D, E and F-2001, Oxygen,

    Iodometric Methods. EPA is proposing these methods because Standard

    Methods has broken down the Winkler titration method into several sections. Sections 4500 O B, D, E and F have been added to provide a more detailed Winkler titration. Section B contains information on how to collect the sample and what pretreatment may be needed for just the

    Winkler titrations. Sections D, E, and F contain specific sample pretreatment for interferences. Section D (see Item 12) is for ferrous iron interferences. Section E (see Item 13) is for samples with a high concentration of Total Suspended Solids. Section F is for samples with large concentrations of biological solids. These sections are similar to the instructions in ASTM D888, AOAC 973.45, and USGS I-1575-78. 12. EPA is proposing to add SM 4500 O D-2001, Oxygen, Permanganate

    Modification. This method for determinations of dissolved oxygen contains the same permanganate pretreatment step that is specified in

    ASTM D 888 and AOAC 973.45. 13. EPA is proposing to add SM 4500 O E-2001, Oxygen, Alum

    Flocculation Modification. This method for dissolved oxygen describes a pretreatment step that removes high concentrations of suspended solids. 14. EPA is proposing to add SM 3500 K C-1997, Potassium, Selective

    Electrode Method. This method uses the same electrochemical procedure to measure Potassium that is used in the Standard Methods for ammonia, chloride, cyanide, and nitrate. Only the electrode construction is different. 15. EPA is proposing to add SM 2540 E-1997 for determinations of

    Residues--Volatile. This fixed and volatile solids method uses the same equipment and procedures to measure this method defined parameter as approved EPA Method 160.4. 16. EPA is proposing to add SM 4500 SiO2E-1997 and SM 4500 SiO2F-1997, Silica. These methods have the same instrument setup and molybdate color reagent as USGS Method I-2700, but utilize different reducing agents to produce molybdenum blue color.

    There are slight modifications in the chemical reaction, but the molybdenum blue final analyte is the same. 17. EPA is proposing to add SM 4500 SO4C-1997, D-1997,

    E-1997, F-1997 and G-1997, Sulfate. EPA is proposing to approve the online version of these methods because they are identical to the approved versions published in the 18th, 19th and 20th edition of

    Standard Methods. EPA approved the online versions for drinking water use (73 FR 31616, June 3, 2008). 18. EPA is proposing to add SM 4500 S\2\-B-2000 and C-2000,

    Sulfide. These approved methods have been revised to describe more completely the sample collection, transportation and analysis steps.

  26. Changes to 40 CFR 136.3 To Include New ASTM Methods and New Versions of Previously Approved ASTM Methods

    EPA is proposing to add to the list of approved testing procedures new ASTM methods for existing pollutants in Table IB, such as cyanide, and methods for new pollutants, such as the nonylphenols in Table IC.

    EPA also is

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    proposing new versions of previously approved ASTM methods. 1. EPA is proposing to add ASTM D2036-09 Standard Test Methods for

    Cyanides in Water, Test Method A Total Cyanide after Distillation. In 2009, ASTM revised the version of this method currently listed in part 136. The method measures cyanides that are free, and strong-metal- cyanide complexes (e.g. iron cyanides) that dissociate and release free cyanide when refluxed under strongly acidic conditions. The cyanide in some cyano complexes of transition metals, for example, cobalt, gold, platinum, etc., is not determined. Samples are digested with sulfuric acid in the presence of magnesium chloride in a distillation reaction vessel that consists of a 1-L round bottom flask, with provision for an inlet tube and a condenser connected to a vacuum-type absorber. The flask is heated with an electric heater. Smaller distillation tubes such as 50-mL midi tubes or 6-mL MicroDist\TM\ tubes described in

    D7284-08 can be used if the quality control requirements in D2036-09 are satisfied. After distillation, the cyanide concentration can be determined with titration, ion chromatography, colorimetric procedure

    (spectrophotometric), selective ion electrode, or flow injection analysis with gas diffusion separation and amperometric detection. The inclusion of ion chromatography and gas diffusion separation with amperometric detection as determinative steps (D2036-09, sections 16.5 and 16.6) will give users additional options to measure cyanide after distillation. Furthermore, these determinative steps can be used to mitigate interferences that have been associated with conventional colorimetric test methods. 2. EPA is proposing to add ASTM D6888-09 Standard Test Method for

    Available Cyanide with Ligand Displacement and Flow Injection Analysis

    (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection.

    This method is used to determine the concentration of available inorganic cyanide in an aqueous wastewater or effluent. The method detects the cyanides that are free and metal-cyanide complexes that are easily dissociated into free cyanide ions. The method does not detect the less toxic strong metal-cyanide complexes, cyanides that are not

    ``amenable to chlorination.'' Total cyanide can be determined for samples that have been distilled as described in Test Methods D2036-09,

    Test Method A, Total Cyanides after Distillation. Complex cyanides bound with nickel or mercury are released by ligand displacement with the addition of a ligand displacement agent prior to analysis. Other available cyanide species do not require ligand displacement under the test conditions. If samples are distilled for total cyanide, ligand exchange reagents are not required since the cyanide complexes are dissociated and absorbed into the sodium hydroxide capture solution during distillation. The treated or distilled sample is introduced into a flow injection analysis (FIA) system where it is acidified to form hydrogen cyanide. The hydrogen cyanide gas diffuses through a hydrophobic gas diffusion membrane, from the acidic donor stream into an alkaline acceptor stream. Up to 50-mg/L sulfide is removed during flow injection to mitigate sulfide interference. The captured cyanide is sent to an amperometric flow cell detector with a silver-working electrode. In the presence of cyanide, silver in the working electrode is oxidized at the applied potential. The anodic current measured is proportional to the concentration of cyanide in the standard or sample injected. 3. EPA is proposing to add ASTM D7284-08 Standard Test Method for

    Total Cyanide in Water by Micro Distillation followed by Flow Injection

    Analysis with Gas Diffusion Separation and Amperometric Detection. This method determines the concentration of total cyanide in wastewater, and detects the cyanides that are free and strong-metal-cyanide complexes

    (e.g., iron cyanides) that dissociate and release free cyanide when refluxed under strongly acidic conditions. This method has a range of approximately 2 to 400 [mu]g/L (parts per billion) total cyanide.

    Higher concentrations can be measured with sample dilution or lower injection volume. The determinative step of this method utilizes flow injection with amperometric detection based on ASTM D6888-09. Sample distillation is based on Lachat QuikChem Method 10-204-00-1-X. Prior to analysis, samples must be distilled with a micro-distillation apparatus described in the test method or with a suitable cyanide distillation apparatus specified in Test Methods D 2036-09. The samples are distilled with a strong acid in the presence of magnesium chloride catalyst and captured in sodium hydroxide absorber solution. The absorber solution from the distillation is introduced into a flow injection analysis (FIA) system where it is acidified to form hydrogen cyanide. The hydrogen cyanide gas diffuses through a hydrophobic gas diffusion membrane, from the acidic donor stream into an alkaline acceptor stream. The captured cyanide is sent to an amperometric flow cell detector with a silver-working electrode. In the presence of cyanide, silver in the working electrode is oxidized at the applied potential. The anodic current measured is proportional to the concentration of cyanide. This method has been shown to be less susceptible to interferences compared to conventional spectrophotometric determinations for total cyanide. 4. EPA is proposing to add ASTM D7511-09e2 Standard Test Method for

    Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet

    Digestion and Amperometric Detection. This method determines the concentration of total cyanide in drinking and surface waters, as well as domestic and industrial wastes. Cyanide ion (CN-), hydrogen cyanide in water (HCN(aq)), and the cyano-complexes of zinc, copper, cadmium, mercury, nickel, silver, and iron may be determined by this method.

    Cyanide ions from Au(I), Co(III), Pd(II), and Ru(II) complexes are only partially determined. The applicable range of the method is 3 to 500

    mu g/L cyanide using a 200-[mu]L sample loop. The range can be extended to analyze higher concentrations by sample dilution or by changing the sample loop volume. ASTM D7511-09e2 decomposes complex cyanides by narrow band, low watt UV irradiation in a continuously flowing acidic stream at room temperature. Reducing and complexing reagents, combined with the room temperature narrow band low watt UV, minimize interferences. The hydrogen cyanide generated passes through a hydrophobic membrane into a basic carrier stream. The cyanide concentration is determined by amperometry. This method operates similarly to available cyanide methods OIA1677 and ASTM D6888-09. The available cyanide methods employ a preliminary ligand addition to liberate cyanide ion from weak to moderate metal cyanide complexes.

    These available cyanide methods were developed because they overcome significant interferences caused by the preliminary chlorination and/or distillation processes. Instead of ligands, ASTM D7511-09e2 irradiates the sample causing strong metal cyanide complexes plus all complexes measured by the available cyanide methods to liberate cyanide and generate hydrogen cyanide. Once the sample solution passes from the UV irradiation, the measurement principle is equivalent to OIA1677 and/or

    ASTM D6888-09. 5. Because there were no EPA-approved methods for free cyanide when water quality criteria were

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    established for free cyanide EPA recommended measurement of cyanide after a ``total'' distillation. Analytical methods for free cyanide have been developed, and in today's rule EPA is proposing to add free cyanide as a parameter (24A in Table IB.) For determinations of this parameter, EPA is proposing to allow use of the approved available cyanide method, OIA 1677-09, and two ASTM methods (D4282-02 and D7237- 10.) ASTM D4282-02 Standard Test Method for Determination of Free

    Cyanide in Water and Wastewater by Microdiffusion determines free cyanide as the cyanide that diffuses into a sodium hydroxide solution from a solution at pH 6. It is not applicable to cyanide complexes that resist dissociation, such as hexacyanoferrates and gold cyanide, and it does not include thiocyanate and cyanohydrin. ASTM D7237-10 Standard

    Test Method for Free Cyanide with Flow Injection Analysis (FIA)

    Utilizing Gas Diffusion Separation and Amperometric Detection determines free cyanide with the same instrumentation and technology as approved methods, ASTM D6888-09 and OIA 1677-09, but under milder (less acidic) conditions and without use of ligand replacement reagents. 6. EPA is proposing to add ASTM D888-09 Standard Test Method for

    Dissolved Oxygen in Water. This method determines dissolved oxygen concentrations in water using the titrimetric (Part A), polarographic

    (Part B) and luminescence-based (Part C) detection methods. This standard test method is applicable to the determination of dissolved oxygen between 0.05-20 ppm in influent, effluent or ambient water testing. ASTM recently updated Part C of this method to include a detailed description of the technology and to update calibration procedures to include a two-point calibration and an air saturated water calibration in addition to a water saturated air calibration.

    This method may be used for Biological Oxygen Demand (BOD) and

    Carbonaceous Oxygen Demand (CBOD.) 7. EPA is proposing to add ASTM D7573-09 Standard Test Method for

    Total Carbon and Organic Carbon in Water by High Temperature Catalytic

    Combustion and Infrared Detection. This Method has the same chemical and instrument setup as approved SM 5310 B-2000. 8. EPA is proposing to add in Table IC ASTM D7065-06: Standard Test

    Method for Determination of five chemicals: Nonylphenol (NP), Bisphenol

    A (BPA), p-tert-Octylphenol (OP), Nonylphenol Monoethoxylate (NP1EO), and Nonylphenol Diethoxylate (NP2EO) in Environmental Waters by Gas

    Chromatography Mass Spectrometry. These five chemicals are partitioned into an organic solvent, separated using gas chromatography and detected with mass selective detection. These chemicals or isomer mixtures are qualitatively and quantitatively determined. Although this method adheres to selected ion monitoring mass spectrometry, full scan mass spectrometry has also been shown to work well under these conditions. This method has been multi-laboratory validated for use with surface water and waste treatment effluent samples and is applicable to these matrices. It has not been investigated for use with salt water or solid sample matrices. The reporting limit for nonylphenol is 5 [mu]g/L (ppb); the chronic Freshwater Aquatic Life

    Ambient Water Quality Criterion is 6.6 ppb. 9. EPA is proposing to add in Table IC ASTM D7574-09: Standard Test

    Method for Determination of BPA in Environmental Waters by Liquid

    Chromatography/Tandem Mass Spectrometry. BPA is an organic chemical produced in large quantities. BPA is soluble in water and undergoes degradation in the environment. The reporting limit for BPA is 20 ng/L which is fifty times less than the limit in D7065-06 (see preceding

    Item 8). The method is based on a solid phase extraction (SPE) followed by separation with liquid chromatography and tandem mass spectrometry

    (LC/MS/MS), which reduces the amount of sample required, solvents, the analysis time, and the reporting limits. The method has been tested in effluents from secondary and tertiary publicly owned treatment works

    (POTW), and fresh surface and ground water. 10. EPA is proposing to add in Table IC ASTM D7485-09: Standard

    Test Method for Determination of NP, OP, NP1EO, and NP2EO in

    Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry.

    The method extracts these four chemicals from water with SPE followed by LC/MS/MS separation and detection. These chemicals are qualitatively and quantitatively determined by this method. This method uses single reaction monitoring (SRM) mass spectrometry. Environmental waters tested using this method were sewage treatment plant effluent, river water, seawater, and a modified ASTM D5905 artificial wastewater. The reporting limit for nonylphenol is 100 ng/L, ppt. The Freshwater and

    Saltwater Aquatic Life Ambient acute criterion is 7.0 ppb, and the chronic criterion is 1.7 ppb. 11. EPA is not proposing to include in Table IB two ASTM oil and grease methods, D7066-04 and D7575-10 because neither method uses n- hexane to determine oil and grease as hexane extractable material

    (HEM). As previously explained in the discussion of Method 1664B, HEM is a measurement defined by the solvent (n-hexane) used to extract oil and grease from the sample. D7066-04 employs a proprietary solvent, S- 316, a dimer/trimer of chlorotrifluoroethylene to measure S-316- extractable substances from an acidified sample. Method D7066 may be useful for determinations of total petroleum hydrocarbons (TPH).

    Although TPH has been measured in some applications, EPA has never included it as a Part 136 pollutant nor received any convincing evidence that it should do so. Although S-316 is not the same solvent as the fluorocarbon, Freon[supreg], it is a fluorochlorohydrocarbon.

    Instead of n-hexane, ASTM D7575-10 uses a different extracting process, an extracting membrane, followed by infrared measurement of the materials in the sample that can pass through the membrane. Several other steps in D7575-10 significantly differ from 1664 including: Use of 10-mL sample aliquot from sample bottle vs. entire contents of 1-L sample; homogenization of samples; and the challenge of pushing solid oil and grease samples through a membrane. The results of a multi- laboratory study (OSS 2009) that the developer conducted as part of

    ASTM's evaluation of D7575 are in the docket.

  27. Changes to 40 CFR 136.3 To Include Alternate Test Procedures

    To promote method innovation, EPA maintains a program whereby method developers may apply for an EPA review and potentially for approval of alternate test procedures. This Alternate Test Procedure

    (ATP) program is described for Clean Water Act applications at Parts 136.4 and 136.5. EPA has reviewed and is proposing for nationwide use eight alternate test procedures. These proposed new methods include:

    Hach Company's Method 10360 Luminescence Measurement of Dissolved

    Oxygen (LDO[supreg]) in Water, In-Situ Incorporated's Method 1002-8- 2009 Dissolved Oxygen (DO) Measurement by Optical Probe, Method 1003-8- 2009 Biochemical Oxygen Demand (BOD) Measurement by Optical Probe, and

    Method 1004-8-2009 Carbonaceous Biochemical Oxygen Demand (CBOD)

    Measurement by Optical Probe August 2009, Mitchell Method M5271 and

    M5331 for measuring turbidity in wastewater; Thermo Scientific's Orion

    Method

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    AQ4500 for measuring turbidity in wastewater; and Systea Scientific,

    LLC's Systea Easy (1-Reagent) Nitrate Method. Descriptions of these new methods included for approval are as follows: 1. EPA is proposing to approve Hach Company's Method 10360

    Luminescence Measurement of Dissolved Oxygen (LDO[supreg]) in wastewater, Revision 1.1 dated January 4, 2006. EPA has reviewed this method and the data generated in a multi-laboratory validation study performed by Hach Company and is proposing to approve it for use in measuring dissolved oxygen. EPA is also proposing to approve the Hach method 10360 to be used for Dissolved Oxygen (DO) when determining BOD and CBOD.

    This method uses an optical probe to measure the light emission characteristics from a luminescence-based reaction that takes place at the sensor-water interface. A light emitting diode (LED) provides incident light required to excite the luminophore substrate. In the presence of dissolved oxygen, the reaction is suppressed. The resulting dynamic lifetime of the excited luminophore is evaluated and equated to

    DO concentration.

    The method involves the following steps:

    Calibration of the probe using water-saturated air, and

    Measurement of the dissolved oxygen in the sample using the probe.

    Approved methods for measuring dissolved oxygen are listed at 40

    CFR 136.3, Table IB. The performance characteristics of the Hach

    Company Method 10360 were compared to the characteristics of the methods listed at 40 CFR 136.3, Table IB for measurement of dissolved oxygen. Because the Hach Company Method 10360 is equally effective relative to the methods already promulgated in the regulations, EPA is proposing to include this method in the list of methods approved for measuring dissolved oxygen concentrations in wastewater when determining BOD and CBOD. 2. EPA is proposing to approve In-Situ Incorporated's Method 1002- 8-2009 Dissolved Oxygen Measurement by Optical Probe. EPA has reviewed this method and the data generated in a multi-laboratory validation study performed by In-Situ Incorporated and is proposing to approve it for use in measuring dissolved oxygen. In-Situ Method 1002-8-2009 uses a new form of electrode based on the luminescence emission of a photoactive chemical compound and the quenching of that emission by oxygen to measure dissolved oxygen concentration.

    The method involves the following steps:

    Calibration of the probe using water-saturated air, and

    Measurement of the dissolved oxygen in the sample using the probe.

    Approved methods for measuring dissolved oxygen are listed at 40

    CFR 136.3, Table IB. The performance characteristics of the In Situ

    Method 1002-8-2009 were compared to the characteristics of the methods listed at 40 CFR 136.3, Table IB for measurement of dissolved oxygen.

    Because the In-Situ Method 1002-8-2009 is equally effective relative to the methods already promulgated in the regulations, EPA is proposing

    In-Situ Method 1002-8-2009 for inclusion in the list of methods approved for measuring dissolved oxygen concentrations in wastewater. 3. EPA is proposing to approve In-Situ Incorporated's Method 1003- 8-2009 Biochemical Demand (BOD) Measurement by Optical Probe. EPA has reviewed this method and the data generated in a multi-laboratory validation study performed by In-Situ Incorporated and is proposing to approve it for measuring BOD.

    In-Situ Method 1003-8-2009 uses a new form of electrode based on the luminescence emission of a photoactive chemical compound and the quenching of that emission by oxygen to measure dissolved oxygen concentration when performing the 5-day BOD test.

    The method involves the following steps:

    Filling a BOD bottle with diluted seeded sample,

    Measuring the dissolved oxygen in the sample using an optical DO probe,

    Sealing and incubating the bottle for five days,

    Measuring the dissolved oxygen with an optical probe after the five day incubation period, and

    Calculating the BOD from the difference between the initial and final dissolved oxygen measurements.

    Approved methods for measuring BOD are listed at 40 CFR 136.3,

    Table IB. The performance characteristics of In-Situ Method 1003-8-2009 were compared to the characteristics of the methods listed at 40 CFR 136.3, Table IB for measurement of BOD. Because In-Situ Method 1003-8- 2009 is equally effective relative to the methods already promulgated in the regulations, EPA is proposing In-Situ Method 1003-8-2009 for inclusion in the list of methods approved for measuring BOD. 4. EPA is proposing to approve In-Situ Incorporated's Method 1004- 8-2009 Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by

    Optical Probe. EPA has reviewed this method and the data generated in a multi-laboratory validation study performed by In-Situ Incorporated and is proposing to approve it for use in measuring carbonaceous biochemical oxygen demand (CBOD). In-Situ Method 1004-8-2009 uses a new form of electrode based on the luminescence emission of a photoactive chemical compound and the quenching of that emission by oxygen to measure dissolved oxygen concentration when performing the CBOD test.

    The method involves the following steps:

    Filling a BOD bottle with diluted seeded sample,

    Adding a chemical nitrification inhibitor,

    Measuring the dissolved oxygen in the sample using an optical dissolved oxygen probe,

    Sealing and incubating the bottle for five days,

    Measuring the dissolved oxygen with an optical probe after the five day incubation period, and

    Calculating the CBOD from the difference between the initial and final dissolved oxygen measurements.

    Approved methods for measuring CBOD are listed at 40 CFR 136.3,

    Table IB. The performance characteristics of In Situ-Method 1004-8-2009 were compared to the characteristics of the methods listed for measurement of CBOD. Because In-Situ Method 1004-8-2009 is equally effective relative to the methods already promulgated in the regulations, EPA is proposing In-Situ Method 1004-8-2009 for inclusion in the list of methods approved for measuring CBOD. 5. EPA is proposing to approve the Mitchell Method M5271 dated July 31, 2008. This method uses laser based nephelometry to measure turbidity in drinking water and wastewater. The method involves the following steps for instruments other than on-line continuous models:

    Mixing the sample to thoroughly disperse the solids,

    Waiting until air bubbles disappear,

    Pouring a sample into a turbidimeter tube, and

    Reading turbidity directly from the instrument scale or from the appropriate calibration curve.

    Approved methods for turbidity are listed at 40 CFR 136.3 Table 1B.

    The performance characteristics of Mitchell Method M5271 were compared to the performance characteristics of EPA Method 180.1 listed at 40 CFR 136.3 for measurement of turbidity. Comparisons were based on results obtained from turbidimeters placed in series which took measurements at one minute

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    intervals over a 20 to 30 hour time period at three different public water supply systems (in one case measurements were taken at 15 minute intervals). Testing included source water from one ground water source and two surface water sources and included at least one natural filter event (back-flush) in lieu of artificially calibrated spikes using a primary standard spiking solution. Additionally, a demonstration of performance at higher turbidities was conducted by making replicate measurements of primary standards at four levels (5 NTU, 10 NTU, 20 NTU and 40 NTU). Results showed excellent correlation between measurements made using a tungsten filament incandescent bulb as specified in EPA

    Method 180.1 and those made using the laser light source specified in

    Mitchell Method M5271. Based on the results of these studies, EPA has determined that Mitchell Method M5271 is as effective as the methods already promulgated in the regulations. EPA is proposing to add this method to the list of methods approved for measurement of turbidity in wastewater. 6. EPA is proposing Mitchell Method M5331 dated July 31, 2008. This method uses LED based nephelometry to measure turbidity. The method involves the following steps for instruments other than on-line continuous models:

    Mixing the sample to thoroughly disperse the solids,

    Waiting until air bubbles disappear,

    Pouring the sample into turbidimeter tube, and

    Reading turbidity directly from the instrument scale or from the appropriate calibration curve.

    Approved methods for turbidity are listed at 40 CFR 136.1 Table 1B.

    The performance characteristics of Mitchell Method 5331 were compared to the performance characteristics of EPA Method 180.1 listed at 40 CFR 136.3 for measurement of turbidity. Comparisons were based on results obtained from turbidimeters placed in series, which took measurements at one minute intervals over a 20 to 30 hour time period at three different public water supply systems (in one case measurements were taken at 15 minute intervals). Testing included source water from one ground water source and two surface water sources and included at least one natural filter event (back-flush) in lieu of artificially calibrated spikes using a primary standard spiking solution.

    Additionally, a demonstration of performance at higher turbidities was conducted by making replicate measurements of primary standards at four levels (5 NTU, 10 NTU, 20 NTU and 40 NTU). Results showed excellent correlation between measurements made using a tungsten filament incandescent bulb as specified in EPA Method 180.1 and the LED light source specified in Mitchell Method M5331. Based on the results of these studies, EPA has determined that Mitchell Method M5331 is equally effective relative to the methods already promulgated in the regulations. EPA is proposing to add this method to the list of methods approved for measurement of turbidity in wastewater. 7. EPA is proposing to approve Thermo Scientific's Orion Method

    AQ4500 dated March 12, 2009. This method uses LED-based nephelometry to measure turbidity. The method involves the following steps:

    Calibration of the instrument using a primary calibration standard,

    Placing the sample into the sample chamber, and

    Reading the turbidity result displayed on the instrument.

    Approved methods for turbidity are listed at 40 CFR 136.3 Table IB.

    The performance characteristics of Thermo Scientific's Orion Method

    AQ4500 were compared to the performance characteristics of EPA Method 180.1 listed at 40 CFR 136.3 for measurement of turbidity. Comparisons were based on an ASTM round robin study comparing results from analyses of 28 different samples of various types including formazin standards, styrene divinyl benzene (SDVB) co-polymer bead standards and real world samples ranging from approximately 2 NTU to over 1,000 NTU. These analyses were conducted using turbidimeters with various light sources including tungsten filament incandescent bulbs as specified in EPA

    Method 180.1 and white LEDs as specified in Thermo Scientific's Orion

    Method AQ4500. Additionally, a demonstration of performance at lower turbidities was conducted by making 20 replicate measurements of dilute formazin standards at four levels (0.2 NTU, 0.5 NTU, 1 NTU, and 2 NTU) using turbidimeters with tungsten filament incandescent bulbs as specified in EPA Method 180.1 and turbidimeters using white LEDs as specified in Thermo Scientific Orion Method AQ4500. Results showed significant correlation between measurements made using a tungsten filament incandescent bulb as specified in EPA Method 180.1 and those made using the LED light source specified in Thermo Scientific's Orion

    Method AQ4500. Based on the results of these studies, EPA has determined that Thermo Scientific's Orion Method AQ4500 is as effective as the methods already promulgated in the regulations. EPA is proposing to add this method to the list of methods approved for measurement of turbidity in wastewater. 8. EPA is proposing to approve Systea Scientific, LLC's Systea Easy

    (1-Reagent) Nitrate Method dated February 4, 2009. This is a method that uses automated discrete analysis, and spectrophotometry to determine concentrations of nitrate and nitrite combined or singly. The method involves the following steps:

    Reduction of nitrate in a sample to nitrite using a non- hazardous proprietary reagent,

    Diazotizing the nitrite originally in the sample plus the reduced nitrate with sulfanilamide followed by coupling with N-(1- napthyl) ethylenediamine dihydrochloride under acidic conditions to form a highly colored azo dye,

    Colorimetric determination in which the absorbance of color at 546 nm is directly proportional to the concentration of the nitrite plus the reduced nitrate in the sample,

    Measurement of nitrite singly, if needed, by analysis of the sample while eliminating the reduction step, and

    Subtraction of the nitrite value from that of the combined nitrate plus nitrite value to measure nitrate singly if needed.

    Approved methods for nitrate, nitrite and combined nitrate/nitrite are listed at 40 CFR 136.3, Table 1B. The performance characteristics of the Systea Easy (1-Reagent) Nitrate Method were compared to the characteristics of the methods listed at 40 CFR 136.3 for nitrate and nitrite. Based on the results of the comparative studies, EPA has determined that the Systea Easy (1-Reagent) Nitrate Method is as effective as the methods already promulgated in the regulations for use in determining concentrations of nitrate and nitrite and combined nitrate/nitrite. The method is a ``green'' alternative to other approved methods that use cadmium, a known carcinogen, for the reduction of nitrate to nitrite. The performance of Systea Easy (1-

    Reagent) Nitrate Method is equivalent to other methods already approved for measurement of nitrate, nitrite and combined nitrate/nitrite in wastewater.

  28. Clarifications and Corrections to Previously Approved Methods in 40

    CFR 136.3

    EPA is proposing a clarification to procedures for measuring orthophosphate, and is proposing to correct typographical or other citation errors in part 136. 1. EPA is clarifying the purpose of the immediate filtration requirement in

    Page 58034

    orthophosphate measurements, which is to assess the dissolved or bio- available form of orthophosphorus (i.e., that which passes through a 0.45 micron filter), hence the requirement to filter the sample immediately upon collection. This filtration excludes any particulate forms of phosphorus that might hydrolyze into orthophosphorus in a slightly acidic sample during the allowed 48 hour holding time. Each grab sample must be filtered within 15 minutes of collection to prevent orthophosphate formation. Specifically, filtration may not be delayed until the final grab sample is collected; each grab sample must be filtered upon collection. However, the filtered grab samples may be held for compositing up to the 48-hour holding time. 2. EPA is proposing to correct missing citations to the table of microbiological methods for ambient water monitoring which are specified in Table IH at 40 CFR 136.3. Stakeholders asked EPA to separately specify the microbiological methods that EPA has approved for wastewater (Table IA) from those for ambient water. On August 15, 2005 (70 FR 48256), EPA proposed to move microbial (bacterial and protozoan) methods which were applicable to ambient water to a new table, Table IH. However, in the final rule of March 26, 2007 (72 FR 14220), EPA inadvertently omitted fecal coliform, total coliform, and fecal streptococcus methods from the table. EPA is proposing to add these methods to Table IH. 3. EPA is proposing to correct several other typographical or minor citation errors, such as incomplete or incorrect method citations.

  29. Proposed Revisions in Table II at 40 CFR 136.3(e) to Required

    Containers, Preservation Techniques, and Holding Times

    EPA is proposing revisions to Table II at 136.3(e) to clarify how to resolve conflicts between instructions in this table and instructions in an approved method or other source, and to amend some of the current requirements in Table II. 1. The introductory text to Table II at 136.3(e) specifies that the instructions in the table take precedence over other sources of this information. EPA publishes holding time and related instructions in

    Table II to provide a consistent set of instructions, and for other reasons. Not all methods contain complete instructions, and some otherwise equivalent methods (or methods for the same parameter) have conflicting instructions. For example, Table II instructions specify the 48 hour BOD holding time while some Part 136 methods recommend 24 hours. In this instance Table II instructions take precedence. EPA recognizes that there may be cases where new technologies or advancements in current technologies may produce approved methods with instructions for a specific parameter that differ from Table II instructions, and provide better results. Cyanide determinations and some automated methods may fall into this category. Therefore, EPA is proposing to revise the text at 136.3(e) to allow a party to submit documentation to their permitting or other authority that supports use of an alternative approach. EPA is proposing to revise the introductory text to the table to read as follows: ``Information in this table takes precedence over instructions provided in specific methods or elsewhere unless a party documents the acceptability of an alternative to the

    Table II instructions. The nature, timing and extent of the required documentation (i.e. how to apply and review as well as the amount of supporting data) are left to the discretion of the permitting authority

    (State Agency or EPA Region) or other authority and may rely on instructions, such as those provided for method modifications at 136.6.'' Thus, an alternate sample container, preservation and/or holding time may be considered at the discretion of the permitting authority or other authority. 2. Some stakeholders have asked EPA to extend the holding time for

    Escherichia coli and Enterococcus. In 2006, EPA conducted a nationwide holding time study (EPA 2006) for fresh and marine ambient waters and concluded that, on a nationwide basis, the Agency was unable to justify extending the holding time for Escherichia coli or Enterococcus in these water matrices. However, EPA is proposing to provide some relief by revising footnote 22 to Table II, which applies to bacterial tests.

    This footnote currently reads as follows: ``Sample analysis should begin immediately, preferably within 2 hours of collection. The maximum transport time to the laboratory is 6 hours, and samples should be processed (in incubator) within 2 hours of receipt at the laboratory.''

    Stakeholders have commented that laboratories must meet the two- hour analysis start time, even if they receive the samples early enough that they could start after two hours and still meet the overall six- hour time limit. EPA is proposing to revise the footnote to read

    ``Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection.'' 3. EPA is proposing to revise the cyanide sample handling instructions in Footnote 5 of Table II to recommend the treatment options for samples containing oxidants described in ASTM's sample handling practice for cyanide samples, D7365-09a. This practice advises analysts to add a reducing agent only if an oxidant is present, and use of the reducing agents sodium thiosulfate

    (Na2S2O3), ascorbic acid, sodium arsenite (NaAsO2), or sodium borohydride (NaBH4). 4. EPA is proposing to revise the cyanide sample handling instructions in Footnote 6 of Table II to describe options available when the interference mitigation instructions in D7365-09a are not effective. EPA proposes to allow use of any technique for removal or suppression of interference, provided the laboratory demonstrates and documents that the alternate technique more accurately measures cyanide through quality control measures described in the analytical test method. 5. EPA is proposing to revise footnote 16 of Table II instructions for handling Whole Effluent Toxicity (WET) samples to be consistent with the November 19, 2002 (67 FR 69951) ``Guidelines for Establishing

    Test Procedures for the Analysis of Pollutants; Whole Effluent Toxicity

    Test Methods; Final Rule,'' as well as the three toxicity methods

    (Methods for Measuring the Acute Toxicity of Effluents and Receiving

    Waters to Freshwater and Marine Organisms (5th Edition, October 2002),

    Short-term Methods for Estimating the Chronic Toxicity of Effluents and

    Receiving Waters to Freshwater Organisms (4th Edition, October 2002), and Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms (3rd Edition,

    October 2002). In the 2002 final rule, EPA established the acceptable range for the current sampling holding temperature for aquatic toxicity tests as 0 to 6 [deg]C based on current National Environmental

    Laboratory Accreditation Conference (NELAC) standards. EPA also clarified in the final rule that hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 [deg]C prior to test initiation. Section 8.5.1 of all three WET methods listed previously states, ``Unless the samples are used in an on-site toxicity test the day of collection (or hand delivered to the testing laboratory for use on the day of collection) it is recommended that they be held at 0 to 6

    deg

    C until used to inhibit microbial degradation, chemical transformation, and loss of highly volatile toxic substances.'' EPA is proposing to add two sentences to the

    Page 58035

    end of Footnote 16 of Table II based on this information. The two sentences are ``Aqueous samples must not be frozen. Hand-delivered samples used on the day of collection do not need to be cooled to 0 to 6 [deg]C prior to test initiation.'' In addition, EPA will post, on the

    WET Web site, corrections to errata in the ``Short-term Methods for

    Estimating the Chronic Toxicity of Effluents and Receiving Waters to

    Freshwater Organisms'' manual (EPA 2010e.) 6. EPA is proposing to add a sentence to footnote 4 of Table II to clarify the sample holding time for the Whole Effluent Toxicity (WET) samples for the three toxicity methods (Methods for Measuring the Acute

    Toxicity of Effluents and Receiving Waters to Freshwater and Marine

    Organisms (5th Edition, October 2002), Short-term Methods for

    Estimating the Chronic Toxicity of Effluents and Receiving Waters to

    Freshwater Organisms (4th Edition, October 2002), and Short-term

    Methods for Estimating the Chronic Toxicity of Effluents and Receiving

    Waters to Marine and Estuarine Organisms (3rd Edition, October 2002) to indicate that one sample of the minimum of three required samples may be used for the renewal of the test solutions and that the sample holding time refers to first use of each sample collected for the toxicity test. The sentence to be added is, ``For static-renewal toxicity tests, each grab or composite sample may also be used to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after first use, if stored at 0-6 [deg]C, with minimum head space.''

  30. Proposed Revisions to 40 CFR 136.4 and 136.5

    EPA is proposing to revise Sec. Sec. 136.4 and 136.5 to describe the procedures for obtaining review and EPA approval for the use of alternate test procedures (alternate methods or ATPs). The proposed changes would revise 40 CFR 136.4 to establish the procedures for obtaining approval for nationwide use of an ATP. The proposed changes would modify 40 CFR 136.5 to establish the procedures for obtaining approval for use of an ATP in a State within a particular EPA Region.

    It should be noted that in its ATP program, EPA considers for review only those methods for which EPA has published an ATP protocol.

    Presently, EPA has published protocols for chemistry, radiochemical, and culture microbiological methods. EPA does not have ATP protocols for Whole Effluent Toxicity (WET) methods or genetic methods.

    In today's rule, EPA proposes to clarify that the intent of the limited use authority is to allow limited use of an alternate method for a specific application at a facility or type of discharge without requiring the same level of supporting test data that would be required for approval for nationwide use. Thus, limited use authority is not intended to be used as a means of avoiding the full examination of comparability that is required when EPA considers a method for nationwide use and decides to amend its list of approved CWA methods at 40 CFR part 136 to include alternative test procedures. In the event that EPA decides not to approve an application for approval of an alternate method for nationwide use, the Regional Alternate Test

    Procedures Coordinator may choose to reconsider any previous limited use approvals of the alternate method. Based on this reconsideration, the Regional Coordinator will notify the user, if the limited use approval is withdrawn.

  31. Proposed Revisions to Method Modification Provisions at 40 CFR 136.6

    EPA encourages regulatory authorities to allow analysts the flexibility to modify CWA methods without prior approval provided the user has documented equivalent or better performance of the method in the matrix type to which the user will apply the modified method. EPA recognizes that addressing specific matrix interferences may require modifications to approved methods that do not require the extensive review and approval process specified for an alternate test procedure at 136.4 and 136.5. Based on users' experiences with 136.6, since it was promulgated on March 12, 2007 (72 FR 11199), EPA proposes to revise this section to provide more examples of allowed and prohibited method modifications. Acceptable reasons for an analyst to modify a method include analytical practices that lower detection limits, improve precision, reduce interferences, lower laboratory costs, and promote environmental stewardship by reducing generation of laboratory wastes.

    Acceptable modifications may use existing or emerging analytical technologies that achieve these ends provided that they do not depart substantially from the underlying chemical principles employed in methods currently approved in 40 CFR part 136. Analysts may use the examples in this section to assess and document that their modification is acceptable and does not depart substantially from the chemical principles in the method being modified. EPA specifically invites comment on the examples of flexibility specified at 136.6 and the documentation that a method modifier must have to demonstrate the equivalency of the modified method. In particular, EPA is interested in public comment on what additional controls, if any, should be applied when changing pH, purge times, buffers, or applying the relative standard error calibration alternative.

    I. Proposed New Quality Assurance and Quality Control Language at 40

    CFR 136.7

    EPA is proposing to specify ``essential'' quality control at Sec. 136.7 for use in conducting an analysis with an approved method and when insufficient instructions are contained in an approved method.

    Auditors, co-regulators, laboratory personnel, and the regulated community have noted the different amounts and types of quality assurance (QA) and quality control (QC) procedures practiced by laboratories that use 40 CFR part 136 methods. Some of these methods are published by voluntary consensus standards bodies, such as the

    Standard Methods Committee, and ASTM International. ASTM and Standard

    Methods are contained in printed compendium volumes, electronic compendium volumes, or as individual online files. Each organization has its unique compendium structure. QA and QC method guidance or requirements may be listed directly in the approved consensus method, or, as is more often the case, these requirements are listed in other parts of the compendium. For example, the publisher of Standard Methods for the Examination of Water and Wastewater consolidates the general quality assurance and quality control requirements for all methods.

    Each specific Part and section can contain additional QA and QC requirements (for example, see part 2020, 3020, 6020, and 9020). ASTM specifies QA and QC requirements in the analyte method's Referenced

    Documents section and in the analyte method. Both organizations require the analyst to reference this additional information within the respective compendiums to achieve the QA and QC expected for valid results.

    Regardless of the publisher, edition or source of an analytical method approved for CWA compliance monitoring, analysts must use suitable QA/QC procedures whether EPA or other method publishers have specified these procedures in a specific part 136 method, or referenced these procedures by other means. Consequently, EPA

    Page 58036

    expects that an analyst using these consensus body methods for reporting under the CWA will also comply with the quality assurance and quality control requirements listed in the appropriate sections in the consensus body compendium. EPA's approval of use of these voluntary consensus standard body methods contemplated that any analysis using such methods would also meet the quality assurance and quality control requirements prescribed for the particular method. Thus, not following the applicable and appropriate quality assurance and quality control requirements of the respective method means that the analysis would not comply with the requirements in EPA's NPDES regulations to monitor in accordance with the procedures of 40 CFR part 136 for analysis of pollutants.

    For methods that have insufficient QA/QC requirements, analysts could refer to and follow the QC published in several public sources.

    Examples of these sources include the instructions in an equivalent approved EPA method or standards published by the National

    Environmental Laboratory Accreditation Conference (cf. Chapter 5 of the compendium published in 2003.)

    In addition to and regardless of the source of the laboratory's QA and QC instructions, EPA is proposing at 136.7 to specify twelve essential quality control checks that must be in the laboratory's documented quality system unless a written rationale is provided to explain why these controls are inappropriate for a specific analytical method or application. This written rationale will be included in the laboratory's Standard Operating Procedure (SOP) for each method to which specific controls do not apply (e.g., internal standards, surrogate standards or tracers do not apply to analyses of inorganic parameters) as well as being included with the monitoring data produced using each method. These twelve essential quality control checks must be clearly documented in the written SOP (or method) along with a performance specification or description for each of the twelve checks.

  32. Proposed Withdrawal of Appendices at 40 CFR 136

    EPA is proposing to incorporate by reference all of the methods printed in 40 CFR part 136 appendices A and C, and to remove most of the information in Appendix D. EPA is proposing to remove EPA Method numbers 601 through 613, 624, 625, 1613B, 1624B and 1625B from Appendix

  33. All of these methods are readily accessible from a variety of sources including EPA's CWA methods Web site http://www.epa.gov/ waterscience/methods/. Removing this appendix would decrease the resources associated with the annual publication of 40 CFR part 136 regulations. EPA would incorporate these methods by reference in Tables

    IC and ID at 136.3(a).

    EPA is proposing to remove Appendix C--Method 200.7 Inductively

    Couple Plasma--Atomic Emission Spectrometric Method for Trace Element

    Analysis of Water and Waste Method because this method has been superseded by Rev. 5.4 of Method 200.7, which is incorporated by reference in Table IB.

    Finally, EPA is proposing to remove from Appendix D the data for all EPA methods that are no longer approved. This would result in

    Appendix D containing Precision and Recovery Statements only for EPA

    Method 279.2 for thallium and EPA Method 289.2 for zinc. EPA will correct any typographical errors in the Appendix, such as the misspelling of thallium. EPA requests comment on whether to publish and make available, at least temporarily, the current version of Appendix D online at the CWA methods Web site for historical purposes.

  34. Proposed Revisions at 40 CFR 423

    EPA is proposing two changes to part 423, Steam Electric Power

    Generating Point Source Category. First, EPA proposes to revise the definitions for total residual chlorine and free available chlorine at

    Sec. Sec. 423.11(a) and 423.11(l), respectively. The current definitions restrict the permittee to the use of the specific amperometric titration method cited in the definitions. The revised definitions will allow the permittee flexibility to use additional approved methods. EPA proposes to revise the definitions as follows: a. The term total residual chlorine (or total residual oxidants for intake water with bromides) means the value obtained using any of the

    ``chlorine--total residual'' methods in Table IB 136.3(a), or other methods approved by the permitting authority. b. The term free available chlorine means the value obtained using any of the ``chlorine--free available'' methods in Table IB 136.3(a) where the method has the capability of measuring free available chlorine, or other methods approved by the permitting authority.

    Second, EPA is proposing to move the current citations of methods from Part 423 and reference a new parameter, ``chlorine-free available'', in Table IB at 136.3(a). Under this parameter, EPA will list any Part 136 methods for total residual chlorine that also provide instructions for determining free chlorine. The tables at 136.3 are well known as the source of most methods that are approved for CWA programs. For this reason EPA is proposing to move the citations of specific methods from part 423 to Table IB, and as described in the following sections, also for Parts 430 and 435.

    L. Proposed Revisions at 40 CFR 430

    EPA is proposing several editorial changes to 40 CFR part 430, The

    Pulp, Paper, and Paperboard Point Source Category. Currently the complete text of EPA Methods 1650 and 1653 are published in Appendix A of part 430. EPA is proposing to cite these two methods in Table IC, at

    Sec. 136.3, and to incorporate by reference the full text of these methods. EPA will list these two methods in Table IC--List of Approved

    Test Procedures for Non-Pesticide Organic Compounds, under adsorbable organic halides (AOX) by Method 1650 and chlorinated phenolics by

    Method 1653. This action would remove Appendix A at 40 CFR part 430, and organize the analytical methods for the Pulp, Paper, and Paperboard category into one part, the Part 136 CWA methods tables, of the CFR.

    To help users more readily identify approved compliance monitoring methods, EPA is proposing to cite at part 430 the Part 136 methods that are approved for these pollutants: Chloroform, 2,3,7,8- tetrachlorodibenzo-p-dioxin (TCDD), and 2,3,7,8- tetrachlorodibenzo-p- furan (TCDF).

  35. Proposed Revisions at 40 CFR 435

    EPA is proposing several changes to Part 435, Oil and Gas

    Extraction Point Source Category. EPA is proposing to move, and in two cases revise, the methods from 40 CFR part 435, subpart A (Offshore

    Subcategory) to an EPA document (``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013), which is included in the record for this rulemaking. This proposed approach organizes the analytical methods for the Offshore Subcategory into one document and allows for easier access to the methods for this category.

    The following table lists the methods EPA proposes to move from Part 435 to the cited document, EPA-821-R-09-013.

    Page 58037

    EPA Method Numbers for Oil and Gas Extraction Point Source Category Analytical Methods and Prior CFR References

    EPA method

    Date first

    Analytical/test method

    number

    promulgated

    Previous CFR references

    Static Sheen Test.....................

    1617

    1993 Subpart A, Appendix 1.

    Drilling Fluids Toxicity Test.........

    1619

    1993 Subpart A, Appendix 2.

    Procedure for Mixing Base Fluids With

    1646

    2001 Subpart A, Appendix 3.

    Sediments.

    Protocol for the Determination of

    1647

    2001 Subpart A, Appendix 4.

    Degradation of Non Aqueous Base

    Fluids in a Marine Closed Bottle

    Biodegradation Test System: Modified

    ISO 11734:1995.

    Determination of Crude Oil

    1655

    2001 Subpart A, Appendix 5.

    Contamination in Non-Aqueous Drilling

    Fluids by Gas Chromatography/Mass

    Spectrometry (GC/MS).

    Reverse Phase Extraction (RPE) Method

    1670

    2001 Subpart A, Appendix 6. for Detection of Oil Contamination in

    Non-Aqueous Drilling Fluids (NAF).

    Determination of the Amount of Non-

    1674

    2001 Subpart A, Appendix 7.

    Aqueous Drilling Fluid (NAF) Base

    Fluid from Drill Cuttings by a Retort

    Chamber (Derived from API Recommended

    Practice 13B-2).

    EPA is also proposing to incorporate additional quality assurance procedures in the marine anaerobic biodegradation analytic method

    (Appendix 4 of Subpart A of Part 435) and to correct some erroneous references and omissions in the method for identification of crude oil contamination (Appendix 5 of Subpart A of Part 435). EPA is proposing to include these revisions in the EPA document (EPA-821-R-09-013).

    EPA promulgated the use of the marine anaerobic biodegradation analytic method (closed bottle test, ISO 11734:1995 as clarified by

    Appendix 4 to Subpart A of Part 435) in 2001 because it most closely modeled the ability of a drilling fluid to biodegrade anaerobically in marine environments (January 22, 2001; 66 FR 6864). Subsequent to this promulgation, EPA incorporated additional quality assurance procedures for the marine anaerobic biodegradation analytic method in the NPDES permit for the Western Gulf of Mexico (``Final NPDES General Permit for

    New and Existing Sources and New Dischargers in the Offshore

    Subcategory of the Oil and Gas Extraction Category for the Western

    Portion of the Outer Continental Shelf of the Gulf of Mexico,''

    GMG290000, Appendix B). The additional quality assurance instructions in the GMG290000 more clearly describe the sample preparation and compliance determination steps. Specifically, these additional quality assurance procedures clarify that users must only use headspace gas to determine compliance with the Part 435 effluent guidelines.

    Additionally, EPA is proposing to correct some erroneous references and omissions in the method for identification of crude oil contamination (Appendix 5 of Subpart A of Part 435). Specifically, EPA is proposing to: a. Add a schematic flow for qualitative identification of crude oil, which was erroneously omitted in Appendix 5 to Subpart A of Part 435, b. Correct erroneous citations in sections 9.5, 9.6, 11.3, and 11.3.1 of Appendix 5, and c. Add a missing ``11) followed by any of the following:

    Nesslerization..... ...................... ..................... D1426-08 (A)......... 973.49,\3\ I-3520- 85.\2\

    Titration.......... ...................... 4500-NH3 C-1997......

    Electrode.......... ...................... 4500-NH3 D-1997 or E- D1426-08 (B)......... 1997.

    Manual phenate,

    ...................... 4500-NH3 F-1997...... ..................... See Footnote.\60\ salicylate, or other substituted phenols in

    Berthelot reaction based methods.

    Automated phenate, 350.1,\30\ Rev. 2.0

    4500-NH3 G-1997 4500- ..................... I-4523-85.\2\ salicylate, or

    (1993).

    NH3 H-1997. other substituted phenols in

    Berthelot reaction based methods.

    Automated electrode ...................... ..................... ..................... See footnote 7.

    Ion Chromatography. ...................... ..................... D6919-09............. 5. Antimony--Total,\4\ mg/L........ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration \36\.

    AA furnace......... ...................... 3113-2004............

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    Page 58043

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\ 6. Arsenic--Total,\4\ mg/L......... Digestion \4\ followed 206.5 (Issued by any of the

    1978).\1\ following:

    AA gaseous hydride. ...................... 3114 B-2009 or C-2009 D2972-08 (B)......... I-3062-85.\2\

    AA furnace......... ...................... 3113-2004............ D2972-08 (C)......... I-4063-98.\49\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07.............

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    Colorimetric (SDDC) ...................... 3500-As B-1997....... D2972-08 (A)......... I-3060-85.\2\ 7. Barium--Total,\4\ mg/L.......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999.......... ..................... I-3084-85.\2\ aspiration \36\.

    AA furnace......... ...................... 3113-2004............ D4382-02(07).

    .....................

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ ..................... I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP \36\........... ...................... ..................... ..................... See footnote.\34\ 8. Beryllium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999 or E-1999 D3645-08 (A)......... I-3095-85.\2\ aspiration.

    AA furnace......... ...................... 3113-2004............ D3645-08 (B).........

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP................ ...................... ..................... D4190-08............. See footnote.\34\

    Colorimetric

    ...................... ..................... ..................... See footnote.\61\

    (aluminon). 9. Biochemical oxygen demand

    Dissolved Oxygen

    ...................... 5210 B-2001.......... D888-09.............. 973.44,\3\ p. 17,\9\

    (BOD5), mg/L.

    Depletion.

    I-1578-78,\8\ See footnote.\10\ \63\ 10. Boron--Total,\37\ mg/L......... Colorimetric

    ...................... 4500-B B-2000........ ..................... I-3112-85.\2\

    (curcumin).

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP................ ...................... ..................... D4190-08............. See footnote.\34\ 11. Bromide, mg/L.................. Electrode............. ...................... ..................... D1246-05............. I-1125-85.\2\

    Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000, C-2000, D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    D-2000.

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 12. Cadmium--Total,\4\ mg/L........ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D3557-02(07) (A or B) 974.27,\3\ p. 37.\9\, aspiration \36\.

    I-3135-85 \2\ or

    I-3136-85.\2\

    AA furnace......... ...................... 3113-1999............ D3557-02(07) (D)..... I-4138-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-1472-85 \2\ or

    (2003); 200.7, Rev.

    I-4471-97.\50\ 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Voltametry \11\.... ...................... ..................... D3557-02(07)(C)......

    Page 58044

    Colorimetric

    ...................... 3500 Cd-D 1990.......

    (Dithizone). 13. Calcium--Total,\4\ mg/L........ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... D511-08(B)........... I-3152-85.\2\ aspiration.

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ ..................... I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    DCP................ ...................... ..................... ..................... See footnote.\34\

    Titrimetric (EDTA). ...................... 3500-Ca-1997......... D511-08(A)...........

    Ion Chromatography. ...................... ..................... D6919-09............. 14. Carbonaceous biochemical oxygen Dissolved Oxygen

    ...................... 5210 B-2001.......... D888-09.............. See footnote.\35\ demand (CBOD5), mg/L.\12\

    Depletion with

    \63\ nitrification inhibitor. 15. Chemical oxygen demand (COD),

    Titrimetric........... 410.3 (Rev. 1978) \1\. 5220 B-1997 or C-1997 D1252-06 (A)......... 973.46,\3\ p. 17 \9\ mg/L.

    I-3560-85.\2\

    Spectrophotometric,

    410.4, Rev. 2.0 (1993) 5220 D-1997.......... D1252-06 (B)......... See footnotes.\13\ manual or automatic.

    \14\

    I-3561-85.\2\ 16. Chloride, mg/L................. Titrimetric: (silver

    ...................... 4500-Cl- B-1997...... D512-04 (B).......... I-1183-85.\2\ nitrate).

    (Mercuric nitrate).... ...................... 4500-Cl- C-1997...... D512-04 (A).......... 973.51,\3\ I-1184- 85.\2\

    Colorimetric: manual.. ...................... ..................... ..................... I-1187-85.\2\

    Automated

    ...................... 4500-Cl- E-1997...... ..................... I-2187-85.\2\

    (Ferricyanide).

    Potentiometric

    ...................... 4500-Cl- D-1997......

    Titration.

    Ion Selective

    ...................... ..................... D512-04 (C)..........

    Electrode.

    Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30,\3\ I-2057- and 300.1, Rev. 1.0

    90.\51\

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 17. Chlorine--Total residual, mg/L. Amperometric direct... ...................... 4500-Cl D-2000....... D1253-08.............

    Amperometric direct

    ...................... 4500-Cl E-2000.......

    (low level).

    Iodometric direct..... ...................... 4500-Cl B-2000.......

    Back titration ether

    ...................... 4500-Cl C-2000....... end-point \15\.

    DPD-FAS............... ...................... 4500-Cl F-2000.......

    Spectrophotometric,

    ...................... 4500-Cl G-2000.......

    DPD.

    Electrode............. ...................... ..................... ..................... See footnote.\16\ 17A. Chlorine--Free Available, mg/L Amperometric direct... ...................... 4500-Cl D-2000....... D1253-08.............

    Amperometric direct

    ...................... 4500-Cl E-2000.......

    (low level).

    DPD-FAS............... ...................... 4500-Cl F-2000.......

    Spectrophotometric,

    ...................... 4500-Cl G-2000.......

    DPD. 18. Chromium VI dissolved, mg/L.... 0.45-micron Filtration followed by any of the following:

    AA chelation-

    ...................... 3111 C-1999.......... ..................... I-1232-85.\2\ extraction.

    Ion Chromatography. 218.6, Rev. 3.3 (1994) 3500-Cr C-2009....... D5257-03............. 993.23.

    Colorimetric

    ...................... 3500-Cr B-2009....... D1687-02(07)(A)...... I-1230-85.\2\

    (Diphenyl- carbazide). 19. Chromium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... D1687-02(07) (B)..... 974.27,\3\ I-3236- aspiration \36\.

    85.\2\

    AA chelation-

    ...................... 3111 C-1999.......... extraction.

    AA furnace......... ...................... 3113-1999............ D1687-02(07)(C)...... I-3233-93.\46\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Page 58045

    Colorimetric

    ...................... 3500-Cr B-2009.......

    (Diphenyl- carbazide). 20. Cobalt--Total,\4\ mg/L......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D3558-08 (A or B).... p. 37,\9\ I-3239- aspiration.

    85.\2\

    AA furnace......... ...................... 3113-2004............ D3558-08 (C)......... I-4243-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07............. I-4471-97.\50\

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    DCP................ ...................... ..................... D4190-08............. See footnote.\34\ 21. Color, platinum cobalt units or Colorimetric (ADMI)... ...................... ..................... ..................... See footnote.\18\ dominant wavelength, hue, luminance purity.

    (Platinum cobalt)..... ...................... 2120 B-2001.......... ..................... I-1250-85.\2\

    Spectrophotometric.... 22. Copper--Total,\4\ mg/L......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D1688-07 (A or B).... 974.27 \3\ p. 37 \9\ aspiration.\36\

    I-3270-85 \2\ or

    I-3271-85.\2\

    AA furnace......... ...................... 3113-2004............ D1688-07 (C)......... I-4274-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Colorimetric

    ...................... 3500-Cu B-1999.......

    (Neocuproine).

    (Bathocuproine).... ...................... 3500-Cu C-1999....... ..................... See footnote.\19\ 23. Cyanide--Total, mg/L........... Automated UV digestion/ ...................... ..................... ..................... Kelada-01.\55\ distillation and

    Colorimetry.

    Segmented Flow

    ...................... ..................... D7511-09e2...........

    Injection, In-Line

    Ultraviolet Digestion followed by gas diffusion amperometry.

    Manual distillation

    335.4, Rev. 1.0 (1993) 4500-CN- B-1999 or C- D2036-09(A), D7284-08 10-204-00-1-X.\56\ with MgCl2 followed

    \57\.

    1999. by any of the following:

    Flow Injection, gas ...................... ..................... D2036-09(A) D7284-08. diffusion amperometry.

    Titrimetric........ ...................... 4500-CN- D-1999...... D2036-09(A).......... p. 22.\9\

    Spectrophotometric, ...................... 4500-CN- E-1999...... D2036-09(A).......... I-3300-85.\2\ manual.

    Semi-Automated \20\ 335.4, Rev. 1.0 (1993) ..................... ..................... 10-204-00-1-X,\56\ I-

    \57\.

    4302-85.\2\

    Ion Chromatography. ...................... ..................... D2036-09(A)..........

    Ion Selective

    ...................... 4500-CN- F-1999...... D2036-09(A)..........

    Electrode. 24. Cyanide-Available, mg/L........ Cyanide Amenable to

    ...................... 4500-CN- G-1999...... D2036-09(B)..........

    Chlorination (CATC);

    Manual distillation with MgCl2 followed by Titrimetric or

    Spectrophotometric.

    Flow injection and

    ...................... ..................... D6888-09............. OIA-1677-09.\44\ ligand exchange, followed by gas diffusion amperometry

    \59\.

    Page 58046

    Automated Distillation ...................... ..................... ..................... Kelada-01.\55\ and Colorimetry (no

    UV digestion). 24.A Cyanide-Free, mg/L............ Flow Injection,

    ...................... ..................... D7237-10............. OIA-1677-09.\44\ followed by gas diffusion amperometry.

    Manual micro-diffusion ...................... ..................... D4282-02............. and colorimetry. 25. Fluoride--Total, mg/L.......... Manual distillation

    ...................... 4500-F- B-1997.......

    \6\ followed by any of the following:

    Electrode, manual.. ...................... 4500-F- C-1997....... D1179-04(B)..........

    Electrode,

    ...................... ..................... ..................... I-4327-85.\2\ automated.

    Colorimetric,

    ...................... 4500-F- D-1997....... D1179-04(A)..........

    (SPADNS).

    Automated

    ...................... 4500-F- E-1997....... complexone.

    Ion Chromatography. 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    (1997).

    CIE/UV............. ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 26. Gold--Total,\4\ mg/L........... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration,.

    AA furnace,........ 231.2 (Rev. 1978) \1\. 3113-2004............

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    DCP................ ...................... ..................... ..................... See footnote.\34\ 27. Hardness--Total, as CaCO3, mg/L Automated

    130.1 (Issued 1971) colorimetric,.

    \1\.

    Titrimetric (EDTA).... ...................... 2340 C-1997.......... D1126-02(07)......... 973.5 2B,\3\ I-1338- 85.\2\

    Ca plus Mg as their

    ...................... 2340 B-1997.......... carbonates, by inductively coupled plasma or AA direct aspiration. (See

    Parameters 13 and 33). 28. Hydrogen ion (pH), pH units.... Electrometric

    ...................... 4500-H\+\-2000....... D1293-99 (A or B).... 973.41,\3\ I-1586- measurement.

    85.\2\

    Automated electrode... 150.2 (Dec. 1982) \1\. ..................... ..................... See footnote,\21\

    I-2587-85.\2\ 29. Iridium--Total,\4\ mg/L........ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration.

    AA furnace......... 235.2 (Issued 1978).\1\

    ICP/MS............. ...................... 3125-2009............ 30. Iron--Total,\4\ mg/L........... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D1068-05 (A or B).... 974.27,\3\ I-3381- aspiration \36\.

    85.\2\

    AA furnace......... ...................... 3113-1999............ D1068-05(C)..........

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Colorimetric

    ...................... 3500-Fe-1997......... D1068-05 (D)......... See footnote.\22\

    (Phenanthroline). 31. Kjeldahl Nitrogen \5\--Total,

    Manual digestion \20\ ...................... 4500-Norg B-1997 or C- D3590-02(06)(A)...... I-4515-91.\45\

    (as N), mg/L.

    and distillation or

    1997 and 4500-NH3 B- gas diffusion

    1997. followed by any of the following:

    Titration.......... ...................... 4500-NH3 C-1997...... ..................... 973.48.\3\

    Nesslerization..... ...................... ..................... D1426-08(A)..........

    Electrode.......... ...................... 4500-NH3 D-1997 or E- D1426-08(B).......... 1997.

    Page 58047

    Semi-automated

    350.1 Rev. 2.0 1993... 4500-NH3 G-1997 4500- phenate.

    NH3 H-1997.

    Manual phenate,

    ...................... 4500-NH3 F-1997...... ..................... See Footnote.\60\ salicylate, or other substituted phenols in

    Berthelot reaction based methods.

    Automated Methods for TKN that do not require manual distillation

    Automated phenate,

    351.1, (Rev. 1978) \1\ ..................... ..................... I-4551-78.\8\ salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation).

    Semi-automated block 351.2, Rev. 2.0 (1993) 4500-Norg D-1997..... D3590-02(06) (B)..... I-4515-91.\45\ digestor colorimetric

    (distillation not required).

    Block digester,

    ...................... ..................... ..................... See footnote.\39\ followed by Auto distillation and

    Titration.

    Block digester,

    ...................... ..................... ..................... See footnote.\40\ followed by Auto distillation and

    Nesslerization.

    Block Digester,

    ...................... ..................... ..................... See footnote.\41\ followed by Flow injection gas diffusion

    (distillation not required). 32. Lead--Total,\4\ mg/L........... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D3559-08(A or B)..... 974.27,\3\ I-3399- aspiration.\36\

    85.\2\

    AA furnace......... ...................... 3113-1999............ D3559-08(D).......... I-4403-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Voltametry \11\.... ...................... ..................... D3559-08(C)..........

    Colorimetric

    ...................... 3500-Pb B-1997.......

    (Dithizone). 33. Magnesium--Total,\4\ mg/L...... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... D511-08(B)........... 974.27,\3\ I-3447- aspiration.

    85.\2\

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    DCP................ ...................... ..................... ..................... See footnote.\34\

    Gravimetric........

    Ion Chromatography. ...................... ..................... D6919-09............. 34. Manganese--Total,\4\ mg/L...... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... D858-07(A or B)...... 974.27,\3\ I-3454- aspiration \36\.

    85.\2\

    AA furnace......... ...................... 3113-2004............ D858-07(C)...........

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Page 58048

    Colorimetric

    ...................... 3500-Mn B-1999....... ..................... 920.203.\3\

    (Persulfate).

    (Periodate)........ ...................... ..................... ..................... See footnote.\23\ 35. Mercury--Total,\4\ mg/L........ Cold vapor, Manual.... 245.1, Rev. 3.0 (1994) 3112-2009............ D3223-07............. 977.22,\3\ I-3462- 85.\2\

    Cold vapor, Automated. 245.2 (Issued 1974)...

    Cold vapor atomic

    245.7, Rev. 2.0 (2005) ..................... ..................... I-4464-01. fluorescence

    \17\. spectrometry (CVAFS).

    Purge and Trap CVAFS.. 1631E.\43\

    ICP/AES \36\.......... 200.7, Rev. 4.4 (1994) 3120-1999............ ..................... I-4471-97.\50\

    ICP/MS................ ...................... 3125-2009............ 36. Molybdenum--Total,\4\ mg/L..... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999.......... ..................... I-3490-85.\2\ aspiration.

    AA furnace......... ...................... 3113-2004............ ..................... I-3492-96.\47\

    ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07............. I-4471-97.\50\

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP................ ...................... ..................... ..................... See footnote.\34\ 37. Nickel--Total,\4\ mg/L......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D1886-08(A or B)..... I-3499-85.\2\ aspiration \36\.

    AA furnace......... ...................... 3113-2004............ D1886-08(C).......... I-4503-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\ 38. Nitrate (as N), mg/L........... Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\

    Ion Selective

    ...................... 4500-NO3- D-2000.....

    Electrode.

    Colorimetric (Brucine 352.1 \1\............. ..................... ..................... 973.50,\3\ 419D,\1\ sulfate).

    \7\ p. 28.\9\

    Nitrate-nitrite N

    ...................... ..................... ..................... See footnote.\62\ minus Nitrite N (See parameters 39 and 40). 39. Nitrate-nitrite (as N), mg/L... Cadmium reduction,

    ...................... 4500-NO3- E-2000..... D3867-04(B)..........

    Manual.

    Cadmium reduction,

    353.2, Rev. 2.0 (1993) 4500-NO3- F-2000..... D3867-04(A).......... I-2545-90.\2\

    Automated.

    Automated hydrazine... ...................... 4500-NO3- H-2000.....

    Reduction/Colorimetric ...................... ..................... ..................... See footnote.\62\

    Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 40. Nitrite (as N), mg/L........... Spectrophotometric:

    ...................... 4500-NO2- B-2000..... ..................... See footnote.\25\

    Manual.

    Automated

    ...................... ..................... ..................... I-4540-85,\2\ See

    (Diazotization).

    footnote.\62\

    Automated (*bypass

    353.2, Rev. 2.0 (1993) 4500-NO3- F-2000..... D3867-04 (A)......... I-4545-85.\2\ cadmium reduction).

    Manual (*bypass

    ...................... 4500-NO3- E-2000..... D3867-04 (B)......... cadmium reduction).

    Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev.2.\54\ 41. Oil and grease--Total

    Hexane extractable

    1664B \42\............ 5520 B-2001.\38\ recoverable, mg/L.

    material (HEM): n-

    Hexane extraction and gravimetry.

    Page 58049

    Silica gel treated HEM 1664B \42\............ 5520 B-2001 \38\ and

    (SGT-HEM): Silica gel

    5520 F-2001.\38\ treatment and gravimetry. 42. Organic carbon--Total (TOC), mg/ Combustion............ ...................... 5310 B-2000.......... D7573-09............. 973.47,\3\ p. 14.\24\

    L.

    Heated persulfate or

    ...................... 5310 C 2000 5310 D

    D4839-03............. 973.47,\3\ p. 14.\24\

    UV persulfate

    2000. oxidation. 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.......... 365.1, Rev. 2.0 (1993) 4500-P F-1999 or G-

    ..................... 973.56,\3\ I-4601- 1999.

    85.\2\

    Manual single

    ...................... 4500-P E-1999........ D515-88(A)........... 973.55.\3\ reagent.

    Manual two reagent. 365.3 (Issued 1978).\1\

    Ion Chromatography. 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\ and 300.1, Rev. 1.0

    (1997).

    CIE/UV............. ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 45. Osmium--Total,\4\ mg/L......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999.......... aspiration.

    AA furnace......... 252.2 (Issued 1978)

    \1\ 46. Oxygen, dissolved, mg/L........ Winkler (Azide

    ...................... 4500-O B-2001, C-

    D888-09(A)........... 973.45B,\3\ I-1575- modification).

    2001, D-2001, E-

    78.\8\ 2001, F-2001.

    Electrode............. ...................... 4500-O G-2001........ D888-09(B)........... I-1576-78.\8\

    Luminescence Based

    ...................... ..................... D888-09 \68\ (C)..... See footnote \63\

    Sensor.

    \68\ See footnote.\64\ 47. Palladium--Total,\4\ mg/L...... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration.

    AA furnace......... 253.2 \1\ (Issued 1978).

    ICP/MS............. ...................... 3125-2009............

    DCP................ ...................... ..................... ..................... See footnote.\34\ 48. Phenols, mg/L.................. Manual distillation

    420.1 \1\ (Rev. 1978). 5530B-2005........... D1783-01.............

    \26\ followed by any of the following:

    Colorimetric (4AAP) 420.1 \1\ (Rev. 1978). 5530D-2005 \27\...... D1783-01(A or B)..... manual.

    Automated

    420.4, Rev. 1.0 (1993) colorimetric

    (4AAP). 49. Phosphorus (elemental), mg/L... Gas-liquid

    ...................... ..................... ..................... See footnote.\28\ chromatography. 50. Phosphorus--Total, mg/L........ Persulfate digestion

    ...................... 4500-P B(5)-1999..... ..................... 973.55.\3\

    \20\ followed by any of the following:

    Manual............. 365.3 \1\ (Issued

    4500-P E-1999........ D515-88(A)........... 1978).

    Automated ascorbic 365.1, Rev. 2.0 (1993) 4500-P F-1999, G-

    ..................... 973.56,\3\ I-4600- acid reduction.

    1999, H-1999.

    85.\2\

    ICP/AES \4\ \36\... 200.7, Rev. 4.4 (1994) 3120-1999............ ..................... I-4471-97.\50\

    Semi-automated

    365.4 \1\ (Issued

    ..................... D515-88(B)........... I-4610-91.\48\ block digestor

    1974).

    (TKP digestion). 51. Platinum--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration.

    AA furnace......... 255.2.\1\

    ICP/MS............. ...................... 3125-2009............

    DCP................ ...................... ..................... ..................... See footnote.\34\ 52. Potassium--Total,\4\ mg/L...... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... ..................... 973.53,\3\ I-3630- aspiration.

    85.\2\

    Page 58050

    ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    Flame photometric.. ...................... 3500-K B-1997........

    Electrode.......... ...................... 3500-K C-1997........

    Ion Chromatography. ...................... ..................... D6919-09............. 53. Residue--Total, mg/L........... Gravimetric, 103-

    ...................... 2540 B-1997.......... ..................... I-3750-85.\2\ 105[deg]. 54. Residue--filterable, mg/L...... Gravimetric, 180[deg]. ...................... 2540 C-1997.......... D5907-03............. I-1750-85.\2\ 55. Residue--non-filterable (TSS), Gravimetric, 103-

    ...................... 2540 D-1997.......... D5907-03............. I-3765-85.\2\ mg/L.

    105[deg] post washing of residue. 56. Residue--settleable, mg/L...... Volumetric, (Imhoff

    ...................... 2540 F-1997.......... cone), or gravimetric. 57. Residue--Volatile, mg/L........ Gravimetric, 550[deg]. 160.4 \1\............. 2540-E-1997.......... ..................... I-3753-85.\2\ 58. Rhodium--Total,\4\ mg/L........ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration, or.

    AA furnace......... 265.2.\1\

    ICP/MS............. ...................... 3125-2009............ 59. Ruthenium--Total,\4\ mg/L...... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration, or.

    AA furnace......... 267.2.\1\

    ICP/MS............. ...................... 3125-2009............ 60. Selenium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA furnace......... ...................... 3113-2004............ D3859-08 (B)......... I-4668-98.\49\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07.............

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05

    AA gaseous hydride. ...................... 3114 B-2009, or C-

    D3859-08 (A)......... I-3667-85.\2\ 2009. 61. Silica--Dissolved,\37\ mg/L.... 0.45 micron filtration followed by any of the following:

    Colorimetric,

    ...................... 4500-SiO2 C-1997..... D859-05.............. I-1700-85.\2\

    Manual.

    Automated

    ...................... 4500-SiO2 E-1997 or F- ..................... I-2700-85.\2\

    (Molybdosilicate).

    1997.

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ ..................... I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\ 62. Silver--Total,4 31 mg/L........ Digestion 4 29 followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 ..................... 974.27,\3\ p. 37,\9\ aspiration.

    I-3720-85.\2\

    AA furnace......... ...................... 3113 -1999........... ..................... I-4724-89.\51\

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\

    DCP................ ...................... ..................... ..................... See footnote.\34\ 63. Sodium--Total,\4\ mg/L......... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... ..................... 973.54,\3\ I-3735- aspiration.

    85.\2\

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ ..................... I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    Page 58051

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\

    DCP................ ...................... ..................... ..................... See footnote.\34\

    Flame photometric.. ...................... 3500-Na B-1997.......

    Ion Chromatography. ...................... ..................... D6919-09............. 64. Specific conductance, micromhos/ Wheatstone bridge..... 120.1 \1\ (Rev. 1982). 2510 -1997........... D1125-99 (A)......... 973.40,\3\ I-2781- cm at 25 [deg]C.

    85.\2\ 65. Sulfate (as SO4), mg/L......... Automated colorimetric 375.2, Rev. 2.0 (1993) 4500-SO42- F-1997 or

    G-1997.

    Gravimetric........... ...................... 4500-SO42- C-1997 or ..................... 925.54.\3\

    D-1997.

    Turbidimetric......... ...................... 4500-SO42- E-1997.... D516-07..............

    Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30,\3\ I-4020-05. and 300.1, Rev. 1.0

    (1997).

    CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\ 66. Sulfide (as S), mg/L........... Sample Pretreatment... ...................... 4500-S 2- B, C-2000..

    Titrimetric (iodine).. ...................... 4500-S 2- F-2000..... ..................... I-3840-85.\2\

    Colorimetric

    ...................... 4500-S 2- D-2000.....

    (methylene blue).

    Ion Selective

    ...................... 4500-S 2- G-2000..... D4658-08.............

    Electrode. 67. Sulfite (as SO3), mg/L......... Titrimetric (iodine-

    ...................... 4500-SO32- B-2000.... iodate). 68. Surfactants, mg/L.............. Colorimetric

    ...................... 5540 C-2000.......... D2330-02.............

    (methylene blue). 69. Temperature, [deg]C............ Thermometric.......... ...................... 2550 B-2000.......... ..................... See footnote.\32\ 70. Thallium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... aspiration.

    AA furnace......... 279.2 \1\ (Issued

    3113-2004............ 1978).

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07.............

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471- 97.\50\ 71. Tin--Total,\4\ mg/L............ Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999.......... ..................... I-3850-78.\8\ aspiration.

    AA furnace......... ...................... 3113-2004............

    STGFAA............. 200.9, Rev. 2.2 (1994)

    ICP/AES............ 200.5, Rev. 4.2

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\ 72. Titanium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999.......... aspiration.

    AA furnace......... 283.2 \1\(Issued 1978)

    DCP................ ...................... ..................... ..................... See footnote.\34\

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\ 73. Turbidity, NTU \53\............ Nephelometric......... 180.1, Rev. 2.0 (1993) 2130-2001............ D1889-00............. I-3860-85.\2\ See footnote.\65\ See footnote.\66\ See footnote.\67\ 74. Vanadium--Total,\4\ mg/L....... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 D-1999.......... aspiration.

    AA furnace......... ...................... 3113-2004............ D3373-03(07).........

    ICP/AES............ 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    DCP................ ...................... ..................... D4190-08............. See footnote.\34\

    Page 58052

    Colorimetric

    ...................... 3500-V B-1997........

    (Gallic Acid). 75. Zinc--Total,\4\ mg/L........... Digestion \4\ followed by any of the following:

    AA direct

    ...................... 3111 B-1999 or C-1999 D1691-02(07) (A or B) 974.27,\3\ p. 37,\9\ aspiration \36\.

    I-3900-85.\2\

    AA furnace......... 289.2\1\ (Issued 1978)

    ICP/AES \36\....... 200.5, Rev. 4.2

    3120-1999............ D1976-07............. I-4471-97.\50\

    (2003); 200.7, Rev. 4.4 (1994).

    ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.

    DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\

    Colorimetric

    (Dithizone).

    (Zincon)........... ...................... 3500-Zn-1997......... ..................... See footnote.\33\ 76. Acid Mine Drainage............. ...................... 1627..................

    Table 1B Notes:

    \1\ ``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.

    \2\ 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.

    \3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' Methods Manual, Sixteenth Edition, 4th Revision, 1998.

    \4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in

    Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as

    Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in

    EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or 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.

    \5\ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.

    \6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to resolve any controversies. In general, the analytical method should be consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is defined as 0.2.

    \28\ 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.

    \29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.

    \30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method specified quality control acceptance criteria are met.

    \31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH >7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.

    \32\ 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.

    \33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.

    \34\ ``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.

    \35\ In-Situ Method 1004-8-2009, ``Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe''. Available from In-Situ, Incorporated, 221 E. Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970-498-1500.

    \36\ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. ``Closed Vessel Microwave Digestion of Wastewater

    Samples for Determination of Metals'', CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation.

    \37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.

    \38\ Only use n-hexane (n-Hexane -- 85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining

    Oil and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664B). Use of other extraction solvents is prohibited.

    \39\ 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.

    \40\ 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.

    \41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/96, OI Analytical/ALPKEM, P.O. Box 9010,

    College Station, TX 77842.

    \42\ Method 1664, Revision B is the revised version of EPA Method 1664A.

    \43\ 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.

    \44\ Available Cyanide, Method OIA-1677-09, ``Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,'' ALPKEM, A Division of OI

    Analytical, P.O. Box 9010, College Station, TX 77842-9010.

    \45\ ``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.

    \46\ ``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.

    \47\ ``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.

    \48\ ``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.

    \49\ ``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.

    \50\ ``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.

    \51\ ``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.

    \52\ Unless otherwise indicated, 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.

    \53\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.

    \54\ Method D6508, 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.

    \55\ Kelada-01, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,'' EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.

    \56\ QuikChem Method 10-204-00-1-X, ``Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of

    Cyanide by Flow Injection Analysis'' is available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414-358-4200.

    Page 58054

    \57\ When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to distillation.

    \58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method, approved digestion and/or distillation are required prior to analysis.

    \59\ Samples analyzed for available cyanide using Methods OIA-1677-09 or D6888-09 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.

    \60\ Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color reagent in Berthelot Reaction (``phenol-hypochlorite reaction'') colorimetric ammonium determination methods. For example when phenol is used as the color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively--see, C.J. Patton and S.R. Crouch, Anal. Chem.

    (1977) 49, 464-469. These reaction parameters increase to pH >12.6 and 665 nm when salicylate is used as the color reagent--see, M.D. Krom, Analyst

    (1980) 105, 305-316.

    \61\ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may be used. This method has poorer precision and bias than the methods of choice.

    \62\ Systea Easy (1-Reagent) Nitrate Method, February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific, LLC., 900 Jorie Blvd., Suite 35, Oak Brook, IL 60523.

    \63\ Hach Method 10360, ``Luminescence Measurement of Dissolved Oxygen (LDO[supreg]) in Water and Wastewater, Revision 1.1 dated January 4, 2006''.

    Available from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539, Telephone: 970-669-3050.

    \64\ In-Situ Method 1002-8-2009, ``Dissolved Oxygen (DO) Measurement by Optical Probe'', 1003-8-2009. Available from In-Situ, Incorporated, 221 E.

    Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970-498-1500.

    \65\ Mitchell Method M5331, ``Determination of Turbidity by Nephlometry'', Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 656

    Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630-645-0600.

    \66\ Mitchell Method M5271, ``Determination of Turbidity by Nephlometry'', Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 656

    Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630-645-0600.

    \67\ Thermo Scientific's Orion Method AQ4500, Revision 5, March 12, 2009, ``Determination of Turbidity by Nephlometry''. Available from Thermo

    Scientific, 166 Cummings Center, Beverly, MA 01915, Phone: 1-800-225-1480, http://www.thermo.com.

    \68\ This method may be used to measure dissolved oxygen when performing methods approved in Table 1B for measurement of biochemical oxygen demand for compliance monitoring under the Clean Water Act.

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

    Parameter \1\

    Method

    EPA \2\ \7\

    Standard methods

    ASTM

    Other

    1. Acenaphthene.................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 2. Acenaphthylene.................. GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 3. Acrolein........................ GC.................... 603...................

    GC/MS................. 624,\4\ 1624B......... 4. Acrylonitrile................... GC.................... 603...................

    GC/MS................. 624,\4\ 1624B......... 5. Anthracene...................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440B-00............. D4657-92 (99)........ 6. Benzene......................... GC.................... 602................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 7. Benzidine....................... Spectrophotometric.... ...................... ..................... ..................... See footnote,\3\ p.1.

    GC/MS................. 625,\5\ 1625B......... 6410 B-00............

    HPLC.................. 605................... 8. Benzo(a)anthracene.............. GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 9. Benzo(a)pyrene.................. GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 10. Benzo(b)fluoranthene........... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 11. Benzo(g,h,i)perylene........... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 12. Benzo(k)fluoranthene........... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 13. Benzylchloride................. GC.................... ...................... ..................... ..................... See footnote,\3\ p. 130.

    Page 58055

    GC/MS................. ...................... ..................... ..................... See footnote,\6\ p.

    S102. 14. Butyl benzyl phthalate......... GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 15. Bis(2-chloroethoxy) methane.... GC.................... 611...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 16. Bis(2-chloroethyl) ether....... GC.................... 611...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 17. Bis(2-ethylhexyl) phthalate.... GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 18. Bromodichloromethane........... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 19. Bromoform...................... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 20. Bromomethane................... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 21. 4-Bromophenyl phenyl ether..... GC.................... 611...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 22. Carbon tetrachloride........... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 23. 4-Chloro-3-methylphenol........ GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 24. Chlorobenzene.................. GC.................... 601, 602.............. 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 25. Chloroethane................... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 26. 2-Chloroethylvinyl ether....... GC.................... 601...................

    GC/MS................. 624, 1624B............ 27. Chloroform..................... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 28. Chloromethane.................. GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 29. 2-Chloronaphthalene............ GC.................... 612................... 6410 B-00............

    GC/MS................. 625, 1625B............ ..................... ..................... See footnote,\9\ p. 27. 30. 2-Chlorophenol................. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 31. 4-Chlorophenyl phenyl ether.... GC.................... 611...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 32. Chrysene....................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 33. Dibenzo(a,h)anthracene......... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 34. Dibromochloromethane........... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 35. 1,2-Dichlorobenzene............ GC.................... 601,602............... 6200 C-97............

    GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p. 27. 36. 1,3-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-97............

    GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p. 27. 37. 1,4-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-97............

    GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p. 27. 38. 3,3-Dichlorobenzidine.......... GC/MS................. 625, 1625B........... 6410 B-00............

    HPLC.................. 605...................

    Page 58056

    39. Dichlorodifluoromethane........ GC.................... 601...................

    GC/MS................. ...................... 6200 C-97............ 40. 1,1-Dichloroethane............. GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 41. 1,2-Dichloroethane............. GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 42. 1,1-Dichloroethene............. GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 43. trans-1,2-Dichloroethene....... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 44. 2,4-Dichlorophenol............. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 45. 1,2-Dichloropropane............ GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 46. cis-1,3-Dichloropropene........ GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 47. trans-1,3-Dichloropropene...... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 48. Diethyl phthalate.............. GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 49. 2,4-Dimethylphenol............. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 50. Dimethyl phthalate............. GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 51. Di-n-butyl phthalate........... GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 52. Di-n-octyl phthalate........... GC.................... 606...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 53. 2,3-Dinitrophenol.............. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ 54. 2,4-Dinitrotoluene............. GC.................... 609...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 55. 2,6-Dinitrotoluene............. GC.................... 609...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 56. Epichlorohydrin................ GC.................... ...................... ..................... ..................... See footnote,\3\ p. 130.

    GC/MS................. ...................... ..................... ..................... See footnote,\6\ p.

    S102. 57. Ethylbenzene................... GC.................... 602................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 58. Fluoranthene................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 59. Fluorene....................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 60. 1,2,3,4,6,7,8-Heptachloro-

    GC/MS................. 1613B................. dibenzofuran. 61. 1,2,3,4,7,8,9-Heptachloro-

    GC/MS................. 1613B................. dibenzofuran. 62. 1,2,3,4,6,7,8-

    GC/MS................. 1613B.................

    Heptachlorodibenzo-p-dioxin. 63. Hexachlorobenzene.............. GC.................... 612...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 64. Hexachlorobutadiene............ GC.................... 612...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 65. Hexachlorocyclopentadiene...... GC.................... 612...................

    GC/MS................. 625,\5\ 1625B......... 6410 B-00............ ..................... See footnote,\9\ p. 27. 66. 1,2,3,4,7,8-

    GC/MS................. 1613B.................

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

    GC/MS................. 1613B.................

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

    GC/MS................. 1613B.................

    Hexachlorodibenzofuran.

    Page 58057

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

    GC/MS................. 1613B.................

    Hexachlorodibenzofuran. 70. 1,2,3,4,7,8-Hexachlorodibenzo-p- GC/MS................. 1613B................. dioxin. 71. 1,2,3,6,7,8-Hexachlorodibenzo-p- GC/MS................. 1613B................. dioxin. 72. 1,2,3,7,8,9-Hexachlorodibenzo-p- GC/MS................. 1613B................. dioxin. 73. Hexachloroethane............... GC.................... 612...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 74. Ideno(1,2,3-cd) pyrene......... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 75. Isophorone..................... GC.................... 609...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 76. Methylene chloride............. GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 77. 2-Methyl-4,6-dinitrophenol..... GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 78. Naphthalene.................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ 79. Nitrobenzene................... GC.................... 609...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. ...................... ..................... D4657-92 (99)........ 80. 2-Nitrophenol.................. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 81. 4-Nitrophenol.................. GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 82. N-Nitrosodimethylamine......... GC.................... 607...................

    GC/MS................. 625 \5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p. 27. 83. N-Nitrosodi-n-propylamine...... GC.................... 607...................

    GC/MS................. 625\5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p. 27. 84. N-Nitrosodiphenylamine......... GC.................... 607...................

    GC/MS................. 625 \5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p. 27. 85. Octachlorodibenzofuran......... GC/MS................. 1613B \10\............ 86. Octachlorodibenzo-p-dioxin..... GC/MS................. 1613B \10\............ 87. 2,2'-Oxybis(2-chloropropane)

    GC.................... 611...................

    also known as bis(2- chloroisopropyl) ether

    .

    GC/MS................. 625, 1625B............ 6410 B-00............ 88. PCB-1016....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\

    GC/MS................. 625................... 6410 B-00............ 89. PCB-1221....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\

    GC/MS................. 625................... 6410 B-00............ 90. PCB-1232....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\

    GC/MS................. 625................... 6410 B-00............ 91. PCB-1242....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\

    GC/MS................. 625................... 6410 B-00............ 92. PCB-1248....................... GC.................... 608...................

    GC/MS................. 625................... 6410 B-00............ 93. PCB-1254....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\

    GC/MS................. 625................... 6410 B-00............

    Page 58058

    94. PCB-1260....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p. 43; See footnote.\8\.

    GC/MS................. 625................... 6410 B-00............ 95. 1,2,3,7,8-Pentachloro-

    GC/MS................. 1613B................. dibenzofuran. 96. 2,3,4,7,8-Pentachloro-

    GC/MS................. 1613B................. dibenzofuran. 97. 1,2,3,7,8,-Pentachlorodibenzo-p- GC/MS................. 1613B................. dioxin. 98. Pentachlorophenol.............. GC.................... 604................... 6420 B-00............ ..................... See footnote,\3\ p. 140.

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 99. Phenanthrene................... GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 100. Phenol........................ GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 101. Pyrene........................ GC.................... 610...................

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27.

    HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........ 102. 2,3,7,8-Tetra-

    GC/MS................. 1613B................. chlorodibenzofuran. 103. 2,3,7,8-Tetra-chlorodibenzo-p- GC/MS................. 613, 625,\5a\ 1613B... dioxin. 104. 1,1,2,2-Tetra-chloro ethane... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 105. Tetrachloroethene............. GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 106. Toluene....................... GC.................... 602................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 107. 1,2,4-Trichlorobenzene........ GC.................... 612................... ..................... ..................... See footnote,\3\ p. 130.

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 108. 1,1,1-Trichloroethane......... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 109. 1,1,2-Trichloroethane......... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p. 130.

    GC/MS................. 624, 1624B............ 6200 B-97............ 110. Trichloroethene............... GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 111. Trichlorofluoromethane........ GC.................... 601................... 6200 C-97............

    GC/MS................. 624................... 6200 B-97............ 112. 2,4,6-Trichlorophenol......... GC.................... 604................... 6420 B-00............

    GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p. 27. 113. Vinyl chloride................ GC.................... 601................... 6200 C-97............

    GC/MS................. 624, 1624B............ 6200 B-97............ 114. Nonylphenol................... GC/MS................. ...................... ..................... D7065-06.............

    LC/MS/MS.............. ...................... ..................... D7485-09............. 115. Bisphenol A (BPA)............. GC/MS................. ...................... ..................... D7065-06.............

    LC/MS/MS.............. ...................... ..................... D7574-09............. 116. p-tert-Octylphenol (OP)....... GC/MS................. ...................... ..................... D7065-06.............

    LC/MS/MS.............. ...................... ..................... D7485-09............. 117. Nonylphenol Monoethoxylate

    GC/MS................. ...................... ..................... D7065-06.............

    (NP1EO).

    LC/MS/MS.............. ...................... ..................... D7485-09............. 118. Nonylphenol Diethoxylate

    GC/MS................. ...................... ..................... D7065-06.............

    (NP2EO).

    LC/MS/MS.............. ...................... ..................... D7485-09............. 119. Polybrominated diphenyl ethers HRGC/HRMS............. 1614A.................

    (PBDEs) 49 congeners. 120. Polychlorinated biphenyls

    HRGC/HRMS............. 1668C.................

    (PCBs) 209 Congeners. 121. Adsorbable Organic Halides

    Adsorption and

    1650..................

    (AOX).

    Coulometric Titration.

    Page 58059

    122. Chlorinated Phenolics......... In Situ Acetylation

    1653.................. and GC/MS.

    Table IC notes:

    \1\ All parameters are expressed in micrograms per liter ([mu]g/L) except for Method 1613B in which the parameters are expressed in picograms per liter

    (pg/L).

    \2\ The full text of Methods 601-613, 624, 625, 1624B, and 1625B, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The full text of Method 1613B is incorporated by reference into this Part 136 and is available from the National Technical Information

    Services as stock number PB95-104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection Limit,'' of this Part 136. The full text of Methods 1613B, 1614A, 1650, 1653, and 1668C are available from EPA Office of Water (4303T) 1200 Pennsylvannia Ave, NW, Washington, DC 20460.

    \3\ ``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection

    Agency, September, 1978.

    \4\ Method 624 may be used for definitive determination of Acrolein and Acrylonitrile.

    \5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.

    \5a\ 625, screening only.

    \6\ ``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).

    \7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624B, and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

    \8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore \TM\ Disk'' 3M Corporation Revised 10/28/94.

    \9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic

    Constituents in Water and Fluvial Sediments,'' U.S. Geological Survey, Open File Report 93-125.

    \10\ Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities.

    Table ID--List of Approved Test Procedures for Pesticides \1\

    Parameter

    Method

    EPA 2 7 10

    Standard methods

    ASTM

    Other

    1. Aldrin......................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-96

    See footnote,\3\ p.

    (02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 2. Ametryn........................ GC........................ 507, 619............. ..................... .................... See footnote,\3\ p. 83; See footnote,\9\ O-3106- 93; See footnote,\6\ p.

    S68.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\14\ O- 1121-91. 3. Aminocarb...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 94; See footnote,\6\ p.

    S60.

    HPLC...................... 632.................. 4. Atraton........................ GC........................ 619.................. ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68. 5. Atrazine....................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68; See footnote,\9\ O-3106- 93.

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95. 6. Azinphos methyl................ GC........................ 614, 622, 1657....... ..................... .................... See footnote,\3\ p. 25; See footnote,\6\ p.

    S51.

    GC MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 7. Barban......................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 8. [alpha]-BHC.................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\8\ 3M0222.

    GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\11\ O- 1126-95. 9. [beta]-BHC..................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\8\ 96(02).

    3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 10. [delta]-BHC................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\8\ 96(02).

    3M0222.

    Page 58060

    GC/MS..................... 625.................. 6410 B-00............ 11. [gamma]-BHC (Lindane)......... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\11\ O- 1126-95. 12. Captan........................ GC........................ 617.................. 6630 B-00............ D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7. 13. Carbaryl...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 94, See footnote,\6\ p.

    S60.

    HPLC...................... 531.1, 632...........

    HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O- 2060-01.

    GC/MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 14. Carbophenothion............... GC........................ 617.................. 6630 B-00............ .................... See footnote,\6\ p.

    S73. 15. Chlordane..................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 16. Chloropropham................. TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 17. 2,4-D......................... GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p. 115; See footnote,\4\ O-3105- 83.

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 18. 4,4'-DDD...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3105-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 19. 4,4'-DDE...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ .................... See footnote,\11\ O- 1126-95. 20. 4,4'-DDT...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 21. Demeton-O..................... GC........................ 614, 622............. ..................... .................... See footnote,\3\ p. 25; See footnote,\6\ p.

    S51. 22. Demeton-S..................... GC........................ 614, 622............. ..................... .................... See footnote,\3\ p. 25; See footnote,\6\ p.

    S51. 23. Diazinon...................... GC........................ 507, 614, 622, 1657.. ..................... .................... See footnote,\3\ p. 25; See footnote,\4\ O-3104- 83; See footnote,\6\ p.

    S51.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95. 24. Dicamba....................... GC........................ 615.................. ..................... .................... See footnote,\3\ p. 115.

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 25. Dichlofenthion................ GC........................ 622.1................ ..................... .................... See footnote,\6\ p.

    S73. 26. Dichloran..................... GC........................ 608.2, 617........... 6630 B-00............ .................... See footnote,\3\ p. 7. 27. Dicofol....................... GC........................ 617.................. 6630 B-00............ .................... See footnote,\4\ O- 3104-83. 28. Dieldrin...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ .................... See footnote,\11\ O- 1126-95. 29. Dioxathion.................... GC........................ 614.1, 1657.......... ..................... .................... See footnote,\6\ p.

    S73. 30. Disulfoton.................... GC........................ 507, 614, 622, 1657.. ..................... .................... See footnote,\3\ p. 25; See footnote,\6\ p.

    S51.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95. 31. Diuron........................ TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O- 2060-01. 32. Endosulfan I.................. GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M022.

    GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\13\ O- 2002-01. 33. Endosulfan II................. GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\8\ 3M0222.

    GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\13\ O- 2002-01. 34. Endosulfan Sulfate............ GC........................ 608, 617............. 6630 C-00............ .................... See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............

    Page 58061

    35. Endrin........................ GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 1656.

    96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 525.1, 525.2, 625 \5\ 6410 B-00............ 36. Endrin aldehyde............... GC........................ 608, 617............. 6630 C-00............ .................... See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 37. Ethion........................ GC........................ 614, 614.1,1657...... ..................... .................... See footnote,\6\ p.

    S73.

    GC/MS..................... ..................... ..................... .................... See footnote,\13\ O- 2002-01. 38. Fenuron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 39. Fenuron-TCA................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 40. Heptachlor.................... GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 1656.

    96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 525.1, 525.2, 625.... 6410 B-00............ 41. Heptachlor epoxide............ GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\6\ p.

    S73; See footnote,\8\ 3M0222.

    GC/MS..................... 625.................. 6410 B-00............ 42. Isodrin....................... GC........................ 617.................. 6630 B-00 & C-00..... .................... See footnote,\4\ O- 3104-83; See footnote,\6\ p.

    S73. 43. Linuron....................... GC........................ ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O- 2060-01.

    GC/MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 44. Malathion..................... GC........................ 614, 1657............ 6630 B-00............ .................... See footnote,\3\ p. 25; See footnote,\6\ p.

    S51.

    GC/MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 45. Methiocarb.................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 94; See footnote,\6\ p.

    S60.

    HPLC...................... 632..................

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 46. Methoxychlor.................. GC........................ 505, 508, 608.2, 617, 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 1656.

    96(02).

    7; See footnote,\4\

    O-3104-83; See footnote,\8\ 3M0222.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95. 47. Mexacarbate................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 94; See footnote,\6\ p.

    S60.

    HPLC...................... 632.................. 48. Mirex......................... GC........................ 617.................. 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7; See footnote,\4\

    O-3104-83. 49. Monuron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 50. Monuron-TCA................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 51. Neburon....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 52. Parathion methyl.............. GC........................ 614, 622, 1657....... 6630 B-00............ .................... See footnote,\3\ p. 25.

    GC/MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 53. Parathion ethyl............... GC........................ 614.................. 6630 B-00............ .................... See footnote,\3\ p. 25.

    GC/MS..................... ..................... ..................... .................... See footnote,\11\ O- 1126-95. 54. PCNB.......................... GC........................ 608.1, 617........... 6630 B-00............ D3086-90, D5812-

    See footnote,\3\ p. 96(02).

    7. 55. Perthane...................... GC........................ 617.................. 6630 B-00............ D3086-90, D5812-

    See footnote,\4\ O- 96(02).

    3104-83. 56. Prometon...................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68; See footnote,\9\ O-3106- 93.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95.

    Page 58062

    57. Prometryn..................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68; See footnote,\9\ O-3106- 93.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\13\ O- 2002-01. 58. Propazine..................... GC........................ 507, 619, 1656....... ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68; See footnote,\9\ O-3106- 93.

    GC/MS..................... 525.1, 525.2......... 59. Propham....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 60. Propoxur...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 94; See footnote,\6\ p.

    S60.

    HPLC...................... 632.................. 61. Secbumeton.................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68.

    GC........................ 619.................. 62. Siduron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632..................

    HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O- 2060-01. 63. Simazine...................... GC........................ 505, 507, 619, 1656.. ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68; See footnote,\9\ O-3106- 93.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95. 64. Strobane...................... GC........................ 617.................. 6630 B-00 & C-00..... .................... See footnote,\3\ p. 7. 65. Swep.......................... TLC....................... ..................... ..................... .................... See footnote,\3\ p. 104; See footnote,\6\ p.

    S64.

    HPLC...................... 632.................. 66. 2,4,5-T....................... GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p. 115; See footnote,\4\ O-3105- 83. 67. 2,4,5-TP (Silvex)............. GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p. 115; See footnote,\4\ O-3105- 83. 68. Terbuthylazine................ GC........................ 619, 1656............ ..................... .................... See footnote,\3\ p. 83; See footnote,\6\ p.

    S68.

    GC/MS..................... ..................... ..................... .................... See footnote,\13\ O- 2002-01. 69. Toxaphene..................... GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812-

    See footnote,\3\ p. 1656.

    96(02).

    115; See footnote,\4\ O-3105- 83.

    GC/MS..................... 525.1, 525.2, 625.... 6410 B-00............ 70. Trifluralin................... GC........................ 508, 617, 627, 1656.. 6630 B-00............ .................... See footnote,\3\ p. 7; See footnote,\9\

    O-3106-93.

    GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O- 1126-95.

    Table ID notes:

    \1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where entries are listed by chemical name.

    \2\ The full text of Methods 608 and 625 are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection Limit,'' of this Part 136.

    \3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection

    Agency, September 1978. This EPA publication includes thin-layer chromatography (TLC) methods.

    \4\ ``Methods for Analysis of Organic Substances in Water and Fluvial Sediments,'' Techniques of Water-Resources Investigations of the U.S. Geological

    Survey, Book 5, Chapter A3 (1987).

    \5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,

    Method 608 is the preferred method.

    \6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of

    Standard Methods for the Examination of Water and Wastewater (1981).

    \7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625

    (See Appendix A of this Part 136) in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on- going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

    \8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'', 3M Corporation, Revised 10/28/94.

    \9\ USGS Method 0-3106-93 from ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Triazine and

    Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors'' U.S. Geological Survey Open File Report 94-37.

    \10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in ``Methods for the Determination of Nonconventional

    Pesticides in Municipal and Industrial Wastewater,'' EPA 821-R-92-002, April 1992.

    Page 58063

    \11\ O-1126-95 GC/MS: Zaugg, S.D., Sandstrom, M.W., Smith, S.G., and Fehlberg, K.M., 1995, Methods of Analysis by the U.S. Geological Survey National

    Water Quality Laboratory--Determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring: U.S. Geological Survey Open-File Report 95-181, Method O-1126-95, 49 p.

    \12\ O-2060-01 LC/MS: Furlong, E.T., Anderson, B.D., Werner, S.L., Soliven, P.P., Coffey, L.J., and Burkhardt, M.R., 2001, Methods of Analysis by the

    U.S. Geological Survey National Water Quality Laboratory-Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and

    High-Performance Liquid Chromatography/Mass Spectrometry: U.S. Geological Survey Water-Resources Investigations Report 01-4134 Method O-2060-01, 73 p.

    \13\ O-2002-01 Sandstrom, M.W., Stroppel, M.E., Foreman, W.T., and Schroeder, M.P., 2001, Methods of Analysis by the U.S. Geological Survey National

    Water Quality Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/ mass spectrometry: U.S. Geological Survey Water-Resources Investigations Report 01-4098, Method O-2002-01, 70 p.

    \14\ O-1121-91: Sandstrom, M.W., Wydoski, D.S., Schroeder, M.P., Zamboni, J.L., and Foreman, W.T., 1992, Methods of Analysis by the U.S. Geological

    Survey National Water Quality Laboratory--Determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring,: U.S. Geological Survey Open-File Report 91-519; O-1121-91, 34 p.

    * * * * *

    Table IG--Test Methods for Pesticide Active Ingredients

    40 CFR 455

    EPA survey code

    Pesticide name

    CAS No.

    EPA analytical method No.(s)

    8........................... Triadimefon.....................

    43121-43-3 507/633/525.1/525.2/1656 12.......................... Dichlorvos......................

    62-73-7 1657/507/622/525.1/525.2 16.......................... 2,4-D; 2,4-D Salts and Esters

    94-75-7 1658/515.1/615/515.2/555

    2,4-Dichloro-phenoxyacetic acid

    . 17.......................... 2,4-DB; 2,4-DB Salts and Esters

    94-82-6 1658/515.1/615/515.2/555

    2,4-Dichlorophenoxybutyric acid

    . 22.......................... Mevinphos.......................

    7786-34-7 1657/507/622/525.1/525.2 25.......................... Cyanazine.......................

    21725-46-2 629/507 26.......................... Propachlor......................

    1918-16-7 1656/508/608.1/525.1/525.2 27.......................... MCPA; MCPA Salts and Esters [2-

    94-74-6 1658/615/555

    Methyl-4-chlorophenoxyacetic acid]. 30.......................... Dichlorprop; Dichlorprop Salts

    120-36-5 1658/515.1/615/515.2/555 and Esters [2-(2,4-

    Dichlorophenoxy) propionic acid]. 31.......................... MCPP; MCPP Salts and Esters [2-

    93-65-2 1658/615/555

    (2-Methyl-4-chlorophenoxy) propionic acid]. 35.......................... TCMTB [2-(Thiocyanomethylthio)

    21564-17-0 637 benzo-thiazole]. 39.......................... Pronamide.......................

    23950-58-5 525.1/525.2/507/633.1 41.......................... Propanil........................

    709-98-8 632.1/1656 45.......................... Metribuzin......................

    21087-64-9 507/633/525.1/525.2/1656 52.......................... Acephate........................

    30560-19-1 1656/1657 53.......................... Acifluorfen.....................

    50594-66-6 515.1/515.2/555 54.......................... Alachlor........................

    15972-60-8 505/507/645/525.1/525.2/1656 55.......................... Aldicarb........................

    116-06-3 531.1 58.......................... Ametryn.........................

    834-12-8 507/619/525.1/525.2 60.......................... Atrazine........................

    1912-24-9 505/507/619/525.1/525.2/1656 62.......................... Benomyl.........................

    17804-35-2 631 68.......................... Bromacil; Bromacil Salts and

    314-40-9 507/633/525.1/525.2/1656

    Esters. 69.......................... Bromoxynil......................

    1689-84-5 1625/1661 69.......................... Bromoxynil octanoate............

    1689-99-2 1656 70.......................... Butachlor.......................

    23184-66-9 507/645/525.1/525.2/1656 73.......................... Captafol........................

    2425-06-1 1656 75.......................... Carbaryl [Sevin]................

    63-25-2 531.1/632/553 76.......................... Carbofuran......................

    1563-66-2 531.1/632 80.......................... Chloroneb.......................

    2675-77-6 1656/508/608.1/525.1/525.2 82.......................... Chlorothalonil..................

    1897-45-6 508/608.2/525.1/525.2/1656 84.......................... Stirofos........................

    961-11-5 1657/507/622/525.1/525.2 86.......................... Chlorpyrifos....................

    2921-88-2 1657/508/622 90.......................... Fenvalerate.....................

    51630-58-1 1660 103......................... Diazinon........................

    333-41-5 1657/507/614/622/525.1/525.2 107......................... Parathion methyl................

    298-00-0 1657/614/622 110......................... DCPA [Dimethyl 2,3,5,-

    1861-32-1 508/608.2/525.1/525.2/515.1/ tetrachloro-terephthalate].

    515.2/1656 112......................... Dinoseb.........................

    88-85-7 1658/515.1/615/515.2/555 113......................... Dioxathion......................

    78-34-2 1657/614.1 118......................... Nabonate [Disodium cyanodithio-

    138-93-2 630.1 imidocarbonate]. 119......................... Diuron..........................

    330-54-1 632/553 123......................... Endothall.......................

    145-73-3 548/548.1 124......................... Endrin..........................

    72-20-8 1656/505/508/608/617/525.1/525.2 125......................... Ethalfluralin...................

    55283-68-6 1656/627 Note 1 126......................... Ethion..........................

    563-12-2 1657/614/614.1 127......................... Ethoprop........................

    13194-48-4 1657/507/622/525.1/525.2 132......................... Fenarimol.......................

    60168-88-9 507/633.1/525.1/525.2/1656 133......................... Fenthion........................

    55-38-9 1657/622 138......................... Glyphosate [N-(Phosphonomethyl)

    1071-83-6 547 glycine].

    Page 58064

    140......................... Heptachlor......................

    76-44-8 1656/505/508/608/617/525.1/525.2 144......................... Isopropalin.....................

    33820-53-0 1656/627 148......................... Linuron.........................

    330-55-2 553/632 150......................... Malathion.......................

    121-75-5 1657/614 154......................... Methamidophos...................

    10265-92-6 1657 156......................... Methomyl........................

    16752-77-5 531.1/632 158......................... Methoxychlor....................

    72-43-5 1656/505/508/608.2/617/525.1/ 525.2 172......................... Nabam...........................

    142-59-6 630/630.1 173......................... Naled...........................

    300-76-5 1657/622 175......................... Norflurazon.....................

    27314-13-2 507/645/525.1/525.2/1656 178......................... Benfluralin.....................

    1861-40-1 \1\1656/\1\627 182......................... Fensulfothion...................

    115-90-2 1657/622 183......................... Disulfoton......................

    298-04-4 1657/507/614/622/525.1/525.2 185......................... Phosmet.........................

    732-11-6 1657/622.1 186......................... Azinphos Methyl.................

    86-50-0 1657/614/622 192......................... Organo-tin pesticides...........

    12379-54-3 Ind-01/200.7/200.9 197......................... Bolstar.........................

    35400-43-2 1657/622 203......................... Parathion.......................

    56-38-2 1657/614 204......................... Pendimethalin...................

    40487-42-1 1656 205......................... Pentachloronitrobenzene.........

    82-68-8 1656/608.1/617 206......................... Pentachlorophenol...............

    87-86-5 625/1625/515.2/555/515.1/525.1/ 525.2 208......................... Permethrin......................

    52645-53-1 608.2/508/525.1/525.2/1656/1660 212......................... Phorate.........................

    298-02-2 1657/622 218......................... Busan 85 [Potassium

    128-03-0 630/630.1 dimethyldithiocarbamate]. 219......................... Busan 40 [Potassium N-

    51026-28-9 630/630.1 hydroxymethyl-N- methyldithiocarbamate]. 220......................... KN Methyl [Potassium N-methyl-

    137-41-7 630/630.1 dithiocarbamate]. 223......................... Prometon........................

    1610-18-0 507/619/525.1/525.2 224......................... Prometryn.......................

    7287-19-6 507/619/525.1/525.2 226......................... Propazine.......................

    139-40-2 507/619/525.1/525.2/1656 230......................... Pyrethrin I.....................

    121-21-1 1660 232......................... Pyrethrin II....................

    121-29-9 1660 236......................... DEF [S,S,S-Tributyl

    78-48-8 1657 phosphorotrithioate]. 239......................... Simazine........................

    122-34-9 505/507/619/525.1/525.2/1656 241......................... Carbam-S [Sodium

    128-04-1 630/630.1 dimethyldithiocarbanate]. 243......................... Vapam [Sodium

    137-42-8 630/630.1 methyldithiocarbamate]. 252......................... Tebuthiuron.....................

    34014-18-1 507/525.1/525.2 254......................... Terbacil........................

    5902-51-2 507/633/525.1/525.2/1656 255......................... Terbufos........................

    13071-79-9 1657/507/614.1/525.1/525.2 256......................... Terbuthylazine..................

    5915-41-3 619/1656 257......................... Terbutryn.......................

    886-50-0 507/619/525.1/525.2 259......................... Dazomet.........................

    533-74-4 630/630.1/1659 262......................... Toxaphene.......................

    8001-35-2 1656/505/508/608/617/525.1/525.2 263......................... Merphos [Tributyl

    150-50-5 1657/507/525.1/525.2/622 phosphorotrithioate]. 264......................... Trifluralin.....................

    1582-09-8 1656/508/617/627/525.1/525.2 268......................... Ziram [Zinc

    137-30-4 630/630.1 dimethyldithiocarbamate].

    \1\ Monitor and report as total Trifluralin.

    Table IH--List of Approved Microbiological Methods for Ambient Water

    Parameter and units

    Method \1\

    EPA

    Standard methods

    AOAC, ASTM, USGS

    Other

    Bacteria: 1. Coliform (fecal), number

    Most Probable Number p. 132 \3\......... 9221 C E-2006...... per 100 mL or number per

    (MPN), 5 tube, 3 gram dry weight.

    dilution, or.

    Membrane filter (MF) p. 124 \3\......... 9222 D-1997........ B-0050-85.\4\

    \2\, single step. 2. Coliform (fecal) in

    MPN, 5 tube, 3

    p. 132 \3\......... 9221 C E-2006...... presence of chlorine, number dilution, or. per 100 mL.

    MF \2\, single step. p. 124 \3\......... 9222 D-1997........ 3. Coliform (total), number

    MPN, 5 tube, 3

    p. 114 \3\......... 9221 B-2006........ per 100 mL.

    dilution, or.

    MF \2\, single step p. 108 \3\......... 9222 B-1997........ B-0025-85.\4\ or two step.

    Page 58065

    4. Coliform (total), in

    MPN, 5 tube, 3

    p. 114 \3\......... 9221 B-2006........ presence of chlorine, number dilution, or. per 100 mL.

    MF \2\ with

    p. 111 \3\......... 9222 (B+B.5c)-1997. enrichment. 5. E. coli, number per 100 mL MPN 6 8 14, multiple ................... 9221 B.1-2006/9221 tube.

    F-2006.11 13

    Multiple tube/

    ................... 9223 B-2004 \12\... 991.15 \10\........ Colilert[supreg].12 16 multiple well.

    Colilert-18[supreg].12 15 16

    MF 2 5 6 7 8, two

    1103.1 \19\........ 9222 B-1997/9222 G- D5392-93.\9\ step, or.

    1997,\18\ 9213 D- 1997.

    Single step......... 1603 \20\, 1604

    9213 D-2007....... ................... mColiBlue-24[supreg].\17\

    \21\. 6. Fecal streptococci, number MPN, 5 tube, 3

    p. 139 \3\......... 9230 B-2007........ per 100 mL.

    dilution,.

    MF \2\, or.......... p. 136 \3\......... 9230 C-2007........ B-0055-85.\4\

    Plate count......... p. 143.\3\ 7. Enterococci, number per

    MPN 6 8, multiple

    ................... 9230 B-2007........ 100 mL.

    tube.

    Multiple tube/

    ................... ................... D6503-99 \9\....... Enterolert[supreg].12 22 multiple well.

    MF 2 5 6 7 8 two

    1106.1 \23\........ 9230 C-2007....... D5259-92.\9\ step.

    Single step, or..... 1600.\24\

    Plate count......... p. 143.\3\

    Protozoa: 8. Cryptosporidium........... Filtration/IMS/FA... 1622,\25\ 1623.\26\ 9. Giardia................... Filtration/IMS/FA... 1623.\26\

    \1\ The method must be specified when results are reported.

    \2\ A 0.45 [micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.

    \3\ 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.

    \4\ 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 the Interior, Reston, VA.

    \5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.

    \6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.

    \7\ When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.

    \8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.

    \9\ 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.

    \10\ 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.

    \11\ 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.

    \12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]- glucuronidase produced by E. coli.

    \13\ 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 [mu]g/mL of MUG may be used.

    \14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.

    \15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.

    \16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX

    Laboratories Inc. 1 IDEXX Drive, Westbrook, ME 04092.

    \17\ A description of the mColiBlue24[supreg] test may be obtained from Hach Company, 100 Dayton Ave., Ames, IA 50010.

    \18\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.

    \19\ USEPA. March 2010. 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-10-002.

    \20\ USEPA. December 2009. 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-09-007.

    \21\ 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. September 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.

    Page 58066

    \22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc. 1 IDEXX Drive, Westbrook, ME 04092.

    \23\ USEPA. December 2009. 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-09-015.

    \24\ USEPA. December 2009. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI).

    U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-09-016.

    \25\ Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.

    USEPA. December 2005. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington,

    DC EPA-821-R-05-001.

    \26\ Method 1623 uses a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of Cryptosporidium and Giardia oocysts and cysts. USEPA. December 2005. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.

    Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-05-002.

    * * * * *

    (b) * * *

    (1) The full texts of the CWA U.S. EPA methods are available at http://epa.gov/waterscience/methods/method. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part 136.

    * * * * *

    (54) USEPA. March 2010. 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-621-R-10-002. Available at http:// www.epa.gov/waterscience/methods/method. Table IH, Note 19.

    (55) USEPA. December 2009. 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-621-R-09-015. Available at http://www.epa.gov/ waterscience/methods/method. Table IH, Note 23.

    (56) USEPA. December 2009. 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-09-007. Available at http://www.epa.gov/waterscience/methods/method. Table IA, Note 20;

    Table IH, Note 20.

    * * * * *

    (59) USEPA. December 2009. Method 1600: Enterococci in Water by

    Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-

    Glucoside Agar (mEI). U.S. Environmental Protection Agency, Office of

    Water, Washington, DC EPA-821-R-09-016. Available at http:// www.epa.gov/waterscience/methods/method. Table IA, Note 23; Table IH,

    Note 24.

    (60) USEPA. December 2005. Method 1622: Cryptosporidium in Water by

    Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of

    Water, Washington, DC EPA-821-R-05-001. Available at http:// www.epa.gov/waterscience/methods/method. Table IA, Note 25.

    (61) USEPA. December 2005. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency,

    Office of Water, Washington, DC EPA-821-R-05-002. Available at http:// www.epa.gov/waterscience/methods/method. Table IA, Note 26.

    * * * * *

    (70) USEPA. April 2010. Method 1680: Fecal Coliforms in Sewage

    Sludge (Biosolids) by Multiple-Tube Fermentation using Lauryl Tryptose

    Broth (LTB) and EC Medium. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-10-003. Available at http:// www.epa.gov/waterscience/methods/method. Table IA, Note 13.

    * * * * *

    (73) EPA Method 200.5, Revision 4.2. ``Determination of Trace

    Elements in Drinking Water by Axially Viewed Inductively Coupled

    Plasma-Atomic Emission Spectrometry.'' 2003. EPA/600/R-06/115.

    (Available at http://www.epa.gov/nerlcwww/ordmeth.htm.)

    * * * * *

    (e) Sample preservation procedures, container materials, and maximum allowable holding times for parameters are cited in Tables IA,

    IB, IC, ID, IE, IF, IG and IH are prescribed in Table II. Information in this table takes precedence over information provided in specific methods or elsewhere unless a party documents the acceptability of an alternative to the Table II instructions. Such alternatives may include a change from the prescribed preservation techniques, container materials, and maximum holding times applicable to samples collected from a specific discharge. The nature and extent of the documentation of such changes (how to apply as well as supporting data) is left to the discretion of the permitting authority (state agency or EPA region) or other authority and may rely on instructions, such as those provided for method modifications at Sec. 136.6.

    Table II--Required Containers, Preservation Techniques, and Holding Times

    Maximum

    Parameter number/name

    Container \1\

    Preservation 2 3

    holding time

    (in hours) \4\

    Table IA--Bacterial Tests: 1-5. Coliform, total, fecal, and E. PA, G..................... Cool, 16-C18internal olefin drilling fluid means a C16-C18internal olefin drilling fluid formulated as specified in Appendix 1 of Subpart A of this part.

    * * * * *

    (uu) Analytic Methods for the Oil and Gas Extraction Point Source

    Category is the EPA document, EPA-821-R-09-013, that compiles analytic methods for this category. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected 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. A copy may also be inspected at EPA's

    Page 58074

    Water Docket, 1200 Pennsylvania Ave., NW., Washington, DC 20460. 19. In Sec. 435.12, the first footnote to the table is revised to read as follows:

    Sec. 435.12 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best practicable control technology currently available (BPT).

    * * * * *

    BPT Effluent Limitations--Oil and Grease

    * * * * *

    * * * * *

    \1\ No discharge of free oil. See Sec. 435.11(x).

    * * * * * 20. In Sec. 435.13, footnotes 2, 3, and 5 through 11 to the table are revised to read as follows:

    Sec. 435.13 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best available technology economically achievable (BAT).

    * * * * *

    BAT Effluent Limitations

    * * * *

    \2\ As determined by the suspended particulate phase (SPP) toxicity test. See Sec. 435.11(gg).

    \3\ As determined by the static sheen test. See Sec. 435.11(hh).

    * * * * *

    \5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) of stock base fluid as determined by EPA Method 1654, Revision A, [specified at

    Sec. 435.11(u)] entitled ``PAH Content of Oil by HPLC/UV,'' December 1992, which is published in ``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \6\ Base fluid sediment toxicity ratio = 10-day LC50 of C16-C18 internal olefin/10-day LC50 of stock base fluid as determined by ASTM E 1367-92

    specified at Sec. 435.11(ee)

    method: ``Standard Guide for

    Conducting 10-day Static Sediment Toxicity Tests with Marine and

    Estuarine Amphipods,'' 1992, after preparing the sediment according to the procedure specified in EPA Method 1646, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \7\ Biodegradation rate ratio = Cumulative headspace gas production (ml) of C16-C18 internal olefin/Cumulative headspace gas production (ml) of stock base fluid, both at 275 days as determined by EPA Method 1647, which is published in ``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(e) and (uu).

    \8\ Drilling fluid sediment toxicity ratio = 4-day LC50 of C16-C18 internal olefin drilling fluid/4-day LC50 of drilling fluid removed from drill cuttings at the solids control equipment as determined by

    ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static

    Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992, with Leptocheirus plumulosus as the test organism and sediment preparation procedures specified in EPA Method 1646, which is published in ``Analytic Methods for the Oil and Gas Extraction Point

    Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu).

    \9\ As determined before drilling fluids are shipped offshore by the GC/

    MS compliance assurance method (EPA Method 1655), and as determined prior to discharge by the RPE method (EPA Method 1670) applied to drilling fluid removed from drill cuttings. If the operator wishes to confirm the results of the RPE method (EPA Method 1670), the operator may use the GC/MS compliance assurance method (EPA Method 1655).

    Results from the GC/MS compliance assurance method (EPA Method 1655) shall supersede the results of the RPE method (EPA Method 1670). EPA

    Method 1655 and 1670 are published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \10\ Maximum permissible retention of non-aqueous drilling fluid (NAF) base fluid on wet drill cuttings averaged over drilling intervals using NAFs as determined by EPA Method 1674, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation is applicable for NAF base fluids that meet the base fluid sediment toxicity ratio (Footnote 6), biodegradation rate ratio (Footnote 7),

    PAH, mercury, and cadmium stock limitations (C16-C18 internal olefin) defined above in this table.

    \11\ Maximum permissible retention of non-aqueous drilling fluid (NAF) base fluid on wet drill cuttings averaged over drilling intervals using NAFs as determined by EPA Method 1674, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation is applicable for NAF base fluids that meet the ester base fluid sediment toxicity ratio and ester biodegradation rate ratio stock limitations defined as:

    (a) Ester base fluid sediment toxicity ratio = 10-day LC50 of C12-C14 ester or C8 ester/10-day LC50 of stock base fluid as determined by

    ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static

    Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992, with Leptocheirus plumulosus as the test organism and sediment preparation procedures specified in EPA Method 1646, which is published in ``Analytic Methods for the Oil and Gas Extraction Point

    Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu);

    (b) Ester biodegradation rate ratio = Cumulative headspace gas production (ml) of C12-C14 ester or C8 ester/Cumulative headspace gas production (ml) of stock base fluid, both at 275 days as determined by

    EPA Method 1647, which is published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(e) and (uu); and (c) PAH mass ratio (Footnote 5), mercury, and cadmium stock limitations (C16-C18 internal olefin) defined above in this table. 21. In Sec. 435.14, footnote 2 to the table is revised to read as follows:

    Sec. 435.14 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best conventional pollutant control technology (BCT).

    * * * * *

    BAT Effluent Limitations

    * * * *

    \2\ As determined by the static sheen test. See Sec. 435.11(hh).

    * * * * * 22. In Sec. 435.15, footnotes 2, 3, and 5 through 11 to the table are revised to read as follows:

    Sec. 435.15 Standards of performance for new sources (NSPS).

    * * * * *

    New Source Performance Standards

    * * * * *

    \2\ As determined by the suspended particulate phase (SPP) toxicity test. See Sec. 435.11(gg).

    \3\ As determined by the static sheen test. See Sec. 435.11(hh).

    * * * * *

    \5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) of stock base fluid as determined by EPA Method 1654, Revision A, [specified at

    Sec. 435.11(u)] entitled ``PAH Content of Oil by HPLC/UV,'' December 1992, which is published in ``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \6\ Base fluid sediment toxicity ratio = 10-day LC50 of C16-C18 internal olefin/10-day LC50 of stock base fluid as determined by ASTM E 1367-92

    specified at Sec. 435.11(ee)

    method: ``Standard Guide for

    Conducting 10-day Static Sediment Toxicity Tests with Marine and

    Estuarine Amphipods,'' 1992, after preparing the sediment according to the procedure specified in EPA Method 1646, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \7\ Biodegradation rate ratio = Cumulative headspace gas production (ml) of C16-C18 internal olefin/Cumulative headspace gas production (ml) of stock base fluid, both at 275 days as determined by EPA Method 1647, which is published in ``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(e) and (uu).

    \8\ Drilling fluid sediment toxicity ratio = 4-day LC50 of C16-C18 internal olefin drilling fluid/4-day LC50 of drilling fluid removed from drill cuttings at the solids control equipment as determined by

    ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static

    Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992, with Leptocheirus plumulosus as the test organism and sediment preparation procedures specified in EPA Method 1646, which is published in ``Analytic Methods for the Oil and Gas Extraction Point

    Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu).

    Page 58075

    \9\ As determined before drilling fluids are shipped offshore by the GC/

    MS compliance assurance method (EPA Method 1655), and as determined prior to discharge by the RPE method (EPA Method 1670) applied to drilling fluid removed from drill cuttings. If the operator wishes to confirm the results of the RPE method (EPA Method 1670), the operator may use the GC/MS compliance assurance method (EPA Method 1655).

    Results from the GC/MS compliance assurance method (EPA Method 1655) shall supersede the results of the RPE method (EPA Method 1670). EPA

    Method 1655 and 1670 are published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).

    \10\ Maximum permissible retention of non-aqueous drilling fluid (NAF) base fluid on wet drill cuttings averaged over drilling intervals using NAFs as determined by EPA Method 1674, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation is applicable for NAF base fluids that meet the base fluid sediment toxicity ratio (Footnote 6), biodegradation rate ratio (Footnote 7),

    PAH, mercury, and cadmium stock limitations (C16-C18 internal olefin) defined above in this table.

    \11\ Maximum permissible retention of non-aqueous drilling fluid (NAF) base fluid on wet drill cuttings average over drilling intervals using

    NAFs as determined by EPA Method 1674, which is published in

    ``Analytic Methods for the Oil and Gas Extraction Point Source

    Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation is applicable for NAF base fluids that meet the ester base fluid sediment toxicity ratio and ester biodegradation rate ratio stock limitations defined as:

    (a) Ester base fluid sediment toxicity ratio = 10-day LC50 of C12-C14 ester or C8 ester/10-day LC50 of stock base fluid as determined by

    ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static

    Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992, with Leptocheirus plumulosus as the test organism and sediment preparation procedures specified in EPA Method 1646, which is published in ``Analytic Methods for the Oil and Gas Extraction Point

    Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu);

    (b) Ester biodegradation rate ratio = Cumulative headspace gas production (ml) of C12-C14 ester or C8 ester/Cumulative headspace gas production (ml) of stock base fluid, both at 275 days as determined by

    EPA Method 1647, which is published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec. 435.11(e) and (uu); and (c) PAH mass ratio (Footnote 5), mercury, and cadmium stock limitations (C16-C18 internal olefin) defined above in this table. 23. Subpart A of part 435 is amended by removing Appendices 1 through 7. 24. Subpart A of part 435 is amended by redesignating Appendix 8 as

    Appendix 1.

    Subpart D--Coastal Subcategory 25. Section 435.41 is amended, a. By revising paragraph (d). b. By revising paragraph (e). c. By revising paragraph (k). d. By revising paragraph (m)(2). e. By revising paragraph (q). f. By revising paragraph (r). g. By revising paragraph (y). h. By revising paragraph (ee). i. By revising paragraph (ff). j. By adding paragraph (mm).

    Sec. 435.41 Specialized definitions.

    * * * * *

    (d) Base fluid retained on cuttings as applied to BAT effluent limitations and NSPS refers to the ``Determination of the Amount of

    Non-Aqueous Drilling Fluid (NAF) Base Fluid from Drill Cuttings by a

    Retort Chamber (Derived from API Recommended Practice 13B-2)'', EPA

    Method 1674, which is published in ``Analytic Methods for the Oil and

    Gas Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph

    (mm) of this section.

    (e) Biodegradation rate as applied to BAT effluent limitations and

    NSPS for drilling fluids and drill cuttings refers to the ``Protocol for the Determination of Degradation of Non Aqueous Base Fluids in a

    Marine Closed Bottle Biodegradation Test System: Modified ISO 11734:1995,'' EPA Method 1647, supplemented with ``Procedure for Mixing

    Base Fluids With Sediments,'' EPA Method 1646. Both EPA Method 1646 and 1647 are published in ``Analytic Methods for the Oil and Gas Extraction

    Point Source Category,'' EPA-821-R-09-013. See paragraph (mm) of this section.

    * * * * *

    (k) Diesel oil refers to the grade of distillate fuel oil, as specified in the American Society for Testing and Materials Standard

    Specification for Diesel Fuel Oils D975-91, that is typically used as the continuous phase in conventional oil-based drilling fluids. This incorporation by reference was approved by the Director of the Federal

    Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be obtained from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428. Copies may be inspected 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. A copy may also be inspected at EPA's Water Docket, 1200 Pennsylvania Ave., NW.,

    Washington, DC 20460.

    * * * * *

    (m) * * *

    (2) Dry drill cuttings means the residue remaining in the retort vessel after completing the retort procedure specified in EPA Method 1674, which is published in ``Analytic Methods for the Oil and Gas

    Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph

    (mm) of this section.

    * * * * *

    (q) Formation oil means the oil from a producing formation which is detected in the drilling fluid, as determined by the GC/MS compliance assurance method, EPA Method 1655, when the drilling fluid is analyzed before being shipped offshore, and as determined by the RPE method, EPA

    Method 1670, when the drilling fluid is analyzed at the offshore point of discharge. The GC/MS compliance assurance method and the RPE method approved for use with this part are published in the ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09- 013. See paragraph (mm) of this section. Detection of formation oil by the RPE method may be confirmed by the GC/MS compliance assurance method, and the results of the GC/MS compliance assurance method shall supersede those of the RPE method.

    (r) Garbage means all kinds of victual, domestic, and operational waste, excluding fresh fish and parts thereof, generated during the normal operation of coastal oil and gas facility and liable to be disposed of continuously or periodically, except dishwater, graywater, and those substances that are defined or listed in other Annexes to

    MARPOL 73/78. A copy of MARPOL may be inspected at EPA's Water Docket, 1200 Pennsylvania Ave., NW., Washington, DC 20460.

    * * * * *

    (y) No discharge of free oil means that waste streams may not be discharged that contain free oil as evidenced by the monitoring method specified for that particular stream, e.g., deck drainage or miscellaneous discharges cannot be discharged when they would cause a film or sheen upon or discoloration of the surface of the receiving water; drilling fluids or cuttings may not be discharged when they fail

    EPA Method 1617 (Static Sheen Test), which is published in ``Analytic

    Methods for the Oil and Gas Extraction Point Source Category,'' EPA- 821-R-09-013. See paragraph (mm) of this section.

    * * * * *

    (ee) SPP toxicity as applied to BAT effluent limitations and NSPS for drilling fluids and drill cuttings refers to the bioassay test procedure, ``Suspended Particulate Phase (SPP) Toxicity Test,'' presented in EPA Method 1619, which is published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09- 013. See paragraph (mm) of this section.

    (ff) Static sheen test means the standard test procedure that has been

    Page 58076

    developed for this industrial subcategory for the purpose of demonstrating compliance with the requirement of no discharge of free oil. The methodology for performing the static sheen test is presented in EPA Method 1617, which is published in ``Analytic Methods for the

    Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph (mm) of this section.

    * * * * *

    (mm) Analytic Methods for the Oil and Gas Extraction Point Source

    Category is the EPA document, EPA-821-R-09-013, that compiles analytic methods for this category. This incorporation by reference was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected 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. A copy may also be inspected at EPA's

    Water Docket, 1200 Pennsylvania Ave., NW., Washington, DC 20460. 26. In Sec. 435.42, footnote 1 to the table is revised to read as follows:

    Sec. 435.42 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best practicable control technology currently available (BPT).

    * * * * *

    \1\ No discharge of free oil. See Sec. 435.41(y).

    * * * * * 27. In Sec. 435.43, footnotes 2 and 4 are revised to read as follows:

    Sec. 435.43 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best available technology economically achievable (BAT).

    * * * * *

    Bat Effluent Limitations

    * * * * *

    \2\ As determined by the static sheen test. See Sec. 435.41(ff).

    * * * * *

    \4\ As determined by the suspended particulate phase (SPP) toxicity test. See Sec. 435.41(ee).

    * * * * * 28. In Sec. 435.44 footnote 2 to the table is revised to read as follows:

    Sec. 435.44 Effluent limitations guidelines representing the degree of effluent reduction attainable by the application of the best conventional pollutant control technology (BCT).

    * * * * *

    Bat Effluent Limitations

    * * * * *

    \2\ As determined by the static sheen test. See Sec. 435.41(ff).

    * * * * * 29. In Sec. 435.45, footnotes 2 and 4 to the table are revised to read as follows:

    Sec. 435.45 Standards of performance for new sources (NSPS).

    * * * * *

    NSPS Effluent Limitations

    * * * * *

    \2\ As determined by the static sheen test. See Sec. 435.41(ff).

    * * * * *

    \4\ As determined by the suspended particulate phase (SPP) toxicity test. See Sec. 435.41(ee).

    * * * * *

    FR Doc. 2010-20018 Filed 9-22-10; 8:45 am

    BILLING CODE 6560-50-P

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