[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:

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