99-33627. Guidelines Establishing Test Procedures for the Analysis of Pollutants; Available Cyanide in Water  

  • [Federal Register Volume 64, Number 250 (Thursday, December 30, 1999)]
    [Rules and Regulations]
    [Pages 73414-73423]
    From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
    [FR Doc No: 99-33627]
    
    
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    ENVIRONMENTAL PROTECTION AGENCY
    
    40 CFR Part 136
    
    [FRL-6478-1]
    RIN 2040-AC76
    
    
    Guidelines Establishing Test Procedures for the Analysis of 
    Pollutants; Available Cyanide in Water
    
    AGENCY: Environmental Protection Agency (EPA).
    
    ACTION: Final rule.
    
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    SUMMARY: This final rule amends the ``Guidelines Establishing Test 
    Procedures for the Analysis of Pollutants'' under section 304(h) of the 
    Clean Water Act by adding Method OIA-1677: Available Cyanide by Flow 
    Injection, Ligand Exchange, and Amperometry (hereafter Method OIA-
    1677). Method OIA-1677 employs flow injection analysis (FIA) to measure 
    ``available cyanide.'' Method OIA-1677 is an additional test procedure 
    for measuring the same cyanide species as are measured by currently 
    approved methods for cyanide amenable to chlorination (CATC). In some 
    matrices, CATC methods are subject to test interferences. EPA is 
    approving Method OIA-1677 because it is more specific for available 
    cyanide, is more rapid, measures cyanide at lower concentrations, 
    offers improved safety, reduces laboratory waste, and is more precise 
    and accurate than currently approved CATC methods.
    
    EFFECTIVE DATE: This regulation is effective on January 31, 2000. For 
    judicial review purposes, this final rule is promulgated as of 1 p.m. 
    Eastern Standard Time on January 13, 2000 in accordance with 40 CFR 
    23.2.
        The incorporation by reference of Method OIA-1677 listed in the 
    rule is approved by the Director of the Federal Register January 31, 
    2000.
    
    ADDRESSES: Copies of the public comments received, EPA responses, and 
    all other supporting documents (including references included in this 
    document) are available for review at the U.S. Environmental Protection 
    Agency, Water Docket, 401 M Street SW., Washington, DC 20460. For 
    access to docket materials, call 202-260-3027 on Monday through Friday, 
    excluding Federal holidays, between 9:00 a.m. and 3:30 p.m. Eastern 
    Time for an appointment.
        Copies of Method OIA-1677 are available from the National Technical 
    Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 
    22161, (703) 605-6000 or (800) 553-6847; or from ALPKEM, Box 9010, 
    College Station, TX 77842-9010. The NTIS publication number is PB99-
    132011.
        An electronic version of Method OIA-1677 is also available via the 
    Internet at http://www.epa.gov/OST/Methods.
    
    FOR FURTHER INFORMATION CONTACT: For information regarding Method OIA-
    1677, contact Maria Gomez-Taylor, Ph.D., Engineering and Analysis 
    Division (4303), USEPA Office of Science and Technology, 401 M Street, 
    SW., Washington, DC 20460, or call (202) 260-1639.
    
    SUPPLEMENTARY INFORMATION:
    
    Potentially Regulated Entities
    
        EPA Regions, as well as States, Territories and Tribes authorized 
    to implement the National Pollutant Discharge Elimination System 
    (NPDES) program, issue permits that comply with the technology-based 
    and water quality-based requirements of the Clean Water Act. In doing 
    so, the NPDES permitting authority, including authorized States, 
    Territories, and Tribes, make a number of discretionary choices 
    associated with permit writing, including the selection
    
    [[Page 73415]]
    
    of pollutants to be measured and, in many cases, limited in permits. If 
    EPA has ``approved'' (i.e., promulgated through rulemaking) 
    standardized testing procedures for a given pollutant, the NPDES permit 
    must specify one of the approved testing procedures or an approved 
    alternate test procedure. Permitting authorities may, at their 
    discretion, require the use of any method approved at 40 CFR part 136 
    in the permits they issue. Therefore, dischargers with NPDES permits 
    could be affected by the standardization of testing procedures in this 
    rulemaking because NPDES permits may incorporate the testing procedures 
    in today's rulemaking. In addition, when a State, Territory, or 
    authorized Tribe provides certification of Federal licenses under Clean 
    Water Act section 401, States, Territories and Tribes are directed to 
    use the standardized testing procedures. Categories and entities that 
    may ultimately be affected include:
    
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                                                 Examples of potentially
                    Category                        regulated entities
    ------------------------------------------------------------------------
    Regional, State and Territorial          States, Territories, and Tribes
     Governments and Indian Tribes.           authorized to administer the
                                              NPDES permitting program;
                                              States, Territories, and
                                              Tribes providing certification
                                              under Clean Water Act section
                                              401; Governmental NPDES
                                              permittees.
    Industry...............................  Industrial NPDES permittees.
    Municipalities.........................  Publicly-owned treatment works
                                              with NPDES permits.
    ------------------------------------------------------------------------
    
        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 the types of entities that EPA is now aware 
    could potentially be affected by this action. Other types of entities 
    not listed in the table could also be affected. If you have questions 
    regarding the applicability of this action to a particular entity, 
    consult the person listed in the preceding FOR FURTHER INFORMATION 
    CONTACT section.
    
    Outline of Preamble
    
    I. Authority
    II. Summary of the Final Rule
        A. Introduction
        B. Summary of Method OIA-1677
        C. Comparison of Method OIA-1677 to Current Methods
        D. Quality Control
        E. Performance-Based Measurement System
    III. Improvements and Changes to Method OIA-1677 Since Proposal
    IV. Public Participation and Response to Comments
        A. Definition of Cyanide
        B. Method Detection Limit
        C. Regulatory Compliance Implications of Method OIA-1677
        D. Proprietary Reagents
        E. Cyanide Species Measured
        F. Sample Pretreatment Issues
        G. Interferences
        H. Alternative Methods
        I. Data Quality
        J. Laboratory Safety
        K. Miscellaneous
    V. References
    VI. Regulatory Requirements
        A. Executive Order 12866
        B. Unfunded Mandates Reform Act
        C. Regulatory Flexibility Act (RFA), as amended by the Small 
    Business Regulatory Enforcement Fairness Act of 1996 (SBREFA), 5 
    U.S.C. 601 et seq.
        D. Paperwork Reduction Act
        E. Submission to Congress and the General Accounting Office
        F. National Technology Transfer and Advancement Act
        G. Executive Order 13045
        H. Executive Order 13132
        I. Executive Order 13084
    
    I. Authority
    
        EPA promulgates today's regulation pursuant to the authority of 
    sections 301, 304(h), 307, and 501(a) of the Clean Water Act (CWA) or 
    the ``Act,'' 33 U.S.C. 1314(h), 1317, and 1361(a). Section 301 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 
    applications 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 his (her) function under this Act.'' EPA 
    publishes CWA analytical methods regulations at 40 CFR part 136. The 
    Administrator also has made these test procedures applicable to 
    monitoring and reporting of NPDES permits (40 CFR part 122, sections 
    122.21, 122.41, 122.44, and 123.25), and implementation of the 
    pretreatment standards issued under section 307 of the Act (40 CFR part 
    403, sections 403.10 and 402.12).
    
    II. Summary of the Final Rule
    
    A. Introduction
    
        Today's action makes available at 40 CFR part 136 an additional 
    test procedure for measurement of available cyanide. Currently approved 
    methods for measurement of available cyanide are based on sample 
    chlorination. Method OIA-1677 uses a flow injection/ligand exchange 
    technique to measure available cyanide. Although Method OIA-1677 and 
    chlorination methods both measure available cyanide, it is possible 
    that the results produced by the two techniques will vary slightly, as 
    detailed in the proposed rule (63 FR 36809, July 7, 1998). EPA offers 
    Method OIA-1677 as another testing procedure for several purposes, 
    including permit applications and compliance monitoring under the NPDES 
    program under CWA section 402; ambient water quality monitoring; CWA 
    section 401 certifications; development of new effluent limitations 
    guidelines, pretreatment standards, and new source performance 
    standards; and for general laboratory use.
        This rulemaking does not repeal any of the currently approved 
    methods that test for available cyanide. For an NPDES permit, the 
    permitting authority can decide which method is appropriate for the 
    specific NPDES permit based on the circumstances of the particular 
    effluent measured. If the permitting authority does not specify the 
    method to be used for the determination of available cyanide, a 
    discharger would be able to use Method OIA-1677 or any of the presently 
    approved cyanide amenable to chlorination (CATC) methods.
    
    B. Summary of Method OIA-1677
    
        Method OIA-1677 is divided into two parts: sample pretreatment and 
    cyanide quantification via amperometric detection. In the sample 
    pretreatment step, ligand-exchange reagents are added to a 100-mL 
    sample. The ligand-exchange reagents displace cyanide ions 
    (CN-) from weak and intermediate strength metallo-cyanide 
    complexes.
        In the flow-injection analysis system, a 200-L aliquot of 
    the pretreated sample is injected into the flow injection manifold. The 
    addition of hydrochloric acid converts cyanide ion to hydrogen cyanide 
    (HCN). The hydrogen cyanide diffuses through a membrane into an 
    alkaline receiving solution where it is converted back to cyanide ion 
    (CN-). The amount of cyanide ion in the alkaline receiving 
    solution is measured amperometrically with a silver working electrode, 
    silver/silver chloride reference electrode, and platinum counter 
    electrode at an applied potential of zero volt. The current generated 
    in the cell is proportional to the concentration of cyanide in the 
    original sample, as determined by calibration.
    
    [[Page 73416]]
    
    C. Comparison of Method OIA-1677 to Current Methods
    
        Methods currently approved for determination of available cyanide 
    all test for CATC. Although they represent the best methods available 
    to date, these methods are prone to matrix interference problems. EPA 
    considers Method OIA-1677 to be a significant addition to the suite of 
    analytical testing procedures for available cyanide because it (1) has 
    greater specificity for cyanide in matrices where interferences have 
    been encountered using currently approved methods; (2) has improved 
    precision and accuracy compared to currently approved CATC cyanide 
    methods; (3) measures available cyanide at lower concentrations; (4) 
    offers improved analyst safety; (5) shortens sample analysis time; and 
    (6) reduces laboratory waste.
        Method OIA-1677 is not subject to known interferences from organic 
    species. The flow-injection technique of Method OIA-1677 excludes known 
    interferences, except sulfide. Sulfide is eliminated by treating the 
    sample with lead carbonate and removing the insoluble lead sulfide by 
    filtration prior to introduction of the sample to the amperometric cell 
    used for cyanide detection.
        Method OIA-1677 was tested against and compared to two existing 
    cyanide methods: EPA Method 335.1, an EPA-approved CATC method, and 
    Standard Method (SM) 4500 CN-I, a weak-acid dissociable 
    (WAD) cyanide method. Comparative recovery and precision data were 
    generated from simple metallo-cyanide species in reagent water. 
    Recovery and precision of each method was comparable for the easily 
    dissociable cyanide species. Results of these tests were included in 
    the docket at proposal (63 FR 36809, July 7, 1998). Method OIA-1677 
    showed superior precision and recoveries of mercury cyanide complexes.
        While EPA Method 335.1 does not specify a method detection limit, 
    colorimetric detection is ``sensitive'' to approximately 5 g/
    L. The method detection limit (MDL), as determined in a multi-
    laboratory study using the procedures described at 40 CFR part 136, 
    appendix B, is 0.5 g/L for Method OIA-1677.
        Method OIA-1677 offers improved analyst safety for two reasons. The 
    first reason is the reduced generation of hydrogen cyanide gas, a 
    highly toxic compound. Although the proposed flow-injection analysis 
    (FIA) method and currently approved CATC methods all generate HCN, the 
    currently approved methods generate a larger quantity of gas during 
    distillation in an open distillation system. As such, extra care is 
    necessary to prevent accidental release of HCN into the laboratory 
    atmosphere. Method OIA-1677 possesses an advantage because it tests a 
    much smaller sample and, therefore, generates significantly less HCN 
    than currently approved methods. In addition, the gas is contained in a 
    closed system with little possibility for release. The second safety 
    improvement is the reduced use of hazardous substances. Currently 
    approved CATC methods require use of hazardous substances in the 
    distillation and color developing processes. These hazardous substances 
    include hydrochloric acid, pyridine, barbituric acid, chloramine-T, and 
    pyrazolone. Method OIA-1677 requires only hydrochloric acid and at a 
    much lower concentration than used in CATC procedures.
        Method OIA-1677 offers a reduced analysis time, which should 
    increase sample throughput in the laboratory. Method OIA-1677 uses 
    automated mixing of the sample with hydrochloric acid and exposure to 
    the gas diffusion membrane to determine the sample concentration. This 
    process takes approximately two minutes per sample. As a comparison, 
    EPA Method 335.1 requires a one-hour distillation procedure plus the 
    time necessary to add and develop the sample color to determine the 
    presence of cyanide.
        Less laboratory waste is generated in Method 1667 because it 
    requires a much smaller sample size for testing. EPA Method 335.1 
    requires handling a sample size of 500 mL for distillation. Method OIA-
    1677 requires the addition of the ligand exchange reagents to 100 mL of 
    sample, from which 40 to 250 L are used for analysis. This 
    reduces the amount of both hazardous sample and toxic reagents that 
    must be handled and subsequently disposed.
    
    D. Quality Control
    
        The quality control (QC) in Method OIA-1677 is more extensive than 
    the QC in currently approved methods for CATC. Method OIA-1677 contains 
    all of the standardized QC tests proposed in EPA's streamlining 
    initiative (62 FR 14976, March 28, 1997) and used in the 40 CFR part 
    136, appendix A methods. An initial demonstration of laboratory 
    capability is required and consists of (1) an MDL study to demonstrate 
    that the laboratory is able to achieve the MDL and minimum level of 
    quantification (ML) specified in Method OIA-1677; and (2) an initial 
    precision and recovery (IPR) test, consisting of the analysis of four 
    reagent water samples spiked with the reference standard, to 
    demonstrate the laboratory's ability to generate acceptable precision 
    and recovery. An important component of these and other QC tests 
    required in Method OIA-1677 is the use of mercuric cyanide 
    (Hg(CN)2) as the reference standard for spiking. Mercuric 
    cyanide was chosen because it is fully recovered in Method OIA-1677 and 
    weak-acid dissociable (WAD) methods, whereas mercuric cyanide is only 
    partially recovered in the CATC method. Therefore, mercuric cyanide 
    demonstrates the ability of the ligand-exchange reagents to liberate 
    cyanide from moderately strong metal-cyano complexes. Method OIA-1677 
    requires the use of standards of known composition and purity, which 
    facilitates more accurate determination of recovery and precision and 
    minimizes variability that may be introduced from spiking substances of 
    unknown or indeterminate purity.
        Ongoing QC consists of the following tests that would need to 
    accompany each analytical batch, i.e., a set of 10 samples or less 
    pretreated at the same time:
         Verification of calibration of the flow injection 
    analysis/amperometric detection system, to verify that instrument 
    response has not deviated significantly from that obtained during 
    calibration.
         Analysis of a matrix spike (MS) and matrix spike duplicate 
    (MSD) to demonstrate method accuracy and precision and to monitor 
    matrix interferences. Hg(CN)2 is the reference standard used 
    for spiking.
         Analysis of a laboratory blank to demonstrate freedom from 
    contamination.
         Analysis of a laboratory control sample to demonstrate 
    that the method remains under control.
        Method OIA-1677 contains QC acceptance criteria for all QC tests. 
    Compliance with these criteria allows a data user to evaluate the 
    quality of the results. This increases the reliability of results and 
    provides a means for laboratories and data users to monitor analytical 
    performance, thereby providing a basis for sound, defensible data.
    
    E. Performance-Based Measurement System
    
        On March 28, 1997, EPA proposed a rule (62 FR 14976) to streamline 
    approval procedures and use of analytic methods in water programs 
    through a performance-based approach to environmental measurements. On 
    October 7, 1997, EPA published a Notice of the Agency's intent to 
    implement a Performance Based Measurement System (PBMS) in all
    
    [[Page 73417]]
    
    media programs to the extent feasible (62 FR 52098). EPA's water 
    program offices are developing plans to implement PBMS. Although EPA 
    has not yet promulgated a final rule to implement PBMS in water 
    programs, Method OIA-1677 incorporates the QA and QC acceptance 
    criteria to be used as a basis for assessment of method performance. 
    When PBMS is in place, Method OIA-1677 could serve as a reference 
    method for demonstrating equivalency for subsequent modifications to 
    the method.
        The analyst has flexibility to modify the Method provided all 
    performance criteria are met. Demonstrating equivalency involves two 
    sets of tests, one set with reference standards and the other with the 
    sample matrix. In addition, if the detection limit would be affected by 
    the modification, performance of an MDL study would be required to 
    demonstrate that the modified procedure could achieve an MDL less than 
    or equal to the MDL in Method OIA-1677 or, for those instances in which 
    the regulatory compliance limit is greater than the ML in the method, 
    one-third the regulatory compliance limit. (For a discussion of these 
    levels, see the streamlining proposal (62 FR 14976, March 28, 1997).)
    
    III. Improvements and Changes to Method OIA-1677 Since Proposal
    
        EPA has revised Method OIA-1677 based on comments received on the 
    proposal (63 FR 36809, July 7, 1998). Minor changes were made to 
    correct typographical errors and for clarification:
         Section 4.5 was reworded to clarify how to mitigate 
    sulfide ion interference.
         Potassium nickel (II) cyanide, a quality control reagent 
    was added as section 7.5.
         Mercury (II) cyanide stock solution (section 7.12.1) 
    mixing directions were rewritten to better explain the steps.
         Section 8.2.1 was revised to require that samples that 
    contain particulate matter be filtered prior to sulfide removal and 
    that the particulate matter be recombined with the treated filtrate 
    prior to shipment to the laboratory. This procedure is necessary to 
    assure that cyanide associated with particulate matter will be included 
    in the measurement.
         Laboratory control sample (LCS) of the mercury (II) 
    cyanide stock solution was described more concisely.
         A note was added to section 11 to explain ligand-exchange 
    reagents and their use.
         Reference materials were updated in section 15.
         In Table 2, units were corrected from mg/L to g/
    mL CN-.
         A definition for ``discharge'' was added under section 
    18.2.
         The sections on Pollution Prevention and Waste Management 
    were separated and expanded.
         Section 12.2 was reworded to clarify the reporting of 
    analytical results.
    
    IV. Public Participation and Response to Comments
    
        EPA proposed Method OIA-1677 for use on July 7, 1998 (63 FR 36809). 
    The public comment period closed on September 8, 1998. Significant 
    comments are summarized below, along with EPA's responses. To the 
    extent practicable, the comments have been categorized by subject. 
    Detailed comments and their accompanying responses are included in the 
    Docket for today's final rule.
        EPA thanks commenters for constructive suggestions. EPA believes 
    that the version of Method OIA-1677 promulgated today will provide 
    reliable data for compliance monitoring.
    
    A. Definition of Cyanide
    
        Comment: The endorsement by EPA of yet another operational method, 
    in this case what its developers term ``available cyanide,'' does not 
    resolve the confusion that exists regarding the appropriateness of the 
    various cyanide measurements for discharge permits and water quality 
    assessments.
        Response: EPA explained use of the term ``available cyanide'' in 
    the preamble to the proposal of Method OIA-1677. The term ``available 
    cyanide'' reflects that it is the cyanide species available for 
    dissociation that is measured by Method OIA-1677. The same cyanide 
    species are measured by the CATC and WAD methods. In today's document, 
    EPA further clarifies that ``available'' cyanide includes ``cyanide 
    amenable to chlorination'' and ``weak-acid dissociable'' cyanides. EPA 
    continues to use the term ``total cyanide'' for cyanides determined 
    after total distillation. The reason that a change to ``available'' 
    cyanide was necessary is that the chlorination reaction used in methods 
    for ``cyanide amenable to chlorination'' is not used in Method OIA-
    1677. The term ``weak-acid dissociable'' (WAD) cyanide was considered 
    but not used in anticipation that future methods could use technologies 
    other than weak-acid dissociation.
    
    B. Method Detection Limit
    
        Comment: If EPA wishes to expand the use of the method detection 
    limit (MDL) approach for the new purpose of deriving a detection level 
    for Method OIA-1677, the Administrative Procedure Act (APA) demands 
    that it provide the public an opportunity to review and comment on the 
    justification for that decision.
        Response: EPA has used the MDL procedure, as described at 40 CFR 
    part 136, appendix B, for the purpose of deriving detection limits in 
    analytical methods for the past 20 years. Use of the MDL procedure for 
    this purpose is therefore not new. By proposing Method OIA-1677 and 
    including the MDL therein, EPA provided the public the opportunity for 
    review and comment on the MDL in Method OIA-1677 and the data that 
    support this MDL estimate.
        EPA has used the MDL successfully for estimating the lowest level 
    at which a substance can be detected since the peer-reviewed article on 
    the MDL was published in 1980 (Environmental Science and Technology 15 
    1426-1435). The MDL procedure is subjected to public comment with every 
    MDL that EPA publishes in nearly every method proposed in the Federal 
    Register for use in EPA's various programs. The MDL procedure is 
    referenced in those methods. The MDL procedure has widespread 
    acceptance and use throughout the analytical community. No other 
    detection or quantitation limit procedure or concept has achieved this 
    level of acceptance and use.
        Comment: Effluent limitations should never be imposed in an 
    enforceable manner below concentrations at which accurate and 
    consistent measurement is possible. EPA must adequately justify the 
    manner in which it proposes to derive detection and quantification 
    levels. EPA has failed to justify its proposal and to allow for public 
    comment.
        Response: EPA proposed to approve Method OIA-1677 as an additional 
    test procedure for use in its water programs. This new analytical 
    method is more sensitive than currently approved methods for the 
    determination of available cyanide and, therefore, EPA believes that 
    this method is suitable for accurate and consistent measurements. The 
    performance of this method was demonstrated through an inter-laboratory 
    validation study. The manner in which EPA derives detection and 
    quantitation levels is through use of the MDL procedure published at 40 
    CFR part 136, appendix B. EPA has used the minimum level of 
    quantitation (ML) in previous rulemakings. The ML is consistent with 
    the limit of quantitation (LOQ) developed by the American Chemical 
    Society. EPA allows comment on the derivation of detection and
    
    [[Page 73418]]
    
    quantification levels through the public comment process every time it 
    proposes a new method. EPA is currently evaluating different approaches 
    to detection and quantification, and may propose one or more alternate 
    approaches in a future rulemaking.
    
    C. Regulatory Compliance Implications of Method OIA-1677
    
        Comment: EPA should clarify that Method OIA-1677 does not indicate 
    that the species measured represent an environmental risk, and that the 
    method should not be used by regulators for measuring the risk 
    associated with particular cyanide species.
        Response: Today's action approves Method OIA-1677 for use in CWA 
    programs because EPA believes that Method OIA-1677 can be used for 
    reliable determination of available cyanide. Analytical methods measure 
    the presence and concentration of pollutants, not risk. In this case, 
    Method OIA-1677 measures dissociable cyanide species.
        Comment: A better measurement of toxicological significance is 
    needed. A regulatory view based on the presence or absence of 
    ``available cyanide'' would not be reflective of environmental 
    conditions that may affect biological organisms. Cyanide species-
    specific methods, such as ion chromatography and the ASTM diffusible 
    cyanide method, provide more scientifically defensible data. EPA and/or 
    instrument manufacturers should pursue development of such techniques 
    as EPA approved methods. For acute toxicity determination, the ``free 
    cyanide'' method by microdiffusion may well be the best approach since 
    it measures HCN and CN species.
        Response: Measurements of toxicological significance and improved 
    tests for toxicological significance are beyond the scope of Method 
    OIA-1677. Method OIA-1677 was developed as an alternative to currently 
    approved methods that measure dissociable cyanide species.
        Regarding cyanide-specific methods such as ion chromatography and 
    diffusible cyanide, EPA believes that these methods may have utility in 
    toxicological testing. However, for testing of wastewaters, methods 
    such as Method OIA-1677 and the total cyanide methods have the 
    advantage that they capture multiple cyanides in a single measurement. 
    These methods are generally less expensive to practice than those 
    methods that resolve the various cyanide forms and species. However, if 
    an instrument manufacturer, discharger, or other interested entity 
    desires to pursue approval of one or more of the cyanide-specific 
    methods, the entity may submit the method under EPA's alternate test 
    procedure program described at 40 CFR part 136.
        Comment: The proposed rule section on regulatory effects is 
    erroneous. Method OIA-1677 will likely produce a result higher than the 
    result produced by a CATC method if a cyanide of nickel, mercury, or 
    silver is present at a high enough concentration. In this instance a 
    permit limit for cyanide would probably be violated.
        EPA must provide specific regulatory language regarding comparison 
    of inconsistent results which impact compliance. EPA recognizes that 
    the new method and the CATC method can produce different results. For 
    example, if a discharger uses the CATC method which shows compliance, 
    while a regulator uses the new method which indicates a violation, EPA 
    suggests that the discharger refer to the preamble language of the 
    proposed rule to convince the regulator that no violation has occurred. 
    As EPA is aware, preamble language is not binding authority as is the 
    actual regulatory language.
        Response: In the proposed rule, EPA stated that interferences in 
    the CATC methods can produce an inflated result for cyanide and that 
    Method OIA-1677 is nearly immune to the interferences that inflate 
    results from CATC methods. Therefore, the result of an analysis using 
    Method OIA-1677 will nearly always be lower, and therefore closer to 
    the true value for cyanide than a result from an analysis using a CATC 
    method. EPA detailed the only exception to this situation as an 
    analysis in which interferences are not present but certain cyanides of 
    nickel, mercury, or silver are present at concentrations greater than 2 
    mg/L. At these concentrations, Method OIA-1677 recovers these cyanides 
    at near 100 percent whereas the CATC methods recover them at 55-85 
    percent, resulting in concentrations that could be 15-45% greater with 
    Method OIA-1677. The scenario described at proposal is very unlikely 
    because the difference in recoveries are not that significant at permit 
    quantities.
        Therefore, in order for a violation to occur, a cyanide of nickel, 
    mercury, or silver would need to be present at greater than 2 mg/L, 
    there would need to be no interferences present, and the permit limit 
    would need to be 2 mg/L or greater. EPA believes that this situation is 
    highly unlikely and believes that, if it ever should occur, it can be 
    handled on a case-by-case basis. Regarding differential use of methods 
    by the permittee and the regulatory authority, EPA notes that permits 
    often specify a particular test method to measure compliance. 
    Compliance with a permit constitutes compliance with the CWA. 
    Dischargers will be held accountable for results from the methods 
    specified in their permits.
    
    D. Proprietary Reagents
    
        Comment: The use of a proprietary reagent as a chelating agent in a 
    significant step in the procedure is an unfortunate precedent in what 
    is supposed to be a scientific process.
        Response: While Method OIA-1677 employs proprietary reagents, the 
    method clearly states that changes to the method (including use of 
    alternative reagents) can be made provided that the analyst 
    demonstrates that the performance achieved is equivalent or superior to 
    the performance of the unmodified method. The process for demonstrating 
    acceptable performance is specified in section 9 of the Method.
        Comment: As presented at the 19th U.S. EPA Conference on Analysis 
    of Pollutants in the Environment (J.R. Sebroski, Bayer Corporation), 
    the proprietary ligand exchange reagents used in the proposed method 
    can suffer from false positive results if the sample is not injected 
    into the flow injection system immediately. For example, after 12 hours 
    residence time in reagent water, the combination of Ligand Exchange 
    Reagent A and B showed an average of 7.57 g/L cyanide.
        Response: The ligand exchange reagents should be tested in NaOH 
    solution, similar to the testing of cyanide samples (pH 12). The method 
    developer has shown that signals due to the reagents are less than the 
    minimum level (ML) of Method OIA-1677 provided the samples are analyzed 
    within 2 hours of reagent addition. Method OIA-1677 has been modified 
    to include statements that specify that the reagents have an 
    approximate lifetime of 6 months after opening, that the reagents 
    should be stored in a refrigerator at 0-4  deg.C, and that samples 
    should be analyzed within 2 hours of adding the ligand-exchange 
    reagents. This is sufficient time for sample preparation even if an 
    auto-sampling system is utilized. Supporting data are included in the 
    docket for the final rule.
        Comment: In order to evaluate the efficiency of a front-end method 
    change or the use of ``equivalent'' ligand exchange reagents, mercury 
    (II) cyanide alone would not be sufficient to demonstrate method 
    equivalency, since this only verifies ligand exchange reagent B and not 
    ligand exchange reagent A which specifically displaces the cyanide 
    species containing nickel. In order to alleviate the problem, several
    
    [[Page 73419]]
    
    ligand exchange reagents from the literature were evaluated for their 
    effectiveness to displace nickel and mercury cyanide species with 
    Method OIA-1677 because the composition of the proprietary reagents is 
    unknown. Our research revealed that tetraethylenepentamine (TEP) and 
    dithizone (diphenylthiocarbazone) were effective at displacing the 
    cyanide species containing nickel and mercury, respectively, up to 400 
    g/L as CN-. The TEP and dithizone combination of 
    ligand exchange reagents did not suffer from any interferences or false 
    positive results, and the reagents have a shelf-life of approximately 6 
    months.
        Response: EPA agrees and has revised Method OIA-1677 to state that 
    a modification to the method must be demonstrated on the cyanide 
    species to which the modification will be applied.
    
    E. Cyanide Species Measured
    
        Comment: While Method OIA-1677 demonstrates some performance 
    characteristics superior to currently available methods (notably the 
    speed of the procedure), cyanide chemistry is too complex to generalize 
    that the proposed method measures the ``same cyanide species'' as the 
    CATC method or that the species measured under either test reflect 
    actual environmental risk.
        Response: Based on the information presented in section II C of the 
    preamble at proposal (63 FR 36810) and data presented in the literature 
    (Environmental Science and Technology, 1995, Vol. 29, 426-430) and at 
    technical conferences (Goldberg, et al.; Goldberg and Clayton), and 
    with the exceptions noted in the preamble at proposal and detailed in a 
    response to Comment IV C above, Method OIA-1677 and the CATC and WAD 
    methods measure the same cyanide species.
        Comment: A fundamental difficulty with the determination of various 
    forms of cyanide is that the analytical methods in use are not defined 
    in terms of specific cyanide species being measured, but rather in 
    terms of whatever the analytical method reports.
        Response: EPA agrees. Method OIA-1677 is actually the first method 
    available that can be defined in terms of the cyanide species being 
    measured because it recovers cyanide completely throughout the 
    analytical range of the Method (2 g/L to 5000 g/L) 
    from the following cyano-species: HCN, CN-, 
    [Zn(CN)4]2-, [Cd(CN)4]2-, 
    [Cu(CN)4]3-, [Ag(CN)2]-, 
    [Ni(CN)4]2-, [Hg(CN)4]2- 
    and Hg(CN)2. In addition, the recoveries are concentration 
    independent, which is not the case with either the CATC or WAD 
    procedures.
        Comment: We believe that the characterization of WAD and CATC 
    analytical methods as deficient is inappropriate because the methods 
    themselves provide operational definitions of cyanide species that 
    comprise weak-acid dissociable cyanide. As such, the fact that the EPA 
    Method OIA-1677 recovers additional metal cyanide complexes does not 
    qualify it as better or more appropriate.
        Response: The WAD and CATC methods are not deficient because they 
    provide an operational definition of cyanide species that comprise 
    weak-acid dissociable cyanide. Rather, the CATC and WAD methods are 
    merely more susceptible to known interferences. The discussion in the 
    preamble of the proposed rule illustrated the problems with the methods 
    that utilize distillation to separate the analyte from potential 
    interferences. Also, Method OIA-1677 does not recover cyanide from 
    additional metal complexes when compared to the WAD and CATC 
    procedures. Rather, it recovers the same metal cyano complexes 
    completely (100%) throughout the analytical range of the method whereas 
    the WAD and CATC procedures recover these species only partially at 
    high concentrations.
    
    F. Sample Pretreatment Issues
    
        Comment: The method currently does not supply any information on 
    the amount of lead carbonate to be used to eliminate sulfide 
    interference.
        Response: The amount of lead carbonate needed depends on the amount 
    of the sulfide interference in each sample. Because the concentration 
    of the sulfide interference is not known in advance, the amount of lead 
    carbonate needed must be determined by the analyst or sampler.
        Comment: Please clarify what preservation must be performed in the 
    field and what preservation can take place back in the laboratory. For 
    example, must the lead acetate paper test, lead carbonate treatment, 
    and filtration for sulfide be performed in the field?
        Response: All preservation must be performed at the time of 
    sampling due to rapid degradation of cyanide in unpreserved samples. If 
    the sample can be transported to a laboratory or other facility within 
    15 minutes of sampling, preservation may be performed in the laboratory 
    or other facility. See footnote 4 to Table II in 40 CFR 136.3 (e) for 
    information on preservation.
        Comment: The procedure for sulfide containing samples is confusing. 
    Is there a concentration below which suspected sulfide ion is not a 
    problem? The method indicates that two samples ``should'' be collected 
    and that both samples ``must'' be analyzed. Is collecting two samples 
    optional or required? When two samples are collected and analyzed, 
    which result should be reported? Or, should both results be reported? 
    If the samples are tested within 24 hours, is one sample sufficient?
        Response: EPA does not know the concentration below which sulfide 
    is not a problem. Collection of two samples is required if sulfide ion 
    is not detected by the lead acetate paper test (See section 8.2.1 of 
    the method). If sulfide ion is detected and removed with lead 
    carbonate, the collection and analysis of a second sample is not 
    required. The result that must be reported is the lower of the two 
    results because the presence of sulfide ion will inflate a result. One 
    sample is sufficient if tested within 24 hours, per footnote 6 of Table 
    II at 40 CFR 136.3(e).
        Comment: Paragraph II F is totally misleading when it states that 
    ``Method OIA-1677 takes approximately two minutes to perform,'' as this 
    time does not include pretreatment (e.g., filtering to eliminate 
    interference from sulfide).
        Response: Pretreatment to remove sulfide interferences is performed 
    at the time of sampling (usually in the field) and the time to perform 
    this pretreatment is not included in analysis time for Method OIA-1677. 
    Analysis of the sample using Method OIA-1677 is performed in the 
    laboratory.
    
    G. Interferences
    
        Comment: The preamble at proposal of Method OIA-1677 states that 
    the Method is not subject to interferences from organic species. While 
    we suspect that the interference that we have encountered may be due to 
    a release of a sulfur-containing or other inorganic gas through the 
    membrane from the acidic flow stream, we cannot be sure that it is not 
    caused by a volatile organic compound.
        Response: EPA does not know if the interference that the commenter 
    is experiencing is a volatile organic compound or a sulfur-containing 
    or other inorganic gas. To date, EPA has not had any reports of 
    interference from organic species. However, one of the developers of 
    Method OIA-1677 speculates that if the electrochemistry at the silver 
    working electrode and the volatility of certain organic species are 
    examined, some interferences from organic species could be encountered. 
    For examples, acetonitrile (CH3CN) could possibly pass 
    through the membrane and would almost certainly aid the oxidation of 
    silver at the
    
    [[Page 73420]]
    
    working potential, producing an analytical signal; low molecular weight 
    aliphatic mercaptans might also pass through the membrane and be active 
    at the working electrode. As a result of these possibilities, EPA 
    believes that it is appropriate to modify its previous statement to 
    state that interference from organic compounds may be possible but that 
    EPA does not have evidence of such organic interferences to date.
        Comment: Use of Method OIA-1677 in the precious metal ore process 
    offers significant improvements over CATC methods with respect to 
    interferences from thiocyanate, sulfide, carbonates, formaldehyde, and 
    metals. While CATC might result in lower cyanide concentrations due to 
    lower metal recoveries, the advantages of Method OIA-1677 with respect 
    to the above interferences should be clarified in the preamble. Mines 
    should be given every opportunity to use the method that provides the 
    best defensible analytical results for those cyanide complexes present 
    in precious metal ore process solutions.
        Response: EPA recognizes the significant advantages of Method OIA-
    1677 over existing methods with respect to interferences. Section IIB-D 
    of the preamble at proposal discussed the interference problems with 
    current methods and the advantage of Method OIA-1677 (63 FR 36811-
    36812). In section IIE of that preamble, EPA stated that use of Method 
    OIA-1677 will likely produce a lower result than the CATC methods 
    because it is nearly interference free. EPA's approval of Method OIA-
    1677 includes its use for the precious metal ore processing industry 
    and for other industries.
    
    H. Alternative Methods
    
        Comment: Any effort funded by EPA and its contractors should result 
    in the technology and methodology that is freely available and fully 
    described via publications of voluntary consensus standards bodies or 
    via scientific literature. Method OIA-1677 is neither of these things. 
    The ASTM method is, by the Rule's own admission, required to take 
    precedence over any method developed by a single vendor by the 
    requirement of the National Technology Transfer and Advancement Act 
    (NTTAA) of 1995.
        Response: EPA did not fund the development of Method OIA-1677. 
    Other than identifying test samples and offering assistance to the 
    method developer on the requirements for validation described in EPA's 
    streamlining proposal (62 FR 13976, March 28, 1997), EPA did not 
    participate in the development of Method OIA-1677. Details of the 
    technology in Method OIA-1677 were published in the scientific 
    literature (Environmental Science and Technology, 1995, 29, 426-430). 
    The NTTAA requires EPA to consider methods from voluntary consensus 
    standard bodies, and to provide a justification if an available method 
    is not selected.
        To date, ASTM has not approved a flow-injection, ligand-exchange 
    method for available cyanide. If ASTM or any other voluntary consensus 
    standard body (VCSB) approves such a method and the quality control and 
    other features of the method meet EPA's requirements, EPA may propose 
    the VCSB method in a future rulemaking.
    
    I. Data Quality
    
        Comment: In 6 of 9 samples in Table 3 on page 36823, the added CN 
    concentrations are 30 times higher than the background concentrations 
    of cyanide in the sample. This ratio seems excessive for calculating 
    spike recoveries.
        Response: Because all samples tested, except the mining tailings 
    pond effluent, had low or undetectable concentrations of cyanide, EPA 
    recommended to the method developer that the range of concentrations 
    tested in the round-robin should encompass the dynamic range of the 
    method (2 to 5000 g/L) so that the efficacy of the ligand-
    exchange reagents in high concentration samples could be evaluated and 
    so that spike recoveries could be determined reliably. Therefore, some 
    samples were spiked at concentrations considerably above the background 
    concentration of cyanide.
        Comment: Method OIA-1677 will not improve data quality.
        Response: Method OIA-1677 is less susceptible to interferences than 
    other methods for available cyanide, including CATC and WAD methods. 
    Therefore, Method OIA-1677 will not subject dischargers to violations 
    for those instances in which an interference with a CATC or WAD method 
    would inflate a cyanide concentration above a permit limit. EPA 
    believes that any method that is less susceptible to interferences and 
    thereby comes closer to determining the true value of a pollutant will 
    improve the quality of analytical data.
    
    J. Laboratory Safety
    
        Comment: EPA promotes the use of mercury cyanide for spiking 
    without any discourse on laboratory safety or disposal problems. 
    Current methods use potassium cyanide for spiking whereby cyanide is 
    the only hazardous substance. However, with mercuric cyanide, there is 
    not only cyanide to consider, but now also mercury. Does it make sense 
    to replace a ``singly'' hazardous compound with a ``doubly'' hazardous 
    compound?
        Response: Mercuric cyanide was chosen because the CATC and WAD 
    methods do not completely recover cyanide from these species, whereas 
    Method OIA-1677 does, and because mercuric cyanide exercises the 
    ligand-exchange reagents used in Method OIA-1677. All methods for 
    determination of cyanide generate cyanide waste and the metal in these 
    wastes is not identified in cyanide determination. Therefore the wastes 
    from all methods must be treated as hazardous unless it is shown that 
    cyanide is not present above disposable levels. Section 14.0 of Method 
    OIA-1677 requires proper handling and disposal of these wastes.
    
    K. Miscellaneous
    
        Comment: To date, there have not been contract laboratories set up 
    to run proposed Method OIA-1677 and there are no commercial 
    laboratories in the U.S. set up to run the new test method.
        Response: There are numerous laboratories in the U.S. that have the 
    instrumentation and can run Method OIA-1677 as written. Nine of these 
    laboratories participated in the round-robin study. Generally, 
    laboratory capacity expands after a method is approved for use in EPA's 
    programs. EPA is not requiring use of Method OIA-1677 in any rules or 
    withdrawing approval for use of any of the methods presently approved. 
    EPA is simply approving another method for use at 40 CFR part 136.
        Comment: The text clearly states that samples with cyanide 
    concentrations higher than 2 mg/L will be reported with a high bias 
    whenever Method OIA-1677 is used. For samples with cyanide 
    concentrations less than 0.2 mg/L, the CATC and Method OIA-1677 methods 
    report approximately the same values. Because most environmental 
    samples have cyanide concentrations less than 0.2 mg/L, e.g., the Safe 
    Drinking Water Act (SDWA) maximum contaminant level (MCL), what is the 
    advantage of Method OIA-1677?
        Response: The bias that occurs with high concentrations of certain 
    cyanides was addressed above in section IV C. Regarding the advantage 
    of Method OIA-1677 over other approved methods for cyanides, EPA has 
    documented through the round-robin validation study that Method OIA-
    1677 offers significant advantages over existing distillation-based 
    methods, including speed, freedom from interferences that
    
    [[Page 73421]]
    
    may occur in highly complex wastewater matrices, and complete recovery 
    of metal cyano complexes.
        Comment: What is the validity of the section III C item 5 of the 
    preamble: ``EPA considers Method OIA-1677 to be a significant addition 
    to the suite of analytical testing procedures for available cyanide 
    because it * * * (5) shortens sample analysis time'' because of the 120 
    second analysis time of Method OIA-1677 versus the 90 second analysis 
    time of another cyanide analysis method (Alpken's Colorimetric RFA)?
        Response: Method OIA-1677 has the shortest analysis time of any 
    method approved for determination of available cyanide. Alpken's 
    Colorimetric RFA method, cited in the comment, is not approved for use 
    at 40 CFR part 136.
    
    V. References
    
        1. Solujic, Lj.; Milosavljevic, E.B.; Hendrix, J.L.; Straka, 
    M.R.; Gallagher, N.P.; ``Cyanide Determination Methods: Distillation 
    vs. Flow Injection Analysis,'' Randol Gold Forum `96, Squaw Creek, 
    CA, April, 1996, 167-173.
        2. Beck, M.T.; ``Critical Survey of Stability Constants of Cyano 
    Complexes,'' Pure & Appl. Chem. 1987, 59, 1703-1720.
        3. Milosavljevic, E.B.; Solujic, Lj.; Hendrix, J.L.; ``Rapid 
    Distillationless `Free Cyanide' Determination by a Flow Injection 
    Ligand Exchange Method,'' Environ. Sci. & Technol. 1995, 29, 426-
    430.
        4. J.C. Wilmot, et al.; ``Formation of Thiocyanate During 
    Removal of Sulfide as Lead Sulfide Prior to Cyanide Determination,'' 
    Analyst, 1996, 121, 799-801.
        5. Goldberg, M.M.; Clayton, C.A.; Potter, B.B.; ``The Effect of 
    Multiple Interferences on the Determination of Total Cyanide in 
    Simulated Electroplating Waste by EPA Method 335.4,'' Proceedings of 
    The Seventeenth Annual EPA Conference On Analysis Of Pollutants in 
    the Environment, Norfolk, VA, 1994, pp. 395-427.
        6. Goldberg, M.M. and Clayton, C.A.; ``Effects of Metals, 
    Ligands, and Oxidants on Cyanide Analysis: Gold Mining Waste Case 
    Study,'' Proceedings of The Eighteenth Annual EPA Conference On 
    Analysis Of Pollutants in the Environment, Norfolk, VA, 1995, pp. 
    87-126.
    
    VI. Regulatory Requirements
    
    A. Executive Order 12866
    
        Under Executive Order 12866 (58 FR 51735 October 4, 1993), the 
    Agency must determine whether a regulatory action is ``significant'' 
    and therefore subject to OMB review and the requirements of the 
    Executive Order. The Order defines ``significant regulatory action'' as 
    one that is likely to result in a rule that may: (1) Have an annual 
    effect on the economy of $100 million or more or adversely affect in a 
    material way the economy, a sector of the economy, productivity, 
    competition, jobs, the environment, public health or safety, or State, 
    local, or Tribal governments or communities; (2) create a serious 
    inconsistency or otherwise interfere with an action taken or planned by 
    another agency; (3) materially alter the budgetary impact of 
    entitlements, grants, user fees, or loan programs or the rights and 
    obligations of recipients thereof; or (4) raise novel legal or policy 
    issues arising out of legal mandates, the President's priorities, or 
    the principles set forth in the Executive Order.
        It has been determined that this rule is not a ``significant 
    regulatory action'' under the terms of Executive Order 12866 and is 
    therefore not subject to OMB review.
    
    B. Unfunded Mandates Reform Act
    
        Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Public 
    Law 104-4, establishes requirements for Federal agencies to assess the 
    effects of their regulatory actions on State, local, and Tribal 
    governments and the private sector. Under section 202 of the UMRA, EPA 
    generally must prepare a written statement, including a cost-benefit 
    analysis, for proposed and final rules with ``Federal mandates'' that 
    may result in expenditures to State, local, and Tribal governments, in 
    the aggregate, or to the private sector, of $100 million or more in any 
    one year. Before promulgating an EPA rule for which a written statement 
    is needed, section 205 of the UMRA generally requires EPA to identify 
    and consider a reasonable number of regulatory alternatives and adopt 
    the least costly, most cost-effective or least burdensome alternative 
    that achieves the objectives of the rule. The provisions of section 205 
    do not apply when they are inconsistent with applicable law. Moreover, 
    section 205 allows EPA to adopt an alternative other than the least 
    costly, most cost-effective or least burdensome alternative if the 
    Administrator publishes with the final rule an explanation why that 
    alternative was not adopted. Before EPA establishes any regulatory 
    requirements that may significantly or uniquely affect small 
    governments, including Tribal governments, it must have developed under 
    section 203 of UMRA a small government agency plan. The plan must 
    provide for notifying potentially affected small governments, enabling 
    officials of affected small governments to have meaningful and timely 
    input in the development of EPA regulatory proposals with significant 
    Federal intergovernmental mandates, and informing, educating, and 
    advising small governments on compliance with the regulatory 
    requirements.
        Today's final rule contains no Federal mandates (under the 
    regulatory provisions of Title II of UMRA) for State, local, or Tribal 
    governments or the private sector. EPA has determined that this rule 
    contains no regulatory requirements that might significantly or 
    uniquely affect small governments. This rule would impose no 
    enforceable duty on any State, local or Tribal governments or the 
    private sector, nor would it significantly or uniquely affect them. 
    This rule makes available an additional analytical test procedure which 
    would merely augment the testing options and standardize the procedures 
    when testing is otherwise required by a regulatory agency. Therefore, 
    today's rule is not subject to the requirements of sections 202, 203 
    and 205 of UMRA.
    
    C. Regulatory Flexibility Act (RFA), as Amended by the Small Business 
    Regulatory Enforcement Fairness Act of 1996 (SBREFA), 5 U.S.C. 601 et 
    seq.
    
        The RFA generally requires an agency to prepare a regulatory 
    flexibility analysis of any rule subject to notice and comment 
    rulemaking requirements under the Administrative Procedure Act or any 
    other statute unless the agency certifies that the rule will not have a 
    significant economic impact on a substantial number of small entities. 
    Small entities include small businesses, small organizations, and small 
    governmental jurisdictions.
        For purposes of assessing the impacts of today's rule on small 
    entities, we defined: (1) Small businesses according to SBA size 
    standards; (2) small governmental jurisdictions as governments of a 
    city, county, town, school district or special district with a 
    population less than 50,000; and (3) small organizations as any not-
    for-profit enterprise which is independently owned and operated and is 
    not dominant in its field.
        After considering the economic impacts of today's final rule on 
    small entities, I certify that this action will not have a significant 
    economic impact on a substantial number of small entities. This final 
    rule will not impose any requirements on small entities. This final 
    rule approves an additional testing procedure for the measurement of 
    available cyanide in wastewater. However, this regulation does not 
    require its use. Rather, the final rule merely provides another option 
    because any of the testing procedures currently approved at 40 CFR part 
    136 can be used if monitoring is otherwise required for this pollutant 
    under the CWA.
    
    [[Page 73422]]
    
    D. Paperwork Reduction Act
    
        This rule contains no information collection requirements. 
    Therefore, no information collection request has been submitted to the 
    Office of Management and Budget (OMB) for review and approval under the 
    Paperwork Reduction Act of 1980, 44 U.S.C. 3501 et seq..
    
    E. Submission to Congress and the General Accounting Office
    
        The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the 
    Small Business Regulatory Enforcement Fairness Act of 1996, generally 
    provides that before a rule may take effect, the agency promulgating 
    the rule must submit a rule report, which includes a copy of the rule, 
    to each House of the Congress and to the Comptroller General of the 
    United States. EPA will submit a report containing this rule and other 
    required information to the U.S. Senate, the U.S. House of 
    Representatives and the Comptroller General of the United States prior 
    to publication of the rule in the Federal Register. A major rule cannot 
    take effect until 60 days after it is published in the Federal 
    Register. This rule is not a ``major rule'' as defined by 5 U.S.C. 
    804(2). This rule will be effective on January 31, 2000.
    
    F. National Technology Transfer and Advancement Act
    
        As noted in the proposed rule, section 12(d) of the National 
    Technology Transfer and Advancement Act of 1995 (NTTAA), Public Law 
    104-113, section 12(d) (15 U.S.C. 272 note) directs EPA to use 
    voluntary consensus standards in its regulatory activities unless to do 
    so would be inconsistent with applicable law or otherwise impractical. 
    Voluntary consensus standards are technical standards (e.g., materials 
    specifications, test methods, sampling procedures and business 
    practices) that are developed or adopted by voluntary consensus 
    standard bodies. The NTTAA directs EPA to provide Congress, through the 
    Office of Management and Budget (OMB), explanations when the Agency 
    decides not to use available and applicable voluntary consensus 
    standards. This rule involves technical standards. Therefore, the 
    Agency conducted a search to identify potentially applicable voluntary 
    consensus standards. However, we identified no such standards for 
    measuring ``available cyanide,'' and none were brought to our attention 
    in comments. Therefore, EPA has decided to use Method OIA-1677.
        The American Society of Testing and Materials (ASTM) is in the 
    balloting process for approval of a voluntary consensus standard method 
    for ``available cyanide.'' The ASTM method may differ slightly from 
    Method OIA-1677. If ASTM or another voluntary consensus standard body 
    approves such a method and EPA determines that the method is suitable 
    for compliance monitoring and other purposes, EPA would promulgate the 
    method in a subsequent rulemaking.
    
    G. Executive Order 13045
    
        Executive Order 13045, ``Protection of Children from Environmental 
    Health Risks and Safety Risks,'' (62 FR 19885, April 23, 1997) applies 
    to any rule that: (1) Is determined to be ``economically significant'' 
    as defined under Executive Order 12866, and (2) concerns an 
    environmental health or safety risk that EPA has reason to believe may 
    have a disproportionate effect on children. If the regulatory action 
    meets both criteria, the Agency must evaluate the environmental health 
    or safety effects of the planned rule on children, and explain why the 
    planned regulation is preferable to other potentially effective and 
    reasonably feasible alternatives considered by the Agency. This rule is 
    not subject to Executive Order 13045 because it is not economically 
    significant as defined under Executive Order 12866.
    
    H. Executive Order 13132
    
        Executive Order 13132, entitled ``Federalism'' (64 FR 43255, August 
    10, 1999), requires EPA to develop an accountable process to ensure 
    ``meaningful and timely input by State and local officials in the 
    development of regulatory policies that have federalism implications.'' 
    ``Policies that have federalism implications'' is defined in the 
    Executive Order to include regulations that have ``substantial direct 
    effects on the States, on the relationship between the national 
    government and the States, or on the distribution of power and 
    responsibilities among the various levels of government.'' Under 
    Executive Order 13132, EPA may not issue a regulation that has 
    federalism implications, that imposes substantial direct compliance 
    costs, and that is not required by statute, unless the Federal 
    government provides the funds necessary to pay the direct compliance 
    costs incurred by State and local governments, or EPA consults with 
    State and local officials early in the process of developing the 
    proposed regulation. EPA also may not issue a regulation that has 
    federalism implications and that preempts State law unless the Agency 
    consults with State and local officials early in the process of 
    developing the proposed regulation.
        If EPA complies by consulting, Executive Order 13132 requires EPA 
    to provide to the Office of Management and Budget (OMB), in a 
    separately identified section of the preamble to the rule, a federalism 
    summary impact statement (FSIS). The FSIS must include a description of 
    the extent of EPA's prior consultation with State and local officials, 
    a summary of the nature of their concerns and the agency's position 
    supporting the need to issue the regulation, and a statement of the 
    extent to which the concerns of State and local officials have been 
    met. Also, when EPA transmits a draft final rule with federalism 
    implications to OMB for review pursuant to Executive Order 12866, EPA 
    must include a certification from the agency's Federalism Official 
    stating that EPA has met the requirements of Executive Order 13132 in a 
    meaningful and timely manner.
        This final rule will not have substantial direct effects on the 
    States, on the relationship between the national government and the 
    States, or on the distribution of power and responsibilities among the 
    various levels of government, as specified in Executive Order 13132. 
    Today's rule merely approves an additional testing procedure for the 
    measurement of available cyanide in wastewater. Today's action does 
    not, however, require use of the alternative method. The rule provides 
    laboratory analysts with another option to the list of currently 
    approved testing procedures 40 CFR part 136, which can be used if 
    monitoring is otherwise required for this pollutant under the CWA. 
    Thus, the requirements of section 6 of the Executive Order do not apply 
    to this rule.
    
    I. Executive Order 13084
    
        Under Executive Order 13084, ``Consultation and Coordination with 
    Indian Tribal Governments,'' EPA may not issue a regulation that is not 
    required by statute, that significantly or uniquely affects the 
    communities of Indian Tribal governments, and that imposes substantial 
    direct compliance costs on those communities, unless the Federal 
    government provides the funds necessary to pay the direct compliance 
    costs incurred by the Tribal governments, or EPA consults with those 
    governments. If EPA complies by consulting, Executive Order 13084 
    requires EPA to provide to the Office of Management and Budget, in a 
    separately identified section of the preamble to the rule, a 
    description of the extent of EPA's prior consultation with 
    representatives
    
    [[Page 73423]]
    
    of affected Tribal governments, a summary of the nature of their 
    concerns, and a statement supporting the need to issue the regulation. 
    In addition, Executive Order 13084 requires EPA to develop an effective 
    process permitting elected and other representatives of Indian Tribal 
    governments ``to provide meaningful and timely input in the development 
    of regulatory policies on matters that significantly or uniquely affect 
    their communities.''
        Today's rule does not significantly or uniquely affect the 
    communities of Indian Tribal governments. Further, this rule does not 
    impose substantial direct compliance costs on Tribal governments. This 
    rule makes available an additional testing procedure which would be 
    used when testing is otherwise required by a regulatory agency to 
    demonstrate compliance with permit limits for cyanide. Accordingly, the 
    requirements of section 3(b) of Executive Order 13084 do not apply to 
    this rule.
    
    List of Subjects in 40 CFR Part 136
    
        Environmental protection, Analytical methods, Incorporation by 
    reference, Monitoring, Reporting and recordkeeping requirements, Waste 
    treatment and disposal, Water pollution control.
    
        Dated: December 20, 1999.
    Carol M. Browner,
    Administrator.
    
        In consideration of the preceding, EPA amends 40 CFR part 136 as 
    follows:
    
    PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS 
    OF POLLUTANTS
    
        1. The authority citation of 40 CFR part 136 continues to read as 
    follows:
    
        Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91 
    Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water 
    Pollution Control Act Amendments of 1972 as amended by the Clean 
    Water Act of 1977).
    
        2. Section 136.3 is amended in paragraph (a), Table IB.--List of 
    Approved Inorganic Test Procedures, by revising entry 24 and adding a 
    new footnote 44 and by adding a new paragraph (b)(43) to read as 
    follows:
    
    
    Sec. 136.3  Identification of test procedures.
    
        (a) * * *
    
                                                      Table IB.--List of Approved Inorganic Test Procedures
    --------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                  Reference (method number or page)
        Parameter, units and method     --------------------------------------------------------------------------------------------------------------------
                                            EPA 1 35         STD methods 18th ed.                ASTM                       USGS 2                 Other
    --------------------------------------------------------------------------------------------------------------------------------------------------------
     
                       *                  *                  *                  *                  *                  *                  *
    24. Available Cyanide, mg/L
        Cyanide amenable to                       335.1  4500-CN G..................  D2036-91(B).
         chlorination (CATC), Manual
         distillation with MgCl2
         followed by titrimetry or
         spectrophotometry.
        Flow injection and ligand                                                     ..........................  ..........................     44 OIA-1677
         exchange, followed by
         amperometry.
     
                      *                  *                  *                  *                  *                  *                  *
    --------------------------------------------------------------------------------------------------------------------------------------------------------
    \1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-
      CI), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.
    \2\ Fishman, M.J., et al., ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques
      of Water--Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
    *        *        *        *        *        *        *
    \35\ Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC
      method for arsenic are provided in Appendix D of this part titled, ``Precision and Recovery Statements for Methods for Measuring Metals.''
    *        *        *        *        *        *        *
    \44\ Available Cyanide, Method OIA-1677 (Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry), ALPKEM, A Division of OI Analytical,
      P.O. Box 9010, College Station, TX 77842-9010.
    
        (b) * * *
        (43) Method OIA-1677, Available Cyanide by Flow Injection, Ligand 
    Exchange, and Amperometry. August 1999. ALPKEM, OI Analytical, Box 648, 
    Wilsonville, Oregon 97070 (EPA-821-R-99-013). Available from: National 
    Technical Information Service, 5285 Port Royal Road, Springfield, 
    Virginia 22161. Publication No. PB99-132011. Cost: $22.50. Table IB, 
    Note 44.
    
    [FR Doc. 99-33627 Filed 12-29-99; 8:45 am]
    BILLING CODE 6560-50-P
    
    
    

Document Information

Effective Date:
1/31/2000
Published:
12/30/1999
Department:
Environmental Protection Agency
Entry Type:
Rule
Action:
Final rule.
Document Number:
99-33627
Dates:
This regulation is effective on January 31, 2000. For judicial review purposes, this final rule is promulgated as of 1 p.m. Eastern Standard Time on January 13, 2000 in accordance with 40 CFR 23.2.
Pages:
73414-73423 (10 pages)
Docket Numbers:
FRL-6478-1
RINs:
2040-AC76: Guidelines Establishing Test Procedures for the Analysis of Cyanide Under the Clean Water Act
RIN Links:
https://www.federalregister.gov/regulations/2040-AC76/guidelines-establishing-test-procedures-for-the-analysis-of-cyanide-under-the-clean-water-act
PDF File:
99-33627.pdf
CFR: (1)
40 CFR 136.3