[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
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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.
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This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be affected by this
action. This table lists 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