Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures

 
CONTENT

Federal Register, Volume 77 Issue 97 (Friday, May 18, 2012)

Federal Register Volume 77, Number 97 (Friday, May 18, 2012)

Rules and Regulations

Pages 29758-29846

From the Federal Register Online via the Government Printing Office www.gpo.gov

FR Doc No: 2012-10210

Page 29757

Vol. 77

Friday,

No. 97

May 18, 2012

Part II

Environmental Protection Agency

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40 CFR Parts 136, 260, et al.

Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures; Final Rule

Page 29758

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 136, 260, 423, 430, and 435

EPA-HQ-OW-2010-0192; FRL-9664-6

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: Final rule.

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SUMMARY: This rule modifies the testing procedures approved for analysis and sampling under the Clean Water Act. EPA proposed these changes for public comment on September 23, 2010. The changes adopted in this final rule fall into the following categories: New and revised EPA methods and new and revised methods published by voluntary consensus standard bodies (VCSB), such as ASTM International and the Standard Methods Committee; updated versions of currently approved methods; methods reviewed under the alternate test procedures (ATP) program; clarifications to the process for EPA approval for use of alternate procedures for nationwide and Regional use; minimum quality control requirements to improve consistency across method versions; corrections to previously approved methods; and revisions to sample collection, preservation, and holding time requirements. Finally, EPA makes changes to three effluent guideline regulations.

DATES: This regulation is effective on June 18, 2012. The incorporation by reference of these methods is approved by the Director of the Federal Register on June 18, 2012. For judicial review purposes, this final rule is promulgated as of 1:00 p.m. (Eastern time) on June 1, 2012 as provided at 40 CFR 23.2 and 23.7.

ADDRESSES: EPA has established a docket for this action under Docket ID No. EPA-HQ-OW-2010-0192. All documents in the docket are listed on the http://www.regulations.gov Web site. Although listed in the index, some information is not publically available, e.g., CBI or other information whose disclosure is restricted by statute. Certain other materials, such as copyrighted material, are not placed on the Internet and will be publicly available only in hard copy form. Publicly available docket materials are available either electronically through http://www.regulations.gov or in hard copy at the HQ Water Docket Center, EPA/

DC, EPA West, Room 3334, 1301 Constitution Ave. NW., Washington, DC. The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. The telephone number for the Public Reading Room is 202-566-1744, and the telephone number is 202-

566-2426 for the HQ Water Docket.

FOR FURTHER INFORMATION CONTACT: For information regarding the changes to inorganic chemical methods, contact Lemuel Walker, Engineering and Analysis Division (4303T), USEPA Office of Science and Technology, 1200 Pennsylvania Ave. NW., Washington, DC 20460, 202-566-1077 (email: walker.lemuel@epa.gov). For information regarding the changes to organic chemical methods, contact Maria Gomez-Taylor, Engineering and Analysis Division (4303T), USEPA Office of Science and Technology, 1200 Pennsylvania Ave. NW., Washington, DC 20460, 202-566-1005 (email: gomez-taylor.maria@epa.gov). For information regarding the changes to microbiological and whole effluent toxicity methods, contact Robin Oshiro, Engineering and Analysis Division (4303T), USEPA Office of Science and Technology, 1200 Pennsylvania Ave. NW., Washington, DC 20460, 202-566-1075 (email: oshiro.robin@epa.gov).

SUPPLEMENTARY INFORMATION:

  1. General Information

    1. Does this action apply to me?

    EPA Regions, as well as States, Territories and Tribes authorized to implement the National Pollutant Discharge Elimination System (NPDES) program, issue permits with conditions designed to ensure compliance with the technology-based and water quality-based requirements of the Clean Water Act (CWA). These permits may include restrictions on the quantity of pollutants that may be discharged as well as pollutant measurement and reporting requirements. If EPA has approved a test procedure for analysis of a specific pollutant, the NPDES permittee must use an approved test procedure (or an approved alternate test procedure if specified by the permitting authority) for the specific pollutant when measuring the required waste constituent. Similarly, if EPA has established sampling requirements, measurements taken under an NPDES permit must comply with these requirements. Therefore, entities with NPDES permits will potentially be affected by the actions in this rulemaking. Categories and entities that may potentially be affected by the requirements of today's rule include:

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    Examples of potentially affected

    Category entities

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    State, Territorial, and Indian States, Territories, and Tribes

    Tribal Governments. authorized to administer the NPDES

    permitting program; States,

    Territories, and Tribes providing

    certification under Clean Water Act

    section 401; State, Territorial,

    and Indian Tribal owned facilities

    that must conduct monitoring to

    comply with NPDES permits.

    Industry.......................... Facilities that must conduct

    monitoring to comply with NPDES

    permits.

    Municipalities.................... POTWs or other municipality owned

    facilities that must conduct

    monitoring to comply with NPDES

    permits.

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

  2. What process governs judicial review of this rule?

    Under Section 509(b)(1) of the Clean Water Act (CWA), judicial review of today's CWA rule may be obtained by filing a petition for review in a United States Circuit Court of Appeals within 120 days from the date of promulgation of this rule. For judicial review purposes, this final rule is promulgated as of 1 p.m. (Eastern time) on June 1, 2012 as provided at 40 CFR 23.2. The

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    requirements of this regulation may also not be challenged later in civil or criminal proceedings brought by EPA.

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

    AOAC: AOAC International

    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

    ISO: International Organization for Standardization

    MS: Mass Spectrometry

    NIST: National Institute of Standards and Technology

    NPDES: National Pollutant Discharge Elimination System

    QA: Quality Assurance

    QC: Quality Control

    SDWA: Safe Drinking Water Act

    SM: Standard Methods

    SRM: Standard Reference Material

    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 Final Rule

  4. New EPA Methods and New Versions of Previously Approved EPA Methods

  5. New Standard Methods and New Versions of Approved Standard Methods

  6. New ASTM Methods and New Versions of Previously Approved ASTM Methods

  7. New Alternate Test Procedures at 40 CFR 136.3

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

  9. Revisions in Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times

  10. Revisions to 40 CFR 136.4 and 136.5

  11. Revisions to Method Modification Provisions at 40 CFR 136.6

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

  12. Revisions to 40 CFR part 423 (Steam Electric Power Generating Point Source Category)

    III. Changes Between the Proposed Rule and the Final Rule

  13. EPA Is Not Adding EPA Method 1614A

  14. Deferral of Action on EPA Method 1668C

  15. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09

  16. Revisions and Clarifications to EPA Method 200.7

  17. Revisions and Corrections to Certain Citations in Tables IB and ID

  18. Continued Approval of Method 1664 Revision A

  19. Revision to Footnote 63 of Table IB at 40 CFR 136.3

  20. Revision to Footnote 4 of Table IC at 40 CFR 136.3

    I. Revisions to Table II Language

  21. Approval of Alternate Test Procedures for Limited Use at 40 CFR 136.5

  22. Revisions to Language at Sec. 136.6

    L. Revisions to New Quality Assurance and Quality Control Language

  23. Withdrawal of Appendices at 40 CFR part 136

  24. Revisions to 40 CFR Part 430 (Pulp, Paper, and Paperboard Point Source Category)

  25. Revisions to 40 CFR Part 435 (Oil and Gas Extraction Point Source Category)

    IV. Response to Comments

  26. How Standard Methods are Identified in Part 136 Tables

  27. Preservation and Holding Time Requirements for EPA Method 624

  28. Quality Assurance and Quality Control Requirements

    V. Statutory and Executive Order Reviews

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

  30. Paperwork Reduction Act

  31. Regulatory Flexibility Act

  32. Unfunded Mandates Reform Act

  33. Executive Order 13132: Federalism

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

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

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

    I. National Technology Transfer and Advancement Act of 1995

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

  38. Congressional Review Act

    I. Statutory Authority

    EPA is promulgating today's rule pursuant to the authority of sections 301(a), 304(h), and 501(a) of the Clean Water Act (``CWA'' or the ``Act''), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of the Act prohibits the discharge of any pollutant into navigable waters unless the discharge complies with a National Pollutant Discharge Elimination System (NPDES) permit issued under section 402 of the Act. Section 304(h) of the Act requires the Administrator of the EPA to ``* * * promulgate guidelines establishing test procedures for the analysis of pollutants that shall include the factors which must be provided in any certification pursuant to section 401 of this Act or permit application pursuant to section 402 of this Act.'' Section 501(a) of the Act authorizes the Administrator to ``* * * prescribe such regulations as are necessary to carry out this function under the Act.'' EPA generally has codified its test procedure regulations (including analysis and sampling requirements) for CWA programs at 40 CFR part 136, though some requirements are codified in other Parts (e.g., 40 CFR Chapter I, Subchapters N and O).

    II. Summary of Final Rule

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

  39. New EPA Methods and New Versions of Previously Approved EPA Methods

    This rule approves new EPA methods and new versions of already approved EPA methods. The following discussion briefly describes the EPA methods added today to Part 136.

    1. Oil and grease. Today's rule adds a new version of EPA Method 1664, 1664 Revision B: 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. Today, EPA is also amending the RCRA regulations at 40 CFR 260.11, which currently specify the use of Method 1664 Rev. A, to provide additionally for use of the revised version, 1664 Rev. B. As stated in the preamble to the proposal (75 FR 58026, Sept. 23, 2010), EPA encourages that future delistings cite ``Method 1664 Rev. B'' while delistings already granted may continue to use Method 1664 Rev. A.

    On December 14, 2011, EPA published a notice of data availability (NODA) on a new method for oil and grease for use in Clean Water Act programs (see 76 FR 77742). This method, ASTM D-7575-10, uses a different extractant (a membrane filter instead of n-hexane for the extraction of oil and grease material) and a different measurement technique (infrared absorption instead of gravimetry) from the extractant and measurement technique of currently approved methods for oil and grease. The new method was discussed in the September 23, 2010 notice but EPA did not propose it for use as an approved method to be codified at 40 CFR 136.3 because oil and grease is a method-defined parameter. By definition, the measurement results of method-defined parameters are specific to the described method and are not directly comparable to results obtained by another method. However, since publication of the Methods Update Rule proposal, the Agency received additional data and information about this method and is re-considering whether it should add this

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    method to the list of approved methods for oil and grease at 40 CFR 136.3. In the NODA, EPA proposed to include ASTM D-7575 for the measurement of oil and grease based on comments received in response to its September 23, 2010 proposal and the additional data. EPA will make a decision on the inclusion of the new method once it reviews the public comments received in response to the NODA and will then publish that decision in a separate Federal Register notice.

    2. Metals. Today's rule adds EPA Method 200.5 (Revision 4.2): ``Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma--Atomic Emission Spectrometry'' to Table IB. The rule also clarifies that the axial orientation of the torch is allowed for use with EPA Method 200.7. Thus, EPA will allow the use of axial instruments or radial instruments to measure metals in water samples.

    3. Pesticides. Today's rule adds EPA Method 525.2 to Table IG (Test Methods for Pesticide Active Ingredients) as an additional approved method for all parameters for which EPA has previously approved EPA Method 525.1, and also adds Methods 525.1 and 525.2 to Table ID for the same parameters for which EPA had previously approved Method 525.1 in Table IG. The rule also adds some of the methods for Pesticide Active Ingredients (Table IG) to applicable parameters listed in Table ID for general use. These methods are:

    1. EPA Method 608.1, ``The Determination of Organochlorine Pesticides in Municipal and Industrial Wastewater.'' This method measures chlorobenzilate, chloroneb, chloropropylate, dibromochloropropane, etridiazole, PCNB, and propachlor.

    2. EPA Method 608.2, ``The Determination of Certain Organochlorine Pesticides in Municipal and Industrial Wastewater.'' This method measures chlorothalonil, DCPA, dichloran, methoxychlor, and permethrin.

    3. EPA Method 614, ``The Determination of Organophosphorus Pesticides in Municipal and Industrial Wastewater.'' This method measures azinphos methyl, demeton, diazinon, disulfoton, ethion, malathion, parathion methyl, and parathion ethyl.

    4. EPA Method 614.1, ``The Determination of Organophosphorus Pesticides in Municipal and Industrial Wastewater.'' This method measures dioxathion, EPN, ethion, and terbufos.

    5. EPA Method 615, ``The Determination of Chlorinated Herbicides in Municipal and Industrial Wastewater.'' This method measures 2,4-D, dalapon, 2,4-DB, dicamba, dichlorprop, dinoseb, MCPA, MCPP, 2,4,5-T, and 2,4,5-TP.

    6. EPA Method 617, ``The Determination of Organohalide Pesticides and PCBs in Municipal and Industrial Wastewater.'' This method measures aldrin, alpha-BHC, beta-BHC, gamma-BHC (lindane), captan, carbophenothion, chlordane, 4,4'-DDD, 4,4'-DDE, 4,4'-DDT, dichloran, dicofol, dieldrin, endosulfan I, endosulfan II, endosulfan sulfate, endrin, endrin aldehyde, heptachlor, heptachlor epoxide, isodrin, methoxychlor, mirex, PCNB, perthane, strobane, toxaphene, trifluralin, PCB-1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254, and PCB-

      1260.

    7. EPA Method 619, ``The Determination of Triazine Pesticides in Municipal and Industrial Wastewater.'' This method measures ametryn, atraton, atrazine, prometon, prometryn, propazine, sec-bumeton, simetryn, simazine, terbuthylazine, and terbutryn.

    8. EPA Method 622, ``The Determination of Organophosphorus Pesticides in Municipal and Industrial Wastewater.'' This method measures azinphos methyl, bolstar, chlorpyrifos, chlorpyrifos methyl, coumaphos, demeton, diazinon, dichlorvos, disulfoton, ethoprop, fensulfothion, fenthion, merphos, mevinphos, naled, parathion methyl, phorate, ronnel, stirofos, tokuthion, and trichloronate.

    9. EPA Method 622.1, ``The Determination of Thiophosphate Pesticides in Municipal and Industrial Wastewater.'' This method measures aspon, dichlofenthion, famphur, fenitrothion, fonophos, phosmet, and thionazin.

    10. EPA Method 632, ``The Determination of Carbamate and Urea Pesticides in Municipal and Industrial Wastewater.'' This method measures aminocarb, barban, carbaryl, carbofuran, chlorpropham, diuron, fenuron, fenuron-TCA, fluometuron, linuron, methiocarb, methomyl, mexacarbate, monuron, monuron-TCA, neburon, oxamyl, propham, propoxur, siduron, and swep.

      4. Microbiologicals. Today's rule approves the 2005 versions of EPA Method 1622, ``Cryptosporidium in Water by Filtration/IMS/FA'' and EPA Method 1623, ``Cryptosporidium and Giardia in Water by Filtration/IMS/

      FA'' in Table IH for ambient water.

      The rule approves revised versions of EPA Methods 1103.1, 1106.1, 1600, 1603, and 1680 in Table IH. The rule also approves the revised version of EPA Methods 1600, 1603 and 1680 in Table IA. We corrected technical errors in these revisions.

      5. Non-Conventionals. Today's rule adds EPA Method 1627, ``Kinetic Test Method for the Prediction of Mine Drainage Quality'' to Table IB as a new parameter termed ``Acid Mine Drainage.''

      6. Organics. Today's rule approves EPA Method 624, ``Purgeables,'' for the determination of acrolein and acrylonitrile in wastewater and revises footnote 4 to Table IC to specify that the laboratory must provide documentation about its ability to measure these analytes at the levels necessary to comply with associated regulations.

  40. New Standard Methods and New Versions of Approved Standard Methods

    This rule approves the following Standard Methods (SM) for certain pollutants currently listed in Table IB at Part 136. Laboratories performing measurements using any of the approved Standard Methods must follow the quality control (QC) procedures specified in the 20th or 21st edition of Standard Methods. Below is a list of the Standard Methods added to Table IB in Part 136:

    1. SM 5520 B-2001 and SM 5520 F-2001, Oil and Grease, gravimetric

    2. SM 4500-NH3 G-1997, Ammonia (as N) and TKN, automated phenate method

    3. SM 4500-B B-2000, Boron, curcumin method

    4. SM 4140 B-1997, Inorganic Ions (Bromide, Chloride, Fluoride, Orthophosphate, and Sulfate), capillary ion electrophoresis with indirect UV detection

    5. SM 3114 B-2009, Arsenic and Selenium, AA gaseous hydride

    6. SM 3114 C-2009, Arsenic and Selenium, AA gaseous hydride

    7. SM 3111 E-1999, Aluminum and Beryllium, direct aspiration atomic absorption spectrometry

    8. SM 5220 B-1997, Chemical Oxygen Demand (COD), titrimetric

    9. SM 3500-Cr B-2009, Chromium, colorimetric method

    10. SM 4500-Norg D-1997, Kjeldahl Nitrogen, semi-automated block digestor colorimetric

    11. SM 3112 B-2009, Mercury, cold vapor, manual

    12. SM 4500-P G-1999 and SM 4500-P H-1999, Phosphorus, Total, automated ascorbic acid reduction

    13. SM 4500-P E-1999 and SM 4500-P F-1999, Phosphorus, Total, manual, and automated ascorbic acid reduction

    14. SM 4500-O B, D, E and F-2001, Oxygen, Dissolved, Winkler

    15. SM 4500-O D-2001, Oxygen, Dissolved, Winkler

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    16. SM 4500-O E-2001, Oxygen, Dissolved, alum flocculation modification

    17. SM 5530 B-2005, Phenols, manual distillation

    18. SM 5530 D-2005, Phenols, colorimetric

    19. SM 3500-K C-1997, Potassium, Total, selective electrode method

    20. SM 2540 E-1997, Residues--Volatile, gravimetric

    21. SM 4500-SiO2 E-1997 and SM 4500-SiO2 F-1997, Silica, Dissolved, automated molybdosilicate

    22. SM 4500-SO42- C-1997, D-1997, E-1997, F-1997 and G-1997, Sulfate, gravimetric, and automated colorimetric

    23. SM 4500-S2- B-2000 and C-2000, Sulfide, sample pretreatment

  41. New ASTM Methods and New Versions of Previously Approved ASTM Methods

    The rule approves the following ASTM methods for existing pollutants and ASTM methods for new pollutants to 40 CFR part 136, Table IB for inorganic compounds, and Table IC for organic compounds.

    1. ASTM D2036-09 (B), Cyanide--Total, Cyanide amenable to cholorination

    2. ASTM D6888-09, Cyanide--Available, flow injection and ligand exchange

    3. ASTM D7284-08, Cyanide--Total, flow injection

    4. ASTM D7511-09, Cyanide--Total, segmented flow injection

    5. Free cyanide is added as a new parameter (24A in Table IB); two ASTM methods (D4282-02 and D7237-10) are approved, in addition to a new version of OIA 1677(2009) for this parameter. D4282-02 is a Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion, and Method D7237-10 is a Standard Test Method for Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection.

    6. ASTM D888-09 (A), Oxygen Dissolved, Winkler

    7. ASTM D7573-09, Organic Carbon--Total, combustion

    8. ASTM D7065-06, Five new chemicals in water: Nonylphenol (NP), Bisphenol A (BPA), p-tert-Octylphenol (OP), Nonylphenol Monoethoxylate (NP1EO), and Nonylphenol Diethoxylate (NP2EO), Gas Chromatography/Mass Spectrometry

  42. New Alternate Test Procedures at 40 CFR 136.3

    The rule approves eight methods submitted to EPA for review through the alternate test procedures (ATP) program and deemed acceptable based on the evaluation of documented method performance. The eight methods approved are added to Table IB:

    1. Hach Company's Method 10360 Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5, Revision 1.2 dated October 2011

    2. In-Situ Incorporated's Method 1002-8-2009 Dissolved Oxygen Measurement by Optical Probe

    3. In-Situ Incorporated's Method 1003-8-2009 Biochemical Demand (BOD) Measurement by Optical Probe

    4. In-Situ Incorporated's Method 1004-8-2009 Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe

    5. Mitchell Method M5271 dated July 31, 2008 for turbidity

    6. Mitchell Method M5331 dated July 31, 2008 for turbidity

    7. Thermo Scientific's Orion Method AQ4500 dated March 12, 2009 for turbidity

    8. Easy (1-Reagent) Nitrate Method dated November 12, 2011 for nitrate, nitrite and combined nitrate/nitrite

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

    The rule also clarifies the procedures for measuring orthophosphate and corrects typographical or other citation errors in Part 136. Specifically, the rule clarifies the purpose of the immediate filtration requirement in orthophosphate measurements (Table IB, parameter 44), which is to assess the dissolved or bio-available form of orthophosphorus (i.e., that portion which passes through a 0.45-

    micron filter)--hence the requirement to filter the sample immediately upon collection (i.e., within 15 minutes of collection). EPA has added a footnote (24) to Table II providing this clarification. The rule also corrects missing citations to the table of microbiological methods for ambient water monitoring which are specified in Table IH at 40 CFR 136.3. When EPA approved the use of certain microbiological methods on March 26, 2007 (72 FR 14220), EPA inadvertently omitted fecal coliform, total coliform, and fecal streptococcus methods from the table. This omission is corrected in today's rule.

  44. Revisions in Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times

    The rule revises some of the current requirements in Table II at 136.3(e).

    1. The rule revises footnote 4 of Table II to clarify the sample holding time for the Whole Effluent Toxicity (WET) samples for the three toxicity methods by adding the following sentence: ``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 degC, with minimum head space.'' 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).

    2. The rule revises 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.

    3. The rule revises 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, and to allow the 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.

    4. The rule revises footnote 16 of Table II instructions for handling Whole Effluent Toxicity (WET) samples by adding two sentences: ``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 degC prior to test initiation.''

    5. The rule revises footnote 22 to Table II 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.''

    6. The rule adds three entries at the end of Table II with the containers, preservation, and holding times for the alkylated phenols, adsorbable organic halides, and chlorinated phenolics. When EPA proposed ASTM D7065-06 for the alkylated phenols, commenters noted that EPA did not include preservation and holding time information in Table II. When EPA moved EPA Methods 1650 and 1653

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    from 40 CFR part 430 to Table IC, EPA inadvertently omitted the associated parameters to Table II, and is correcting this omission in today's rule. The Table II information for containers, preservation, and holding times for these three new entries are taken from the approved methods.

  45. Revisions to 40 CFR 136.4 and 136.5

    This rule changes Sec. Sec. 136.4 and 136.5 to clarify the procedures for obtaining review and approval for the use of alternate test procedures (alternate methods or ATPs) for those methods for which EPA has published an ATP protocol (there are published protocols for chemistry, radiochemical, and microbiological culture methods). In particular, it establishes separate sections outlining the procedures for obtaining EPA review and approval for nationwide use of an ATP (Sec. Sec. 136.4), and the procedures for obtaining approval for limited use of an ATP (Sec. Sec. 136.5).

    In addition, this rule adds language to Part 136.5 to clarify the purpose and intent of limited use applications. This provision only allows use of an alternate method for a specific application at a facility or type of discharge. The Regional Alternate Test Procedure (ATP) Coordinator or the permitting authority, at his/her discretion, may grant approval to all discharges or facilities specified in the approval letter. However, the appropriate permitting authority within a state may request supporting test data from each discharger or facility prior to allowing any such approvals.

    Today's rule further clarifies that the limited use provision cannot be used to gain nationwide approval and is not a way to avoid the full examination of comparability that is required for alternate test procedures when EPA considers a method for nationwide use with the ultimate goal of listing it as an approved CWA method at 40 CFR part 136. As further clarification, in the event that EPA decides not to approve a method proposed for nationwide use, the Regional ATP Coordinator or the permitting authority may choose to reconsider any previous limited use approvals of the alternate method. Based on this reconsideration, the Regional ATP Coordinator or the permitting authority will notify the user(s) if the limited use approval is withdrawn. Otherwise, the limited use approvals remain in effect.

  46. Revisions to Method Modification Provisions at 40 CFR 136.6

    This section allows users to make certain modifications to an approved method to address matrix interferences without the extensive review and approval process specified for an alternate test procedure at 136.4 and 136.5. Today's rule revises 136.6 to provide more examples of allowed and prohibited method modifications. The intent of today's revisions is to clarify those situations in which an ATP is required and those where it is not. Analysts may use the examples to help assess the need for a formal ATP, and in the event an ATP is not needed to document that their modification is acceptable and does not depart substantially from the chemical principles in the method being modified.

    In response to comments, EPA has included additional examples of allowed and prohibited method modifications and has made some revisions to the text language as discussed in Section III below.

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

    EPA is specifying ``essential'' quality control elements at Sec. 136.7 for use in conducting an analysis for CWA compliance monitoring. This new language is added because auditors, co-regulators, laboratory personnel, and the regulated community have noted the variations in quality assurance (QA) and quality control (QC) procedures practiced by laboratories that use 40 CFR part 136 methods for compliance monitoring. Some of these methods are published by voluntary consensus standards bodies, such as the Standard Methods Committee, and ASTM International. Standard Methods and ASTM are available in printed or electronic compendia, or as individual online files. As mentioned in the proposal, each organization has a 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.

    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 particular Part 136 method, or referenced these procedures by other means. These records must be kept in-house as part of the method testing documentation. Consequently, today's rule clarifies that an analyst using these consensus standard body methods for reporting under the CWA must also comply with the quality assurance and quality control requirements listed in the appropriate sections in that consensus standard 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 does 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 lack QA/QC requirements (as specified in this new section at 40 CFR 136.7), whether developed by EPA, a vendor, or a consensus standard body, analysts can refer to and follow the QA/QC published in several public sources. Examples of these sources include the relevant QA/QC sections of an equivalent approved EPA method, or voluntary consensus standards published as Part 136 approved methods (e.g., Standard Methods, ASTM International, and AOAC). In addition to and regardless of the source of the laboratory's or method's QA and QC instructions, for methods that lack QA/QC requirements, EPA is adding requirements at 136.7 to specify twelve essential quality control elements that must be in the laboratory's documented quality system unless a written rationale is provided to explain why these quality control elements are inappropriate for a specific analytical method or application. 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, as applicable to the specific method. EPA has clarified the language in this section in response to public comments. The revised language is discussed in section III below.

  47. Revisions at 40 CFR Part 423 (Steam Electric Power Generating Point Source Category)

    The rule revises the 40 CFR part 423 definitions for total residual chlorine and free available chlorine at Sec. Sec. 423.11(a) and 423.11(l) to allow the use of ``chlorine--total residual'' and ``chlorine--free available'' methods in Sec. 136.3(a), Table IB, or other methods approved by the permitting authority.

    Page 29763

    III. Changes Between the Proposed Rule and the Final Rule

    Except as noted below, the content of the final rule is the same as that of the proposed rule.

  48. EPA Is Not Adding EPA Method 1614A

    The Agency proposed to add Method 1614A, ``Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS.'' EPA developed this method to determine 49 polybrominated diphenyl ether (PBDE) congeners in aqueous, solid, tissue, and multi-phase matrices. This method uses isotope dilution and internal standard high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The commenters were divided on whether EPA should approve this method. Two commenters stated that Method 1614A would be a valuable addition to the list of approved methods, while two other commenters stated that the method has not been sufficiently validated for use in Clean Water Act programs. Upon further evaluation of the data supporting the use of this test procedure and the peer review comments, EPA agrees with those commenters who stated that additional validation data are needed to fully characterize the performance of this method for various matrices and has decided not to include Method 1614A in today's final rule.

  49. Deferral of Action on EPA Method 1668C

    The Agency proposed to add EPA Method 1668C, ``Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/

    HRMS.'' This method measures individual chlorinated biphenyl congeners in environmental samples by isotope dilution and internal standard high resolution gas chromatography/high resolution mass spectrometry (HRGC/

    HRMS). As discussed in the proposal, Part 136 methods for chlorinated biphenyls (PCBs) only measure a mixture of congeners in seven Aroclors--PCB-1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254, and PCB-1260, while Method 1668C can measure the 209 PCB congeners in these mixtures.

    EPA began development of this method in 1995, initially covering 13 congeners labeled ``toxic'' by the World Health Organization. In 1999, EPA expanded the scope of the method to include all 209 PCB congeners. The method has been used to support several studies, including the 2001 National Sewage Sludge Survey and the National Lake Fish Tissue Survey. Since 1999, EPA has revised the method to incorporate additional information and data collected such as the results of an inter-

    laboratory validation study, peer reviews of the method and the validation study data, additional QC performance criteria and MDL data, and user experiences. In the development and subsequent multi-

    laboratory validation of this method, EPA evaluated method performance characteristics, such as selectivity, calibration, bias, precision, quantitation and detection limits. The Agency is aware that this method is being used in some states in their regulatory programs and by other groups for some projects with good success. For example, in a study of data comparability between two laboratories on samples collected from the Passaic River in New Jersey, in which 151 PCB congeners were identified and measured, accuracy, as measured by analysis of an NIST SRM, was 15% or better. Recoveries of the PCB congeners ranged from 90% to 124% and averaged 105%; precision ranged from 4.2 to 23% (Passaic River 2010). This type of data shows that recoveries and precision for this method are within the performance achievable with other approved methods.

    EPA received comments from thirty-five individuals or organizations on this method. Of these commenters, five (three states, one laboratory, and one laboratory organization) supported the approval of this method. Some states indicated that they are already requiring this method for use in permits and for other purposes. On the other hand, industry and industry groups/associations were critical of the method for various reasons. Commenters opposing the method provided a detailed critique of the method, the inter-laboratory study, the peer reviews and the other supporting documentation. Among the criticisms of the inter-laboratory study, commenters argued that: (1) EPA did not produce documentation supporting changes to the method approved by EPA for the interlaboratory study, (2) the raw data for wastewater and biosolids was poor and is not fit for use in a comprehensive interlaboratory study, (3) EPA cited certain guidelines such as ASTM but deviated from those guidelines (e.g., used only one Youden pair per matrix), (4) the peer reviewers' qualifications were questioned, (5) the addendum and the pooled MDLs/MLs were not subjected to peer review, (6) MDL/ML are flawed, the process to calculate MDLs/MLs for congeners that co-elute was flawed, the MDL/ML ignored the ubiquitous problem of background contamination, and (7) the validation study did not include all matrices in the method (soil and sediment excluded). In addition, some commenters also suggested that EPA should first promulgate new detection and quantitation procedures. Further, commenters raised questions about possible adverse effects of this new method on compliance monitoring as well as concerns about data reporting and costs.

    EPA is still evaluating the large number of public comments and intends to make a determination on the approval of this method at a later date. In the meantime, the Agency has decided to go forward with the promulgation of the other proposed analytical methods to expedite their implementation by the regulated community and laboratories. This decision does not negate the merits of this method for the determination of PCB congeners in regulatory programs or for other purposes when analyses are performed by an experienced laboratory.

  50. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09

    In today's rule, EPA is not adding two proposed ASTM methods, ASTM D7574-09 ``Standard Test Method for Determination of Bisphenol A (BPA),'' and ASTM D7485-09 ``Standard Test Method for Determination of NP, OP, NP1EO, and NP2EO.'' These two methods involve liquid chromatography and tandem mass spectrometry (LC/MS/MS). The methods have been tested by a single laboratory in several environmental waters, and may be useful for many applications. However, EPA has decided to postpone approval of these two methods for general use until completion of a full inter-laboratory validation study designed to fully characterize the performance of these methods across multiple laboratories and matrices.

  51. Revisions and Clarifications to EPA Method 200.7

    EPA Method 200.5 ``Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma--Atomic Emission Spectrometry'' employs a plasma torch viewed in the axial orientation to measure chemical elements (metals). As stated earlier in today's rule, EPA is adding Method 200.5 for some metals in Table IB. Both Methods 200.5 and 200.7 are acceptable methods under Part 136 and both methods employ ICP/AES technology. However, Method 200.5 includes performance data for the axial configuration that is not in Method 200.7 because the axial technology torch

    Page 29764

    results were not available when Method 200.7 was developed. For some parameters listed in Table IB, the axial orientation using ICP/AES technology results in greater sensitivity and lower detection limits than the radial orientation. Thus, today's approval of Method 200.5 and the additional flexibility to modify Method 200.7 to use the axial orientation discussed in the proposal will allow laboratories to use either axial instruments or radial instruments to measure metals in water samples with Method 200.7. In response to EPA's proposal to allow the use of the axial orientation of the torch with EPA Method 200.7, commenters expressed support for this added flexibility. Thus, today's rule clarifies that the use of the axial orientation of the torch to measure metals is an acceptable modification to Method 200.7. EPA has added new text at Part 136.6(b)(5) to allow the use of the axial orientation of the torch for Method 200.7 as an acceptable method modification that does not require an ATP application.

    EPA further notes that there was a typographical error in Section II.J of the proposed rule which stated that the version of EPA Method 200.7 (which the Agency proposed to remove; with Appendix C, see section IIIM below) has been superseded by Revision 5.4 of Method 200.7. Today's final rule reflects that the correct reference is Revision 4.4 of EPA Method 200.7. In today's rule, EPA has added Method 200.7 Revision 4.4 as an additional approved method for the measurement of titanium. As some commenters pointed out, EPA Method 200.7 covers this parameter and exclusion of this method for the measurement of titanium in Table IB was an oversight.

    In addition, EPA has removed EPA Method 200.7 from Table IB for the measurement of mercury. The addition of EPA Method 200.7 to the list of approved methods for mercury in Table IB was an error. Although this pollutant is on the list of analytes in EPA Method 200.7, mercury may be lost to the atmosphere through the use of the approved total recoverable metals digestion procedures (e.g., EPA Method 200.2, or the digestion procedures listed in EPA Method 200.7) that must be applied to the wastewater samples of interest under the Clean Water Act program. Such losses can lead to poor recovery in the samples compared to the sample preparation procedures included in other mercury methods approved at 40 CFR part 136. Therefore, EPA Method 200.7 has not been included in Table IB for mercury.

  52. Revisions and Corrections to Certain Citations in Tables IA, IB, IC, ID, and IG

    EPA proposed some additions to Table IB which include some new Standard Methods or new versions of approved Standard Methods. Today's rule revises the applicability of some methods and makes some corrections to the method citations. Specifically, EPA removed SM 3120 and SM 3125 for the measurement of mercury because mercury is not on the list of analytes for these methods. In addition, EPA corrected the citation of SM 3113 to SM 3113B-2004 in the final rule and has added SM 3113B-2004 for the measurement of cadmium, chromium, iron, lead, and silver, because these analytes are covered by the method and they exhibit acceptable analytical performance. These omissions were an oversight.

    EPA also deleted from Table ID an EPA GC/MS method, Method 525.1, for the measurement of ametryn, diazinon, disulfoton, prometon, and trifluoralin. These analytes are not listed within the scope of this method and their inclusion in the proposal was an error.

    EPA has corrected a number of typographical errors in the tables and footnotes, correcting spelling and method availability information, method title names, and document identification numbers. A complete list of these changes has been included in a memo to the docket.

  53. Continued Approval of Method 1664 Rev. A

    EPA proposed to replace Method 1664 Rev. A for the measurement of oil and grease with a revised version (Method 1664 Rev. B). This new version of the method describes modifications that are allowed and modifications that are not allowed when using this method for compliance with Clean Water Act regulations. Comments were generally supportive of the revised method but some commenters recommended that Method 1664 Rev. A not be withdrawn immediately because many permits currently specify the use of this method. In response to these comments, EPA will continue to allow the use of Method 1664 Rev. A for current permits because this method is not significantly different from the revised version of the method. However, EPA strongly encourages the use of the revised method (Method 1664 Rev. B) in the future. EPA may revisit this decision in a future rulemaking.

  54. Revision to Footnote 63 of Table IB at 40 CFR 136.3

    EPA received comments that the Hach Method 10360, described in footnote 63 of Table IB, is a dissolved oxygen procedure, and as such, should only be listed as a procedure for dissolved oxygen, and not for BOD and CBOD. EPA disagrees with these commenters because the method on its face is clearly applicable to dissolved oxygen measurements in conjunction with BOD and CBOD analyses, as described in the method. As a result, in today's final rule, EPA added language to the end of this footnote to clarify that Part 136 allows the use of Hach Method 10360 for measurement of dissolved oxygen in conjunction with the methods approved for measurement of biochemical demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).

  55. Revision to Footnote 4 of Table IC at 40 CFR 136.3

    EPA received comments on the proposed approval of Method 624 for the definitive determination of acrolein and acrylonitrile. Commenters agreed with the addition of these two analytes, but one of these commenters expressed concern about a blanket approval without requiring a demonstration of adequate performance and appropriate sample introduction techniques. This commenter recommended that performance criteria and information about appropriate sample introduction techniques be added to footnote 4 of Table IC. EPA agrees with this commenter's suggestions because this requirement would ensure that the laboratory has the ability to measure these analytes at the levels necessary to comply with any associated regulations. In response to these concerns, in today's rule, the Agency revised the footnote to add a statement requiring documentation of the ability to quantitatively measure these analytes and advising analysts that other sample introduction techniques may be required to achieve adequate performance.

    I. Revisions to Table II Language

    EPA proposed to revise the text at 136.3(e) to allow any party to modify sample preservation and holding times after submitting documentation to its permitting or other authority that supports use of an alternative approach. Commenters expressed concern that this change would present a burden both to permitting authorities to review and approve changes, and for laboratories that work in different states because each state could have different requirements. In response to public comments, EPA has removed the proposed language at 136.3(e) that would have allowed such modifications based on documentation and procedures

    Page 29765

    determined by individual permitting authorities. Instead, such modifications must continue to be requested via a limited use ATP application to the Regional Alternate Test Procedure Coordinator or permitting authority, as appropriate. Thus, approval of any changes in sample preservation procedures, container materials, and maximum allowable holding time will remain unchanged and continue to be the responsibility of EPA through its Alternate Test Procedure program. EPA clarified language regarding the limited use application process procedure. Additionally, in today's rule, EPA added a clarifying sentence at the end of the current language to emphasize that an analyst cannot modify any sample preservation or holding time requirements in an approved method unless the requirements in Section 136.3(e) are met.

    EPA also revised footnote 4 to Table II to delete the parenthetical statement specifying that samples analyzed for fecal coliforms may be held up to six hours prior to commencing analysis. That statement in footnote 4 is inconsistent with the requirement for an eight-hour holding time, as pointed out by a commenter.

    In response to comments, EPA included a new entry in Table II for the alkylated phenols (parameters 114 to 118 in Table IC) that was inadvertently omitted from the proposal. Similarly, when EPA moved EPA Methods 1650 and 1653 to Table IC, EPA inadvertently omitted to add the parameters adsorbable organic halides (AOX) and chlorinated phenolics to Table II. The Table II information for containers, preservation, and holding times for these three new entries are taken from the approved methods.

  56. Approval of Alternate Test Procedures for Limited Use at 40 CFR 136.5

    EPA proposed changes to 40 CFR 136.4 and 136.5 that establish the procedures for obtaining approval for use of a nationwide or limited use ATP. The proposed revisions established separate sections outlining the procedures for obtaining EPA review and approval for nationwide use of an ATP (Sec. Sec. 136.4), and the procedures for obtaining approval for limited use of an ATP (Sec. Sec. 136.5). The proposal also included language to clarify that limited use approvals do not require the same level of supporting data that would be required for nationwide approvals and that limited use approvals are not intended to be used as a means to avoid the full examination of comparability that is required for an application for approval of an alternative test procedure for nationwide use.

    Today's rule finalizes these sections as proposed with one exception. EPA received comments that the proposed language under Sec. 136.5 does not require that comparability data be submitted when seeking a Regional limited use ATP approval. EPA agrees that comparability data is an essential component of the ATP approval process and had inadvertently omitted this language. As a result, the Agency added language in today's final rule that requires an applicant to provide comparability data specific to the limited use for the performance of the proposed alternative test procedure relative to the performance of the reference method.

  57. Revisions to Language at Sec. 136.6

    EPA proposed to revise the section on method modification provisions at 40 CFR 136.6 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 in methods currently approved in 40 CFR part 136. Analysts may use the examples in this section to help assess whether the modifications require an ATP and if not, to document that their modification is acceptable. The additional examples provide further guidance to laboratories and permittees on allowable method modifications that do not require an application through the ATP program. Proposal comments generally expressed support for allowing the flexibility to make certain changes to methods and for the specific examples of allowable changes included in the proposal. In addition, some commenters suggested revisions to clarify EPA's intent in Sections (b)(4) and (b)(5) of 40 CFR 136.6. EPA reviewed the suggestions and agrees with commenters that the revisions will provide additional clarity. In addition, as discussed in Section III.D of this preamble, EPA added the use of axially viewed torch as an allowable modification to Method 200.7. Today's rule includes the following revisions to the regulatory text:

    (a) Adds language to Section (b)(3) to clarify that modifications to sample collection, preservation, and holding time do not fall within the scope of 136.6,

    (b) Revises the language at (b)(4)(T) be more specific with respect to the use of gas diffusion across a hydrophobic semi-permeable membrane to separate the analyte of interest from the sample matrix in place of manual or automated distillation for the analysis of certain analytes,

    (c) Revises the equation for Relative Standard Error (RSE) in (b)(4)(J) to make it consistent with the description in other EPA methods, and

    (d) Adds the use of an axially viewed torch with Method 200.7 as an allowable modification.

    L. Revisions to New Quality Assurance and Quality Control Language

    For today's rule, EPA added some introductory language to this section to clarify the new requirements. EPA added this language to provide some additional clarity as to when the new requirements are applicable and, thus, must be incorporated into the laboratory's documented standard operating procedures. Additional discussion of the revisions is provided under section IV.C below.

  58. Withdrawal of Appendices at 40 CFR Part 136

    EPA proposed to incorporate by reference in Table IB all of the methods printed in 40 CFR part 136 Appendices A and C, and to remove most of the information in Appendix D. The methods in Appendix A are EPA Method Numbers 601 through 613, 624, 625, 1613B, 1624B, and 1625B. Appendix C contains EPA Method 200.7, ``Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma--

    Atomic Emission Spectrometry''. However, Federal regulations at 1 CFR part 51.7(c)(1) prohibit the incorporation by reference of material previously published in the Federal Register. Thus, EPA is not withdrawing Appendices A or C. Because EPA Method 200.7 has been revised, EPA is replacing the current version of this method in Appendix C with Rev. 4.4 of Method 200.7. All of these methods are readily accessible from a variety of sources, including EPA's CWA methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm.

    The rule also removes most of the data from Appendix D for all EPA methods that are no longer approved, and retains only the Precision and Recovery Statements for EPA Method 279.2 for thallium and EPA Method 289.2 for zinc, and corrects

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    typographical errors in the Appendix. The current version of Appendix D will be available online at the CWA methods Web site for historical purposes.

  59. Revisions at 40 CFR Part 430 (Pulp, Paper, and Paperboard Point Source Category)

    EPA also proposed to remove Appendix A at 40 CFR part 430 and to incorporate by reference the methods in this Appendix. Appendix A contains two methods, EPA Method 1650 for adsorbable organic halides or AOX, and EPA Method 1653 for chlorinated phenolics. As explained above, we cannot incorporate by reference this material, so Appendix A remains unchanged in the Code of Federal Regulations. These methods are also readily available from a variety of sources, including EPA's CWA methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm. EPA is also adding these two methods to Table IC for general use.

  60. Revisions at 40 CFR Part 435 (Oil and Gas Extraction Point Source Category)

    The rule makes several changes to Part 435, Oil and Gas Extraction Point Source Category. First, EPA is moving the methods and associated quality assurance requirements 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-11-004), and incorporating by reference this document in the revised regulation at 40 CFR part 435. This 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 moved from part 435 to the cited document, EPA-821-R-11-004.

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

    ----------------------------------------------------------------------------------------------------------------

    Date first

    Analytical/Test method EPA Method No. 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 Degradation 1647 2001 Subpart A, Appendix 4.

    of Non-Aqueous Base Fluids in a Marine Closed

    Bottle Biodegradation Test System: Modified

    ISO 11734:1995.

    Determination of Crude Oil Contamination in 1655 2001 Subpart A, Appendix 5.

    Non-Aqueous Drilling Fluids by Gas

    Chromatography/Mass Spectrometry (GC/MS).

    Reverse Phase Extraction (RPE) Method for 1670 2001 Subpart A, Appendix 6.

    Detection of Oil Contamination in Non-Aqueous

    Drilling Fluids (NAF).

    Determination of the Amount of Non-Aqueous 1674 2001 Subpart A, Appendix 7.

    Drilling Fluid (NAF) Base Fluid from Drill

    Cuttings by a Retort Chamber (Derived from

    API Recommended Practice 13B-2).

    ----------------------------------------------------------------------------------------------------------------

    As noticed in the proposed rule, EPA is also incorporating additional quality assurance procedures in the marine anaerobic biodegradation method (Appendix 4 of Subpart A of part 435) and is correcting some erroneous references and omissions in the method for identification of crude oil contamination (Appendix 5 of Subpart A of part 435) into the new document (EPA-821-R-11-004).

    EPA promulgated the use of the marine anaerobic biodegradation method (closed bottle test, ISO 11734:1995 as clarified by Appendix 4 to Subpart A of part 435) as an Appendix to the rule 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 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. EPA worked with the same industry consortium that assisted EPA in the development of the analytical methods used in the effluent guidelines for the Oil and Gas Extraction point source category (40 CFR part 435) to develop these additional quality assurance measures. Thus, the quality assurance procedures are generally applicable to this industry.

    Additionally, as noticed in the proposed rule, EPA is correcting some erroneous references and omissions in the method for identification of crude oil contamination (Appendix 5 of Subpart A of Part 435), as follows:

    1. Adding a schematic flow for qualitative identification of crude oil, which was erroneously omitted in Appendix 5 to Subpart A of part 435,

    2. Correcting erroneous citations in sections 9.5, 9.6, 11.3, and 11.3.1 of Appendix 5, and

    3. Adding a missing `` 3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC media

      supplemented in the laboratory with 50 mug/mL of MUG may be used.

      \15\ Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-

      10-003. April 2010. U.S. EPA.

      \16\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and

      dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilertsupreg may be enumerated with

      the multiple-well procedures, Quanti-Traysupreg, Quanti-Traysupreg/2000, and the MPN calculated from the table provided by the manufacturer.

      \17\ Colilert-18supreg is an optimized formulation of the Colilertsupreg for the determination of total coliforms and E. coli that provides results

      within 18 h of incubation at 35 degC rather than the 24 h required for the Colilertsupreg test and is recommended for marine water samples.

      \18\ Descriptions of the Colilertsupreg, Colilert-18supreg, Quanti-Traysupreg, and Quanti-Traysupreg/2000 may be obtained from IDEXX

      Laboratories, Inc.

      \19\ A description of the mColiBlue24supreg test, is available from Hach Company.

      \20\ Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.

      \21\ Recommended for enumeration of target organism in wastewater effluent.

      \22\ Method 1603: Escherichia coli (E. coli ) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (modified

      mTEC), EPA-821-R-09-007. December 2009. U.S. EPA.

      \23\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-06-014. July 2006. U.S.

      EPA.

      \24\ A description of the Enterolertsupreg test may be obtained from IDEXX Laboratories Inc.

      \25\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-beta-D-Glucoside Agar (mEI), EPA-821-R-09-016.

      December 2009. U.S. EPA.

      \26\ Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA-821-R-02-012. Fifth Edition,

      October 2002. U.S. EPA.

      \27\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. EPA-821-R-02-013. Fourth Edition,

      October 2002. U.S. EPA.

      \28\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. EPA-821-R-02-014. Third

      Edition, October 2002. U.S. EPA.

      Table IB--List of Approved Inorganic Test Procedures

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Parameter Methodology \58\ EPA \52\ Standard methods ASTM USGS/AOAC/Other

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      1. Acidity, as CaCO3, mg/L......... Electrometric endpoint ...................... 2310 B-1997.......... D1067-06............. I-1020-85.\2\

      or phenolphthalein

      endpoint.

      2. Alkalinity, as CaCO3, mg/L...... Electrometric or ...................... 2320 B-1997.......... D1067-06............. 973.43 \3\, I-1030-

      Colorimetric 85.\2\

      titration to pH 4.5,

      Manual.

      Automatic............. 310.2 (Rev. 1974)\1\.. ..................... ..................... I-2030-85.\2\

      3. Aluminum--Total,\4\ mg/L........ Digestion,\4\ followed

      by any of the

      following:

      AA direct aspiration ...................... 3111 D-1999 or 3111 E- ..................... I-3051-85.\2\

      \36\ 1999.

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      97.\50\

      Direct Current ...................... ..................... D4190-08............. See footnote.\34\

      Plasma (DCP) \36\.

      Colorimetric ...................... 3500-Al B-2001.......

      (Eriochrome

      cyanine R).

      4. Ammonia (as N), mg/L............ Manual distillation 350.1, Rev. 2.0 (1993) 4500-NH3 B-1997...... ..................... 973.49\3\.

      \6\ or gas diffusion

      (pH > 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 ..................... I-4523-85.\2\

      salicylate, or (1993). 4500-NH3 H-1997......

      other substituted

      phenols in

      Berthelot reaction

      based methods.

      Page 29775

      Automated electrode Ion Chromatography.... ..................... D6919-09............. See footnote.\7\

      5. Antimony--Total,\4\ mg/L........ Digestion,\4\ followed

      by any of the

      following:

      AA direct ...................... 3111 B-1999..........

      aspiration \36\.

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      97.\50\

      6. Arsenic-Total,\4\ mg/L.......... Digestion,\4\ followed 206.5 (Issued 1978)

      by any of the \1\.

      following:

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

      3114 C-2009..........

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07.............

      \68\; 200.7, Rev. 4.4

      (1994).

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

      05.\70\

      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 B-2004.......... D4382-02(07).........

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... ..................... I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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....... D3645-08 (A)......... I-3095-85.\2\

      aspiration. 3111 E-1999..........

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

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

      ICP/AES............ 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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.......... ..................... 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 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 300.1-1, Rev 1.0 D-2000.

      (1997).

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

      12. Cadmium--Total,\4\ mg/L........ Digestion,\4\ followed

      by any of the

      following:

      Page 29776

      AA direct ...................... 3111 B-1999.......... D3557-02(07) (A or B) 974.27,\3\ p. 37.\9\,

      aspiration \36\. or 3111 C-1999....... I-3135-85 \2\ or I-

      3136-85.\2\

      AA furnace......... ...................... 3113 B-2004.......... D3557-02(07) (D)..... I-4138-89.\51\

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-1472-85 \2\ or I-

      \68\; 200.7, Rev. 4.4 4471-97.\50\

      (1994).

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

      97.\50\

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

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

      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 (2003) 3120 B-1999.......... ..................... I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

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

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

      Ion Chromatography. ...................... ..................... D6919-09.............

      14. Carbonaceous biochemical oxygen Dissolved Oxygen ...................... 5210 B-2001.......... ..................... See footnote.\35,63\

      demand (CBOD5), mg/L\12\. Depletion with

      nitrification

      inhibitor.

      15. Chemical oxygen demand (COD), Titrimetric........... 410.3 (Rev. 1978)\1\.. 5220 B-1997.......... D1252-06 (A)......... 973.46,\3\ p. 17,\9\

      mg/L. or C-1997............ I-3560-85.\2\

      Spectrophotometric, 410.4, Rev. 2.0 (1993) 5220 D-1997.......... D1252-06 (B)......... See footnotes.\13,14\

      manual or automatic. 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....... D4327-03............. 993.30\3\ , I-2057-

      and 300.1-1, Rev 1.0 4110 C-2000.......... 90.\51\

      (1997).

      CIE/UV................ ...................... 4140 B-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-carbazid

      e).

      19. Chromium--Total,\4\ mg/L....... Digestion,\4\ followed

      by any of the

      following:

      Page 29777

      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 B-2004.......... D1687-02(07) (C)..... I-3233-93.\46\

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

      ICP/AES \36\....... 200.5, Rev 4.2 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      (2003),\68\ 200.7,

      Rev. 4.4 (1994).

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

      05.\70\

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

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

      (Diphenyl-carbazid

      e).

      20. Cobalt--Total,\4\ mg/L......... Digestion,\4\ followed

      by any of the

      following:

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

      aspiration. 1999. 85.\2\

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      05.\70\

      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....... D1688-07 (A or B).... 974.27,\3\ p. 37,\9\

      aspiration \36\. 3111 C-1999.......... I-3270-85 \2\ or I-

      3271-85.\2\

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      05.\70\

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

      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)..........

      Page 29778

      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\.

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

      distillation,\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 300.1-1, Rev 1.0

      (1997).

      CIE/UV............. ...................... 4140 B-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 (Issued 1978)\1\ 3113 B-2004..........

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

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

      27. Hardness--Total, as CaCO3, mg/L Automated colorimetric 130.1 (Issued 1971)\1\

      Titrimetric (EDTA).... ...................... 2340 C-1997.......... D1126-02(07)......... 973.52B,\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\+\ B-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 B-2009..........

      30. Iron--Total,\4\ mg/L........... Digestion,\4\ followed

      by any of the

      following:

      AA direct ...................... 3111 B-1999 or....... D1068-05 (A or B).... 974.27,\3\ I-3381-

      aspiration \36\. 3111 C-1999.......... 85.\2\

      AA furnace......... ...................... 3113 B-2004.......... D1068-05 (C).........

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      Page 29779

      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.

      Semi-automated 350.1 Rev 2.0 1993.... 4500-NH3 G-1997.

      phenate. 4500-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....... D3559-08 (A or B).... 974.27,\3\ I-3399-

      aspiration \36\. 3111 C-1999.......... 85.\2\

      AA furnace......... ...................... 3113 B-2004.......... D3559-08 (D)......... I-4403-89.\51\

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

      ICP/AES \36\....... 200.5, Rev 4.2 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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:

      Page 29780

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

      aspiration \36\. 85.\2\

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      97.\50\

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

      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 B-2009.......... D3223-02(07)......... 977.22,\3\ I-3462-

      85.\2\

      Cold vapor, Automated. 245.2 (Issued 1974)\1\

      Cold vapor atomic 245.7 Rev. 2.0 ..................... ..................... I-4464-01.\71\

      fluorescence (2005)\17\.

      spectrometry (CVAFS).

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

      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 B-2004.......... ..................... I-3492-96.\47\

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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....... D1886-08 (A or B).... I-3499-85.\2\

      aspiration \36\. 3111 C-1999..........

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

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

      ICP/AES \36\....... 200.5, Rev 4.2 (2003) 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      \68\; 200.7, Rev. 4.4

      (1994).

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

      05.\70\

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

      38. Nitrate (as N), mg/L........... Ion Chromatography.... 300.0, Rev 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\

      and 300.1-1, Rev 1.0

      (1997).

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

      Ion Selective ...................... 4500-NO3- D-2000.....

      Electrode.

      Colorimetric 352.1 (Issued 1971)\1\ ..................... ..................... 973.50,\3\ 419D\1,7\,

      (Brucine sulfate). 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.\51\

      Automated.

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

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

      Colorimetric.

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

      and 300.1-1, Rev 1.0

      (1997).

      CIE/UV............. ...................... 4140 B-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\

      Page 29781

      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 300.1-1, Rev 1.0

      (1997).

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

      41. Oil and grease--Total Hexane extractable 1664 Rev. A; 1664 Rev. 5520 B-2001\38\......

      recoverable, mg/L. material (HEM): n- B\42\.

      Hexane extraction and

      gravimetry.

      Silica gel treated 1664 Rev. A; 1664 Rev. 5520 B-2001\38\ and

      HEM (SGT-HEM): B\42\. 5520 F-2001\38\.

      Silica gel

      treatment and

      gravimetry.

      42. Organic carbon--Total (TOC), mg/ Combustion............ ...................... 5310 B-2000.......... D7573-09............. 973.47\3\, p. 14.\24\

      L.

      Heated persulfate ...................... 5310 C 2000.......... D4839-03............. 973.47\3,\, p.

      or UV persulfate 5310 D 2000.......... 14.\24\

      oxidation.

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

      (Parameter 31) minus

      ammonia N (Parameter

      4).

      44. Ortho-phosphate (as P), mg/L... Ascorbic acid method:

      Automated.......... 365.1, Rev. 2.0 (1993) 4500-P F-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 300.1-1, Rev 1.0

      (1997).

      CIE/UV............. ...................... 4140 B-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 (C).......... See footnote\63\

      Sensor. 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 B-2009..........

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

      48. Phenols, mg/L.................. Manual 420.1\1\(Rev. 1978)... 5530 B-2005.......... D1783-01.............

      distillation\26\,

      followed by any of

      the following:

      Colorimetric (4AAP) 420.1\1\(Rev. 1978)... 5530 D-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........ Digestion\20\, ...................... 4500-P B(5)-1999..... ..................... 973.55.\3\

      followed by any of

      the following:

      Manual............. 365.3\1\(Issued 1978). 4500-P E-1999........ D515-88 (A)..........

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

      Page 29782

      Semi-automated 365.4\1\ (Issued 1974) ..................... D515-88 (B).......... I-4610-91.\48\

      block digestor

      (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 (Issued 1978)\1\

      ICP/MS............. ...................... 3125 B-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\

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

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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\

      105deg.

      54. Residue--filterable, mg/L...... Gravimetric, 180deg. ...................... 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. 105deg post washing

      of residue.

      56. Residue--settleable, mg/L...... Volumetric, (Imhoff ...................... 2540 F-1997..........

      cone), or gravimetric.

      57. Residue--Volatile, mg/L........ Gravimetric, 550deg. 160.4 (Issued 1971)\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 (Issued 1978)\1\

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

      60. Selenium--Total,\4\ mg/L....... Digestion\4\, followed

      by any of the

      following:

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

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

      ICP/AES\36\........ 200.5, Rev 4.2 3120 B-1999.......... D1976-07.............

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

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

      05.\70\

      AA gaseous hydride. ...................... 3114 B-2009, or 3111 D3859-08 (A)......... I-3667-85.\2\

      C-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 B-1999.......... ..................... I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 ..................... 974.27\3\, p. 37\9\,

      aspiration. 3111 C-1999.......... I-3720-85.\2\

      AA furnace......... ...................... 3113 B-2004.......... ..................... I-4724-89.\51\

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

      Page 29783

      ICP/AES............ 200.5, Rev 4.2 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 B-1999.......... ..................... I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 B-1997.......... D1125-95(99) (A)..... 973.40\3\, I-2781-

      cm at 25degC. 85.\2\

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

      or G-1997.

      Gravimetric........ ...................... 4500-SO4\2-\ C-1997 ..................... 925.54.\3\

      or D-1997.

      Turbidimetric...... ...................... 4500-SO4\2-\ 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-

      and 300.1-1, Rev 1.0 05.\70\

      (1997).

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

      66. Sulfide (as S), mg/L........... Sample Pretreatment... ...................... 4500-S2- B, C-2000...

      Titrimetric ...................... 4500-S2-F-2000....... ..................... I-3840-85.\2\

      (iodine).

      Colorimetric ...................... 4500-S2-D-2000.......

      (methylene blue).

      Ion Selective ...................... 4500-S2-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, degC............ 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 1978). 3113 B-2004..........

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

      ICP/AES............ 200.7, Rev. 4.4 3120 B-1999.......... D1976-07.............

      (1994); 200.5 Rev.

      4.2 (2003)\68\.

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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 B-2004..........

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

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

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

      ICP/MS............. 200.8, Rev. 5.4 (1994) 3125 B-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).

      ICP/AES............ 200.7, Rev. 4.4 (1994)

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

      Page 29784

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

      73. Turbidity, NTU\53\............. Nephelometric......... 180.1, Rev. 2.0 (1993) 2130 B-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 B-2004.......... D3373-03(07).........

      ICP/AES............ 200.5, Rev 4.2 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

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

      05.\70\

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

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

      aspiration\36\. 1999. I-3900-85.\2\

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

      ICP/AES\36\........ 200.5, Rev 4.2 3120 B-1999.......... D1976-07............. I-4471-97.\50\

      (2003)\68\; 200.7,

      Rev. 4.4 (1994).

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

      05.\70\

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

      Colorimetric ...................... 3500 Zn B-1997....... ..................... See footnote.\33\

      (Zincon).

      76. Acid Mine Drainage............. ...................... 1627\69\..............

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Table IB Notes:

      \1\ Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.

      \2\ Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological

      Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.

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

      International.

      \4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion

      procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable

      form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in

      Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to

      gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a

      combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as

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

      EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain

      elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic

      absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced

      method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission

      spectrometry (ICP-AES), the direct current plasma (DCP) technique or 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\ Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography, Journal of Chromatography,

      47(3):421-426.

      \29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as

      an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble

      in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be

      diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the

      approved method is satisfactory.

      \30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method

      specified quality control acceptance criteria are met.

      \31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in

      solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2

      to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent

      the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with

      reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as

      well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the

      cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.

      \32\ ``Water Temperature-Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.

      Geological Survey, Book 1, Chapter D1. 1975. USGS.

      \33\ Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.

      \34\ Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised

      1991. Thermo Jarrell Ash Corporation.

      \35\ In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

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

      Samples for Determination of Metals. April 16, 1992. CEM Corporation

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

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

      and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of

      other extraction solvents is prohibited.

      \39\ Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical.

      \40\ Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.

      \41\ Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical.

      \42\ Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable

      Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-

      821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane

      Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001.

      \43\ Method 1631, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August

      2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality

      Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations.

      \44\ Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.

      \45\ Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonium Plus

      Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS.

      \46\ Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by

      Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.

      \47\ Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by

      Graphite Furnace Atomic Absorption Spectrophotometry. 1997.. USGS.

      \48\ Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by

      Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS.

      \49\ Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium

      in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS.

      \50\ Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-

      water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS.

      \51\ Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and

      Organic Constituents in Water and Fluvial Sediments. 1993.. USGS.

      \52\ Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1-1, are published in U.S. EPA. May 1994. Methods for the Determination of

      Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in

      Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of

      Inorganic Ions in Drinking Water by Ion Chromatography.

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

      substitutes for formazin.

      \54\ Method D6508, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate

      Electrolyte. December 2000. Waters Corp.

      Page 29786

      \55\ Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001.

      US EPA. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control

      (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the

      method, provided that the QC acceptance criteria are met.

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

      Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Lachat Instruments.

      \57\ When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to

      distillation.

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

      approved digestion and/or distillation are required prior to analysis.

      \59\ Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-09 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, Patton, C.J. and S.R. Crouch. March 1977.

      Anal. Chem. 49:464-469. These reaction parameters increase to pH > 12.6 and 665 nm when salicylate is used as the color reagent--see, Krom, M.D. April

      1980. The Analyst 105:305-316.

      \61\ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may

      be used. This method has poorer precision and bias than the methods of choice.

      \62\ Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.

      \63\ Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5.

      Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for

      measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).

      \64\ In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.

      \65\ Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

      \66\ Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

      \67\ Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.

      \68\ EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/

      600/R-06/115. Revision 4.2, October 2003. US EPA.

      \69\ Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. US EPA.

      \70\ Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell

      Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis,

      2006. USGS.

      \71\ Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination

      of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water With Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.

      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-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      2. Acenaphthylene.................. GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      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-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440B-2000........... D4657-92 (98)........ .....................

      6. Benzene......................... GC.................... 602................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      7. Benzidine....................... Spectro-photometric... ...................... ..................... ..................... See footnote \3\,

      p.1.

      GC/MS................. 625 \5\, 1625B........ 6410 B-2000. .....................

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

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

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      9. Benzo(a)pyrene.................. GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      10. Benzo(b)fluoranthene........... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      11. Benzo(g,h,i)perylene........... GC.................... 610.

      Page 29787

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      12. Benzo(k)fluoranthene........... GC.................... 610.

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      13. Benzyl chloride................ GC.................... ...................... ..................... ..................... See footnote \3\, p.

      130.

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

      S102.

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

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      15. bis(2-Chloroethoxy) methane.... GC.................... 611. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      16. bis(2-Chloroethyl) ether....... GC.................... 611. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      17. bis(2-Ethylhexyl) phthalate.... GC.................... 606. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      18. Bromodichloromethane........... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      19. Bromoform...................... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      20. Bromomethane................... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      21. 4-Bromophenyl phenyl ether..... GC.................... 611. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      22. Carbon tetrachloride........... GC.................... 601................... 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      23. 4-Chloro-3-methyl phenol....... GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000. See footnote \9\, p.

      27.

      24. Chlorobenzene.................. GC.................... 601, 602.............. 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      25. Chloroethane................... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      26. 2-Chloroethylvinyl ether....... GC.................... 601. .....................

      GC/MS................. 624, 1624B. .....................

      27. Chloroform..................... GC.................... 601................... 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      28. Chloromethane.................. GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      29. 2-Chloronaphthalene............ GC.................... 612. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      30. 2-Chlorophenol................. GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      31. 4-Chlorophenyl phenyl ether.... GC.................... 611. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      32. Chrysene....................... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      33. Dibenzo(a,h)anthracene......... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      34. Dibromochloromethane........... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      35. 1,2-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-1997. .....................

      Page 29788

      GC/MS................. 624, 1625B............ 6200 B-1997.......... ..................... See footnote \9\, p.

      27.

      36. 1,3-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-1997. .....................

      GC/MS................. 624, 1625B............ 6200 B-1997.......... ..................... See footnote \9\, p.

      27.

      37. 1,4-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-1997. .....................

      GC/MS................. 624, 1625B............ 6200 B-1997.......... ..................... See footnote \9\, p.

      27.

      38. 3,3'-Dichlorobenzidine......... GC/MS................. 625, 1625B............ 6410 B-2000. .....................

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

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

      GC/MS................. ...................... 6200 C-1997. .....................

      40. 1,1-Dichloroethane............. GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      41. 1,2-Dichloroethane............. GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      42. 1,1-Dichloroethene............. GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      43. trans-1,2-Dichloroethene....... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      44. 2,4-Dichlorophenol............. GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      45. 1,2-Dichloropropane............ GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      46. cis-1,3-Dichloropropene........ GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      47. trans-1,3-Dichloropropene...... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      48. Diethyl phthalate.............. GC.................... 606. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      49. 2,4-Dimethylphenol............. GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      50. Dimethyl phthalate............. GC.................... 606. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      51. Di-n-butyl phthalate........... GC.................... 606. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      52. Di-n-octyl phthalate........... GC.................... 606. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      53. 2, 4-Dinitrophenol............. GC.................... 604................... 6420 B-2000.......... ..................... See footnote \9\, p.

      27.

      GC/MS................. 625, 1625B............ 6410 B-2000. .....................

      54. 2,4-Dinitrotoluene............. GC.................... 609. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      55. 2,6-Dinitrotoluene............. GC.................... 609. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      56. Epichlorohydrin................ GC.................... ...................... ..................... ..................... See footnote \3\, p.

      130.

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

      S102.

      57. Ethylbenzene................... GC.................... 602................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      58. Fluoranthene................... GC.................... 610. ..................... .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      59. Fluorene....................... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      60. 1,2,3,4,6,7,8-Heptachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

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

      dibenzofuran.

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

      dibenzo-p-dioxin.

      63. Hexachlorobenzene.............. GC.................... 612. .....................

      Page 29789

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      64. Hexachlorobutadiene............ GC.................... 612. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      65. Hexachlorocyclopentadiene...... GC.................... 612. .....................

      GC/MS................. 625 \5\, 1625B........ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      66. 1,2,3,4,7,8-Hexachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      67. 1,2,3,6,7,8-Hexachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      68. 1,2,3,7,8,9-Hexachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      69. 2,3,4,6,7,8-Hexachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      70. 1,2,3,4,7,8-Hexachloro-dibenzo- GC/MS................. 1613B. .....................

      p-dioxin.

      71. 1,2,3,6,7,8-Hexachloro-dibenzo- GC/MS................. 1613B. .....................

      p-dioxin.

      72. 1,2,3,7,8,9-Hexachloro-dibenzo- GC/MS................. 1613B. .....................

      p-dioxin.

      73. Hexachloroethane............... GC.................... 612. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      74. Indeno(1,2,3-c,d) pyrene....... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      75. Isophorone..................... GC.................... 609. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      76. Methylene chloride............. GC.................... 601................... 6200 C-1997. ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      77. 2-Methyl-4,6-dinitrophenol..... GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000. ..................... See footnote \9\, p.

      27.

      78. Naphthalene.................... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27

      HPLC.................. 610................... 6440 B-2000. .....................

      79. Nitrobenzene................... GC.................... 609. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. ...................... ..................... D4657-92 (98)........ .....................

      80. 2-Nitrophenol.................. GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      81. 4-Nitrophenol.................. GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      82. N-Nitrosodimethylamine......... GC.................... 607. .....................

      GC/MS................. 625 \5\, 1625B........ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      83. N-Nitrosodi-n-propylamine...... GC.................... 607. .....................

      GC/MS................. 625 \5\, 1625B........ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      84. N-Nitrosodiphenylamine......... GC.................... 607. .....................

      GC/MS................. 625 \5\, 1625B........ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      85. Octachlorodibenzofuran......... GC/MS................. 1613B.\10\ .....................

      86. Octachlorodibenzo-p-dioxin..... GC/MS................. 1613B.\10\ .....................

      87. 2,2'-Oxybis(2-chloro-propane) GC.................... 611. .....................

      also known as bis(2-

      Chloroisopropyl) ether.

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      88. PCB-1016....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      GC/MS................. 625................... 6410 B-2000. .....................

      89. PCB-1221....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      GC/MS................. 625................... 6410 B-2000. .....................

      90. PCB-1232....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      Page 29790

      GC/MS................. 625................... 6410 B-2000. .....................

      91. PCB-1242....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      GC/MS................. 625................... 6410 B-2000. .....................

      92. PCB-1248....................... GC.................... 608. .....................

      GC/MS................. 625................... 6410 B-2000. .....................

      93. PCB-1254....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      GC/MS................. 625................... 6410 B-2000. .....................

      94. PCB-1260....................... GC.................... 608................... ..................... ..................... See footnote \3\, p.

      43; See footnote.

      \8\

      GC/MS................. 625................... 6410 B-2000. .....................

      95. 1,2,3,7,8-Pentachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      96. 2,3,4,7,8-Pentachloro- GC/MS................. 1613B. .....................

      dibenzofuran.

      97. 1,2,3,7,8,-Pentachloro-dibenzo- GC/MS................. 1613B. .....................

      p-dioxin.

      98. Pentachlorophenol.............. GC.................... 604................... 6420 B-2000.......... ..................... See footnote \3\, p.

      140.

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      99. Phenanthrene................... GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      100. Phenol........................ GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      101. Pyrene........................ GC.................... 610. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      HPLC.................. 610................... 6440 B-2000.......... D4657-92 (98)........ .....................

      102. 2,3,7,8-Tetrachloro- GC/MS................. 1613B.\10\ .....................

      dibenzofuran.

      103. 2,3,7,8-Tetrachloro-dibenzo-p- GC/MS................. 613, 625 \5a\, 1613B.. .....................

      dioxin.

      104. 1,1,2,2-Tetrachloroethane..... GC.................... 601................... 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      105. Tetrachloroethene............. GC.................... 601................... 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      106. Toluene....................... GC.................... 602................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      107. 1,2,4-Trichlorobenzene........ GC.................... 612................... ..................... ..................... See footnote \3\, p.

      130.

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      108. 1,1,1-Trichloroethane......... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      109. 1,1,2-Trichloroethane......... GC.................... 601................... 6200 C-1997.......... ..................... See footnote \3\, p.

      130.

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      110. Trichloroethene............... GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      111. Trichlorofluoromethane........ GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624................... 6200 B-1997. .....................

      112. 2,4,6-Trichlorophenol......... GC.................... 604................... 6420 B-2000. .....................

      GC/MS................. 625, 1625B............ 6410 B-2000.......... ..................... See footnote \9\, p.

      27.

      113. Vinyl chloride................ GC.................... 601................... 6200 C-1997. .....................

      GC/MS................. 624, 1624B............ 6200 B-1997. .....................

      114. Nonylphenol................... GC/MS................. ...................... ..................... D7065-06. .....................

      115. Bisphenol A (BPA)............. GC/MS................. ...................... ..................... D7065-06. .....................

      116. p-tert-Octylphenol (OP)....... GC/MS................. ...................... ..................... D7065-06. .....................

      117. Nonylphenol Monoethoxylate GC/MS................. ...................... ..................... D7065-06. .....................

      (NP1EO).

      118. Nonylphenol Diethoxylate GC/MS................. ...................... ..................... D7065-06. .....................

      (NP2EO).

      119. Adsorbable Organic Halides Adsorption and 1650.\11\ .....................

      (AOX). Coulometric Titration.

      Page 29791

      120. Chlorinated Phenolics......... In Situ Acetylation 1653.\11\ .....................

      and GC/MS.

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Table IC notes:

      \1\ All parameters are expressed in micrograms per liter (mug/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, 1613B, 1624B, and 1625B are provided 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. September 1978. U.S. EPA.

      \4\ Method 624 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate

      the ability to detect and quantify these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample

      introduction techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 should be used when analyzing samples

      for acrolein and acrylonitrile in the absence of such criteria in Method 624.

      \5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi-n-propylamine, and N-

      nitrosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these

      compounds.

      \5a\ Method 625, screening only.

      \6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard

      Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).

      \7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624,

      625, 1624B, and 1625B 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 EmporeTM Disk. Revised October 28, 1994. 3M Corporation.

      \9\ Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of

      Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

      \10\ Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method

      1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and

      Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in Appendix A to 40 CFR Part 136 and at

      http://water.epa.gov/scitech/methods/cwa/index.cfm

      \11\ Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997. U.S. EPA. Method 1653, Chlorinated Phenolics in

      Wastewater by In Situ Acetylation and GCMS. Revision A, 1997. U.S. EPA. The full text for both of these methods is provided at Appendix A in Part 430,

      The Pulp, Paper, and Paperboard Point Source Category.

      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-2000 & C-2000. 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-2000. ....................

      2. Ametryn........................ GC........................ 507, 619............. ..................... .................... See footnote \3\, p.

      83; See footnote

      \9\, O-3106-93; See

      footnote \6\, p.

      S68.

      GC/MS..................... 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-2000 & C-2000. D3086-90, D5812- See footnote \3\, p.

      96(02). 7; See footnote

      \8\, 3M0222.

      GC/MS..................... 625 \5\.............. 6410 B-2000.......... .................... See footnote \11\, O-

      1126-95.

      Page 29792

      9. beta-BHC..................... GC........................ 608, 617............. 6630 B-2000 & C-2000. D3086-90, D5812- See footnote \8\,

      96(02). 3M0222.

      GC/MS..................... 625.................. 6410 B-2000. ....................

      10. delta-BHC................... GC........................ 608, 617............. 6630 B-2000 & C-2000. D3086-90, D5812- See footnote \8\,

      96(02). 3M0222.

      GC/MS..................... 625.................. 6410 B-2000. ....................

      11. gamma-BHC (Lindane)......... GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000.......... .................... See footnote \11\, O-

      1126-95.

      12. Captan........................ GC........................ 617.................. 6630 B-2000.......... 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-2000.......... .................... See footnote \4\,

      page 27; See

      footnote \6\, p.

      S73.

      15. Chlordane..................... GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000. ....................

      16. Chloropropham................. TLC....................... ..................... ..................... .................... See footnote \3\, p.

      104; See footnote

      \6\, p. S64.

      HPLC...................... 632. ....................

      17. 2,4-D......................... GC........................ 615.................. 6640 B-2001.......... .................... 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-2000 & C-2000. 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-2000. ....................

      19. 4,4'-DDE...................... GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000.......... .................... See footnote \11\, O-

      1126-95.

      20. 4,4'-DDT...................... GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000. ....................

      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..................... 525.2................ ..................... .................... 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 \4\,

      page 27; See

      footnote \6\, p.

      S73.

      26. Dichloran..................... GC........................ 608.2, 617........... 6630 B-2000.......... .................... See footnote \3\, p.

      7;

      27. Dicofol....................... GC........................ 617.................. ..................... .................... See footnote \4\, O-

      3104-83.

      28. Dieldrin...................... GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000.......... .................... See footnote \11\, O-

      1126-95.

      29. Dioxathion.................... GC........................ 614.1, 1657.......... ..................... .................... See footnote \4\,

      page 27; See

      footnote \6\, p.

      S73.

      30. Disulfoton.................... GC........................ 507, 614, 622, 1657.. ..................... .................... See footnote \3\, p.

      25; See footnote

      \6\ p. S51.

      GC/MS..................... 525.2................ ..................... .................... 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.

      Page 29793

      32. Endosulfan I.................. GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000.......... .................... See footnote \13\, O-

      2002-01.

      33. Endosulfan II................. GC........................ 608, 617............. 6630 B-2000 & C-2000. D3086-90, D5812- See footnote \3\, p.

      96(02). 7; See footnote

      \8\, 3M0222.

      GC/MS..................... 625 \5\.............. 6410 B-2000.......... .................... See footnote \13\,

      O-2002-01.

      34. Endosulfan Sulfate............ GC........................ 608, 617............. 6630 C-2000.......... .................... See footnote \8\,

      3M0222.

      GC/MS..................... 625.................. 6410 B-2000.......... .................... ....................

      35. Endrin........................ GC........................ 505, 508, 608, 617, 6630 B-2000 & C-2000. 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-2000. ....................

      36. Endrin aldehyde............... GC........................ 608, 617............. 6630 C-2000.......... .................... See footnote \8\,

      3M0222.

      GC/MS..................... 625. ....................

      37. Ethion........................ GC........................ 614, 614.1,1657...... ..................... .................... See footnote \4\,

      page 27; 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-2000 & C-2000. 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-2000. ....................

      41. Heptachlor epoxide............ GC........................ 608, 617............. 6630 B-2000 & C-2000. 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-2000. ....................

      42. Isodrin....................... GC........................ 617.................. 6630 B-2000 & C-2000. .................... 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-2000.......... .................... 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-2000 & C-2000. 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-2000 & C-2000. 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-2000.......... .................... See footnote \4\,

      page 27; See

      footnote \3\, p.

      25.

      Page 29794

      GC/MS..................... ..................... ..................... .................... See footnote \11\, O-

      1126-95.

      53. Parathion ethyl............... GC........................ 614.................. 6630 B-2000.......... .................... See footnote \4\,

      page 27; See

      footnote \3\, p.

      25.

      GC/MS..................... ..................... ..................... .................... See footnote \11\, O-

      1126-95.

      54. PCNB.......................... GC........................ 608.1, 617........... 6630 B-2000 & C-2000. D3086-90, D5812- See footnote \3\, p.

      96(02). 7.

      55. Perthane...................... GC........................ 617.................. ..................... 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..................... 525.2................ ..................... .................... See footnote \11\, O-

      1126-95.

      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-2000 & C-2000. .................... 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-2001.......... .................... See footnote \3\, p.

      115; See footnote

      \4\, O-3105-83.

      67. 2,4,5-TP (Silvex)............. GC........................ 615.................. 6640 B-2001.......... .................... 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-2000 & C-2000. D3086-90, D5812- See footnote \3\, p.

      1656. 96(02). 7; See footnote

      \8\; See footnote

      \4\, O-3105-83.

      GC/MS..................... 525.1, 525.2, 625.... 6410 B-2000. ....................

      70. Trifluralin................... GC........................ 508, 617, 627, 1656.. 6630 B-2000.......... .................... See footnote \3\, p.

      7; See footnote

      \9\, O-3106-93.

      GC/MS..................... 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 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. September 1978. U.S. EPA. This EPA

      publication includes thin-layer chromatography (TLC) methods.

      \4\ Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S.

      Geological Survey, Book 5, Chapter A3. 1987. USGS.

      \5\ The method may be extended to include 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 15th Edition of Standard

      Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).

      Page 29795

      \7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625

      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 Empore \TM\ Disk. Revised October 28, 1994. 3M Corporation.

      \9\ Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of

      Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography With Nitrogen Phosphorus Detectors. 1994. USGS.

      \10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional

      Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. The full text of Methods 608 and 625 are provided at

      Appendix A, Test Procedures for Analysis of Organic Pollutants, of this Part 136. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for

      the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA Method 525.2

      is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry,

      Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial

      Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA.

      \11\ Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination

      of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995.

      USGS.

      \12\ Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality

      Laboratory--Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass

      Spectrometry. 2001. USGS.

      \13\ Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality

      Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass

      spectrometry. 2001. USGS.

      \14\ Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination

      of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion

      monitoring. 1992. USGS.

      * * * * *

      Table IG--Test Methods for Pesticide Active Ingredients (40 CFR Part 455)

      ----------------------------------------------------------------------------------------------------------------

      EPA survey code Pesticide name CAS No. EPA analytical method No.(s) \3\

      ----------------------------------------------------------------------------------------------------------------

      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......................... 834-12-8 507/619/525.2

      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 1657/507/614/622/525.2

      107......................... Parathion methyl................ 298-00-0 1657/614/622

      110......................... DCPA Dimethyl 2,3,5,6- 1861-32-1 508/608.2/525.1/525.2/515.1 \2\/

      tetrachloro-terephthalate. 515.2 \2\/1656

      Page 29796

      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 See footnote 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.

      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 1656/627 See footnote 1

      182......................... Fensulfothion................... 115-90-2 1657/622

      183......................... Disulfoton...................... 298-04-4 1657/507/614/622/525.2

      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........................ 1610-18-0 507/619/525.2

      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 dimethyldithio- 128-04-1 630/630.1

      carbamate.

      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 \1\................. 1582-09-8 1656/508/617/627/525.2

      268......................... Ziram Zinc 137-30-4 630/630.1

      dimethyldithiocarbamate.

      ----------------------------------------------------------------------------------------------------------------

      Table 1G notes:

      \1\ Monitor and report as total Trifluralin.

      \2\ Applicable to the analysis of DCPA degradates.

      \3\ EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are available in Methods For The Determination

      of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, Revision I,

      August 1993, U.S. EPA. EPA Methods 200.9 and 505 through 555 are available in Methods For The Determination of

      Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, August 1993,

      U.S. EPA. The full text of Methods 608, 625 and 1625 are provided at Appendix A of this Part 136. The full

      text of Method 200.7 is provided at Appendix C of this Part 136.

      Page 29797

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

      \5\.

      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.

      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, or. F-2006 11,13.

      Multiple tube/ ................... 9223 B-2004 \12\... 991.15 \10\........ Colilertsupreg12,16, Colilert-

      multiple well, or. 18supreg12,15,16.

      MF 2,5,6,7,8, two 1103.1 \19\........ 9222 B-1997/9222 G- D5392-93 \9\. ................................

      step, or. 1997 \18\, 9213 D-

      2007.

      Single step......... 1603 \20\, 1604 ................... ................... mColiBlue-24supreg\17\.

      \21\.

      6. Fecal streptococci, number MPN, 5 tube, 3 p. 139 \3\......... 9230 B-2007. ................................

      per 100 mL. dilution, or.

      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 ................... ................... D6503-99 \9\....... Enterolertsupreg12,22.

      100 mL. tube/multiple well,

      or.

      MF 2,5,6,7,8 two 1106.1 \23\........ 9230 C-2007........ D5259-92 \9\. ................................

      step, or.

      Single step, or..... 1600 \24\.......... 9230 C-2007. ................................

      Plate count......... p. 143 \3\. ................................

      Protozoa:

      8. Cryptosporidium........... Filtration/IMS/FA... 1622 \25\, 1623 ................................

      \26\.

      9. Giardia................... Filtration/IMS/FA... 1623 \26\ ................................

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Table 1H notes:

      \1\ The method must be specified when results are reported.

      \2\ A 0.45-microm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of

      extractables which could interfere with their growth.

      \3\ Microbiological Methods for Monitoring the Environment, Water, and Wastes. EPA/600/8-78/017. 1978. US EPA.

      \4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of

      Aquatic Biological and Microbiological Samples. 1989. USGS.

      \5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to

      resolve any controversies.

      \6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes

      to account for the quality, character, consistency, and anticipated organism density of the water sample.

      \7\ When the MF method has 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\ Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.

      \10\ Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.

      \11\ The multiple-tube fermentation test is used in 9221B.1-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25

      parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-

      positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase

      on 10 percent of all total coliform-positive tubes on a seasonal basis.

      \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.1-2006, all presumptive tubes or bottles showing any amount of gas,

      growth or acidity within 48 h 3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC media

      supplemented in the laboratory with 50 microg/mL of MUG may be used.

      Page 29798

      \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 Colilertsupreg may be enumerated with

      the multiple-well procedures, Quanti-Traysupreg or Quanti-Traysupreg/2000, and the MPN calculated from the table provided by the manufacturer.

      \15\ Colilert-18supreg is an optimized formulation of the Colilertsupreg for the determination of total coliforms and E. coli that provides results

      within 18 h of incubation at 35 degC, rather than the 24 h required for the Colilertsupreg test, and is recommended for marine water samples.

      \16\ Descriptions of the Colilertsupreg, Colilert-18supreg, Quanti-Traysupreg, and Quanti-Traysupreg/2000 may be obtained from IDEXX

      Laboratories Inc.

      \17\ A description of the mColiBlue24supreg test may be obtained from Hach Company.

      \18\ Subject total coliform positive samples determined by 9222B-1997 or other membrane filter procedure to 9222G-1997 using NA-MUG media.

      \19\ Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-10-

      002. March 2010. US EPA.

      \20\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified

      mTEC), EPA-821-R-09-007. December 2009. US EPA.

      \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 Method 1604: Total Coliforms and

      Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium), EPA 821-R-02-024, September 2002,

      US EPA.

      \22\ A description of the Enterolertsupreg test may be obtained from IDEXX Laboratories Inc.

      \23\ Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), EPA-821-R-09-015. December 2009.

      US EPA.

      \24\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-beta-D-Glucoside Agar (mEI), EPA-821-R-09-016.

      December 2009. US EPA.

      \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.

      Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. US EPA.

      \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. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002. December

      2005. US EPA.

      (b) The documents required in this section are incorporated by reference into this section with approval of the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the documents may be obtained from the sources listed in paragraph (b) of this section. Documents may be inspected at EPA's Water Docket, EPA West, 1301 Constitution Avenue NW., Room B102, Washington, DC (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. These test procedures are incorporated as they exist on the day of approval and a notice of any change in these test procedures will be published in the Federal Register. The full texts of the methods from the following references which are cited in Tables IA, IB, IC, ID, IE, IF, IG and IH are incorporated by reference into this regulation and may be obtained from the source identified. All costs cited are subject to change and must be verified from the indicated source.

      (1) Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161

      (i) Microbiological Methods for Monitoring the Environment, Water, and Wastes. 1978. EPA/600/8-78/017, Pub. No. PB-290329/A.S.

      (A) Part III Analytical Methodology, Section B Total Coliform Methods, page 108. Table IA, Note 3; Table IH, Note 3.

      (B) Part III Analytical Methodology, Section B Total Coliform Methods, 2.6.2 Two-Step Enrichment Procedure, page 111. Table IA, Note 3; Table IH, Note 3.

      (C) Part III Analytical Methodology, Section B Total Coliform Methods, 4 Most Probable Number (MPN) Method, page 114. Table IA, Note 3; Table IH, Note 3.

      (D) Part III Analytical Methodology, Section C Fecal Coliform Methods, 2 Direct Membrane Filter (MF) Method, page 124. Table IA, Note 3; Table IH, Note 3.

      (E) Part III, Analytical Methodology, Section C Fecal Coliform Methods, 5 Most Probable Number (MPN) Method, page 132. Table IA, Note 3; Table IH, Note 3.

      (F) Part III Analytical Methodology, Section D Fecal Streptococci, 2 Membrane Filter (MF) Method, page 136. Table IA, Note 3; Table IH, Note 3.

      (G) Part III Analytical Methodology, Section D Fecal Streptococci, 4 Most Probable Number Method, page 139. Table IA, Note 3; Table IH, Note 3.

      (H) Part III Analytical Methodology, Section D Fecal Streptococci, 5 Pour Plate Method, page 143. Table IA, Note 3; Table IH, Note 3.

      (ii) Reserved

      (2) Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.

      (i) Method 300.1 (including Errata Cover Sheet, April 27, 1999), Determination of Inorganic Ions in Drinking Water by Ion Chromatography, Revision 1.0, 1997. Table IB, Note 52.

      (ii) Method 551, Determination of Chlorination Disinfection Byproducts and Chlorinated Solvents in Drinking Water by Liquid-Liquid Extraction and Gas Chromatography With Electron-Capture Detection. 1990. Table IF.

      (3) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available from http://water.epa.gov/scitech/methods/cwa/index.cfm or from the National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Telephone: 800-553-6847.

      (i) Methods for the Determination of Inorganic Substances in Environmental Samples. August 1993. EPA/600/R-93/100, Pub. No. PB 94120821. Table IB, Note 52.

      (A) Method 180.1, Determination of Turbidity by Nephelometry. Revision 2.0. Table IB, Note 52.

      (B) Method 300.0, Determination of Inorganic Anions by Ion Chromatography. Revision 2.1. Table IB, Note 52.

      (C) Method 335.4, Determination of Total Cyanide by Semi-Automated Colorimetry. Revision 1.0. Table IB, Notes 52 and 57.

      (D) Method 350.1, Determination of Ammonium Nitrogen by Semi-

      Automated Colorimetry. Revision 2.0. Table IB, Notes 30 and 52.

      (E) Method 351.2, Determination of Total Kjeldahl Nitrogen by Semi-

      Automated Colorimetry. Revision 2.0. Table IB, Note 52.

      (F) Method 353.2, Determination of Nitrate-Nitrite Automated Colorimetry. Revision 2.0. Table IB, Note 52.

      Page 29799

      (G) Method 365.1, Determination of Phosphorus by Automated Colorimetry. Revision 2.0. Table IB, Note 52.

      (H) Method 375.2, Determination of Sulfate by Automated Colorimetry. Revision 2.0. Table IB, Note 52.

      (I) Method 410.4, Determination of Chemical Oxygen Demand by Semi-

      Automated Colorimetry. Revision 2.0. Table IB, Note 52.

      (ii) Methods for the Determination of Metals in Environmental Samples, Supplement I. May 1994. EPA/600/R-94/111, Pub. No. PB 95125472. Table IB, Note 52.

      (A) Method 200.7, Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission Spectrometry. Revision 4.4. Table IB, Note 52.

      (B) Method 200.8, Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma Mass Spectrometry. Revision 5.3. Table IB, Note 52.

      (C) Method 200.9, Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry. Revision 2.2. Table IB, Note 52.

      (D) Method 218.6, Determination of Dissolved Hexavalent Chromium in Drinking Water, Groundwater, and Industrial Wastewater Effluents by Ion Chromatography. Revision 3.3. Table IB, Note 52.

      (E) Method 245.1, Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry. Revision 3.0. Table IB, Note 52.

      (4) National Exposure Risk Laboratory-Cincinnati, U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.

      (i) EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry. Revision 4.2, October 2003. EPA/600/R-06/115. Table IB, Note 68.

      (ii) EPA Method 525.2, Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry. Revision 2.0, 1995. Table ID, Note 10.

      (5) Office of Research and Development, Cincinnati OH. U.S. Environmental Protection Agency, Cincinnati OH (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from ORD Publications, CERI, U.S. Environmental Protection Agency, Cincinnati OH 45268.

      (i) Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol, and Pesticides in Water and Wastewater. 1978. Table IC, Note 3; Table ID, Note 3.

      (ii) Methods for Chemical Analysis of Water and Wastes. March 1979. EPA-600/4-79-020. Table IB, Note 1.

      (iii) Methods for Chemical Analysis of Water and Wastes. Revised March 1983. EPA-600/4-79-020. Table IB, Note 1.

      (A) Method 120.1, Conductance, Specific Conductance, mumhos at 25 degC. Revision 1982. Table IB, Note 1.

      (B) Method 130.1, Hardness, Total (mg/L as CaCO3), Colorimetric, Automated EDTA. Issued 1971. Table IB, Note 1.

      (C) Method 150.2, pH, Continuous Monitoring (Electrometric). December 1982. Table IB, Note 1.

      (D) Method 160.4, Residue, Volatile, Gravimetric, Ignition at 550 degC. Issued 1971. Table IB, Note 1.

      (E) Method 206.5, Arsenic, Sample Digestion Prior to Total Arsenic Analysis by Silver Diethyldithiocarbamate or Hydride Procedures. Issued 1978. Table IB, Note 1.

      (F) Method 231.2, Gold, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (G) Method 245.2, Mercury, Automated Cold Vapor Technique. Issued 1974. Table IB, Note 1.

      (H) Method 252.2, Osmium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (I) Method 253.2, Palladium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (J) Method 255.2, Platinum, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (K) Method 265.2, Rhodium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (L) Method 279.2, Thallium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (M) Method 283.2, Titanium, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (N) Method 289.2, Zinc, Atomic Absorption, Furnace Technique. Issued 1978. Table IB, Note 1.

      (O) Method 310.2, Alkalinity, Colorimetric, Automated, Methyl Orange. Revision 1974. Table IB, Note 1.

      (P) Method 351.1, Nitrogen, Kjeldahl, Total, Colorimetric, Automated Phenate. Revision 1978. Table IB, Note 1.

      (Q) Method 352.1, Nitrogen, Nitrate, Colorimetric, Brucine. Issued 1971. Table IB, Note 1.

      (R) Method 365.3, Phosphorus, All Forms, Colorimetric, Ascorbic Acid, Two Reagent. Issued 1978. Table IB, Note 1.

      (S) Method 365.4, Phosphorus, Total, Colorimetric, Automated, Block Digestor AA II. Issued 1974. Table IB, Note 1.

      (T) Method 410.3, Chemical Oxygen Demand, Titrimetric, High Level for Saline Waters. Revision 1978. Table IB, Note 1.

      (U) Method 420.1, Phenolics, Total Recoverable, Spectrophotometric, Manual 4-AAP With Distillation. Revision 1978. Table IB, Note 1.

      (iv) Prescribed Procedures for Measurement of Radioactivity in Drinking Water. 1980. EPA-600/4-80-032. Table IE.

      (A) Method 900.0, Gross Alpha and Gross Beta Radioactivity. Table IE.

      (B) Method 903.0, Alpha-Emitting iRadio Isotopes. Table IE.

      (C) Method 903.1, Radium-226, Radon Emanation Technique. Table IE.

      (D) Appendix B, Error and Statistical Calculations. Table IE.

      (6) Office of Science and Technology, U.S. Environmental Protection Agency, Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.

      (i) Method 1625C, Semivolatile Organic Compounds by Isotope Dilution GCMS. 1989. Table IF.

      (ii) Reserved

      (7) Office of Water, U.S. Environmental Protection Agency, Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161.

      (i) Method 1631, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry. Revision E, August 2002. EPA-821-R-02-019, Pub. No. PB2002-108220. Table IB, Note 43.

      (ii) Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate. Revision 1.2, August 2001. EPA 821-B-01-009, Pub. No. PB 2001-108275. Table IB, Note 55.

      (iii) In the compendium Analytical Methods for the Determination of Pollutants in Pharmaceutical Manufacturing Industry Wastewaters. July 1998. EPA 821-B-98-016, Pub. No. PB95201679. Table IF, Note 1.

      (A) EPA Method 1666, Volatile Organic Compounds Specific to the Pharmaceutical Industry by Isotope Dilution GC/MS. Table IF, Note 1.

      (B) EPA Method 1667, Formaldehyde, Isobutyraldehyde, and Furfural by Derivatization Followed by High Performance Liquid Chromatography. Table IF.

      (C) Method 1671, Volatile Organic Compounds Specific to the

      Page 29800

      Pharmaceutical Manufacturing Industry by GC/FID. Table IF.

      (iv) Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I. Revision I, August 1993. EPA 821-R-93-010A, Pub. No. PB 94121654. Tables ID, IG.

      (A) Method 608.1, Organochlorine Pesticides. Table ID, Note 10; Table IG, Note 3.

      (B) Method 608.2, Certain Organochlorine Pesticides. Table ID, Note 10; Table IG, Note 3.

      (C) Method 614, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.

      (D) Method 614.1, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.

      (E) Method 615, Chlorinated Herbicides. Table ID, Note 10; Table IG, Note 3.

      (F) Method 617, Organohalide Pesticides and PCBs. Table ID, Note 10; Table IG, Note 3.

      (G) Method 619, Triazine Pesticides. Table ID, Note 10; Table IG, Note 3.

      (H) Method 622, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.

      (I) Method 622.1, Thiophosphate Pesticides. Table ID, Note 10; Table IG, Note 3.

      (J) Method 627, Dinitroaniline Pesticides. Table ID, Note 10; Table IG, Notes 1 and 3.

      (K) Method 629, Cyanazine. Table IG, Note 3.

      (L) Method 630, Dithiocarbamate Pesticides. Table IG, Note 3.

      (M) Method 630.1, Dithiocarbamate Pesticides. Table IG, Note 3.

      (N) Method 631, Benomyl and Carbendazim. Table IG, Note 3.

      (O) Method 632, Carbamate and Urea Pesticides. Table ID, Note 10; Table IG, Note 3.

      (P) Method 632.1, Carbamate and Amide Pesticides. Table IG, Note 3.

      (Q) Method 633, Organonitrogen Pesticides. Table IG, Note 3.

      (R) Method 633.1, Neutral Nitrogen-Containing Pesticides. Table IG, Note 3.

      (S) Method 637, MBTS and TCMTB. Table IG, Note 3.

      (T) Method 644, Picloram. Table IG, Note 3.

      (U) Method 645, Certain Amine Pesticides and Lethane. Table IG, Note 3.

      (V) Method 1656, Organohalide Pesticides. Table ID, Note 10; Table IG, Notes 1 and 3.

      (W) Method 1657, Organophosphorus Pesticides. Table ID, Note 10; Table IG, Note 3.

      (X) Method 1658, Phenoxy-Acid Herbicides. Table IG, Note 3.

      (Y) Method 1659, Dazomet. Table IG, Note 3.

      (Z) Method 1660, Pyrethrins and Pyrethroids. Table IG, Note 3.

      (AA) Method 1661, Bromoxynil. Table IG, Note 3.

      (BB) Ind-01. Methods EV-024 and EV-025, Analytical Procedures for Determining Total Tin and Triorganotin in Wastewater. Table IG, Note 3.

      (v) Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume II. August 1993. EPA 821-R-

      93-010B, Pub. No. PB 94166311. Table IG.

      (A) Method 200.9, Determination of Trace Elements by Stabilized Temperature Graphite Furnace Atomic Absorption Spectrometry. Table IG, Note 3.

      (B) Method 505, Analysis of Organohalide Pesticides and Commercial Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and Gas Chromatography. Table ID, Note 10; Table IG, Note 3.

      (C) Method 507, The Determination of Nitrogen- and Phosphorus-

      Containing Pesticides in Water by Gas Chromatography with a Nitrogen-

      Phosphorus Detector. Table ID, Note 10; Table IG, Note 3.

      (D) Method 508, Determination of Chlorinated Pesticides in Water by Gas Chromatography with an Electron Capture Detector. Table ID, Note 10; Table IG, Note 3.

      (E) Method 515.1, Determination of Chlorinated Acids in Water by Gas Chromatography with an Electron Capture Detector. Table IG, Notes 2 and 3.

      (F) Method 515.2, Determination of Chlorinated Acids in Water Using Liquid-Solid Extraction and Gas Chromatography with an Electron Capture Detector. Table IG, Notes 2 and 3.

      (G) Method 525.1, Determination of Organic Compounds in Drinking Water by Liquids-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry. Table ID, Note 10; Table IG, Note 3.

      (H) Method 531.1, Measurement of N-Methylcarbamoyloximes and N-

      Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-

      Column Derivatization. Table ID, Note 10; Table IG, Note 3.

      (I) Method 547, Determination of Glyphosate in Drinking Water by Direct-Aqueous-Injection HPLC, Post-Column Derivatization, and Fluorescence Detection. Table IG, Note 3.

      (J) Method 548, Determination of Endothall in Drinking Water by Aqueous Derivatization, Liquid-Solid Extraction, and Gas Chromatography with Electron-Capture Detector. Table IG, Note 3.

      (K) Method 548.1, Determination of Endothall in Drinking Water by Ion-Exchange Extraction, Acidic Methanol Methylation and Gas Chromatography/Mass Spectrometry. Table IG, Note 3.

      (L) Method 553, Determination of Benzidines and Nitrogen-Containing Pesticides in Water by Liquid-Liquid Extraction or Liquid-Solid Extraction and Reverse Phase High Performance Liquid Chromatography/

      Particle Beam/Mass Spectrometry Table ID, Note 10; Table IG, Note 3.

      (M) Method 555, Determination of Chlorinated Acids in Water by High Performance Liquid Chromatography With a Photodiode Array Ultraviolet Detector. Table IG, Note 3.

      (vi) In the compendium Methods for the Determination of Organic Compounds in Drinking Water. Revised July 1991, December 1998. EPA-600/

      4-88-039, Pub. No. PB92-207703. Table IF.

      (A) EPA Method 502.2, Volatile Organic Compounds in Water by Purge and Trap Capillary Column Gas Chromatography with Photoionization and Electrolytic Conductivity Detectors in Series. Table IF.

      (B) Reserved

      (vii) In the compendium Methods for the Determination of Organic Compounds in Drinking Water-Supplement II. August 1992. EPA-600/R-92-

      129, Pub. No. PB92-207703. Table IF.

      (A) EPA Method 524.2, Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry. Table IF.

      (B) Reserved

      (viii) Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, Fifth Edition. October 2002. EPA 821-R-02-012, Pub. No. PB2002-108488. Table IA, Note 26.

      (ix) Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition. October 2002. EPA 821-R-02-013, Pub. No. PB2002-108489. Table IA, Note 27.

      (x) Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, Third Edition. October 2002. EPA 821-R-02-014, Pub. No. PB2002-108490. Table IA, Note 28.

      (8) Office of Water, U.S. Environmental Protection Agency, Washington DC (US EPA). Available at

      Page 29801

      http://water.epa.gov/scitech/methods/cwa/index.cfm.

      (i) Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry. Revision 2.0, February 2005. EPA-821-R-05-

      001. Table IB, Note 17.

      (ii) Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). March 2010. EPA-621-R-10-002. Table IH, Note 19.

      (iii) Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). December 2009. EPA-621-R-09-015. Table IH, Note 23.

      (iv) Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-beta-D-Glucoside Agar (mEI). December 2009. EPA-821-R-09-016. Table IA, Note 25; Table IH, Note 24.

      (v) Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified mTEC). December 2009. EPA-821-R-09-007. Table IA, Note 22; Table IH, Note 20.

      (vi) Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration Using a Simultaneous Detection Technique (MI Medium). September 2002. EPA-821-R-02-024. Table IH, Note 21.

      (vii) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. December 2005. EPA-821-R-05-001. Table IH, Note 25.

      (viii) Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. December 2005. EPA-821-R-05-002. Table IH, Note 26.

      (ix) Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality. December 2011. EPA-821-R-09-002. Table IB, Note 69.

      (x) Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. Revision A, February 1999. EPA-821-R-98-002. Table IB, Notes 38 and 42.

      (xi) Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. Revision B, February 2010. EPA-821-R-10-001. Table IB, Notes 38 and 42.

      (xii) Method 1669, Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels. July 1996. Table IB, Note 43.

      (xiii) Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using Lauryl Tryptose Broth (LTB) and EC Medium. April 2010. EPA-821-R-10-003. Table IA, Note 15.

      (xiv) Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. July 2006. EPA 821-R-06-

      013. Table IA, Note 20.

      (xv) Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. July 2006. EPA 821-R-06-014. Table IA, Note 23.

      (9) American National Standards Institute, 1430 Broadway, New York NY 10018.

      (i) ANSI. American National Standard on Photographic Processing Effluents. April 2, 1975. Table IB, Note 9.

      (ii) Reserved

      (10) American Public Health Association, 1015 15th Street NW., Washington, DC 20005. Standard Methods Online is available through the Standard Methods Web site (http://www.standardmethods.org).

      (i) Standard Methods for the Examination of Water and Wastewater. 14th Edition, 1975. Table IB, Notes 17 and 27.

      (ii) Standard Methods for the Examination of Water and Wastewater. 15th Edition, 1980, Table IB, Note 30; Table ID.

      (iii) Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and Wastewater. 1981. Table IC, Note 6; Table ID, Note 6.

      (iv) Standard Methods for the Examination of Water and Wastewater. 18th Edition, 1992. Tables IA, IB, IC, ID, IE, and IH.

      (v) Standard Methods for the Examination of Water and Wastewater. 19th Edition, 1995. Tables IA, IB, IC, ID, IE, and IH.

      (vi) Standard Methods for the Examination of Water and Wastewater. 20th Edition, 1998. Tables IA, IB, IC, ID, IE, and IH.

      (vii) Standard Methods for the Examination of Water and Wastewater. 21st Edition, 2005. Table IB, Notes 17 and 27.

      (viii) 2120, Color. 2001. Table IB.

      (ix) 2130, Turbidity. 2001. Table IB.

      (x) 2310, Acidity. 1997. Table IB.

      (xi) 2320, Alkalinity. 1997. Table IB.

      (xii) 2340, Hardness. 1997. Table IB.

      (xiii) 2510, Conductivity. 1997. Table IB.

      (xiv) 2540, Solids. 1997. Table IB.

      (xv) 2550, Temperature. 2000. Table IB.

      (xvi) 3111, Metals by Flame Atomic Absorption Spectrometry. 1999. Table IB.

      (xvii) 3112, Metals by Cold-Vapor Atomic Absorption Spectrometry. 2009. Table IB.

      (xviii) 3113, Metals by Electrothermal Atomic Absorption Spectrometry. 2004. Table IB.

      (xix) 3114, Arsenic and Selenium by Hydride Generation/Atomic Absorption Spectrometry. 2009. Table IB.

      (xx) 3120, Metals by Plasma Emission. 1999. Table IB.

      (xxi) 3125, Metals by Inductively Coupled Plasma-Mass Spectrometry. 2009. Table IB.

      (xxii) 3500-Al, Aluminum. 2001. Table IB.

      (xxiii) 3500-As, Arsenic. 1997. Table IB.

      (xxiv) 3500-Ca, Calcium. 1997. Table IB.

      (xxv) 3500-Cr, Chromium. 2009. Table IB.

      (xxvi) 3500-Cu, Copper. 1999. Table IB.

      (xxvii) 3500-Fe, Iron. 1997. Table IB.

      (xxviii) 3500-Pb, Lead. 1997. Table IB.

      (xxix) 3500-Mn, Manganese. 1999. Table IB.

      (xxx) 3500-K, Potassium. 1997. Table IB.

      (xxxi) 3500-Na, Sodium. 1997. Table IB.

      (xxxii) 3500-V, Vanadium. 1997. Table IB.

      (xxxiii) 3500-Zn, Zinc. 1997. Table IB.

      (xxxiv) 4110, Determination of Anions by Ion Chromatography. 2000. Table IB.

      (xxxv) 4140, Inorganic Anions by Capillary Ion Electrophoresis. 1997. Table IB.

      (xxxvi) 4500-B, Boron. 2000. Table IB.

      (xxxvii) 4500-Cl-, Chloride. 1997. Table IB.

      (xxxviii) 4500-Cl, Chlorine (Residual). 2000. Table IB.

      (xxxix) 4500-CN-, Cyanide. 1999. Table IB.

      (xl) 4500-F-, Fluoride. 1997. Table IB.

      (xli) 4500-H\+\, pH Value. 2000. Table IB.

      (xlii) 4500-NH3, Nitrogen (Ammonia). 1997. Table IB.

      (xliii) 4500-NO2-, Nitrogen (Nitrite). 2000. Table IB.

      (xliv) 4500-NO3-, Nitrogen (Nitrate). 2000. Table IB.

      (xlv) 4500-Norg, Nitrogen (Organic). 1997. Table IB.

      (xlvi) 4500-O, Oxygen (Dissolved). 2001. Table IB.

      (xlvii) 4500-P, Phosphorus. 1999. Table IB.

      (xlviii) 4500-SiO2, Silica. 1997. Table IB.

      Page 29802

      (xlix) 4500-S2-, Sulfide. 2000. Table IB.

      (l) 4500-SO32-, Sulfite. 2000. Table IB.

      (li) 4500-SO42-, Sulfate. 1997. Table IB.

      (lii) 5210, Biochemical Oxygen Demand (BOD). 2001. Table IB.

      (liii) 5220, Chemical Oxygen Demand (COD). 1997. Table IB.

      (liv) 5310, Total Organic Carbon (TOC). 2000. Table IB.

      (lv) 5520, Oil and Grease. 2001. Table IB.

      (lvi) 5530, Phenols. 2005. Table IB.

      (lvii) 5540, Surfactants. 2000. Table IB.

      (lviii) 6200, Volatile Organic Compounds. 1997. Table IC.

      (lix) 6410, Extractable Base/Neutrals and Acids. 2000. Tables IC, ID.

      (lx) 6420, Phenols. 2000. Table IC.

      (lxi) 6440, Polynuclear Aromatic Hydrocarbons. 2000. Table IC.

      (lxii) 6630, Organochlorine Pesticides. 2000. Table ID.

      (lxiii) 6640, Acidic Herbicide Compounds. 2001. Table ID.

      (lxiv) 7110, Gross Alpha and Gross Beta Radioactivity (Total, Suspended, and Dissolved). 2000. Table IE.

      (lxv) 7500, Radium. 2001. Table IE.

      (lxvi) 9213, Recreational Waters. 2007. Table IH.

      (lxvii) 9221, Multiple-Tube Fermentation Technique for Members of the Coliform Group. 2006. Table IA, Notes 12 and 14; Table IH, Notes 11 and 13.

      (lxviii) 9222, Membrane Filter Technique for Members of the Coliform Group. 1997. Table IA; Table IH, Note 18.

      (lxix) 9223, Enzyme Substrate Coliform Test. 2004. Table IA; Table IH.

      (lxx) 9230, Fecal Enterococcus/Streptococcus Groups. 2007. Table IA; Table IH.

      (11) The Analyst, The Royal Society of Chemistry, RSC Publishing, Royal Society of Chemistry, Thomas Graham House, Science Park, Milton Road, Cambridge CB4 0WF, United Kingdom. (Also available from most public libraries.)

      (i) Spectrophotometric Determination of Ammonia: A Study of a Modified Berthelot Reaction Using Salicylate and Dichloroisocyanurate. Krom, M.D. 105:305-316, April 1980. Table IB, Note 60.

      (ii) Reserved

      (12) Analytical Chemistry, ACS Publications, 1155 Sixteenth St. NW., Washington DC 20036. (Also available from most public libraries.)

      (i) Spectrophotometric and Kinetics Investigation of the Berthelot Reaction for the Determination of Ammonia. Patton, C.J. and S.R. Crouch. 49(3):464-469, March 1977. Table IB, Note 60.

      (ii) Reserved

      (13) AOAC International, 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.

      (i) Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998.

      (A) 920.203, Manganese in Water, Persulfate Method. Table IB, Note 3.

      (B) 925.54, Sulfate in Water, Gravimetric Method. Table IB, Note 3.

      (C) 973.40, Specific Conductance of Water. Table IB, Note 3.

      (D) 973.41, pH of Water. Table IB, Note 3.

      (E) 973.43, Alkalinity of Water, Titrimetric Method. Table IB, Note 3.

      (F) 973.44, Biochemical Oxygen Demand (BOD) of Water, Incubation Method. Table IB, Note 3.

      (G) 973.45, Oxygen (Dissolved) in Water, Titrimetric Methods. Table IB, Note 3.

      (H) 973.46, Chemical Oxygen Demand (COD) of Water, Titrimetric Methods. Table IB, Note 3.

      (I) 973.47, Organic Carbon in Water, Infrared Analyzer Method. Table IB, Note 3.

      (J) 973.48, Nitrogen (Total) in Water, Kjeldahl Method. Table IB, Note 3.

      (K) 973.49, Nitrogen (Ammonia) in Water, Colorimetric Method. Table IB, Note 3.

      (L) 973.50, Nitrogen (Nitrate) in Water, Brucine Colorimetric Method. Table IB, Note 3.

      (M) 973.51, Chloride in Water, Mercuric Nitrate Method. Table IB, Note 3.

      (N) 973.52, Hardness of Water. Table IB, Note 3.

      (O) 973.53, Potassium in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.

      (P) 973.54, Sodium in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.

      (Q) 973.55, Phosphorus in Water, Photometric Method. Table IB, Note 3.

      (R) 973.56, Phosphorus in Water, Automated Method. Table IB, Note 3.

      (S) 974.27, Cadmium, Chromium, Copper, Iron, Lead, Magnesium, Manganese, Silver, Zinc in Water, Atomic Absorption Spectrophotometric Method. Table IB, Note 3.

      (T) 977.22, Mercury in Water, Flameless Atomic Absorption Spectrophotometric Method. Table IB, Note 3.

      (U) 991.15. Total Coliforms and Escherichia coli in Water Defined Substrate Technology (Colilert) Method. Table IA, Note 10; Table IH, Note 10.

      (V) 993.14, Trace Elements in Waters and Wastewaters, Inductively Coupled Plasma-Mass Spectrometric Method. Table IB, Note 3.

      (W) 993.23, Dissolved Hexavalent Chromium in Drinking Water, Ground Water, and Industrial Wastewater Effluents, Ion Chromatographic Method. Table IB, Note 3.

      (X) 993.30, Inorganic Anions in Water, Ion Chromatographic Method. Table IB, Note 3.

      (ii) Reserved

      (14) Applied and Environmental Microbiology, American Society for Microbiology, 1752 N Street NW., Washington DC 20036. (Also available from most public libraries.)

      (i) New Medium for the Simultaneous Detection of Total Coliforms and Escherichia coli in Water. Brenner, K.P., C.C. Rankin, Y.R. Roybal, G.N. Stelma, Jr., P.V. Scarpino, and A.P. Dufour. 59:3534-3544, November 1993. Table IH, Note 21.

      (ii) Reserved

      (15) ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, or online at http://www.astm.org.

      (i) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1994. Tables IA, IB, IC, ID, IE, and IH.

      (ii) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1996. Tables IA, IB, IC, ID, IE, and IH.

      (iii) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 1999. Tables IA, IB, IC, ID, IE, and IH.

      (iv) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02. 2000. Tables IA, IB, IC, ID, IE, and IH.

      (v) ASTM D511-08, Standard Test Methods for Calcium and Magnesium in Water. November 2008. Table IB.

      (vi) ASTM D512-04, Standard Test Methods for Chloride Ion in Water. July 2004. Table IB.

      (vii) ASTM D515-88, Test Methods for Phosphorus in Water, March 1989. Table IB.

      (viii) ASTM D516-07, Standard Test Method for Sulfate Ion in Water, September 2007. Table IB.

      (ix) ASTM D858-07, Standard Test Methods for Manganese in Water. August 2007. Table IB.

      (x) ASTM D859-05, Standard Test Method for Silica in Water. February 2005. Table IB.

      (xi) ASTM D888-09, Standard Test Methods for Dissolved Oxygen in Water. December 2009. Table IB.

      (xii) ASTM D1067-06, Standard Test Methods for Acidity or Alkalinity of Water. January 2007. Table IB.

      Page 29803

      (xiii) ASTM D1068-05\E1\, Standard Test Methods for Iron in Water. July 2005. Table IB.

      (xiv) ASTM D1125-95 (Reapproved 1999), Standard Test Methods for Electrical Conductivity and Resistivity of Water. December 1995. Table IB.

      (xv) ASTM D1126-02 (Reapproved 2007)\E1\, Standard Test Method for Hardness in Water. August 2007. Table IB.

      (xvi) ASTM D1179-04, Standard Test Methods for Fluoride Ion in Water. July 2004. Table IB.

      (xvii) ASTM D1246-05, Standard Test Method for Bromide Ion in Water. February 2005. Table IB.

      (xviii) ASTM D1252-06, Standard Test Methods for Chemical Oxygen Demand (Dichromate Oxygen Demand) of Water. February 2006. Table IB.

      (xix) ASTM D1253-08, Standard Test Method for Residual Chlorine in Water. October 2008. Table IB.

      (xx) ASTM D1293-99, Standard Test Methods for pH of Water. March 2000. Table IB.

      (xxi) ASTM D1426-08, Standard Test Methods for Ammonia Nitrogen in Water. September 2008. Table IB.

      (xxii) ASTM D1687-02 (Reapproved 2007)\E1\, Standard Test Methods for Chromium in Water. August 2007. Table IB.

      (xxiii) ASTM D1688-07, Standard Test Methods for Copper in Water. August 2007. Table IB.

      (xxiv) ASTM D1691-02 (Reapproved 2007)\E1\, Standard Test Methods for Zinc in Water. August 2007. Table IB.

      (xxv) ASTM D1783-01 (Reapproved 2007), Standard Test Methods for Phenolic Compounds in Water. January 2008). Table IB.

      (xxvi) ASTM D1886-08, Standard Test Methods for Nickel in Water. October 2008. Table IB.

      (xxvii) ASTM D1889-00, Standard Test Method for Turbidity of Water. October 2000. Table IB.

      (xxviii) ASTM D1890-96, Standard Test Method for Beta Particle Radioactivity of Water. April 1996. Table IE.

      (xxix) ASTM D1943-96, Standard Test Method for Alpha Particle Radioactivity of Water. April 1996. Table IE.

      (xxx) ASTM D1976-07, Standard Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy. August 2007. Table IB.

      (xxxi) ASTM D2036-09, Standard Test Methods for Cyanides in Water. October 2009. Table IB.

      (xxxii) ASTM D2330-02, Standard Test Method for Methylene Blue Active Substances. August 2002. Table IB.

      (xxxiii) ASTM D2460-97, Standard Test Method for Alpha-Particle-

      Emitting Isotopes of Radium in Water. October 1997. Table IE.

      (xxxiv) ASTM D2972-08, Standard Tests Method for Arsenic in Water. October 2008. Table IB.

      (xxxv) ASTM D3223-02 (Reapproved 2007)\E1\, Standard Test Method for Total Mercury in Water. August 2007. Table IB.

      (xxxvi) ASTM D3371-95, Standard Test Method for Nitriles in Aqueous Solution by Gas-Liquid Chromatography, February 1996. Table IF.

      (xxxvii) ASTM D3373-03 (Reapproved 2007)\E1\, Standard Test Method for Vanadium in Water. September 2007. Table IB.

      (xxxviii) ASTM D3454-97, Standard Test Method for Radium-226 in Water. February 1998. Table IE.

      (xxxix) ASTM D3557-02 (Reapproved 2007)\E1\, Standard Test Method for Cadmium in Water. September 2007. Table IB.

      (xl) ASTM D3558-08, Standard Test Method for Cobalt in Water. November 2008. Table IB.

      (xli) ASTM D3559-08, Standard Test Methods for Lead in Water. October 2008. Table IB.

      (xlii) ASTM D3590-02 (Reapproved 2006), Standard Test Methods for Total Kjeldahl Nitrogen in Water. February 2007. Table IB.

      (xliii) ASTM D3645-08, Standard Test Methods for Beryllium in Water. October 2008. Table IB.

      (xliv) ASTM D3695-95, Standard Test Method for Volatile Alcohols in Water by Direct Aqueous-Injection Gas Chromatography. April 1995. Table IF.

      (xlv) ASTM D3859-08, Standard Test Methods for Selenium in Water. October 2008. Table IB.

      (xlvi) ASTM D3867-04, Standard Test Method for Nitrite-Nitrate in Water. July 2004. Table IB.

      (xlvii) ASTM D4190-08, Standard Test Method for Elements in Water by Direct-Current Plasma Atomic Emission Spectroscopy. October 2008. Table IB.

      (xlviii) ASTM D4282-02, Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion. August 2002. Table IB.

      (xlix) ASTM D4327-03, Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography. January 2003. Table IB.

      (l) ASTM D4382-02 (Reapproved 2007)\E1\, Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace. September 2007. Table IB.

      (li) ASTM D4657-92 (Reapproved 1998), Standard Test Method for Polynuclear Aromatic Hydrocarbons in Water. January 1993. Table IC.

      (lii) ASTM D4658-08, Standard Test Method for Sulfide Ion in Water. August 2008. Table IB.

      (liii) ASTM D4763-88 (Reapproved 2001), Standard Practice for Identification of Chemicals in Water by Fluorescence Spectroscopy. September 1988. Table IF.

      (liv) ASTM D4839-03, Standard Test Method for Total Carbon and Organic Carbon in Water by Ultraviolet, or Persulfate Oxidation, or Both, and Infrared Detection. January 2003. Table IB.

      (lv) ASTM D5257-03, Standard Test Method for Dissolved Hexavalent Chromium in Water by Ion Chromatography. January 2003. Table IB.

      (lvi) ASTM D5259-92, Standard Test Method for Isolation and Enumeration of Enterococci from Water by the Membrane Filter Procedure. October 1992. Table IH, Note 9.

      (lvii) ASTM D5392-93, Standard Test Method for Isolation and Enumeration of Escherichia coli in Water by the Two-Step Membrane Filter Procedure. September 1993. Table IH, Note 9.

      (lviii) ASTM D5673-05, Standard Test Method for Elements in Water by Inductively Coupled Plasma--Mass Spectrometry. July 2005. Table IB.

      (lix) ASTM D5907-03, Standard Test Method for Filterable and Nonfilterable Matter in Water. July 2003. Table IB.

      (lx) ASTM D6503-99, Standard Test Method for Enterococci in Water Using Enterolert. April 2000. Table IA Note 9, Table IH, Note 9.

      (lxi) ASTM. D6508-00 (Reapproved 2005)\E2\, Standard Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. April 2005. Table IB.

      (lxii) ASTM. D6888-09, Standard Test Method for Available Cyanide with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. October 2009. Table IB, Note 59.

      (lxiii) ASTM. D6919-09, Standard Test Method for Determination of Dissolved Alkali and Alkaline Earth Cations and Ammonium in Water and Wastewater by Ion Chromatography. May 2009. Table IB.

      (lxiv) ASTM. D7065-06, Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters

      Page 29804

      by Gas Chromatography Mass Spectrometry. January 2007. Table IC.

      (lxv) ASTM. D7237-10, Standard Test Method for Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and Amperometric Detection. June 2010. Table IB.

      (lxvi) 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. April 2008). Table IB.

      (lxvii) ASTM. D7365-09a, Standard Practice for Sampling, Preservation, and Mitigating Interferences in Water Samples for Analysis of Cyanide. October 2009. Table II, Notes 5 and 6.

      (lxviii) ASTM. D7511-09\E2\, Standard Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and Amperometric Detection. March 2009. Table IB.

      (lxix) ASTM. D7573-09, Standard Test Method for Total Carbon and Organic Carbon in Water by High Temperature Catalytic Combustion and Infrared Detection. November 2009. Table IB.

      (16) Bran & Luebbe Analyzing Technologies, Inc., Elmsford NY 10523.

      (i) Industrial Method Number 378-75WA, Hydrogen Ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Auto Analyzer II. October 1976. Table IB, Note 21.

      (ii) Reserved

      (17) CEM Corporation, P.O. Box 200, Matthews NC 28106-0200.

      (i) Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. Table IB, Note 36.

      (ii) Reserved

      (18) Craig R. Chinchilla, 900 Jorie Blvd., Suite 35, Oak Brook IL 60523. Telephone: 630-645-0600.

      (i) Nitrate by Discrete Analysis Easy (1-Reagent) Nitrate Method, (Colorimetric, Automated, 1 Reagent). Revision 1, November 12, 2011. Table IB, Note 62.

      (ii) Reserved

      (19) Hach Company, P.O. Box 389, Loveland CO 80537.

      (i) Method 8000, Chemical Oxygen Demand. Hach Handbook of Water Analysis. 1979. Table IB, Note 14.

      (ii) Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Table IB, Note 22.

      (iii) Method 8009, Zincon Method for Zinc. Hach Handbook for Water Analysis. 1979. Table IB, Note 33.

      (iv) Method 8034, Periodate Oxidation Method for Manganese. Hach Handbook for Water Analysis. 1979. Table IB, Note 23.

      (v) Method 8506, Bicinchoninate Method for Copper. Hach Handbook of Water Analysis. 1979. Table IB, Note 19.

      (vi) Method 8507, Nitrogen, Nitrite--Low Range, Diazotization Method for Water and Wastewater. 1979. Table IB, Note 25.

      (vii) Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5. Revision 1.2, October 2011. Table IB, Note 63.

      (viii) m-ColiBlue24supreg Method, for total Coliforms and E. coli. Revision 2, 1999. Table IA, Note 18; Table IH, Note 17.

      (20) IDEXX Laboratories Inc., One Idexx Drive, Westbrook ME 04092.

      (i) Colilertsupreg Method. 2002. Table IA, Notes 17 and 18; Table IH, Notes 14, 15 and 16.

      (ii) Colilert-18supreg Method. 2002. Table IA, Notes 17 and 18; Table IH, Notes 14, 15 and 16.

      (iii) Enterolertsupreg Method. 2002. Table IA, Note 24; Table IH, Note 12.

      (iv) Quanti-Traysupreg Method. 2002. Table IA, Note 18; Table IH, Notes 14 and 16.

      (v) Quanti-Traysupreg/2000 Method. 2002. Table IA, Note 18; Table IH, Notes 14 and 16.

      (21) In-Situ Incorporated, 221 E. Lincoln Ave., Ft. Collins CO 80524. Telephone: 970-498-1500.

      (i) In-Situ Inc. Method 1002-8-2009, Dissolved Oxygen Measurement by Optical Probe. 2009. Table IB, Note 64.

      (ii) In-Situ Inc. Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. Table IB, Note 10.

      (iii) In-Situ Inc. Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. Table IB, Note 35.

      (22) Journal of Chromatography, Elsevier/North-Holland, Inc., Journal Information Centre, 52 Vanderbilt Avenue, New York NY 10164. (Also available from most public libraries.

      (i) Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography. Addison, R.F. and R.G. Ackman. 47(3): 421-426, 1970. Table IB, Note 28.

      (ii) Reserved

      (23) Lachat Instruments, 6645 W. Mill Road, Milwaukee WI 53218, Telephone: 414-358-4200.

      (i) QuikChem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Table IB, Note 56.

      (ii) Reserved

      (24) Leck Mitchell, Ph.D., P.E., 656 Independence Valley Dr., Grand Junction CO 81507. Telephone: 970-244-8661.

      (i) Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 66.

      (ii) Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 65.

      (25) National Council of the Paper Industry for Air and Stream Improvements, Inc. (NCASI), 260 Madison Avenue, New York NY 10016.

      (i) NCASI Technical Bulletin No. 253, An Investigation of Improved Procedures for Measurement of Mill Effluent and Receiving Water Color. December 1971. Table IB, Note 18.

      (ii) Reserved

      (26) Oceanography International Corporation, 512 West Loop, P.O. Box 2980, College Station TX 77840.

      (i) OIC Chemical Oxygen Demand Method. 1978. Table IB, Note 13.

      (ii) Reserved

      (27) OI Analytical, Box 9010, College Station TX 77820-9010.

      (i) Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). Copyright 2010. Table IB, Note 59.

      (ii) Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. Table IB, Note 39.

      (iii) Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. Table IB, Note 40.

      (iv) Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. Table IB, Note 41.

      (28) ORION Research Corporation, 840 Memorial Drive, Cambridge, Massachusetts 02138.

      (i) ORION Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Table IB, Note 16.

      (ii) Reserved

      (29) Technicon Industrial Systems, Tarrytown NY 10591.

      (i) Industrial Method Number 379-75WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Table IB, Note 7.

      (ii) Reserved

      (30) Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin MA 02038.

      (i) Method AES0029. Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986, Revised 1991. Table IB, Note 34.

      Page 29805

      (ii) Reserved

      (31) Thermo Scientific, 166 Cummings Center, Beverly MA 01915. Telephone: 1-800-225-1480. www.thermoscientific.com.

      (i) Thermo Scientific Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Table IB, Note 67.

      (ii) Reserved

      (32) 3M Corporation, 3M Center Building 220-9E-10, St. Paul MN 55144-1000.

      (i) Organochlorine Pesticides and PCBs in Wastewater Using Empore\TM\ Disk'' Test Method 3M 0222. Revised October 28, 1994. Table IC, Note 8; Table ID, Note 8.

      (ii) Reserved

      (33) U.S. Geological Survey (USGS), U.S. Department of the Interior, Reston, Virginia. Available from USGS Books and Open-File Reports (OFR) Section, Federal Center, Box 25425, Denver, CO 80225.

      (i) OFR 76-177, Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters. 1976. Table IE, Note 2.

      (ii) OFR 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Organonitrogen Herbicides in Water by Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry With Selected-Ion Monitoring. 1992. Table ID, Note 14.

      (iii) OFR 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by a Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. Table IB, Note 48.

      (iv) OFR 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. Table IB, Note 51; Table IC, Note 9.

      (v) OFR 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. Table IB, Note 46.

      (vi) OFR 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Triazine and Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors. 1994. Table ID, Note 9.

      (vii) OFR 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Pesticides in Water by C-18 Solid-Phase Extraction and Capillary-Column Gas Chromatography/

      Mass Spectrometry With Selected-Ion Monitoring. 1995. Table ID, Note 11.

      (viii) OFR 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. Table IB, Note 47.

      (ix) OFR 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-

      Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. Table IB, Note 50.

      (x) OFR 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace--Atomic Absorption Spectrometry. 1999. Table IB, Note 49.

      (xi) OFR 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. Table IB, Note 45.

      (xii) Water-Resources Investigation Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry. 2001. Table ID, Note 13.

      (xiii) Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water With Cold Vapor-Atomic Fluorescence Spectrometry. 2001. Table IB, Note 71.

      (xiv) Water-Resources Investigation Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Pesticides in Water by Graphitized Carbon-

      Based Solid-Phase Extraction and High-Performance Liquid Chormatography/Mass Spectrometry. 2001. Table ID, Note 12.

      (xv) Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, editors, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. Table IB, Note 8.

      (xvi) Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1989. Table IB, Note 2.

      (xvii) Methods for the Determination of Organic Substances in Water and Fluvial Sediments. Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3. 1987. Table IB, Note 24; Table ID, Note 4.

      (xviii) Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/

      Reaction Cell Inductively Coupled Plasma-Mass Spectrometry. Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis. 2006. Table IB, Note 70.

      (xix) U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. Table IA, Note 4; Table IH, Note 4.

      (xx) Water Temperature--Influential Factors, Field Measurement and Data Presentation, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1. 1975. Table IB, Note 32.

      (34) Waters Corporation, 34 Maple Street, Milford MA 01757, Telephone: 508-482-2131, Fax: 508-482-3625.

      (i) Method D6508, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. Revision 2, December 2000. Table IB, Note 54.

      (ii) Reserved

      * * * * *

      (e) Sample preservation procedures, container materials, and maximum allowable holding times for parameters are cited in Tables IA, IB, IC, ID, IE, IF, IG, and IH are prescribed in Table II. Information in the table takes precedence over information in specific methods or elsewhere. Any person may apply for a change from the prescribed preservation techniques, container materials, and maximum holding times applicable to samples taken from a specific discharge. Applications for such limited use changes may be made by letters to the Regional Alternative Test Procedure (ATP) Program Coordinator or the permitting authority in the Region in which the discharge will occur. Sufficient data should be

      Page 29806

      provided to assure such changes in sample preservation, containers or holding times do not adversely affect the integrity of the sample. The Regional ATP Coordinator or permitting authority will review the application and then notify the applicant and the appropriate State agency of approval or rejection of the use of the alternate test procedure. A decision to approve or deny any request on deviations from the prescribed Table II requirements will be made within 90 days of receipt of the application by the Regional Administrator. An analyst may not modify any sample preservation and/or holding time requirements of an approved method unless the requirements of this section are met.

      Table II--Required Containers, Preservation Techniques, and Holding Times

      ----------------------------------------------------------------------------------------------------------------

      Maximum holding time

      Parameter number/name Container \1\ Preservation \2,3\ \4\

      ----------------------------------------------------------------------------------------------------------------

      Table IA--Bacterial Tests:

      1-5. Coliform, total, fecal, and PA, G.................. Cool, 10 5,6,

      reducing agent if

      oxidizer present.

      25. Fluoride..................... P...................... None required.......... 28 days.

      27. Hardness..................... P, FP, G............... HNO3 or H2SO4 to pH 9.

      67. Sulfite...................... P, FP, G............... None required.......... Analyze within 15

      minutes.

      68. Surfactants.................. P, FP, G............... Cool, 0.2 to

      prevent rearrangement to benzidine.

      \13\ Extracts may be stored up to 30 days at i = Calculated concentration at level i

      xi = Actual concentration of the calibration level i

      n = Number of calibration points

      p = Number of terms in the fitting equation (average = 1, linear = 2, quadratic = 3)

      (C) Using the RSE as a metric has the added advantage of allowing the same numerical standard to be applied to the calibration model, regardless of the form of the model. Thus, if a method states that the RSD should be 20 percent. Analyst judgment must be applied to the evaluation of ion ratios because the ratios can be affected by co-eluting compounds present in the sample matrix. The signal-to-noise ratio of the least sensitive ion should be at least 3:1. Retention time in the sample should match within 0.05 minute of an authentic standard analyzed under identical conditions. Matrix interferences can cause minor shifts in retention time and may be evident as shifts in the retention times of the internal standards. The total scan time should be such that a minimum of eight scans are obtained per chromatographic peak.

      (xvi) Changes are allowed in purge-and-trap sample volumes or operating conditions. Some examples are:

      (A) Changes in purge time and purge-gas flow rate. A change in purge time and purge-gas flow rate is allowed provided that sufficient total purge volume is used to achieve the required minimum detectible concentration and calibration range for all compounds. In general, a purge rate in the range 20-200 mL/min and a total purge volume in the range 240-880 mL are recommended.

      (B) Use of nitrogen or helium as a purge gas, provided that the required sensitivities for all compounds are met.

      (C) Sample temperature during the purge state. Gentle heating of the sample during purging (e.g., 40 degC) increases purging efficiency of hydrophilic compounds and may improve sample-to-sample repeatability because all samples are purged under precisely the same conditions.

      (D) Trap sorbent. Any trap design is acceptable, provided that the data acquired meet all QC criteria.

      (E) Changes to the desorb time. Shortening the desorb time (e.g., from 4 minutes to 1 minute) may not affect compound recoveries, and can shorten overall cycle time and significantly reduce the amount of water introduced to the analytical system, thus improving the precision of analysis, especially for water-soluble analytes. A desorb time of four minutes is recommended, however a shorter desorb time may be used, provided that all QC specifications in the method are met.

      (F) Use of water management techniques is allowed. Water is always collected on the trap along with the analytes and is a significant interference for analytical systems (GC and GC/MS). Modern water management techniques (e.g., dry purge or condensation points) can remove moisture from the sample stream and improve analytical performance.

      (xvii) The following modifications are allowable when performing EPA Method 625: The base/neutral and acid fractions may be added together and analyzed as one extract, provided that the analytes can be reliably identified and quantified in the combined extracts; the pH extraction sequence may be reversed to better separate acid and neutral components; neutral components may be extracted with either acid or base components; a smaller sample volume may be used to minimize matrix interferences provided matrix interferences are demonstrated and documented; alternative surrogate and internal standard concentrations other than those specified in the method are acceptable, provided that method performance is not degraded; an alternative concentration range may be used for the calibration other than the range specified in the method; the solvent for the calibration standards may be changed to match the solvent of the final sample extract.

      (xviii) If the characteristics of a wastewater matrix prevent efficient recovery of organic pollutants and prevent the method from meeting QC requirements, the analyst may attempt to resolve the issue by adding salts to the sample, provided that such salts do not react with or introduce the target pollutant into the sample (as evidenced by the analysis of method blanks, laboratory control samples, and spiked samples that also contain such salts), and that all requirements of paragraph (b)(2) of this section are met. Samples having residual chlorine or other halogen must be dechlorinated prior to the addition of such salts.

      (xix) If the characteristics of a wastewater matrix result in poor sample dispersion or reagent deposition on equipment and prevent the analyst from meeting QC requirements, the analyst may attempt to resolve the issue by adding a inert surfactant that does not affect the chemistry of the method, such as Brij-35 or sodium dodecyl sulfate (SDS), provided that such surfactant does not react with or introduce the target pollutant into the sample (as evidenced by the analysis of method blanks, laboratory control samples, and spiked samples that also contain such surfactant) and that all requirements of paragraph (b)(1) and (b)(2) of this section are met. Samples having residual chlorine or other halogen must be dechlorinated prior to the addition of such surfactant.

      (xx) The use of gas diffusion (using pH change to convert the analyte to gaseous form and/or heat to separate an analyte contained in steam from the sample matrix) across a hydrophobic semi-permeable membrane to separate the analyte of interest from the sample matrix may be used in place of manual or automated distillation in methods for analysis such as ammonia, total cyanide, total Kjeldahl nitrogen, and total phenols. These procedures do not replace the digestion procedures specified in the approved methods and must be used in conjunction with those procedures.

      (xxi) Changes in equipment operating parameters such as the monitoring wavelength of a colorimeter or the reaction time and temperature as needed to achieve the chemical reactions defined in the unmodified CWA method. For example, molybdenum blue phosphate methods have two absorbance maxima, one at about 660 nm and another at about 880 nm. The former is about 2.5 times less sensitive than the latter. Wavelength choice provides a cost-effective, dilution-free means to increase sensitivity of molybdenum blue phosphate methods.

      (xxii) Interchange of oxidants, such as the use of titanium oxide in UV-assisted automated digestion of TOC and total

      Page 29813

      phosphorus, as long as complete oxidation can be demonstrated.

      (xxii) Use of an axially viewed torch with Method 200.7.

      0

      7. Add new Sec. 136.7 to read as follows:

      Sec. 136.7 Quality assurance and quality control.

      The permittee/laboratory shall use suitable QA/QC procedures when conducting compliance analyses with any Part 136 chemical method or an alternative method specified by the permitting authority. These QA/QC procedures are generally included in the analytical method or may be part of the methods compendium for approved Part 136 methods from a consensus organization. For example, Standard Methods contains QA/QC procedures in the Part 1000 section of the Standard Methods Compendium. The permittee/laboratory shall follow these QA/QC procedures, as described in the method or methods compendium. If the method lacks QA/

      QC procedures, the permittee/laboratory has the following options to comply with the QA/QC requirements:

      (a) Refer to and follow the QA/QC published in the ``equivalent'' EPA method for that parameter that has such QA/QC procedures;

      (b) Refer to the appropriate QA/QC section(s) of an approved Part 136 method from a consensus organization compendium;

      (c)(1) Incorporate the following twelve quality control elements, where applicable, into the laboratory's documented standard operating procedure (SOP) for performing compliance analyses when using an approved Part 136 method when the method lacks such QA/QC procedures. One or more of the twelve QC elements may not apply to a given method and may be omitted if a written rationale is provided indicating why the element(s) is/are inappropriate for a specific method.

      (i) Demonstration of Capability (DOC);

      (ii) Method Detection Limit (MDL);

      (iii) Laboratory reagent blank (LRB), also referred to as method blank (MB);

      (iv) Laboratory fortified blank (LFB), also referred to as a spiked blank, or laboratory control sample (LCS);

      (v) Matrix spike (MS) and matrix spike duplicate (MSD), or laboratory fortified matrix (LFM) and LFM duplicate, may be used for suspected matrix interference problems to assess precision;

      (vi) Internal standards (for GC/MS analyses), surrogate standards (for organic analysis) or tracers (for radiochemistry);

      (vii) Calibration (initial and continuing), also referred to as initial calibration verification (ICV) and continuing calibration verification (CCV);

      (viii) Control charts (or other trend analyses of quality control results);

      (ix) Corrective action (root cause analysis);

      (x) QC acceptance criteria;

      (xi) Definitions of preparation and analytical batches that may drive QC frequencies; and

      (xii) Minimum frequency for conducting all QC elements.

      (2) These twelve quality control elements must be clearly documented in the written standard operating procedure for each analytical method not containing QA/QC procedures, where applicable.

      0

      8. Revise Appendix C to Part 136 to read as follows.

      APPENDIX C TO PART 136--DETERMINATION OF METALS AND TRACE ELEMENTS IN WATER AND WASTES BY INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRY METHOD 200.7

      1.0 Scope and Application

      1.1 Inductively coupled plasma-atomic emission spectrometry (ICP-AES) is used to determine metals and some nonmetals in solution. This method is a consolidation of existing methods for water, wastewater, and solid wastes.1-4 (For analysis of petroleum products see References 5 and 6, Section 16.0). This method is applicable to the following analytes:

      ------------------------------------------------------------------------

      Chemical abstract

      Analyte services registry

      number (CASRN)

      ------------------------------------------------------------------------

      Aluminum (Al)..................................... 7429-90-5

      Antimony (Sb)..................................... 7440-36-0

      Arsenic (As)...................................... 7440-38-2

      Barium (Ba)....................................... 7440-39-3

      Beryllium (Be).................................... 7440-41-7

      Boron (B)......................................... 7440-42-8

      Cadmium (Cd)...................................... 7440-43-9

      Calcium (Ca)...................................... 7440-70-2

      Cerium \a\ (Cr)................................... 7440-45-1

      Chromium (Cr)..................................... 7440-47-3

      Cobalt (Co)....................................... 7440-48-4

      Copper (Cu)....................................... 7440-50-8

      Iron (Fe)......................................... 7439-89-6

      Lead (Pb)......................................... 7439-92-1

      Lithium (Li)...................................... 7439-93-2

      Magnesium (Mg).................................... 7439-95-4

      Manganese (Mn).................................... 7439-96-5

      Mercury (Hg)...................................... 7439-97-6

      Molybdenum (Mo)................................... 7439-98-7

      Nickel (Ni)....................................... 7440-02-0

      Phosphorus (P).................................... 7723-14-0

      Potassium (K)..................................... 7440-09-7

      Selenium (Se)..................................... 7782-49-2

      Silica \b\ (Si02)................................. 7631-86-9

      Silver (Ag)....................................... 7440-22-4

      Sodium (Na)....................................... 7440-23-5

      Strontium (Sr).................................... 7440-24-6

      Thallium (Tl)..................................... 7440-28-0

      Tin (Sn).......................................... 7440-31-5

      Titanium (Ti)..................................... 7440-32-6

      Vanadium (V)...................................... 7440-62-2

      Zinc (Zn)......................................... 7440-66-6

      ------------------------------------------------------------------------

      \a\ Cerium has been included as method analyte for correction of

      potential interelement spectral interference.

      \b\ This method is not suitable for the determination of silica in

      solids.

      1.2 For reference where this method is approved for use in compliance monitoring programs e.g., Clean Water Act (NPDES) or Safe Drinking Water Act (SDWA) consult both the appropriate sections of the Code of Federal Regulation (40 CFR Part 136 Table 1B for NPDES, and Part 141 Sec. 141.23 for drinking water), and the latest Federal Register announcements.

      1.3 ICP-AES can be used to determine dissolved analytes in aqueous samples after suitable filtration and acid preservation. To reduce potential interferences, dissolved solids should be 50 mg/kg should be treated in a similar manner. Also, the extraction of tin from solid samples should be prepared again using aliquots 3 + HCl) matrix as the total recoverable calibration standards and blank solutions.

      1.10 Detection limits and linear ranges for the elements will vary with the wavelength selected, the spectrometer, and the matrices. Table 1 provides estimated instrument detection limits for the listed wavelengths.\7\ However, actual method detection limits and linear working ranges will be dependent on the sample matrix, instrumentation, and selected operating conditions.

      1.11 Users of the method data should state the data-quality objectives prior to analysis. Users of the method must document and have on file the required initial demonstration performance data described in Section 9.2 prior to using the method for analysis.

      2.0 Summary of Method

      2.1 An aliquot of a well mixed, homogeneous aqueous or solid sample is accurately weighed or measured for sample processing. For total recoverable analysis of a solid or an aqueous sample containing undissolved material, analytes are first solubilized by gentle refluxing with nitric and hydrochloric acids. After cooling, the sample is made up to volume, is mixed and centrifuged or allowed to settle overnight prior to analysis. For the determination of dissolved analytes in a filtered aqueous sample aliquot, or for the ``direct analysis'' total recoverable determination of analytes in drinking water where sample turbidity is 9-12 A reference file of material data handling sheets should also be made available to all personnel involved in the chemical analysis. Specifically, concentrated nitric and hydrochloric acids present various hazards and are moderately toxic and extremely irritating to skin and mucus membranes. Use these reagents in a fume hood whenever possible and if eye or skin contact occurs, flush with large volumes of water. Always wear safety glasses or a shield for eye protection, protective clothing and observe proper mixing when working with these reagents.

      5.2 The acidification of samples containing reactive materials may result in the release of toxic gases, such as cyanides or sulfides. Acidification of samples should be done in a fume hood.

      5.3 All personnel handling environmental samples known to contain or to have been in contact with human waste should be immunized against known disease causative agents.

      5.4 The inductively coupled plasma should only be viewed with proper eye protection from the ultraviolet emissions.

      5.5 It is the responsibility of the user of this method to comply with relevant disposal and waste regulations. For guidance see Sections 14.0 and 15.0.

      6.0 Equipment and Supplies

      6.1 Inductively coupled plasma emission spectrometer:

      6.1.1 Computer-controlled emission spectrometer with background-

      correction capability.

      The spectrometer must be capable of meeting and complying with the requirements described and referenced in Section 2.2.

      6.1.2 Radio-frequency generator compliant with FCC regulations.

      6.1.3 Argon gas supply--High purity grade (99.99%). When analyses are conducted frequently, liquid argon is more economical and requires less frequent replacement of tanks than compressed argon in conventional cylinders.

      6.1.4 A variable speed peristaltic pump is required to deliver both standard and sample solutions to the nebulizer.

      6.1.5 (Optional) Mass flow controllers to regulate the argon flow rates, especially the aerosol transport gas, are highly recommended. Their use will provide more exacting control of reproducible plasma conditions.

      6.2 Analytical balance, with capability to measure to 0.1 mg, for use in weighing solids, for preparing standards, and for determining dissolved solids in digests or extracts.

      6.3 A temperature adjustable hot plate capable of maintaining a temperature of 95 degC.

      6.4 (Optional) A temperature adjustable block digester capable of maintaining a temperature of 95 degC and equipped with 250 mL constricted digestion tubes.

      6.5 (Optional) A steel cabinet centrifuge with guard bowl, electric timer and brake.

      6.6 A gravity convection drying oven with thermostatic control capable of maintaining 180 degC 5 degC.

      6.7 (Optional) An air displacement pipetter capable of delivering volumes ranging from 0.1-2500 muL with an assortment of high quality disposable pipet tips.

      6.8 Mortar and pestle, ceramic or nonmetallic material.

      6.9 Polypropylene sieve, 5-mesh (4 mm opening).

      6.10 Labware--For determination of trace levels of elements, contamination and loss are of prime consideration. Potential contamination sources include improperly cleaned laboratory apparatus and general contamination within the laboratory environment from dust, etc. A clean laboratory work area designated for trace element sample handling must be used. Sample containers can introduce positive and negative errors in the determination of trace elements by contributing contaminants through surface desorption or leaching, or depleting element concentrations through adsorption processes. All reusable labware (glass, quartz, polyethylene, PTFE, FEP, etc.) should be sufficiently clean for the task objectives. Several procedures found to provide clean labware include washing with a detergent solution, rinsing with tap water, soaking for four hours or more in 20% (v/v) nitric acid or a mixture of HNO3 and HCl (1+2+9), rinsing with reagent water and storing clean.2 3 Chromic acid cleaning solutions must be avoided because chromium is an analyte.

      6.10.1 Glassware--Volumetric flasks, graduated cylinders, funnels and centrifuge tubes (glass and/or metal-free plastic).

      6.10.2 Assorted calibrated pipettes.

      6.10.3 Conical Phillips beakers (Corning 1080-250 or equivalent), 250 mL with 50 mm watch glasses.

      6.10.4 Griffin beakers, 250 mL with 75 mm watch glasses and (optional) 75 mm ribbed watch glasses.

      6.10.5 (Optional) PTFE and/or quartz Griffin beakers, 250 mL with PTFE covers.

      6.10.6 Evaporating dishes or high-form crucibles, porcelain, 100 mL capacity.

      6.10.7 Narrow-mouth storage bottles, FEP (fluorinated ethylene propylene) with screw closure, 125 mL to 1 L capacities.

      6.10.8 One-piece stem FEP wash bottle with screw closure, 125 mL capacity.

      7.0 Reagents and Standards

      7.1 Reagents may contain elemental impurities which might affect analytical data. Only high-purity reagents that conform to the American Chemical Society specifications \13\ should be used whenever possible. If the purity of a reagent is in question, analyze for contamination. All acids used for this method must be of ultra high-purity grade or equivalent. Suitable acids are available from a number of manufacturers. Redistilled acids prepared by sub-

      boiling distillation are acceptable.

      7.2 Hydrochloric acid, concentrated (sp.gr. 1.19)--HCl.

      7.2.1 Hydrochloric acid (1+1)--Add 500 mL concentrated HCl to 400 mL reagent water and dilute to 1 L.

      7.2.2 Hydrochloric acid (1+4)--Add 200 mL concentrated HCl to 400 mL reagent water and dilute to 1 L.

      7.2.3 Hydrochloric acid (1+20)--Add 10 mL concentrated HCl to 200 mL reagent water.

      7.3 Nitric acid, concentrated (sp.gr. 1.41)--HNO3.

      7.3.1 Nitric acid (1+1)--Add 500 mL concentrated HNO3 to 400 mL reagent water and dilute to 1 L.

      7.3.2 Nitric acid (1+2)--Add 100 mL concentrated HNO3 to 200 mL reagent water.

      7.3.3 Nitric acid (1+5)--Add 50 mL concentrated HNO3 to 250 mL reagent water.

      7.3.4 Nitric acid (1+9)--Add 10 mL concentrated HNO3 to 90 mL reagent water.

      7.4 Reagent water. All references to water in this method refer to ASTM Type I grade water.\14\

      7.5 Ammonium hydroxide, concentrated (sp.gr. 0.902).

      7.6 Tartaric acid, ACS reagent grade.

      7.7 Hydrogen peroxide, 50%, stabilized certified reagent grade.

      7.8 Standard Stock Solutions--Stock standards may be purchased or prepared from ultra-high purity grade chemicals (99.99-99.999% pure). All compounds must be dried for one hour at 105 degC, unless otherwise specified. It is recommended that stock solutions be stored in FEP bottles. Replace stock standards when succeeding dilutions for preparation of calibration standards cannot be verified.

      CAUTION: Many of these chemicals are extremely toxic if inhaled or swallowed (Section 5.1). Wash hands thoroughly after handling.

      Typical stock solution preparation procedures follow for 1 L quantities, but for the purpose of pollution prevention, the analyst is encouraged to prepare smaller quantities when possible. Concentrations are calculated based upon the weight of the pure element or upon the weight of the compound multiplied by the fraction of the analyte in the compound

      From pure element,

      Page 29817

      GRAPHIC TIFF OMITTED TR18MY12.001

      where: gravimetric factor = the weight fraction of the analyte in the compound

      7.8.1 Aluminum solution, stock, 1 mL = 1000 mug Al: Dissolve 1.000 g of aluminum metal, weighed accurately to at least four significant figures, in an acid mixture of 4.0 mL of (1+1) HCl and 1 mL of concentrated HNO3 in a beaker. Warm beaker slowly to effect solution. When dissolution is complete, transfer solution quantitatively to a 1 L flask, add an additional 10.0 mL of (1+1) HCl and dilute to volume with reagent water.

      7.8.2 Antimony solution, stock, 1 mL = 1000 mug Sb: Dissolve 1.000 g of antimony powder, weighed accurately to at least four significant figures, in 20.0 mL (1+1) HNO3 and 10.0 mL concentrated HCl. Add 100 mL reagent water and 1.50 g tartaric acid. Warm solution slightly to effect complete dissolution. Cool solution and add reagent water to volume in a 1 L volumetric flask.

      7.8.3 Arsenic solution, stock, 1 mL = 1000 mug As: Dissolve 1.320 g of As2O3 (As fraction = 0.7574), weighed accurately to at least four significant figures, in 100 mL of reagent water containing 10.0 mL concentrated NH4OH. Warm the solution gently to effect dissolution. Acidify the solution with 20.0 mL concentrated HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.4 Barium solution, stock, 1 mL = 1000 mug Ba: Dissolve 1.437 g BaCO3 (Ba fraction = 0.6960), weighed accurately to at least four significant figures, in 150 mL (1+2) HNO3 with heating and stirring to degas and dissolve compound. Let solution cool and dilute with reagent water in 1 L volumetric flask.

      7.8.5 Beryllium solution, stock, 1 mL = 1000 mug Be: DO NOT DRY. Dissolve 19.66 g BeSO44H2O (Be fraction = 0.0509), weighed accurately to at least four significant figures, in reagent water, add 10.0 mL concentrated HNO3, and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.6 Boron solution, stock, 1 mL = 1000 mug B: DO NOT DRY. Dissolve 5.716 g anhydrous H3BO3 (B fraction = 0.1749), weighed accurately to at least four significant figures, in reagent water and dilute in a 1 L volumetric flask with reagent water. Transfer immediately after mixing to a clean FEP bottle to minimize any leaching of boron from the glass volumetric container. Use of a nonglass volumetric flask is recommended to avoid boron contamination from glassware.

      7.8.7 Cadmium solution, stock, 1 mL = 1000 mug Cd: Dissolve 1.000 g Cd metal, acid cleaned with (1+9) HNO3, weighed accurately to at least four significant figures, in 50 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool and dilute with reagent water in a 1 L volumetric flask.

      7.8.8 Calcium solution, stock, 1 mL = 1000 mug Ca: Suspend 2.498 g CaCO3 (Ca fraction = 0.4005), dried at 180 degC for one hour before weighing, weighed accurately to at least four significant figures, in reagent water and dissolve cautiously with a minimum amount of (1+1) HNO3. Add 10.0 mL concentrated HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.9 Cerium solution, stock, 1 mL = 1000 mug Ce: Slurry 1.228 g CeO2 (Ce fraction = 0.8141), weighed accurately to at least four significant figures, in 100 mL concentrated HNO3 and evaporate to dryness. Slurry the residue in 20 mL H2O, add 50 mL concentrated HNO3, with heat and stirring add 60 mL 50% H2O2 dropwise in 1 mL increments allowing periods of stirring between the 1 mL additions. Boil off excess H2O2 before diluting to volume in a 1 L volumetric flask with reagent water.

      7.8.10 Chromium solution, stock, 1 mL = 1000 mug Cr: Dissolve 1.923 g CrO3 (Cr fraction = 0.5200), weighed accurately to at least four significant figures, in 120 mL (1+5) HNO3. When solution is complete, dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.11 Cobalt solution, stock, 1 mL = 1000 mug Co: Dissolve 1.000 g Co metal, acid cleaned with (1+9) HNO3, weighed accurately to at least four significant figures, in 50.0 mL (1+1) HNO3. Let solution cool and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.12 Copper solution, stock, 1 mL = 1000 mug Cu: Dissolve 1.000 g Cu metal, acid cleaned with (1+9) HNO3, weighed accurately to at least four significant figures, in 50.0 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool and dilute in a 1 L volumetric flask with reagent water.

      7.8.13 Iron solution, stock, 1 mL = 1000 mug Fe: Dissolve 1.000 g Fe metal, acid cleaned with (1+1) HCl, weighed accurately to four significant figures, in 100 mL (1+1) HCl with heating to effect dissolution. Let solution cool and dilute with reagent water in a 1 L volumetric flask.

      7.8.14 Lead solution, stock, 1 mL = 1000 mug Pb: Dissolve 1.599 g Pb(NO3)2 (Pb fraction = 0.6256), weighed accurately to at least four significant figures, in a minimum amount of (1+1) HNO3. Add 20.0 mL (1+1) HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.15 Lithium solution, stock, 1 mL = 1000 mug Li: Dissolve 5.324 g Li2CO3 (Li fraction = 0.1878), weighed accurately to at least four significant figures, in a minimum amount of (1+1) HCl and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.16 Magnesium solution, stock, 1 mL = 1000 mug Mg: Dissolve 1.000 g cleanly polished Mg ribbon, accurately weighed to at least four significant figures, in slowly added 5.0 mL (1+1) HCl (CAUTION: reaction is vigorous). Add 20.0 mL (1+1) HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.17 Manganese solution, stock, 1 mL = 1000 mug Mn: Dissolve 1.000 g of manganese metal, weighed accurately to at least four significant figures, in 50 mL (1+1) HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.18 Mercury solution, stock, 1 mL = 1000 mug Hg: DO NOT DRY. CAUTION: highly toxic element. Dissolve 1.354 g HgCl2 (Hg fraction = 0.7388) in reagent water. Add 50.0 mL concentrated HNO3 and dilute to volume in 1 L volumetric flask with reagent water.

      7.8.19 Molybdenum solution, stock, 1 mL = 1000 mug Mo: Dissolve 1.500 g MoO3 (Mo fraction = 0.6666), weighed accurately to at least four significant figures, in a mixture of 100 mL reagent water and 10.0 mL concentrated NH4OH, heating to effect dissolution. Let solution cool and dilute with reagent water in a 1 L volumetric flask.

      7.8.20 Nickel solution, stock, 1 mL = 1000 mug Ni: Dissolve 1.000 g of nickel metal, weighed accurately to at least four significant figures, in 20.0 mL hot concentrated HNO3, cool, and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.21 Phosphorus solution, stock, 1 mL = 1000 mug P: Dissolve 3.745 g NH4H2PO4 (P fraction = 0.2696), weighed accurately to at least four significant figures, in 200 mL reagent water and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.22 Potassium solution, stock, 1 mL = 1000 mug K: Dissolve 1.907 g KCl (K fraction = 0.5244) dried at 110 degC, weighed accurately to at least four significant figures, in reagent water, add 20 mL (1+1) HCl and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.23 Selenium solution, stock, 1 mL = 1000 mug Se: Dissolve 1.405 g SeO2 (Se fraction = 0.7116), weighed accurately to at least four significant figures, in 200 mL reagent water and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.24 Silica solution, stock, 1 mL = 1000 mug SiO2: DO NOT DRY. Dissolve 2.964 g (NH4)2SiF6, weighed accurately to at least four significant figures, in 200 mL (1+20) HCl with heating at 85 degC to effect dissolution. Let solution cool and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.25 Silver solution, stock, 1 mL = 1000 mug Ag: Dissolve 1.000 g Ag metal, weighed accurately to at least four significant figures, in 80 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool and dilute with reagent water in a 1 L volumetric flask. Store

      Page 29818

      solution in amber bottle or wrap bottle completely with aluminum foil to protect solution from light.

      7.8.26 Sodium solution, stock, 1 mL = 1000 mug Na: Dissolve 2.542 g NaCl (Na fraction = 0.3934), weighed accurately to at least four significant figures, in reagent water. Add 10.0 mL concentrated HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.27 Strontium solution, stock, 1 mL = 1000 mug Sr: Dissolve 1.685 g SrCO3 (Sr fraction = 0.5935), weighed accurately to at least four significant figures, in 200 mL reagent water with dropwise addition of 100 mL (1+1) HCl. Dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.28 Thallium solution, stock, 1 mL = 1000 mug Tl: Dissolve 1.303 g TlNO3 (Tl fraction = 0.7672), weighed accurately to at least four significant figures, in reagent water. Add 10.0 mL concentrated HNO3 and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.29 Tin solution, stock, 1 mL = 1000 mug Sn: Dissolve 1.000 g Sn shot, weighed accurately to at least four significant figures, in an acid mixture of 10.0 mL concentrated HCl and 2.0 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool, add 200 mL concentrated HCl, and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.30 Titanium solution, stock, 1 mL = 1000 mug Ti: DO NOT DRY. Dissolve 6.138 g (NH4)2TiO(C2O4)2

      H2O (Ti fraction = 0.1629), weighed accurately to at least four significant figures, in 100 mL reagent water. Dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.31 Vanadium solution, stock, 1 mL = 1000 mug V: Dissolve 1.000 g V metal, acid cleaned with (1+9) HNO3, weighed accurately to at least four significant figures, in 50 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool and dilute with reagent water to volume in a 1 L volumetric flask.

      7.8.32 Yttrium solution, stock 1 mL = 1000 mug Y: Dissolve 1.270 g Y2O3 (Y fraction = 0.7875), weighed accurately to at least four significant figures, in 50 mL (1+1) HNO3, heating to effect dissolution. Cool and dilute to volume in a 1 L volumetric flask with reagent water.

      7.8.33 Zinc solution, stock, 1 mL = 1000 mug Zn: Dissolve 1.000 g Zn metal, acid cleaned with (1+9) HNO3, weighed accurately to at least four significant figures, in 50 mL (1+1) HNO3 with heating to effect dissolution. Let solution cool and dilute with reagent water to volume in a 1 L volumetric flask.

      7.9 Mixed Calibration Standard Solutions--For the analysis of total recoverable digested samples prepare mixed calibration standard solutions (see Table 3) by combining appropriate volumes of the stock solutions in 500 mL volumetric flasks containing 20 mL (1+1) HNO3 and 20 mL (1+1) HCl and dilute to volume with reagent water. Prior to preparing the mixed standards, each stock solution should be analyzed separately to determine possible spectral interferences or the presence of impurities. Care should be taken when preparing the mixed standards to ensure that the elements are compatible and stable together. To minimize the opportunity for contamination by the containers, it is recommended to transfer the mixed-standard solutions to acid-cleaned, never-used FEP fluorocarbon (FEP) bottles for storage. Fresh mixed standards should be prepared, as needed, with the realization that concentrations can change on aging. Calibration standards not prepared from primary standards must be initially verified using a certified reference solution. For the recommended wavelengths listed in Table 1 some typical calibration standard combinations are given in Table 3.

      Note: If the addition of silver to the recommended mixed-acid calibration standard results in an initial precipitation, add 15 mL of reagent water and warm the flask until the solution clears. For this acid combination, the silver concentration should be limited to 0.5 mg/L.

      7.10 Blanks--Four types of blanks are required for the analysis. The calibration blank is used in establishing the analytical curve, the laboratory reagent blank is used to assess possible contamination from the sample preparation procedure, the laboratory fortified blank is used to assess routine laboratory performance and a rinse blank is used to flush the instrument uptake system and nebulizer between standards, check solutions, and samples to reduce memory interferences.

      7.10.1 The calibration blank for aqueous samples and extracts is prepared by acidifying reagent water to the same concentrations of the acids as used for the standards. The calibration blank should be stored in a FEP bottle.

      7.10.2 The laboratory reagent blank (LRB) must contain all the reagents in the same volumes as used in the processing of the samples. The LRB must be carried through the same entire preparation scheme as the samples including sample digestion, when applicable.

      7.10.3 The laboratory fortified blank (LFB) is prepared by fortifying an aliquot of the laboratory reagent blank with all analytes to a suitable concentration using the following recommended criteria: Ag 0.1 mg/L, K 5.0 mg/L and all other analytes 0.2 mg/L or a concentration approximately 100 times their respective MDL, whichever is greater. The LFB must be carried through the same entire preparation scheme as the samples including sample digestion, when applicable.

      7.10.4 The rinse blank is prepared by acidifying reagent water to the same concentrations of acids as used in the calibration blank and stored in a convenient manner.

      7.11 Instrument Performance Check (IPC) Solution--The IPC solution is used to periodically verify instrument performance during analysis. It should be prepared in the same acid mixture as the calibration standards by combining method analytes at appropriate concentrations. Silver must be limited to 2; (o) 50 mg/L Ti; (p) 50 mg/L Tl and (q) 50 mg/L V should be prepared in the same acid mixture as the calibration standards and stored in FEP bottles. These solutions can be used to periodically verify a partial list of the on-line (and possible off-

      line) interelement spectral correction factors for the recommended wavelengths given in Table 1. Other solutions could achieve the same objective as well. (Multielement SIC solutions\3\ may be prepared and substituted for the single element solutions provided an analyte is not subject to interference from more than one interferant in the solution.)

      Note: If wavelengths other than those recommended in Table 1 are used, other solutions different from those above (a through q) may be required.

      7.13.2 For interferences from iron and aluminum, only those correction factors (positive or negative) when multiplied by 100 to calculate apparent analyte concentrations that exceed the determined analyte IDL or fall below the lower 3-sigma control limit of the calibration blank need be tested on a daily basis.

      7.13.3 For the other interfering elements, only those correction factors (positive or negative) when multiplied by 10 to calculate apparent analyte concentrations that exceed the determined analyte IDL or fall below the lower 3-sigma control limit of the calibration blank need be tested on a daily basis.

      7.13.4 If the correction routine is operating properly, the determined apparent analyte(s) concentration from analysis of each interference solution (a through q) should fall within a specific concentration range bracketing the calibration blank. This

      Page 29819

      concentration range is calculated by multiplying the concentration of the interfering element by the value of the correction factor being tested and dividing by 10. If after subtraction of the calibration blank the apparent analyte concentration is outside (above or below) this range, a change in the correction factor of more than 10% should be suspected. The cause of the change should be determined and corrected and the correction factor should be updated.

      Note: The SIC solution should be analyzed more than once to confirm a change has occurred with adequate rinse time between solutions and before subsequent analysis of the calibration blank.

      7.13.5 If the correction factors tested on a daily basis are found to be within the 10% criteria for five consecutive days, the required verification frequency of those factors in compliance may be extended to a weekly basis. Also, if the nature of the samples analyzed is such (e.g., finished drinking water) that they do not contain concentrations of the interfering elements at the 10 mg/L level, daily verification is not required; however, all interelement spectral correction factors must be verified annually and updated, if necessary.

      7.13.6 If the instrument does not display negative concentration values, fortify the SIC solutions with the elements of interest at 1 mg/L and test for analyte recoveries that are below 95%. In the absence of measurable analyte, over-correction could go undetected because a negative value could be reported as zero.

      7.14 For instruments without interelement correction capability or when interelement corrections are not used, SIC solutions (containing similar concentrations of the major components in the samples, e.g., 10 mg/L) can serve to verify the absence of effects at the wavelengths selected. These data must be kept on file with the sample analysis data. If the SIC solution confirms an operative interference that is 10% of the analyte concentration, the analyte must be determined using a wavelength and background correction location free of the interference or by another approved test procedure. Users are advised that high salt concentrations can cause analyte signal suppressions and confuse interference tests.

      7.15 Plasma Solution--The plasma solution is used for determining the optimum viewing height of the plasma above the work coil prior to using the method (Section 10.2). The solution is prepared by adding a 5 mL aliquot from each of the stock standard solutions of arsenic, lead, selenium, and thallium to a mixture of 20 mL (1+1) nitric acid and 20 mL (1+1) hydrochloric acid and diluting to 500 mL with reagent water. Store in a FEP bottle.

      8.0 Sample Collection, Preservation, and Storage

      8.1 Prior to the collection of an aqueous sample, consideration should be given to the type of data required, (i.e., dissolved or total recoverable), so that appropriate preservation and pretreatment steps can be taken. The pH of all aqueous samples must be tested immediately prior to aliquoting for processing or ``direct analysis'' to ensure the sample has been properly preserved. If properly acid preserved, the sample can be held up to six months before analysis.

      8.2 For the determination of the dissolved elements, the sample must be filtered through a 0.45 mum pore diameter membrane filter at the time of collection or as soon thereafter as practically possible. (Glass or plastic filtering apparatus are recommended to avoid possible contamination. Only plastic apparatus should be used when the determinations of boron and silica are critical.) Use a portion of the filtered sample to rinse the filter flask, discard this portion and collect the required volume of filtrate. Acidify the filtrate with (1+1) nitric acid immediately following filtration to pH 2, more acid must be added and the sample held for 16 hours until verified to be pH s = fortified sample concentration

      C = sample background concentration

      s = concentration equivalent of analyte added to fortify the sample

      9.4.4 If the recovery of any analyte falls outside the designated LFM recovery range, and the laboratory performance for that analyte is shown to be in control (Section 9.3), the recovery problem encountered with the fortified sample is judged to be matrix related, not system related. The data user should be informed that the result for that analyte in the unfortified sample is suspect due to either the heterogeneous nature of the sample or matrix effects and analysis by method of standard addition or the use of an internal standard(s) (Section 11.5) should be considered.

      9.4.5 Where reference materials are available, they should be analyzed to provide additional performance data. The analysis of reference samples is a valuable tool for demonstrating the ability to perform the method acceptably. Reference materials containing high concentrations of analytes can provide additional information on the performance of the spectral interference correction routine.

      9.5 Assess the possible need for the method of standard additions (MSA) or internal standard elements by the following tests. Directions for using MSA or internal standard(s) are given in Section 11.5.

      9.5.1 Analyte addition test: An analyte(s) standard added to a portion of a prepared

      Page 29821

      sample, or its dilution, should be recovered to within 85% to 115% of the known value. The analyte(s) addition should produce a minimum level of 20 times and a maximum of 100 times the method detection limit. If the analyte addition is 3 to a 20 mL aliquot of sample). Cap the tube and mix. The sample is now ready for analysis (Section 1.3). Allowance for sample dilution should be made in the calculations. (If mercury is to be determined, a separate aliquot must be additionally acidified to contain 1% (vsolv) HCl to match the signal response of mercury in the calibration standard and reduce memory interference effects. Section 1.9).

      Note: If a precipitate is formed during acidification, transport, or storage, the sample aliquot must be treated using the procedure described in Sections 11.2.2 through 11.2.7 prior to analysis.

      11.2 Aqueous Sample Preparation--Total Recoverable Analytes

      11.2.1 For the ``direct analysis'' of total recoverable analytes in drinking water samples containing turbidity 1%, a well mixed, acid preserved aliquot containing no more than 1 g particulate material should be cautiously evaporated to near 10 mL and extracted using the acid-mixture procedure described in Sections 11.3.3 through 11.3.6.

      11.2.3 Add 2 mL (1+1) nitric acid and 1.0 mL of (1+1) hydrochloric acid to the beaker containing the measured volume of sample. Place the beaker on the hot plate for solution evaporation. The hot plate should be located in a fume hood and previously adjusted to provide evaporation at a temperature of approximately but no higher than 85 degC. (See the following note.) The beaker should be covered with an elevated watch glass or other necessary steps should be taken to prevent sample contamination from the fume hood environment.

      Note: For proper heating adjust the temperature control of the hot plate such that an uncovered Griffin beaker containing 50 mL of water placed in the center of the hot plate can be maintained at a temperature approximately but no higher than 85 degC. (Once the beaker is covered with a watch glass the temperature of the water will rise to approximately 95 degC.)

      11.2.4 Reduce the volume of the sample aliquot to about 20 mL by gentle heating at 85 degC. DO NOT BOIL. This step takes about two hours for a 100 mL aliquot with the rate of evaporation rapidly increasing as the sample volume approaches 20 mL. (A spare beaker containing 20 mL of water can be used as a gauge.)

      11.2.5 Cover the lip of the beaker with a watch glass to reduce additional evaporation and gently reflux the sample for 30 minutes. (Slight boiling may occur, but vigorous boiling must be avoided to prevent loss of the HCl-H2O azeotrope.)

      11.2.6 Allow the beaker to cool. Quantitatively transfer the sample solution to a 50 mL volumetric flask, make to volume with reagent water, stopper and mix.

      11.2.7 Allow any undissolved material to settle overnight, or centrifuge a portion of the prepared sample until clear. (If after centrifuging or standing overnight the sample contains suspended solids that would clog the nebulizer, a portion of the sample may be filtered for their removal prior to analysis. However, care should be exercised to avoid potential contamination from filtration.) The sample is now ready for analysis. Because the effects of various matrices on the stability of diluted samples cannot be characterized, all analyses should be performed as soon as possible after the completed preparation.

      11.3 Solid Sample Preparation--Total Recoverable Analytes

      11.3.1 For the determination of total recoverable analytes in solid samples, mix the sample thoroughly and transfer a portion (>20 g) to tared weighing dish, weigh the sample and record the wet weight (WW). (For samples with 35% a larger aliquot 50-100 g is required.) Dry the sample to a constant weight at 60 degC and record the dry weight (DW) for calculation of percent solids (Section 12.6). (The sample is dried at 60 degC to prevent the loss of mercury and other possible volatile metallic compounds, to facilitate sieving, and to ready the sample for grinding.)

      11.3.2 To achieve homogeneity, sieve the dried sample using a 5-

      mesh polypropylene sieve and grind in a mortar and pestle. (The sieve, mortar and pestle should be cleaned between samples.) From the dried, ground material weigh accurately a representative 1.0 0.01 g aliquot (W) of the sample and transfer to a 250 mL Phillips beaker for acid extraction (Sections 1.6, 1.7, 1.8, and 1.9).

      11.3.3 To the beaker add 4 mL of (1+1) HNO3 and 10 mL of (1+4) HCl. Cover the lip of the beaker with a watch glass. Place the beaker on a hot plate for reflux extraction of the analytes. The hot plate should be located in a fume hood and previously adjusted to provide a reflux temperature of approximately 95 degC. (See the following note.)

      Note: For proper heating adjust the temperature control of the hot plate such that an uncovered Griffin beaker containing 50 mL of water placed in the center of the hot plate can be maintained at a temperature approximately but no higher than 85 degC. (Once the beaker is covered with a watch glass the temperature of the water will rise to approximately 95 degC.) Also, a block digester capable of maintaining a temperature of 95 degC and equipped with 250 mL constricted volumetric digestion tubes may be substituted for the hot plate and conical beakers in the extraction step.

      11.3.4 Heat the sample and gently reflux for 30 minutes. Very slight boiling may occur, however vigorous boiling must be avoided to prevent loss of the HCl-H2O azeotrope. Some solution evaporation will occur (3-4 mL).

      11.3.5 Allow the sample to cool and quantitatively transfer the extract to a 100 mL volumetric flask. Dilute to volume with reagent water, stopper and mix.

      11.3.6 Allow the sample extract solution to stand overnight to separate insoluble material or centrifuge a portion of the sample solution until clear. (If after centrifuging or standing overnight the extract solution contains suspended solids that would clog the nebulizer, a portion of the extract solution may be filtered for their removal prior to analysis. However, care should be exercised to avoid potential contamination from filtration.) The sample extract is now ready for analysis. Because the effects of various matrices on the stability of diluted samples cannot be characterized, all analyses should be performed as soon as possible after the completed preparation.

      11.4 Sample Analysis

      11.4.1 Prior to daily calibration of the instrument inspect the sample introduction system including the nebulizer, torch, injector tube and uptake tubing for salt deposits, dirt and debris that would restrict solution flow and affect instrument performance. Clean the system when needed or on a daily basis.

      11.4.2 Configure the instrument system to the selected power and operating conditions as determined in Sections 10.1 and 10.2.

      11.4.3 The instrument must be allowed to become thermally stable before calibration and analyses. This usually requires at least 30 to 60 minutes of operation. After instrument warmup, complete any required optical profiling or alignment particular to the instrument.

      11.4.4 For initial and daily operation calibrate the instrument according to the instrument manufacturer's recommended procedures, using mixed calibration standard solutions (Section 7.9) and the calibration blank (Section 7.10.1). A peristaltic pump must be used to introduce all solutions to the nebulizer. To allow equilibrium to be reached in the plasma, aspirate all solutions for 30 seconds after reaching the plasma before beginning integration of the background corrected signal to accumulate data. When possible, use the average value of replicate integration periods of the signal to be correlated to the analyte concentration. Flush the system with the rinse blank (Section 7.10.4) for a minimum of 60 seconds (Section 4.4) between each standard. The calibration line should consist of a minimum of a calibration blank and a high standard. Replicates of the blank and highest standard provide an optimal distribution of calibration standards to minimize the confidence band for a straight-line calibration in a response region with uniform variance.\20\

      11.4.5 After completion of the initial requirements of this method (Sections 10.3 and 10.4), samples should be analyzed in the same operational manner used in the calibration routine with the rinse blank also being used between all sample solutions, LFBs, LFMs, and check solutions (Section 7.10.4).

      11.4.6 During the analysis of samples, the laboratory must comply with the required quality control described in Sections 9.3 and 9.4. Only for the determination of dissolved analytes or the ``direct analysis'' of drinking water with turbidity of 1 = Signal for fortified aliquot

      S2 = Signal for unfortified aliquot

      V1 = Volume of the standard addition (L)

      V2 = Volume of the sample aliquot (L) used for MSA

      For more than one fortified portion of the prepared sample, linear regression analysis can be applied using a computer or calculator program to obtain the concentration of the sample solution. An alternative to using the method of standard additions is use of the internal standard technique by adding one or more elements (not in the samples and verified not to cause an uncorrected interelement spectral interference) at the same concentration (which is sufficient for optimum precision) to the prepared samples (blanks and standards) that are affected the same as the analytes by the sample matrix. Use the ratio of analyte signal to the internal standard signal for calibration and quantitation.

      12.0 Data Analysis and Calculations

      12.1 Sample data should be reported in units of mg/L for aqueous samples and mg/kg dry weight for solid samples.

      12.2 For dissolved aqueous analytes (Section 11.1) report the data generated directly from the instrument with allowance for sample dilution. Do not report analyte concentrations below the IDL.

      12.3 For total recoverable aqueous analytes (Section 11.2), multiply solution analyte concentrations by the dilution factor 0.5, when 100 mL aliquot is used to produce the 50 mL final solution, and report data as instructed in Section 12.4. If a different aliquot volume other than 100 mL is used for sample preparation, adjust the dilution factor accordingly. Also, account for any additional dilution of the prepared sample solution needed to complete the determination of analytes exceeding 90% or more of the LDR upper limit. Do not report data below the determined analyte MDL concentration or below an adjusted detection limit reflecting smaller sample aliquots used in processing or additional dilutions required to complete the analysis.

      12.4 For analytes with MDLs 20 g) of the sample and dry to constant weight at 103-105 degC.

      12.7 The QC data obtained during the analyses provide an indication of the quality of the sample data and should be provided with the sample results.

      13.0 Method Performance

      13.1 Listed in Table 4 are typical single laboratory total recoverable MDLs determined for the recommended wavelengths using simultaneous ICP-AES and the operating conditions given in Table 5. The MDLs were determined in reagent blank matrix (best case situation). PTFE beakers were used to avoid boron and silica contamination from glassware with the final dilution to 50 mL completed in polypropylene centrifuged tubes. The listed MDLs for solids are estimates and were calculated from the aqueous MDL determinations.

      13.2 Data obtained from single laboratory method testing are summarized in Table 6 for five types of water samples consisting of drinking water, surface water, ground water, and two wastewater effluents. The data presented cover all analytes except cerium and titanium. Samples were prepared using the procedure described in Section 11.2. For each matrix, five replicate aliquots were prepared, analyzed and the average of the five determinations used to define the sample background concentration of each analyte. In addition, two pairs of duplicates were fortified at different concentration levels. For each method analyte, the sample background concentration, mean percent recovery, standard deviation of the percent recovery, and relative percent difference between the duplicate fortified samples are listed in Table 6. The variance of the five replicate sample background determinations is included in the calculated standard deviation of the percent recovery when the analyte concentration in the sample was greater than the MDL. The tap and well waters were processed in Teflon and quartz beakers and diluted in polypropylene centrifuged tubes. The nonuse of borosilicate glassware is reflected in the precision and recovery data for boron and silica in those two sample types.

      13.3 Data obtained from single laboratory method testing are summarized in Table 7 for three solid samples consisting of EPA 884 Hazardous Soil, SRM 1645 River Sediment, and EPA 286 Electroplating Sludge. Samples were prepared using the procedure described in Section 11.3. For each method analyte, the sample background concentration, mean percent recovery of the fortified additions, the standard deviation of the percent

      Page 29824

      recovery, and relative percent difference between duplicate additions were determined as described in Section 13.2. Data presented are for all analytes except cerium, silica, and titanium. Limited comparative data to other methods and SRM materials are presented in Reference 23 of Section 16.0.

      13.4 Performance data for aqueous solutions independent of sample preparation from a multilaboratory study are provided in Table 8.\22\

      13.5 Listed in Table 9 are regression equations for precision and bias for 25 analytes abstracted from EPA Method Study 27, a multilaboratory validation study of Method 200.7.\1\ These equations were developed from data received from 12 laboratories using the total recoverable sample preparation procedure on reagent water, drinking water, surface water and three industrial effluents. For a complete review and description of the study, see Reference 16 of Section 16.0.

      14.0 Pollution Prevention

      14.1 Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation. Numerous opportunities for pollution prevention exist in laboratory operation. The EPA has established a preferred hierarchy of environmental management techniques that places pollution prevention as the management option of first choice. Whenever feasible, laboratory personnel should use pollution prevention techniques to address their waste generation (e.g., Section 7.8). When wastes cannot be feasibly reduced at the source, the Agency recommends recycling as the next best option.

      14.2 For information about pollution prevention that may be applicable to laboratories and research institutions, consult ``Less is Better: Laboratory Chemical Management for Waste Reduction'', available from the American Chemical Society's Department of Government Relations and Science Policy, 1155 16th Street NW., Washington, DC 20036, (202) 872-4477.

      15.0 Waste Management

      15.1 The Environmental Protection Agency requires that laboratory waste management practices be conducted consistent with all applicable rules and regulations. The Agency urges laboratories to protect the air, water, and land by minimizing and controlling all releases from hoods and bench operations, complying with the letter and spirit of any sewer discharge permits and regulations, and by complying with all solid and hazardous waste regulations, particularly the hazardous waste identification rules and land disposal restrictions. For further information on waste management consult ``The Waste Management Manual for Laboratory Personnel'', available from the American Chemical Society at the address listed in the Section 14.2.

      16.0 References

      1. U.S. Environmental Protection Agency. Inductively Coupled Plasma--

      Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes--Method 200.7, Dec. 1982. EPA-600/4-79-020, revised March 1983.

      2. U.S. Environmental Protection Agency. Inductively Coupled Plasma Atomic Emission Spectroscopy Method 6010, SW-846 Test Methods for Evaluating Solid Waste, 3rd Edition, 1986.

      3. U.S. Environmental Protection Agency. Method 200.7: Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma--Atomic Emission Spectrometry, revision 3.3, EPA 600 4-91/010, June 1991.

      4. U.S. Environmental Protection Agency. Inductively Coupled Plasma--

      Atomic Emission Spectrometry Method for the Analysis of Waters and Solids, EMMC, July 1992.

      5. Fassel, V.A. et al. Simultaneous Determination of Wear Metals in Lubricating Oils by Inductively-Coupled Plasma Atomic Emission Spectrometry. Anal. Chem. 48:516-519, 1976.

      6. Merryfield, R.N. and R.C. Loyd. Simultaneous Determination of Metals in Oil by Inductively Coupled Plasma Emission Spectrometry. Anal. Chem. 51:1965-1968, 1979.

      7. Winge, R.K. et al. Inductively Coupled Plasma--Atomic Emission Spectroscopy: An Atlas of Spectral Information, Physical Science Data 20. Elsevier Science Publishing, New York, New York, 1985.

      8. Boumans, P.W.J.M. Line Coincidence Tables for Inductively Coupled Plasma Atomic Emission Spectrometry, 2nd edition. Pergamon Press, Oxford, United Kingdom, 1984.

      9. Carcinogens--Working With Carcinogens, Department of Health, Education, and Welfare, Public Health Service, Center for Disease Control, National Institute for Occupational Safety and Health, Publication No. 77-206, Aug. 1977. Available from the National Technical Information Service (NTIS) as PB-277256.

      10. OSHA Safety and Health Standards, General Industry, (29 CFR 1910), Occupational Safety and Health Administration, OSHA 2206, (Revised, January 1976).

      11. Safety in Academic Chemistry Laboratories, American Chemical Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.

      12. Proposed OSHA Safety and Health Standards, Laboratories, Occupational Safety and Health Administration, Federal Register, July 24, 1986.

      13. Rohrbough, W.G. et al. Reagent Chemicals, American Chemical Society Specifications, 7th edition. American Chemical Society, Washington, DC, 1986.

      14. American Society for Testing and Materials. Standard Specification for Reagent Water, D1193-77. Annual Book of ASTM Standards, Vol. 11.01. Philadelphia, PA, 1991.

      15. Code of Federal Regulations 40, Ch. 1, Pt. 136 Appendix B.

      16. Maxfield, R. and B. Mindak. EPA Method Study 27, Method 200.7 Trace Metals by ICP, Nov. 1983. Available from National Technical Information Service (NTIS) as PB 85-248-656.

      17. Botto, R.I. Quality Assurance in Operating a Multielement ICP Emission Spectrometer. Spectrochim. Acta, 39B(1):95-113, 1984.

      18. Wallace, G.F., Some Factors Affecting the Performance of an ICP Sample Introduction System. Atomic Spectroscopy, Vol. 4, p. 188-192, 1983.

      19. Koirtyohann, S.R. et al. Nomenclature System for the Low-Power Argon Inductively Coupled Plasma, Anal. Chem. 52:1965, 1980.

      20. Deming, S.N. and S.L. Morgan. Experimental Design for Quality and Productivity in Research, Development, and Manufacturing, Part III, pp. 119-123. Short course publication by Statistical Designs, 9941 Rowlett, Suite 6, Houston, TX 77075, 1989.

      21. Winefordner, J.D., Trace Analysis: Spectroscopic Methods for Elements, Chemical Analysis, Vol. 46, pp. 41-42.

      22. Jones, C.L. et al. An Interlaboratory Study of Inductively Coupled Plasma Atomic Emission Spectroscopy Method 6010 and Digestion Method 3050. EPA-600/4-87-032, U.S. Environmental Protection Agency, Las Vegas, Nevada, 1987.

      23. Martin, T.D., E.R. Martin and SE. Long. Method 200.2: Sample Preparation Procedure for Spectrochemical Analyses of Total Recoverable Elements, EMSL ORD, USEPA, 1989.

      17.0 Tables, Diagrams, Flowcharts, and Validation Data

      Page 29825

      Table 1--Wavelengths, Estimated Instrument Detection Limits, and Recommended Calibration

      ----------------------------------------------------------------------------------------------------------------

      Estimated

      Wavelength\a\ detection Calibrate\c\ to

      Analyte (nm) limit\b\ (mug/ (mg/L)

      L)

      ----------------------------------------------------------------------------------------------------------------

      Aluminum.................................................. 308.215 45 10

      Antimony.................................................. 206.833 32 5

      Arsenic................................................... 193.759 53 10

      Barium.................................................... 493.409 2.3 1

      Beryllium................................................. 313.042 0.27 1

      Boron..................................................... 249.678 5.7 1

      Cadmium................................................... 226.502 3.4 2

      Calcium................................................... 315.887 30 10

      Cerium.................................................... 413.765 48 2

      Chromium.................................................. 205.552 6.1 5

      Cobalt.................................................... 228.616 7.0 2

      Copper.................................................... 324.754 5.4 2

      Iron...................................................... 259.940 6.2 10

      Lead...................................................... 220.353 42 10

      Lithium................................................... 670.784 \d\ 3.7 5

      Magnesium................................................. 279.079 30 10

      Manganese................................................. 257.610 1.4 2

      Mercury................................................... 194.227 2.5 2

      Molybdenum................................................ 203.844 12 10

      Nickel.................................................... 231.604 15 2

      Phosphorus................................................ 214.914 76 10

      Potassium................................................. 766.491 \e\ 700 20

      Selenium.................................................. 196.090 75 5

      Silica (SiO2)............................................. 251.611 \d\ 26 (SiO2) 10

      Silver.................................................... 328.068 7.0 0.5

      Sodium.................................................... 588.995 29 10

      Strontium................................................. 421.552 0.77 1

      Thallium.................................................. 190.864 40 5

      Tin....................................................... 189.980 25 4

      Titanium.................................................. 334.941 3.8 10

      Vanadium.................................................. 292.402 7.5 2

      Zinc...................................................... 213.856 1.8 5

      ----------------------------------------------------------------------------------------------------------------

      \a\ The wavelengths listed are recommended because of their sensitivity and overall acceptability. Other

      wavelengths may be substituted if they can provide the needed sensitivity and are treated with the same

      corrective techniques for spectral interference (see Section 4.1).

      \b\ These estimated 3-sigma instrumental detection limits \16\ are provided only as a guide to instrumental

      limits. The method detection limits are sample dependent and may vary as the sample matrix varies. Detection

      limits for solids can be estimated by dividing these values by the grams extracted per liter, which depends

      upon the extraction procedure. Divide solution detection limits by 10 for 1 g extracted to 100 mL for solid

      detection limits.

      \c\ Suggested concentration for instrument calibration.\2\ Other calibration limits in the linear ranges may be

      used.

      \d\ Calculated from 2-sigma data.\5\

      \e\ Highly dependent on operating conditions and plasma position.

      Page 29826

      TABLE 2--On-Line Method Interelement Spectral Interferances Arising From Interferants at the 100 mg/L Level

      ----------------------------------------------------------------------------------------------------------------

      Analyte Wavelength (nm) Interferant*

      ----------------------------------------------------------------------------------------------------------------

      Ag......................................... 328.068 Ce, Ti, Mn

      Al......................................... 308.215 V, Mo, Ce, Mn

      As......................................... 193.759 V, Al, Co, Fe, Ni

      B.......................................... 249.678 None

      Ba......................................... 493.409 None

      Be......................................... 313.042 V, Ce

      Ca......................................... 315.887 Co, Mo, Ce

      Cd......................................... 226.502 Ni, Ti, Fe, Ce

      Ce......................................... 413.765 None

      Co......................................... 228.616 Ti, Ba, Cd, Ni, Cr, Mo, Ce

      Cr......................................... 205.552 Be, Mo, Ni

      Cu......................................... 324.754 Mo, Ti

      Fe......................................... 259.940 None

      Hg......................................... 194.227 V, Mo

      K.......................................... 766.491 None

      Li......................................... 670.784 None

      Mg......................................... 279.079 Ce

      Mn......................................... 257.610 Ce

      Mo......................................... 203.844 Ce

      Na......................................... 588.995 None

      Ni......................................... 231.604 Co, Tl

      P.......................................... 214.914 Cu, Mo

      Pb......................................... 220.353 Co, Al, Ce, Cu, Ni, Ti, Fe

      Sb......................................... 206.833 Cr, Mo, Sn, Ti, Ce, Fe

      Se......................................... 196.099 Fe

      SiO2....................................... 251.611 None

      Sn......................................... 189.980 Mo, Ti, Fe, Mn, Si

      Sr......................................... 421.552 None

      Tl......................................... 190.864 Ti, Mo, Co, Ce, Al, V, Mn

      Ti......................................... 334.941 None

      V.......................................... 292.402 Mo, Ti, Cr, Fe, Ce

      Zn......................................... 213.856 Ni, Cu, Fe

      ----------------------------------------------------------------------------------------------------------------

      * These on-line interferences from method analytes and titanium only were observed using an instrument with

      0.035 nm resolution (see Section 4.1.2). Interferant ranked by magnitude of intensity with the most severe

      interferant listed first in the row.

      TABLE 3--Mixed Standard Solutions

      ----------------------------------------------------------------------------------------------------------------

      Solution Analytes

      ----------------------------------------------------------------------------------------------------------------

      I......................................... Ag, As, B, Ba, Ca, Cd, Cu, Mn, Sb, and Se

      II........................................ K, Li, Mo, Na, Sr, and Ti

      III....................................... Co, P, V, and Ce

      IV........................................ Al, Cr, Hg, SiO2, Sn, and Zn

      V......................................... Be, Fe, Mg, Ni, Pb, and Tl

      ----------------------------------------------------------------------------------------------------------------

      TABLE 4--Total Recoverable Method Detection Limits (MDL)

      ------------------------------------------------------------------------

      MDLs Aqueous, mg/

      Analyte L\(1)\ Solids, mg/kg\(2)\

      ------------------------------------------------------------------------

      Ag.............................. 0.002 0.3

      Al.............................. 0.02 3

      As.............................. 0.008 2

      B............................... 0.003 --

      Ba.............................. 0.001 0.2

      Be.............................. 0.0003 0.1

      Ca.............................. 0.01 2

      Cd.............................. 0.001 0.2

      Ce.............................. 0.02 3

      Co.............................. 0.002 0.4

      Cr.............................. 0.004 0.8

      Cu.............................. 0.003 0.5

      Fe.............................. *0.03 6

      Hg.............................. 0.007 2

      K............................... 0.3 60

      Li.............................. 0.001 0.2

      Mg.............................. 0.02 3

      Mn.............................. 0.001 0.2

      Mo.............................. 0.004 1

      Page 29827

      Na.............................. 0.03 6

      Ni.............................. 0.005 1

      P............................... 0.06 12

      Pb.............................. 0.01 2

      Sb.............................. 0.008 2

      Se.............................. 0.02 5

      SiO2............................ 0.02 --

      Sn.............................. 0.007 2

      Sr.............................. 0.0003 0.1

      Tl.............................. 0.001 0.2

      Ti.............................. 0.02 3

      V............................... 0.003 1

      Zn.............................. 0.002 0.3

      ------------------------------------------------------------------------

      \(1)\ MDL concentrations are computed for original matrix with allowance

      for 2x sample preconcentration during preparation. Samples were

      processed in PTFE and diluted in 50-mL plastic centrifuge tubes.

      \(2)\ Estimated, calculated from aqueous MDL determinations.

      -- Boron not reported because of glassware contamination. Silica not

      determined in solid samples.

      * Elevated value due to fume-hood contamination.

      TABLE 5--Inductively Coupled Plasma Instrument Operating Conditions

      ------------------------------------------------------------------------

      ------------------------------------------------------------------------

      Incident rf power........................ 1100 watts

      Reflected rf power....................... 884

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Ag................................. 1.1 20 98 0.7 1.0 100 96 0.2 0.6

      Al................................. 5080 20 * * 7.2 100 * * 5.4

      As................................. 5.7 20 95 5.4 10.6 100 96 1.4 3.6

      B.................................. 20.4 100 93 2.7 5.3 400 100 2.1 5.5

      Ba................................. 111 20 98 71.4 22.2 100 97 10.0 1.0

      Be................................. 0.66 20 97 0.7 2.3 100 99 0.1 0.2

      Ca................................. 85200 - - - - - - - -

      Cd................................. 2 20 93 0.7 1.0 100 94 0.2 0.4

      Co................................. 5.5 20 96 3.5 7.7 100 93 0.8 2.1

      Cr................................. 79.7 20 87 28.8 16.5 100 104 1.3 1.1

      Cu................................. 113 20 110 16.2 4.4 100 104 4.0 4.2

      Fe................................. 16500 - - - - - - - -

      Hg................................. 286

      --------------------------------------------------------------------------------------------------------------------------------------------------------

      Ag................................. 6 20 96 0.2 0.4 100 93 0.1 0.4

      Al................................. 4980 20 * * 4.4 100 * * 5.6

      As................................. 32 20 94 1.3 0.8 100 97 0.7 1.6

      B.................................. 210 100 113 2.0 1.6 400 98 1.9 3.5

      Ba................................. 39.8 20 0 6.8 0.3 100 0 1.6 5.7

      Be................................. 0.32 20 96 0.2 0.5 100 101 0.7 2.0

      Ca................................. 48500 - - - - - - - -

      Cd................................. 108 20 98 2.5 0.8 100 96 0.5 0.5

      Co................................. 5.9 20 93 2.9 5.7 100 93 0.6 1.5

      Cr................................. 7580 20 * * 0.7 100 * * 1.3

      Cu................................. 806 20 * * 1.5 100 94 8.3 0.7

      Fe................................. 31100 - - - - - - - -

      Hg................................. 6.1 10 90 2.5 4.0 40 97 1.7 4.3

      K.................................. 2390 500 75 8.3 4.0 2000 94 2.9 3.8

      Li................................. 9.1 10 101 2.8 0.5 40 106 1.6 3.1

      Mg................................. 1950 500 110 2.0 0.8 2000 108 2.3 3.2

      Mn................................. 262 20 * * 1.8 100 91 1.2 0.9

      Mo................................. 13.2 20 92 2.1 2.9 100 92 0.3 0.0

      Na................................. 73400 500 * * 1.7 2000 * * 1.4

      Ni................................. 456 20 * * 0.4 100 88 2.7 0.9

      P.................................. 9610 500 * * 2.9 2000 114 7.4 3.4

      Pb................................. 1420 20 * * 2.1 100 * * 1.3

      Sb................................. 50 value allowed as measured in any single sample of the discharged waste stream. Minimum as applied to BPT and BCT effluent limitations and NSPS for sanitary wastes means the minimum concentration value allowed as measured in any single sample of the discharged waste stream.

      * * * * *

      (x) 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this section.

      * * * * *

      (ee) Sediment toxicity as applied to BAT effluent limitations and NSPS for drilling fluids and drill cuttings refers to EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' and sediment preparation procedures specified in EPA Method 1646. EPA Method 1644 is published in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' (see paragraph (uu) of this section) and EPA Method 1646 is published as an appendix to Subpart A of this part.

      * * * * *

      (gg) 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this section.

      (hh) Static sheen test means the standard test procedure that has been 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this section.

      * * * * *

      (ss) C16-C18 internal olefin drilling fluid means a C16-C18 internal 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, ``Analytic Methods for the Oil and Gas Point Source Category,'' December 2011, EPA-821-R-11-004, 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. This method may be obtained

      Page 29836

      at http://water.epa.gov/scitech/methods/cwa/index.cfm.

      0

      18. In Sec. 435.12, Footnote 1 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).

      * * * * *

      \1\ No discharge of free oil. See Sec. 435.11(x).

      * * * * *

      0

      19. In Sec. 435.13:

      0

    4. Remove ``LC5'' and add in its place ``LC50'' wherever it appears.

      0

    5. 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).

      * * * * *

      \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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after preparing the sediment according to the procedure specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. See Sec. 435.11(ee) and (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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after sediment preparation procedures specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after sediment preparation procedures specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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.

      0

      20. 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).

      * * * * *

      \2\ As determined by the static sheen test. See Sec. 435.11(hh).

      * * * * *

      0

      21. In Sec. 435.15:

      0

    6. Remove ``LC5'' and add in its place ``LC50''wherever it appears.

      0

    7. 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).

      * * * * *

      \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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after preparing the sediment according to the procedure specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. See Sec. 435.11(ee) and (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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. See Sec. 435.11(e) and (uu).

      \8\ Drilling fluid sediment toxicity ratio = 4dashday 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after sediment preparation procedures specified in

      Page 29837

      EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-

      821-R-11-004. 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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after sediment preparation procedures specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-

      004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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.

      0

      22. The heading of Appendix 1 to Subpart A of Part 435 is revised to read as follows:

      Appendix 1 to Subpart A of Part 435-- Static Sheen Test (EPA Method 1617)

      * * * * *

      0

      23. Appendix 2 to Subpart A of Part 435 is amended as follows:

      0

    8. Revise the appendix heading.

      0

    9. Remove the fourth sentence from Section II.C.6.

      0

    10. Revise Section III.A.1.

      0

    11. Revise Section III.E.2.

      The revisions read as follows:

      Appendix 2 to Subpart A of Part 435--Drilling Fluids Toxicity Test (EPA Method 1619)

      * * * * *

      III-A. * * *

      (1) Each definitive test consists of 18 test containers: 3 replicates of a control and 5 SPP dilutions. Test containers should be Pyrex or equivalent glass. For definitive tests, 5 SPP dilutions with 3 replicates of at least 500 ml each are required. Twenty mysids per replicate, 360 per definitive test are required.

      * * * * *

      III-E. * * *

      (2) Establish the definitive test concentrations based on results of a range finding test or based on prior experience and knowledge of the mud system.

      * * * * *

      0

      24. The heading of Appendix 3 to Subpart A of Part 435 is amended to read as follows:

      Appendix 3 to Subpart A of Part 435--Procedure for Mixing Base Fluids With Sediments (EPA Method 1646)

      * * * * *

      0

      25. Appendix 4 to Subpart A of Part 435 is revised to read as follows:

      Appendix 4 to Subpart A of Part 435-- 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)

      1.0. Summary of EPA Method 1647

    12. This method determines the anaerobic degradation potential of mineral oils, paraffin oils and non-aqueous fluids (NAF) in sediments. These substrates are base fluids for formulating offshore drilling fluids. The test evaluates base fluid biodegradation rates by monitoring gas production due to microbial degradation of the test fluid in natural marine sediment.

    13. The test procedure places a mixture of marine/estuarine sediment, test substrate (hydrocarbon or controls) and seawater into clean 120 mL (150 mL actual volume) Wheaton serum bottles. The test is run using four replicate serum bottles containing 2,000 mg carbon/kg dry weight concentration of test substrate in sediment. The use of resazurin dye solution (1 ppm) evaluates the anaerobic (redox) condition of the bottles (dye is blue when oxygen is present, reddish in low oxygen conditions and colorless if oxygen free). After capping the bottles, a nitrogen sparge removes air in the headspace before incubation begins. During the incubation period, the sample should be kept at a constant temperature of 29 1degC. Gas production and composition is measured approximately every two weeks. The samples need to be brought to ambient temperature before making the measurements. Measure gas production using a pressure gauge. Barometric pressure is measured at the time of testing to make necessary volume adjustments.

    14. ISO 11734:1995 specifies that total gas is the standard measure of biodegradation. While modifying this test for evaluating biodegradation of NAFs, methane was also monitored and found to be an acceptable method of evaluating biodegradation. Section 7 contains the procedures used to follow biodegradation by methane production. Measurement of either total gas or methane production is permitted. If methane is followed, determine the composition of the gas by using gas chromatography (GC) analysis at each sampling. At the end of the test when gas production stops, or at around 275 days, an analysis of sediment for substrate content is possible. Common methods which have been successfully used for analyzing NAFs from sediments are listed in Section 8.

      2.0 System Requirements

      This environmental test system has three phases, spiked sediment, overlying seawater, and a gas headspace. The sediment/test compound mixture is combined with synthetic sea water and transferred into 120-mL serum bottles. The total volume of sediment/

      sea water mixture in the bottles is 75 mL. The volume of the sediment layer will be approximately 50 mL, but the exact volume of the sediment will depend on sediment characteristics (wet:dry ratio and density). The amount of synthetic sea water will be calculated to bring the total volume in the bottles to 75 mL. The test systems are maintained at a temperature of 29 1degC during incubation. The test systems are brought to ambient temperatures prior to measuring pressure or gas volume.

      2.1 Sample Requirements

    15. The concentration of base fluids are at least 2,000 mg carbon test material/kg dry sediment. Carbon concentration is determined by theoretical composition based on the chemical formula or by chemical analysis by ASTM D5291-96. Sediments with positive, intermediate and negative control substances as well as a C16-

      C18 internal olefin type base fluid will be run in conjunction with test materials under the same conditions. The positive control is ethyl oleate (CAS 111-62-6), the intermediate control is 1-hexadecene (CAS 629-73-2), and the negative control is squalane (CAS 111-01-3). Controls must be of analytical grade or

      Page 29838

      the highest grade available. Each test control concentration should be prepared according to the mixing procedure described in Section 3.1.

    16. Product names will be used for examples or clarification in the following text. Any use of trade or product names in this publication is for descriptive use only, and does not constitute endorsement by EPA or the authors.

      2.2. Seawater Requirements

      Synthetic seawater at a salinity of 25 1 ppt should be used for the test. The synthetic seawater should be prepared by mixing a commercially available artificial seawater mix, into high purity distilled or de-ionized water. The seawater should be aerated and allowed to age for approximately one month prior to use.

      2.3. Sediment Requirements

    17. The dilution sediment must be from a natural estuarine or marine environment and be free of the compounds of interest. The collection location, date and time will be documented and reported. The sediment is prepared by press-sieving through a 2,000-micron mesh sieve to remove large debris, then press-sieving through a 500-

      micron sieve to remove indigenous organisms that may confound test results. The water content of the sediment should be less than 60% (w/w) or a wet to dry ratio of 2.5. The sediment should have a minimum organic matter content of 3% (w/w) as determined by ASTM D2974-07a (Method A and D and calculate organic matter as in Section 8.3 of method ASTM D2974-07a).

    18. To reduce the osmotic shock to the microorganisms in the sediment the salinity of the sediment's pore water should be between 20-30 ppt. Sediment should be used for testing as soon as possible after field collection. If required, sediment can be stored in the dark at 4 degC with 3-6 inches of overlying water in a sealed container for a maximum period of 2 months prior to use.

      3.0 Test Set Up

      The test is set up by first mixing the test or control substrates into the sediment inoculum, then mixing in seawater to make a pourable slurry. The slurry is then poured into serum bottles, which are then flushed with nitrogen and sealed.

      3.1. Mixing Procedure

      Because base fluids are strongly hydrophobic and do not readily mix with sediments, care must be taken to ensure base fluids are thoroughly homogenized within the sediment. All concentrations are weight-to-weight comparisons (mg of base fluid to kg of dry control sediment). Sediment and base fluid mixing will be accomplished by using the following method.

      3.1.1. Determine the wet to dry weight ratio for the control sediment by weighing approximately 10 sub-samples of approximately 1 g each of the screened and homogenized wet sediment into tared aluminum weigh pans. Dry sediment at 105 degC for 18-24 h. Remove the dried sediments and cool in a desiccator. Repeat the drying, cooling, and weighing cycle until a constant weight is achieved (within 4% of previous weight). Re-weigh the samples to determine the dry weight. Calculate the mean wet and dry weights of the 10 sub samples and determine the wet/dry ratio by dividing the mean wet weight by the mean dry weight using Equation 5-1. This is required to determine the weight of wet sediment needed to prepare the test samples.

      GRAPHIC TIFF OMITTED TR18MY12.008

      3.1.2. Determine the density (g/ml) of the wet sediment. This will be used to determine total volume of wet sediment needed for the various test treatments. One method is to tare a 5 ml graduated cylinder and add about 5 ml of homogenized sediment. Carefully record the volume then weigh this volume of sediment. Repeat this a total of three times. To determine the wet sediment density, divide the weight by volume per the following formula:

      GRAPHIC TIFF OMITTED TR18MY12.009

      3.1.3. Determine the amount of base fluid to be spiked into wet sediment in order to obtain the desired initial base fluid concentration of 2,000 mg carbon/kg dry weight. An amount of wet sediment that is the equivalent of 30 g of dry sediment will be added to each bottle. A typical procedure is to prepare enough sediment for 8 serum bottles (3 bottles to be sacrificed at the start of the test, 4 bottles incubated for headspace analysis, and enough extra sediment for 2 extra bottles). Extra sediment is needed because some of the sediment will remain coated onto the mixing bowl and utensils. Experience with this test may indicate that preparing larger volumes of spiked sediment is a useful practice, then the following calculations should be adjusted accordingly.

    19. Determine the total weight of dry sediment needed to add 30 g dry sediment to 8 bottles. If more bottles are used then the calculations should be modified accordingly. For example:

      GRAPHIC TIFF OMITTED TR18MY12.010

    20. Determine the weight of base fluid, in terms of carbon, needed to obtain a final base fluid concentration of 2,000 mg carbon/kg dry weight. For example:

      GRAPHIC TIFF OMITTED TR18MY12.011

    21. i. Convert from mg of carbon to mg of base fluid. This calculation will depend on the % fraction of carbon present in the molecular structure of each base fluid. For the control fluids, ethyl oleate is composed of 77.3% carbon, hexadecene is composed of 85.7% carbon, and squalane is composed of 85.3% carbon. The carbon fraction of each base fluid should be supplied by the manufacturer or determined before use. ASTM D5291-96 or equivalent will be used to determine composition of fluid.

      ii. To calculate the amount of base fluid to add to the sediment, divide the amount of carbon (480 mg) by the percent fraction of carbon in the fluid.

      iii. For example, the amount of ethyl oleate added to 240 g dry weight sediment can be calculated from the following equation:

      Page 29839

      GRAPHIC TIFF OMITTED TR18MY12.012

      iv. Therefore, add 621 mg of ethyl oleate to 240 g dry weight sediment for a final concentration of 2,000 mg carbon/kg sediment dry weight.

      3.1.4. Mix the calculated amount of base fluid with the appropriate weight of wet sediment.

    22. Use the wet:dry ratio to convert from g sediment dry weight to g sediment wet weight, as follows:

      GRAPHIC TIFF OMITTED TR18MY12.013

    23. i. Weigh the appropriate amount of base fluid (calculated in Section 3.1.3.c) into stainless mixing bowls, tare the vessel weight, then add the wet sediment calculated in Equation 5, and mix with a high shear dispersing impeller for 9 minutes.

      ii. The sediment is now mixed with synthetic sea water to form a slurry that will be transferred into the bottles.

      3.2. Creating Seawater/Sediment Slurry

      Given that the total volume of sediment/sea water slurry in each bottle is to be 75 mL, determine the volume of sea water to add to the wet sediment.

      3.2.1. If each bottle is to contain 30 g dry sediment, calculate the weight, and then the volume, of wet sediment to be added to each bottle.

      GRAPHIC TIFF OMITTED TR18MY12.014

      3.2.4. Convert the wet sediment weight from Equation 6 into a volume using the sediment density.

      GRAPHIC TIFF OMITTED TR18MY12.016

      3.2.5. Determine the amount of sea water to mix with the wet sediment.

      GRAPHIC TIFF OMITTED TR18MY12.017

      Mix sea water thoroughly with wet sediment to form a sediment/

      sea water slurry.

      3.3. Bottling the Sediment Seawater Slurry

      The total volume of sediment/sea water slurry in each bottle is to be 75 mL. Convert the volume (mL) of sediment/sea water slurry into a weight (g) using the density of the sediment and the seawater.

      Page 29840

      GRAPHIC TIFF OMITTED TR18MY12.018

      This should provide each bottle with 30 g dry sediment in a total volume of 75 mL.

      3.3.4. Putting the sediment:seawater slurry in the serum bottles.

    24. Note: The slurry will need to be constantly stirred to keep the sediment suspended.

    25. Place a tared serum bottle on a balance and add the appropriate amount of slurry to the bottle using a funnel. Once the required slurry is in the bottle remove the funnel, add 2-3 drops (25 muL) of a 1 gram/L resazurin dye stock solution. Cap the bottle with a butyl rubber stopper (Bellco Glass, Part 2048-11800) and crimp with an aluminum seal (Bellco Glass Part 2048-11020).

    26. Using a plastic tube with a (23-gauge, 1-inch long) needle attached to one side and a nitrogen source to the other, puncture the serum cap with the needle. Puncture the serum cap again with a second needle to sparge the bottle's headspace of residual air for two minutes. The nitrogen should be flowing at no more than 100 mL/

      min to encourage gentle displacement of oxygenated air with nitrogen. Faster nitrogen flow rates would cause mixing and complete oxygen removal would take much longer. Remove the nitrogen needle first to avoid any initial pressure problems. The second (vent) needle should be removed within 30 seconds of removing the nitrogen needle.

    27. Triplicate blank test systems are prepared, with similar quantities of sediment and seawater without any base fluid. Incubate in the dark at a constant temperature of 29 1 degC.

    28. Record the test temperature. The test duration is dependent on base fluid performance, but at a maximum should be no more than 275 days. Stop the test after all base fluids have achieved a plateau of gas production. At termination, base fluid concentrations can be verified in the terminated samples by extraction and GC analysis according to Section 8.

      4.0. Concentration Verification Chemical Analyses

    29. Because of the difficulty of homogeneously mixing base fluid with sediment, it is important to demonstrate that the base fluid is evenly mixed within the sediment sea water slurry that was added to each bottle. Of the seven serum bottles set up for each test or control condition, three are randomly selected for concentration verification analyses. These should be immediately placed at 4 degC and a sample of sediment from each bottle should be analyzed for base fluid content as soon as possible. The coefficient of variation (CV) for the replicate samples must be less than 20%. The results should show recovery of at least 70% of the spiked base fluid. Use an appropriate analytical procedure described in Section 8 to perform the extractions and analyses. If any set of sediments fail the criteria for concentration verification, then the corrective action for that set of sediments is also outlined in Section 8.

    30. The nominal concentrations and the measured concentrations from the three bottles selected for concentration verification should be reported for the initial test concentrations. The coefficient of variation (CV) for the replicate samples must be less than 20%. If base fluid content results are not within the 20% CV limit, the test must be stopped and restarted with adequately mixed sediment.

      5.0. Gas Monitoring Procedures

      Biodegradation is measured by total gas as specified in ISO 11734:1995. Methane production can also be tracked and is described in Section 7.

      5.1. Total Gas Monitoring Procedures

      Bottles should be brought to room temperature before readings are taken. a. The bottles are observed to confirm that the resazurin has not oxidized to pink or blue. Total gas production in the culture bottles should be measured using a pressure transducer (one source is Biotech International). The pressure readings from test and control cultures are evaluated against a calibration curve created by analyzing the pressure created by known additions of gas to bottles established identically to the culture bottles. Bottles used for the standard curve contain 75 mL of water, and are sealed with the same rubber septa and crimp cap seals used for the bottles containing sediment. After the bottles used in the standard curve have been sealed, a syringe needle inserted through the septa is used to equilibrate the pressure inside the bottles to the outside atmosphere. The syringe needle is removed and known volumes of air are injected into the headspace of the bottles. Pressure readings provide a standard curve relating the volume of gas injected into the bottles and headspace pressure. No less than three points may be used to generate the standard curve. A typical standard curve may use 0, 1, 5, 10, 20 and 40 mL of gas added to the standard curve bottles.

    31. The room temperature and barometric pressure (to two digits) should be recorded at the time of sampling. One option for the barometer is Fisher Part 02-400 or 02-401. Gas production by the sediment is expressed in terms of the volume (mL) of gas at standard temperature (0 degC = 273 degK) and pressure (1 atm = 30 inches of Hg) using Eq. 16.

      GRAPHIC TIFF OMITTED TR18MY12.020

      Where:

      V2 = Volume of gas production at standard temperature and pressure

      P1 = Barometric pressure on day of sampling (inches of Hg)

      V1 = Volume of gas measured on day of sampling (mL)

      T2 = Standard temperature = 273 degK

      T1 = Temperature on day of sampling (degC + 273 = degK)

      P2 = Standard pressure = 30 inches Hg

    32. An estimate can be made of the total volume of anaerobic gas that will be produced in the bottles. The gas production measured for each base fluid can be expressed as a percent of predicted total anaerobic gas production.

      5.1.1. Calculate the total amount of carbon in the form of the base fluid present in each bottle.

    33. Each bottle is to contain 30 g dry weight sediment. The base fluid concentration is 2,000 mg carbon/kg dry weight sediment. Therefore:

      Page 29841

      GRAPHIC TIFF OMITTED TR18MY12.021

      5.1.2. Theory states that anaerobic microorganisms will convert 1 mole of carbon substrate into 1 mole of total anaerobic gas production.

    34. Calculate the number of moles of carbon in each bottle.

    35. The molecular weight of carbon is 12 (i.e., 1 mole of carbon = 12 g). Therefore, the number of moles of carbon in each bottle can be calculated.

      GRAPHIC TIFF OMITTED TR18MY12.022

      5.1.3. Calculate the predicted volume of anaerobic gas.

      One mole of gas equals 22.4 L (at standard temperature and pressure), therefore,

      GRAPHIC TIFF OMITTED TR18MY12.023

      5.2. Gas Venting

    36. If the pressure in the serum bottle is too great for the pressure transducer or syringe, some of the excess gas must be wasted. The best method to do this is to vent the excess gas right after measurement. To do this, remove the barrel from a 10-mL syringe and fill it \1/3\ full with water. This is then inserted into the bottle through the stopper using a small diameter (high gauge) needle. The excess pressure is allowed to vent through the water until the bubbles stop. This allows equalization of the pressure inside the bottle to atmospheric without introducing oxygen. The amount of gas vented (which is equal to the volume determined that day) must be kept track of each time the bottles are vented. A simple way to do this in a spreadsheet format is to have a separate column in which cumulative vented gas is tabulated. Each time the volume of gas in the cultures is analyzed, the total gas produced is equal to the gas in the culture at that time plus the total of the vented gas.

    37. To keep track of the methane lost in the venting procedure, multiply the amount of gas vented each time by the corrected % methane determined on that day. The answer gives the volume of methane wasted. This must be added into the cumulative totals similarly to the total gas additions.

      6.0. Test Acceptability and Interpretation

      6.1. Test Acceptability

      At day 275 or when gas production has plateaued, whichever is first, the controls are evaluated to confirm that the test has been performed appropriately. In order for this modification of the closed bottle biodegradation test to be considered acceptable, all the controls must meet the biodegradation levels indicated in Table 1. The intermediate control hexadecene must produce at least 30% of the theoretical gas production. This level may be reexamined after two years and more data has been generated.

      Table 1--Test Acceptability Criteria

      ----------------------------------------------------------------------------------------------------------------

      Concentration Percent biodegradability as a function of gas measurement

      ----------------------------------------------------------------------------------------------------------------

      Squalane negative Hexadecene intermediate

      Positive control control control

      ----------------------------------------------------------------------------------------------------------------

      2,000 mg carbon/kg................. >=60% theoretical..... =30% theoretical.

      ----------------------------------------------------------------------------------------------------------------

      6.2 Interpretation

    38. In order for a fluid to pass the closed bottle test, the biodegradation of the base fluid as indicated by the total amount of total gas (or methane) generated once gas production has plateaued (or at the end of 275 days, which ever is first) must be greater than or equal to the volume of gas (or methane) produced by the reference standard (internal elefin or ester).

    39. The method for evaluating the data to determine whether a fluid has passed the biodegradation test must use the equations:

      GRAPHIC TIFF OMITTED TR18MY12.024

      Where:

      NAF = Stock base fluid being tested for compliance

      Reference fluid = C16-C18 internal olefin or C12 -C14 or C8 ester reference fluid

      7.0. Methane Measurement

      7.1. Methane Monitoring Procedures

    40. The use of total gas production alone may result in an underestimation of the actual metabolism occurring since CO2 is slightly soluble in water. An acceptable alternative method is to monitor methane production and total gas production. This is easily done using GC analysis. A direct injection of headspace gases can be made into a GC using almost any packed or capillary column with an FID detector. Unless volatile fuels or solvents are present in the test material or the inocula, the only component of the headspace gas that can be detected using an FID detector is methane. The percent methane in the headspace gas is determined by comparing the response of the sample injections to the response from injections of known percent methane standards. The percent methane is corrected for water vapor saturation using Eq. 21 and then converted to a volume of dry methane using Eq. 22.

      Page 29842

      GRAPHIC TIFF OMITTED TR18MY12.025

      Where:

      D = The density of water vapor at saturation (g/m\3\, can be found in CRC Handbook of Chemistry and Physics) for the temperature of sampling.

      GRAPHIC TIFF OMITTED TR18MY12.026

      Where:

      VCH4 = Volume of methane in the bottle

      S = Volume of excess gas production (measured with a pressure transducer)

      V = Volume of the headspace in the culture bottle (total volume--

      liquid phase)

      P = Barometric pressure (mm Hg, measured with barometer)

      T = Temperature (degC)

      Pw = Vapor pressure of water at T (mm Hg, can be found in CRC Handbook of Chemistry and Physics)

      CH4 = % methane in headspace gas (after correction for water vapor)

    41. The total volume of serum bottles sold as 125 mL bottles (Wheaton) is 154.8 mL.

    42. The volumes of methane produced are then compared to the volumes of methane in the controls to determine if a significant inhibition of methane production or a significant increase of methane production has been observed. Effective statistical analyses are important, as variability in the results is common due to the heterogeneity of the inoculum's source. It is also common to observe that the timing of the initiation of culture activity is not equal in all of the cultures. Expect a great variability over the period when the cultures are active, some replicates will start sooner than others, but all of the replicates should eventually reach similar levels of base fluid degradation and methane production.

      7.2. Expected Methane Production Calculations

    43. The amount of methane expected can be calculated using the equation of Symons and Buswell (Eq. 23). In the case of complete mineralization, all of the carbon will appear as wither CO2 or CH4, thus the total moles of gas produced will be equal to the total moles of carbon in the parent molecule. The use of the Buswell equation allows you to calculate the effects the redox potential will have on the distribution of the products in methanogenic cultures. More reduced electron donors will allow the production of more methane, while more oxidized electron donors will cause a production of more carbon dioxide.

      GRAPHIC TIFF OMITTED TR18MY12.027

    44. An example calculation of the expected methane volume in a culture fed 2,000 mg/kg hexadecene is as follows. The application of Symons and Buswell's equation reveals that hexadecene (C16H32) will yield 4 moles of CO2 and 12 moles of CH4. Assuming 30 g of dry sediment are added to the bottles with 2,334 mg hexadecene/kg dry sediment (i.e., equivalent to 2,000 mg carbon/kg dry sediment) the calculation is as follows.

      GRAPHIC TIFF OMITTED TR18MY12.028

    45. By subtracting the average amount of methane in control bottles from the test bottles and then dividing by the expected volume an evaluation of the completion of the process may be conducted.

      8.0. Concentration Verification Analysis

      The Concentration Verification analysis is required at the beginning of the test to ensure homogeneity and confirm that the required amount of fluid was delivered to the sediments at the start of the test.

      8.1. Three samples per fluid need to be analyzed and achieve =70% to 10 to C13 n-alkanes and corresponding target aromatics.

      * * * * *

      11.5.4.2 Asphaltene crude oils with API gravity '' before ``11-14'' in Table 1.

      Appendix 8 to Subpart A of Part 435--Reference C16-

      C18 Internal Olefin Drilling Fluid Formulation

      * * * * *

      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 EPA Method 1644: ``Method for Conducting a Sediment Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling Muds'' after sediment preparation procedures specified in EPA Method 1646, which are published as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See Sec. 435.11(ee) and (uu).

      * * * * *

      Subpart D--Coastal Subcategory

      0

      30. Section 435.41 is amended:

      0

    46. By revising paragraph (d).

      0

    47. By revising paragraph (e).

      0

    48. By revising paragraph (k).

      0

    49. By revising paragraph (m)(2).

      0

    50. By revising paragraph (q).

      0

    51. By revising paragraph (r).

      0

    52. By amending paragraph (w) to remove ``LC5'' and add in its place ``LC50''.

      0

    53. By revising paragraph (y).

      0

    54. By revising paragraph (ee).

      0

    55. By revising paragraph (ff).

      0

    56. By adding paragraph (mm).

      Sec. 435.41 Special 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as appendices to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph (mm) of this section.

      (ff) Static sheen test means the standard test procedure that has been

      Page 29846

      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 as an appendix to Subpart A of this part and in ``Analytic Methods for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. 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-11-004, that compiles analytic methods for this category. 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. This method may be obtained at http://water.epa.gov/scitech/methods/cwa/index.cfm.

      0

      31. 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).

      * * * * *

      0

      32. In Sec. 435.43:

      0

    57. Remove ``LC5'' and add in its place ``LC50'' in the table.

      0

    58. Footnotes 2 and 4 to the table 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).

      * * * * *

      \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).

      * * * * *

      0

      33. 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).

      * * * * *

      \2\ As determined by the static sheen test. See Sec. 435.41(ff).

      * * * * *

      0

      34. In Sec. 435.45:

      0

    59. Remove ``LC5'' and add in its place ``LC50''in the table.

      0

    60. Footnotes 2 and 4 to the table are revised to read as follows:

      Sec. 435.45 Standards of performance for new sources (NSPS).

      * * * * *

      \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. 2012-10210 Filed 5-17-12; 8:45 am

      BILLING CODE 6560-50-P