[Federal Register Volume 66, Number 195 (Tuesday, October 9, 2001)]
[Proposed Rules]
[Pages 51518-51528]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 01-24886]
[[Page 51517]]
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Part II
Environmental Protection Agency
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40 CFR Part 136
Guidelines Establishing Test Procedures for the Analysis of Pollutants;
Measurement of Mercury in Water; Revisions to EPA Method 1631; Proposed
Rule
Federal Register / Vol. 66, No. 195 / Tuesday, October 9, 2001 /
Proposed Rules
[[Page 51518]]
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ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 136
[FRL-7074-6]
Guidelines Establishing Test Procedures for the Analysis of
Pollutants; Measurement of Mercury in Water; Revisions to EPA Method
1631; Proposed Rule
AGENCY: Environmental Protection Agency (EPA).
ACTION: Proposed rule.
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SUMMARY: By this action, EPA is proposing modifications to EPA Method
1631, Revision C: Mercury in Water by Oxidation, Purge and Trap, and
Cold Vapor Atomic Fluorescence Spectrometry (Method 1631C), which
measures mercury in aqueous samples. The proposed modifications would
require use of certain ``clean techniques'' and quality control
requirements when using this test method. The Agency is proposing to
modify EPA Method 1631C to fulfill obligations under a Settlement
Agreement designed to resolve litigation challenging an earlier EPA
rulemaking that standardized this test method. The proposed
modifications are intended to improve performance of EPA Method 1631C
by reducing opportunities for contamination during sample collection
and analysis. In addition, EPA is proposing revisions to this test
method based on comments received from method users following method
approval.
DATES: Comments must be postmarked, delivered by hand, or
electronically mailed on or before December 10, 2001. Comments provided
electronically will be considered timely if they are submitted
electronically by 11:59 p.m. Eastern Standard Time (EST) on December
10, 2001.
ADDRESSES: Mail written comments on the proposed rule to ``Method
1631--Proposed Rule'' Comment Clerk (W-01-05), Water Docket (4101);
U.S. Environmental Protection Agency; Ariel Rios Building; 1200
Pennsylvania Avenue, NW., Washington, DC 20460. Hand deliveries should
be delivered to: EPA's Water Docket at 401 M Street, SW., East Tower
Basement (Room EB 57), Washington, DC 20460. If you wish to hand-
deliver your comments, please call (202) 260-3027 between 9:00 a.m. and
4:00 p.m., Monday through Friday, excluding Federal holidays, to
schedule an appointment. Comments also may be submitted electronically
to: [email protected].
FOR FURTHER INFORMATION CONTACT: Maria Gomez-Taylor, Ph.D.; Engineering
and Analysis Division (4303); Office of Science and Technology; Office
of Water; U.S. Environmental Protection Agency; Ariel Rios Building;
1200 Pennsylvania Avenue, NW; Washington, DC 20460, or call (202) 260-
1639 or E-mail at [email protected].
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, NPDES permitting authorities, including authorized States,
Territories, and Tribes, make a number of discretionary choices
associated with permit writing, including the selection 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 permitting
authority must specify one of the approved testing procedures or an
approved alternate test procedure for the measurements required under
the permit. 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
approved testing procedures. Categories and entities that may be
regulated include:
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Examples of potentially
Category regulated entities
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State, Territorial, and Indian Tribal States, Territories, and
Governments. Tribes authorized to
administer the NPDES
permitting program; States,
Territories, and Tribes
providing certification
under Clean Water Act
section 401.
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This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be regulated by this
action. This table lists the types of entities that EPA is now aware
could potentially be regulated by this action. Other types of entities
not listed in the table could also be regulated. 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.
Record and Commenting Procedures
The record for this rulemaking has been established under Docket
Number W-01-05. A copy of the supporting documents cited in this
proposal are available for review at EPA's Water Docket. The record is
available for inspection from 9 a.m. to 4 p.m. EST, Monday through
Friday, excluding Federal holidays at EPA's Water Docket, 401 M Street
SW., East Tower Basement (Room EB 57), Washington, DC 20460. For access
to docket materials, please call (202) 260-3027 to schedule an
appointment.
Commenters are requested to submit any references cited in their
comments. Commenters also are requested to submit an original and three
copies of their written comments and enclosures, and to clearly
identify the specific issue(s) and method section(s) to which the
comment applies. Commenters who want a confirmed receipt of their
comments should include a self-addressed, stamped envelope. All
comments must be postmarked or delivered by hand. No facsimiles (faxes)
will be accepted.
Electronic comments must be submitted as a Word Perfect for Windows
5/6/7/8 file or an ASCII file, avoiding the use of special characters
and any form of encryption. Comments and data also will be accepted on
disks in Word Perfect 5/6/7/8 or ASCII file format. Electronic comments
on this notice may be filed online at many Federal Depository
Libraries. All electronic comments must be identified by docket number.
Electronic comments will be transferred into a paper version for the
official record. EPA will attempt to clarify electronic comments if
there is an apparent error in transmission.
Information on Internet Access
This Federal Register document has been placed on the Internet for
public review and downloading at the following location: http//
www.epa.gov/fedrgstr. Method 1631, Revision C; Draft Method 1631,
Revision D; the Method 1631 Guidance; and a Fact Sheet are available at
www.epa.gov/ost/methods/1631.html or from the EPA Sample Control Center
(SCC), DynCorp I&ET, 6101 Stevenson Ave., Alexandria, VA 22304 (703-
461-2100; [email protected]).
Outline of Notice
I. Statutory Authority
II. Background
A. Regulatory Actions
B. Settlement Agreement
III. Summary of Today's Action
IV. Proposed Revisions Based on the Settlement Agreement
[[Page 51519]]
A. Additional Requirements for Clean Techniques and Quality
Control Provisions
B. Election by a Permittee/Industrial User
V. Proposed Additional Revisions to EPA Method 1631
A. Use of Automated Flow-Injection Systems
B. Blanks
C. Calibration Over a Different Range
D. Sample Preservation, Refrigeration, Headspace, Collection
Containers, and Storage
E. Shipment of Empty Sample Containers
F. Scope of ``Should'' and ``May''
G. Field Filtration for Dissolved Metals
H. Carryover Test
I. Correction of Part Numbers
J. Use of Polyethylene or Polypropylene Vessels for Sample
Digestion
K. Indication of Complete Oxidation
L. Adjustment for Amount of Bromine Monochloride to Blanks
M. Addition of Method 1631 Guidance as a Reference
VI. Proposed Amendment to 40 CFR 136.3(e) Table II
VII. Administrative Requirements
A. Executive Order 12866--Regulatory Planning and Review
B. Regulatory Flexibility Act (RFA), as Amended by the Small
Business Regulatory Enforcement Fairness Act of 1996 (SBREFA), 5
U.S.C. 601 et seq.
C. Unfunded Mandates Reform Act
D. Paperwork Reduction Act
E. National Technology Transfer and Advancement Act
F. Executive Order 13045--Protection of Children from
Environmental Health Risks and Safety Risks
G. Executive Order 13132--Federalism
H. Executive Order 13175--Consultation and Coordination with
Indian Tribal Governments
I. Executive Order 13211--Actions Concerning Regulations That
Significantly Affect Energy Supply, Distribution, or Use
J. Plain Language Directive
VIII. Request for Comments
I. Statutory Authority
Today's proposal is pursuant to the authority of sections 301,
304(h), 307, and 501(a) of the Clean Water Act (CWA), 33 U.S.C. 1311,
1314(h), 1317, 1361(a) (the ``Act''). 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 function under this Act.'' EPA publishes
CWA analytical method regulations at 40 CFR Part 136. The Administrator
also has made these test procedures applicable to monitoring and
reporting of NPDES permits (40 CFR Parts 122, Secs. 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, Secs. 403.10 and
402.12).
II. Background
A. Regulatory Actions
On May 26, 1998, EPA proposed Method 1631 at 40 CFR Part 136 for
use in determining mercury at ambient water quality criteria levels in
EPA's Clean Water Act programs (63 FR 28867). Subsequently, on March 5,
1999, EPA published a Notice of Data Availability that included
additional data supporting the application of Method 1631 to effluent
matrices (64 FR 10596) in response to comments received at proposal. On
June 8, 1999, EPA published a final rule promulgating EPA Method 1631,
Revision B: Mercury in Water by Oxidation, Purge and Trap, and Cold
Vapor Atomic Fluorescence Spectrometry (64 FR 30416) at 40 CFR Part
136. EPA published a technical correction revising EPA Method 1631B to
EPA Method 1631C (66 FR 32774; June 18, 2001) to clarify the method
text regarding the use of field blanks (see Settlement Agreement
discussion below).
B. Settlement Agreement
In response to a petition for judicial review of EPA Method 1631B,
EPA entered into negotiations with several industry groups. On October
19, 2000, EPA entered into a Settlement Agreement with the Alliance of
Automobile Manufacturers, Inc., the Chemical Manufacturers Association,
and the Utility Water Act Group (collectively, Petitioners), and the
American Forest & Paper Association (Intervenor). The Settlement
Agreement (Alliance of Automobile Manufacturers, et al. v. EPA, No. 99-
1420, D.C. Dir.), is included in the rulemaking record in the Water
Docket for today's proposal (see the ADDRESSES section of this proposal
for details on the Water Docket). The Settlement Agreement includes
four clauses that directly affect Method 1631 (Clauses 2, 3, 4, and 5).
Clauses 2 and 3 of the Settlement Agreement committed EPA to sign a
notice of final rulemaking by June 15, 2001, revising sections 12.4.2
and 9.4.3.3 of Method 1631B to clarify the use of field blank
subtraction (section 12.4.2) and the use of multiple field blanks
(section 9.3.3.3) to determine whether test samples are acceptable for
compliance monitoring purposes. EPA complied with that commitment, and
on June 18, 2001, EPA published a final rule; technical correction
notice (66 FR 32774) announcing a revised version of Method 1631
(Revision C; Method 1631C). That notice included the technical
corrections about field blanks required by the Settlement Agreement. At
that time, no other changes were made to the test method.
Clause 4 of the Settlement Agreement requires that EPA sign a
notice for publication in the Federal Register on or before September
30, 2001 to propose additional requirements for certain clean
techniques and quality control (QC) provisions in Method 1631. Today's
proposed rule complies with EPA's obligation under Clause 4 of the
Settlement Agreement. The additional requirements were listed in the
Settlement Agreement as Appendix A and are discussed in Section IV of
this preamble. Clause 4 also requires that EPA propose that ``a
National Pollutant Discharge Elimination System (NPDES) permittee or an
industrial user of a publicly-owned treatment works (POTW) may elect
not to implement such provisions in its discretion and at its peril,
unless specifically provided otherwise by the relevant permitting
agency or pretreatment control authority, as the case may be.''
Clause 5 of the Settlement Agreement required that EPA publish a
guidance document on or before March 1, 2001 specifying procedures for
identifying, reducing, and demonstrating potential matrix
interferences. On February 27, 2001, EPA published Guidance for
Implementation and Use of EPA Method 1631 for the Determination of Low-
Level Mercury (40 CFR Part 136) (EPA 821-R-01-023; March 2001) to
address this clause and to assist regulatory agencies, dischargers,
industrial users, and laboratories in the application of Method 1631 to
ambient water and wastewater. In addition to providing information on
potential matrix interferences, the guidance provides information on
the use of clean techniques and method flexibility, and answers
frequently asked questions regarding method implementation.
III. Summary of Today's Action
This rulemaking proposes to modify EPA Method 1631 to require the
use of certain clean techniques and quality control (QC) provisions in
accordance with clause 4 of the Settlement Agreement. These changes are
in response to the petitioners' concerns
[[Page 51520]]
that results produced by laboratories using EPA Method 1631 would not
be reliable unless the optional clean techniques and QC provisions are
required. These revisions are discussed in Section IV of this proposal
and are included in draft Method 1631, Revision D (Method 1631D).
Today's notice also proposes improvements and clarifications to EPA
Method 1631 to make this test method more consistent with other
approved methods and current practices, and easier to use. These
proposed revisions are based on comments received from method users
since promulgation of Method 1631. The proposed revisions are discussed
in Section V and are included in draft Method 1631D.
IV. Proposed Revisions Based on the Settlement Agreement
A. Additional Requirements for Clean Techniques and Quality Control
Provisions
Clause 4 of the Settlement Agreement requires EPA to sign a notice
for publication in the Federal Register on or before September 30,
2001, proposing to require certain clean techniques and quality control
(QC) provisions in EPA Method 1631. These requirements to propose clean
techniques and QC provisions are listed in Appendix A to the Settlement
Agreement and are reproduced below. The Petitioners believe that these
additional requirements are necessary to prevent samples from becoming
contaminated during the sampling and analysis process. EPA believes
that these techniques may improve test performance. EPA refers readers
to the appropriate section of draft EPA Method 1631, Revision D for the
proposed revised language, which is indicated in the draft revised
method in brackets and italics.
EPA solicits your comments and/or data on the proposed
requirements, collectively or individually, and requests that you
provide a reason to support your position.
1. Proposed Revision to Section 1.4
Item 1 of Appendix A to the Settlement Agreement states, ``Section
1.4 currently explains the importance of minimizing contamination of
ambient water samples and explains that the Method includes suggestions
for improvements to minimize contamination and maximize the ability of
laboratories to make reliable measurements. The notice shall invite
comment on revisions to this section to explain that certain sections
contain suggestions and that other sections contain requirements to
minimize contamination.'' Revision D, as proposed, includes a statement
to that effect in Section 1.4.
2. Proposed Revision to Sections 2.3 and 8.5
Item 2 of Appendix A to the Settlement Agreement states, ``Sections
2.3 and 8.5 currently suggest that a sample used for the determination
of methyl mercury should be preserved with 5 mL/L HCl solution only.
The notice would invite comment on whether to change these sections to
require the use of HCl for preservation if the sample is collected for
the determination of methyl mercury.'' Revision D, as proposed,
includes statements in Sections 2.3 and 8.5 corresponding to this
requirement.
3. Proposed Revision to Section 4.3.3
Item 3 of Appendix A to the Settlement Agreement states, ``Section
4.3.3 currently suggests the use of a clean room or a clean bench. The
notice would invite comment on whether to change this section to
require a clean bench if a clean room is not available. The notice
would not invite comment on whether to require a nonmetal hood because
the Agency believes removal and replacement of existing metal hoods is
unnecessary; use of a plastic awning in the hood prevents contamination
during sample digestion.'' Revision D, as proposed, reflects this
language in Section 4.3.3.
4. Proposed Revision to Section 4.3.4
Item 4 of Appendix A to the Settlement Agreement states, ``Section
4.3.4 currently suggests precautions to minimize exposure of the
apparatus to contamination. The notice would invite comment on whether
to change the `shoulds' to `musts.' '' Revision D, as proposed, changes
the `shoulds' to `musts' in Section 4.3.4.
5. Proposed Revision to Section 4.3.5
Item 5 of Appendix A to the Settlement Agreement states, ``Section
4.3.5 currently recommends cleaning work surfaces before a batch of
samples is processed. The notice would invite comment on whether to
require the laboratory to clean work surfaces after processing a batch
of samples with high levels of mercury.'' Revision D, as proposed,
includes a requirement to this effect in Section 4.3.5.
6. Proposed Revision to Section 4.3.7.1
Item 6 of Appendix A to the Settlement Agreement states, ``Section
4.3.7.1 currently recommends that only fluoropolymer or borosilicate
glass containers be used for samples. The notice would invite comment
on whether to change `should' to `must' to respond to Petitioners'
concern.'' Revision D, as proposed, changes the `should' to `must' in
Section 4.3.7.1.
7. Proposed Revision to Sections 4.3.8.1 and 11.2.4
Item 7 of Appendix A to the Settlement Agreement states, ``Sections
4.3.8.1 and 11.2.4 currently suggest that a bubbler blank be used to
check for carryover after encountering an unusually concentrated
sample. The notice would invite comment on whether to change `should'
to `must' in both sections to require analysis of the bubbler blank.''
Revision D, as proposed, changes the `should' to `must' in Section
4.3.8.1 and also changes Section 11.2 to correspond to this
requirement.
8. Proposed Revision to Section 4.3.8.4
Item 8 of Appendix A to the Settlement Agreement states, ``Section
4.3.8.4 currently suggests that sample processing should occur as far
as possible from sources of airborne contamination. The notice would
invite comment on whether to change the `should' to `must.''' Revision
D, as proposed, changes the `should' to `must' in Section 4.3.8.4.
9. Proposed Revision to Section 4.4.3
Item 9 of Appendix A to the Settlement Agreement states ``Section
4.4.3 currently explains a concern regarding condensation of water in
the gold traps. The section explains that condensation can be avoided
by predrying the gold trap, and by discarding those traps that tend to
absorb large quantities of water vapor. The notice would invite comment
on whether to change this Section to preclude the use of gold traps
that tend to absorb large quantities of water vapor.'' Revision D, as
proposed, changes Section 4.4.3 to include a requirement to this
effect.
10. Proposed Revision to Sections 6.1.2.3 and 9.4.4.1
Item 10 of Appendix A to the Settlement Agreement states,
``Sections 6.1.2.3 and 9.4.4.1 currently recommend the analysis of
bottle blanks. The notice would invite comment on whether to change
`should' to `must' to require analysis of bottle blanks in these
sections.'' Revision D, as proposed, changes the `should' to `must' in
Section 6.1.2.3 and also changes Section 9.4.7 to correspond to this
requirement because the requirements for bottle blanks are presented in
this section.
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11. Proposed Revision to Section 7.2
Item 11 of Appendix A to the Settlement Agreement states, ``Section
7.2 currently lists two ways to assure that laboratory air is low in
both particulate and gaseous mercury: use of outside air that is very
low in mercury and use of inside air recycled through a gold-coated
filter. As presently written, outside air `should' be brought into the
class-100 clean bench air intake. The notice would invite comment on
whether to change this `should' in the outdoor air option to a
`must.''' Revision D, as proposed, changes the `should' to `must' in
Section 7.2.
12. Proposed Revision to Section 8.5.3
Item 12 of Appendix A to the Settlement Agreement states, ``Section
8.5.3 currently requires handling of samples in a mercury-free clean
bench. The notice would invite comment on whether to change `should' to
`must.''' Revision D, as proposed, changes the `should' to `must' in
Section 8.5.3.
13. Proposed Revision to Note at Section 8.5.3
Item 13 of Appendix A to the Settlement Agreement states ``Section
8.5.3 (note) currently states that samples `should' be filtered and
preserved in accordance with the procedures in Method 1669. The notice
would invite comment on whether to change the `should' to `must' but
only for the provisions of Method 1669 related to filtration and
preservation of samples when circumstances prevent overnight sample
shipment (i.e., sections 2.9 and 2.10 of EPA Method 1669).'' Revision
D, as proposed, changes the `should' to `must' in the Section 8.5.3
note.
14. Proposed Revision to Section 8.6
Item 14 of Appendix A to the Settlement Agreement states, ``Section
8.6 currently suggests that sample bottles should be stored in clean
(new) polyethylene bags until sample analysis. The notice would invite
comment on whether to change this section to require storage in clean
bags by changing `should' to `must.''' Revision D, as proposed, changes
the `should' to `must' in Section 8.6.
15. Proposed Revision to Section 9.4.4.2
Item 15 of Appendix A to the Settlement Agreement states, ``Section
9.4.4.2 currently suggests the use of `Clean Hands/Dirty Hands' when
preparing sampler check blanks at the laboratory or cleaning facility.
The notice would invite comment on whether to change `should' to `must'
in this section for low-level mercury measurements.'' Revision D, as
proposed, makes this change in Section 9.4.6.1 because the ``clean
hands/dirty hands'' technique is referenced in that section.
16. Proposed Revision to Section 11.1.2
Item 16 of Appendix A to the Settlement Agreement states, ``Section
11.1.2 currently suggests that there should be 2 matrix spike/matrix
spike duplicate pairs for each analytical batch of 20 samples. The
notice would invite comment on whether to make the matrix spike/matrix
spike duplicate pairs mandatory by changing `should' to `must be a
minimum of' in this section.'' Revision D, as proposed, makes this
change in Section 11.1.2.
B. Election by a Permittee/Industrial User
In EPA's ``Guidance for the Implementation and Use of EPA Method
1631 for the Determination of Low Level Mercury (40 CFR Part 136),''
dated March 2001, EPA recommends that State and Federal agencies
measuring ambient water quality for compliance with water quality
standards at very low concentrations should require, as a matter of
internal agency protocol, that their personnel use clean techniques.
EPA also suggests in this guidance, that NPDES permits specify the use
of clean techniques, on a permit-by-permit basis, depending on the
measurement level of concern, upon request by the permit applicant. The
guidance also states that EPA will propose additional requirements for
clean techniques by October 2001, and that EPA may revise the guidance
in accordance with any requirements that are promulgated as a result.
Clause 4 of the Settlement Agreement requires EPA to propose that
an NPDES permittee or an industrial user of a POTW may elect not to
implement the clean techniques and QC provisions that are listed in
Appendix A to the Settlement Agreement and that are proposed today ``in
its discretion and at its peril, unless specifically provided otherwise
by the relevant permitting agency or pretreatment control authority, as
the case may be.'' Revision D, as proposed, includes this election in
Section 1.13.
As required by the Settlement Agreement, the election is applicable
to the clean techniques and QC provisions designated in Appendix A to
the Settlement Agreement only. These provisions are discussed in
Section IV.A of this notice and are designated throughout draft EPA
Method 1631D by bracketed and italicized text. If Section 1.13 is
promulgated as proposed, any text pertaining to clean techniques and
quality control provisions that is also promulgated as proposed under
the Settlement Agreement, would remain italicized and bracketed in the
approved version of EPA Method 1631D to designate the techniques and
provisions to which the election is applicable.
Users of EPA Method 1631 should be aware that the election in
Clause 4 of the Settlement Agreement would apply to the permittee/
industrial user only, and not to a regulatory/control authority or to
other users of the Method. Regulatory/control authorities and other
users of EPA Method 1631 would be required to use the clean techniques
and QC provisions as designated by the italicized bracketed text in the
affected sections of EPA Method 1631D. Permittees/industrial users
should be aware of the potential disparity that could result if a
sample is analyzed by a permittee/industrial user not using the clean
techniques and QC provisions and also by a regulatory/control authority
using the clean techniques and QC provisions. In addition, if a
regulatory/control authority requires that a permittee/industrial user
use the clean techniques and QC provisions, the burden would be on the
regulatory/control authority to incorporate this requirement into
regulations or permits.
EPA is soliciting comments on this election and on the specific
techniques and provisions to which the election would be applicable.
EPA is soliciting comments particularly from permittees/industrial
users because the users would have the election, and from regulatory/
control authorities and other users of EPA Method 1631 because they
would not. EPA also seeks comment on whether the philosophical change
embodied by the election (i.e., to allow a permittee/industrial user to
not use certain techniques and QC provisions of an analytical method,
yet require regulatory/control authorities and other users to use these
techniques) is desirable, in general. In addition, EPA solicits
comments on alternatives to the Settlement Agreement approach, mainly
on whether the additional clean techniques and QC requirements should
be applicable to all users or whether the additional requirements
should be optional for all users.
V. Proposed Additional Revisions to EPA Method 1631
Since promulgation of EPA Method 1631 in June 1999, EPA has
received many suggestions for method improvement and requests to
clarify certain method procedures. In today's action, EPA is proposing
revisions to clarify and improve the method in
[[Page 51522]]
response to these comments. This section explains the revisions
included in draft EPA Method 1631D in response to these comments. EPA
is soliciting comment on the proposed revisions described below.
A. Use of Automated Flow-Injection Systems
Automated flow-injection systems are currently available and have
been used successfully for performing EPA Method 1631 procedures for
several years. These systems use flow injection and a gas-liquid
separator in place of the bubbler.
EPA has worked with several users of these systems to develop
appropriate calibration and calculation procedures and blank sample
requirements and has included these procedures and requirements in
draft Method 1631D. The revisions incorporate calibration blanks
(Section 9.4.2), calibration procedures (Section 10.2), and result
calculation procedures (Section 2.2) that are specific for flow
injection systems. The proposed method also refers to flow injection
systems throughout the text, and includes a figure depicting the flow-
injection system (Figure 3). The revisions will expand the use of the
Method by providing appropriate procedures for the use of automated
flow injection systems.
B. Blanks
EPA Method 1631C includes the use of bubbler blanks (Section
9.4.1), reagent blanks (Section 9.4.2), field blanks (Section 9.4.3),
equipment blanks (Section 9.4.4), bottle blanks (Section 9.4.4.1), and
sampler check blanks (Section 9.4.4.1). Several commenters noted that
the blanks are not well defined and that blank requirements are
inconsistent with common usage. In addition, commenters noted that the
types and requirements for blanks are not appropriate for use with the
flow-injection systems. To address these comments, EPA added
definitions for all blanks in the Glossary of draft Method 1631D, and
clarified these definitions throughout the Method text. EPA has also
added requirements for calibration blanks (for use with flow injection
systems only) and method blanks (for use with both bubbler and flow
injection systems). The proposed revisions are discussed in the
following sections.
1. Definitions
In response to several comments that the types of blank samples
required by Method 1631 are defined inconsistently throughout the
Method, EPA revised Section 17 of draft Method 1631D to include
definitions for the calibration blank, method blank, reagent blank,
field blank, and bottle blank samples. Section 17 of draft Method 1631D
also includes a revised definition of the bubbler blank to clarify its
specificity for use with bubbler systems. In addition, EPA revised
Section 9.4 in draft Method 1631D to further clarify definitions and
use of blank samples for both bubbler and flow-injection systems.
The proposed revisions address more accurately EPA's intent to
allow the use of both bubbler and flow injection systems for
determination of mercury using Method 1631. The revisions also clarify
the application and use of blank samples to identify and handle
potential contamination.
2. Calibration Blanks
In EPA Method 1631, bubbler blanks are used to establish a
background for the bubbler system (i.e., bubbler, traps, and cold-vapor
atomic fluorescence detector) and can be used to identify potential
carryover from one sample to the succeeding sample (see Section 9.4.1
of EPA Method 1631C). Results of bubbler blanks are subtracted from all
raw calibration and sample results. Bubbler blanks, however, are not
appropriate for flow injection systems. Hence, EPA added a requirement
for calibration blanks, when using a flow injection system. The
performance criteria and application requirements of the calibration
blanks are identical to those for the bubbler blanks.
3. Method and Reagent Blanks
EPA Method 1631 requires reagent blanks to identify contamination
from reagents, but these blanks are required only when a new batch of
reagents is prepared, with verification in triplicate each month, and
are not required with each analytical batch (see Section 9.4.2 of EPA
Method 1631C). Method 1631 also requires field blanks to identify
contamination from sample collection and transport (see Section 9.4.3
of EPA Method 1631C). These field blanks may be used to identify
contamination introduced at some point during the entire measurement
process from sample collection through mercury detection, but cannot
isolate contamination caused by sample collection and transport from
contamination that is introduced during sample processing and analysis.
Several method users commented that laboratories typically use
method blanks to determine potential contamination in the analytical
system during sample preparation and analysis. These method blanks are
prepared and analyzed using procedures identical to those used to
prepare and analyze the corresponding samples.
Because method blanks can be used to identify total analytical
system contamination, and are subjected to all sample processing and
analytical steps including digestion, reduction, and determination, EPA
added a requirement for method blanks to draft Method 1631D. The
proposed method includes a requirement that at least three method
blanks be analyzed with each analytical batch. It also includes a
requirement that any sample requiring increased oxidation (e.g., an
increased amount of reagent) be associated with at least one method
blank that is processed and analyzed using the same amount of increased
oxidation. The performance criteria for the method blanks is identical
to the field blank criteria. This requirement provides method users
with a more appropriate procedure for addressing contamination that may
result during the entire analytical procedure.
EPA also proposes to revise the requirement for the frequency of
reagent blanks. In draft Method 1631D, analysis of reagent blanks is
required only when each new batch of reagents is prepared. EPA believes
that the requirements for method blanks included in draft Method 1631D
will be sufficient to identify contamination that may be introduced by
reagent solutions during processing and analysis of an analytical
batch.
4. Equipment and Bottle Blanks
EPA received several comments on Method 1631 expressing confusion
over the use of the terms ``equipment blank,'' ``sampler check blank,''
and ``bottle blank.'' Commenters also noted that the terms ``equipment
blank'' and ``sampler check'' blank are synonymous and that using two
terms to identify blanks used to check sample collection equipment is
confusing. Additionally, commenters were concerned that bottle blanks
are listed in EPA Method 1631 under blanks specific for determination
of contamination in sample collection equipment. These commenters noted
that bottle blanks also are necessary to determine contamination in
bottles used for sample preparation and analysis, and recommended that
bottle blanks be analyzed at a frequency of at least 20 percent of each
lot used.
In response to these comments, EPA proposes to change the term
``sampler check blank'' to ``equipment blank'' in Section 9.4.6 of
draft Method 1631D, and to revise Section 9.4 of the method to expand
the application of bottle blanks for determination of contamination in
bottles used for both sample collection and analysis (Section
[[Page 51523]]
9.4.7). EPA also included a requirement in draft Method 1631D that a
minimum of 20 percent of the bottles from a given lot shall be tested
and demonstrated to be free of mercury at the Method MDL (Section
6.1.2.4).
C. Calibration Over a Different Range
Several users of Method 1631 stated that they prefer to use EPA
Method 1631 for mercury determination because it is less prone to
interferences than other available methods, and would like to apply EPA
Method 1631 procedures across a higher calibration range. Other users
of the method commented that when they are analyzing samples known to
be within a narrower range of concentrations than that of the current
method (e.g., an analytical run consisting of ambient samples), they
prefer to calibrate the analytical system across the narrower range.
Additional users noted that they desire to calibrate to a lower point
to measure mercury in blanks to a lower level.
In response to these comments and to allow expanded use of EPA
Method 1631, EPA included a provision in draft Method 1631D to allow
calibration over ranges other than the range currently specified
(Section 10.4). EPA included certain criteria with this provision to
ensure that this allowance does not compromise data quality. These
criteria are: (1) there must be a minimum of five, non-zero calibration
points; (2) the difference between successive calibration points must
be no greater than a factor of 10 and no less than a factor of 2 and
should be approximately evenly spaced on a logarithmic scale over the
calibration range; (3) the relative standard deviation (RSD) of the
calibration factors for all calibration points must be less than 15%;
(4) the calibration factor for any calibration point at a concentration
greater than 100 ng/L must be within plus or minus 15% of the average
calibration factor for the points at or below 100 ng/L; (5) the
calibration factor for any point less than 5 ng/L must be within plus
or minus 25% of the average calibration factor for all points; (6) if
the highest calibration point is increased above 100 ng/L, the lowest
calibration point (ML) must be increased commensurately above 0.5 ng/L;
and, (7) if the calibration is to a higher range and this Method is
used for regulatory compliance, the ML must be less than one-third the
regulatory compliance limit.
D. Sample Preservation, Refrigeration, Headspace, Collection
Containers, and Storage
Section 8.5 of the currently approved EPA Method 1631 requires that
samples are preserved upon collection, or alternatively, are collected
only in fluoropolymer bottles, with zero headspace, capped tightly, and
stored at 0-4 deg.C until they can be preserved within 48 hours of
collection.
Since promulgation of EPA Method 1631, EPA has received numerous
comments on the sample preservation, refrigeration, headspace, and
holding time requirements in the method and in Table II at 40 CFR
136.3(e). EPA has considered these comments and has included revisions
in today's draft Method 1631D to address the recommendations from
method users. Specific proposed revisions regarding preservation,
refrigeration, container type, headspace, and holding time requirements
are discussed below. The proposed changes are based on the comments
received from method users and EPA requests data to support whether the
changes would affect the quality of results. EPA is not proposing to
revise the requirements that samples collected for determination of
total mercury must be capped tightly and must be preserved or analyzed
within 48 hours of collection. EPA is requesting comment on whether
this requirement should be kept.
1. Sample Preservation
Sections 2.3 and 8.5 of EPA Method 1631 currently require that
samples are either preserved with hydrochloric acid (HCl) or bromine
monochloride (BrCl) solution immediately upon collection, or
alternatively, are collected and stored under specific conditions
(i.e., zero headspace, fluoropolymer bottles, capped tightly, and
stored at 0-4 deg.C) until they can be preserved in the laboratory
within 48 hours of collection. As discussed in Section IV.A.2, EPA is
also proposing to revise the sample preservation requirement in
Sections 2.3 and 8.5 of the method for the determination of methyl
mercury.
Commenters claim there is no need to preserve samples for total Hg
if BrCl is added to the sample in the laboratory and the sample is
allowed to stand for a minimum of 24 hours to oxidize all forms and
species of mercury to Hg(II). Commenters also noted that the
immediate preservation of samples collected for total or dissolved
mercury determination is unnecessary, provided the samples are
preserved or analyzed within 48 hours of collection, and have requested
elimination of the requirement for preservation so that solutions of
HCl or BrCl do not need to be shipped to the sampling site.
EPA currently is reviewing data that indicate that unpreserved
samples collected for measurement of low level mercury may be stable
for as long as 35 days. Additionally, EPA does not have data
demonstrating that results of samples for total or dissolved mercury
that are not preserved immediately are compromised, and solicits such
data to determine whether immediate preservation should be required.
Therefore, EPA has included revisions in draft Method 1631D (Section
8.5) to eliminate the requirement for immediate preservation of samples
collected for determination of mercury using EPA Method 1631. Today's
proposed method does not include a revision to the requirement for
immediate preservation of samples collected for methyl- and di-methyl
mercury determination.
EPA is also proposing to amend Table II of 40 CFR 136.3(e) to
include requirements for preservation of samples collected for mercury
measurement using Method 1631 within 48 hours of sample collection,
using BrCl or HCl (see Section VI of this notice).
2. Sample Refrigeration
Users of EPA Method 1631 claim that there is no need to refrigerate
unpreserved samples for total or dissolved mercury because the bromine
monochloride (BrCl) digestion converts all forms of Hg to
Hg(II). Therefore, if a given form or species of Hg were
converted to another form or species in the absence of refrigeration
(e.g., through biological activity), the BrCl digestion would convert
the new form, as well as any remaining portion of the old form, to
Hg(II). Commenters have requested that EPA eliminate the
requirement for refrigeration of unpreserved samples because of costs
and logistics problems (i.e., refrigeration requires purchase of ice,
shipment of the sample in a cooler, and testing of the sample at the
laboratory to make certain that the temperature remains in the range
specified, 0-4 deg.C).
EPA currently does not have data demonstrating that refrigeration
of unpreserved samples for measurement of total or dissolved mercury
using Method 1631 is necessary, and is seeking such data to determine
if refrigeration should be required. In the absence of data, EPA has
revised draft Method 1631D (Section 8.5) to eliminate the requirement
for refrigeration of unpreserved samples, provided that the sample is
tightly capped and is either preserved or analyzed within 48 hours of
collection.
EPA also has received comments that samples collected for
measurement of mercury using Method 1631 are stable for up to 30 days
prior to either preservation or analysis. EPA is
[[Page 51524]]
requesting data to support this comment. EPA will consider submitted
data, and if appropriate, will re-evaluate the requirement for
preservation or analysis of samples within 48 hours.
3. Sample Headspace
Section 8.5 of EPA Method 1631 requires that mercury samples are
collected with zero headspace if they are not preserved immediately. A
laboratory involved in the development of EPA Method 1631 commented
that, although it is necessary to collect samples for methyl- and
dimethyl-mercury with zero headspace, it is not necessary to collect
samples for total or dissolved mercury with zero headspace. For total
or dissolved mercury, the partitioning of volatile forms of mercury
into a relatively small headspace volume is negligible.
EPA has removed the requirement for collecting unpreserved samples
with zero headspace in draft Method 1631D (Section 8.5.1), provided the
sample is tightly capped and is preserved or analyzed within 48 hours
of sample collection. The proposed method does not include a revision
of the requirement to collect samples for methyl mercury with no
headspace.
4. Sample Collection Containers
Section 8.5.1 of EPA Method 1631 requires that unpreserved samples
must be collected in fluoropolymer sample containers. Several users of
EPA Method 1631 have commented that, in addition to fluoropolymer
bottles, glass bottles can be used successfully for collection of
unpreserved samples, provided the containers are demonstrated to be
clean, are tightly capped, and are preserved or analyzed within 48
hours of sample collection.
EPA is soliciting data demonstrating that the use of glass
containers for collection of mercury samples that are not preserved
immediately does not compromise the quality of results obtained using
EPA Method 1631. EPA has revised Sections 2.1, 4.3.7.1, and 8.5.1 in
draft Method 1631D, to allow collection of unpreserved samples in
either clean fluoropolymer or clean glass sample containers.
As discussed previously in Section V.D.1 of this document, EPA is
requesting data to support the comment that samples collected for
measurement of mercury using Method 1631 are stable for up to 30 days
prior to preservation or analysis. EPA will consider submitted data,
and if appropriate, will re-evaluate the requirement for preservation
or analysis of samples within 48 hours.
5. Holding Time
Section 8.5 of EPA Method 1631 states that acid- and BrCl-preserved
samples are stable for a period of 28 days. Several laboratories that
assisted in the development of EPA Method 1631 believe that samples are
stable for at least three months and have provided data to EPA
demonstrating this stability in mercury samples that have been
preserved with either BrCl or HCl. These data are included in the
Record supporting today's rule.
EPA revised Section 8.5 of draft Method 1631D to recognize that
acid- or BrCl-preserved samples that are collected for measuring
mercury using Method 1631 are stable for a period of 90 days. EPA is
also proposing to amend Table II of 40 CFR 136.3(e) to include a
maximum holding time of 90 days for samples collected for determination
of mercury using Method 1631 (see Section VI of this preamble).
E. Shipment of Empty Sample Containers
Section 6.1.2.1 of EPA Method 1631 requires that sample bottles be
filled with 0.4% HCl solution and stored until use. EPA Method 1631
also references Section 6.3.1 of EPA Method 1669, which suggests that
clean sample bottles should be filled with reagent water for shipment
to the sampling site prior to sample collection.
Commenters have stated that EPA Methods 1631 and 1669 should allow
shipment of empty sample bottles to avoid shipping acid and to save
shipping weight. As with sample refrigeration and preservation, EPA is
soliciting data demonstrating whether shipping sample bottles full of
dilute acid or reagent water is necessary and should be required. We
have revised Section 6.1.2.1 in draft Method 1631D to allow shipment of
empty bottles for sample collection based on comments from method
users.
F. Scope of ``Should'' and ``May''
The introduction to EPA Method 1631 contains a note that addresses
the performance-based aspects of the Method. The note states that the
terms ``shall'' and ``must'' define procedures required for producing
reliable data at water quality criteria levels and that the terms
``should'' and ``may'' indicate optional steps that may be modified or
omitted if the laboratory can demonstrate that the modified method
produces results equivalent or superior to results produced by the
unmodified method. As discussed in Section IV of today's notice, EPA is
proposing additional requirements for clean techniques and quality
control that would, if implemented, change certain ``should'' and
``may'' to ``shall'' and ``must.''
Some commenters have interpreted the terms ``should'' and ``may''
as limiting the applicability of the performance-based allowances in
the Method. EPA does not intend this restriction. As stated in Sections
1.8 and 9 of EPA Method 1631, any procedure may be modified, except for
procedures required as defined by the terms ``shall'' and ``must'' and
all QC tests.
To preclude ambiguity, EPA has revised the note in draft Method
1631D to clarify that the laboratory is permitted to omit steps or
modify procedures provided that all performance requirements in this
Method are met, but that the laboratory must not omit or modify any
procedure defined by the term ``shall'' or ``must'' and must perform
all quality control tests.
G. Field Filtration for Dissolved Metals
Both EPA Method 1669 (Section 8.3) and the current version of EPA
Method 1631 (Method 1631C, Section 8.5.3) recommend that filtration of
samples collected for dissolved Hg should be performed in the clean
room of the laboratory. In contrast, 40 CFR 136.3(e), Table II,
footnote 7, says that samples for dissolved metals should be filtered
immediately on-site before adding preservative.
Since promulgation of EPA Method 1631, some commenters have noted
that it is preferable to filter samples for dissolved Hg in the
laboratory under controlled clean conditions. Other commenters,
however, have noted that it is preferable to filter samples for
dissolved Hg immediately upon collection, thereby allowing for in-line
filtration and immediate preservation if desired.
EPA believes that filtration of mercury samples in either the field
or laboratory is appropriate, provided the filtration is performed in a
clean area, and provided that samples are accompanied by a blank that
has been filtered under the same conditions. EPA has revised Sections
2.2 and 8.4 of draft Method 1631D to allow for both in-field and
laboratory sample filtration under these provisions.
EPA is also proposing to amend 40 CFR 136.3(e) Table II to include
requirements for filtration of samples for measurement of dissolved
mercury using Method 1631, in a clean area in the laboratory or in the
field (see Section VI of this preamble for proposed revisions to 40 CFR
136.3(e), Table II).
[[Page 51525]]
H. Carryover Test
The bubbler blank carryover test in EPA Method 1631 is recommended
``when an unusually concentrated sample is encountered'' (Method 1631C,
Section 4.3.8.1) or ``after very high samples'' (Method 1631C, Section
11.2.4).
Several commenters stated that ``unusually concentrated'' and
``high sample'' are not defined. Commenters also have noted that it may
not be practical to stop a run and analyze a bubbler blank immediately
after these samples. Often a sample is determined to have a high Hg
concentration that could result in carryover only after subsequent
samples have been analyzed or at the completion of an analytical batch.
To quantify the concentration of mercury in a sample that would
carry a concentration into a subsequent sample, EPA has included a
carryover test in draft Method 1631D (Section 4.3.8.1) that is similar
to that in Section 8.5.1 of EPA Method 1624B for analysis of volatile
organic compounds using a gas chromatograph/mass spectrometer (40 CFR
Part 136, appendix A). In this test, successively greater
concentrations of mercury in reagent water are analyzed to determine
the concentration at which more than 0.2 ng/L (the MDL in Method 1631)
would be measured in a subsequent bubbler blank.
EPA also has included revisions in draft Method 1631D (Section
4.3.8.1 and Section 11.2.1.3) to require that when an unusually
concentrated sample is encountered, a bubbler blank must be analyzed to
check for carryover and that samples run immediately following a sample
that has been determined to result in carryover must be reanalyzed
using a bubbler that is demonstrated to be free of Hg at the 0.2 ng/L
level.
I. Correction of Part Numbers
Users of Method 1631 have informed EPA that the supplier does not
recognize part numbers for the peristaltic pump or tubing suggested in
the method. The supplier has informed us that the leading letter in the
part number signifies the version of the catalog and should be omitted
from the part number. EPA has corrected these part numbers in proposed
Method 1631D (Sections 6.1.3.2 and 6.1.3.3).
J. Use of Polyethylene or Polypropylene Vessels for Sample Digestion
Most methods for determination of metals allow polyethylene bottles
as sample containers (see 40 CFR Part 136, Table II, footnote 1). EPA
Method 1631 requires use of glass or fluoropolymer because mercury can
diffuse in and out of polyethylene bottles (see Section 16.4 of EPA
Method 1631).
Commenters have stated that, although fluoropolymer or glass
bottles are necessary for sample collection, this type of labware is
not necessary for sample digestion and other laboratory uses, because
mercury will not diffuse through these materials in the relatively
short time during which the sample is analyzed. Because polyethylene
and polypropylene is less expensive than fluoropolymer and is less
susceptible to breakage than glass, EPA has included a revision to this
requirement in draft Method 1631D (Section 4.3.7.1) to allow use of
polyethylene or polypropylene labware for sample digestion and
preparation, but not for sample collection.
K. Indication of Complete Oxidation
Section 8.1 of EPA Method 1631 currently states that the pH of all
aqueous samples must be tested immediately before analysis to ensure
that the sample has been properly preserved.
Users of EPA Method 1631 have noted that the pH of a sample
provides an insufficient indication of whether or not the sample is
completely oxidized or ready for analysis, and cite as an example,
samples containing high concentrations of sulfides or other reducing
compounds that can consume BrCl, but still have a pH less than 2. These
commenters have stated that color is a better indication of complete
oxidation (see Sections 11.1.1.1 and 11.1.1.2 of EPA Method 1631).
EPA proposes to revise Section 8.1 in EPA Method 1631D to recognize
that samples must be completely oxidized prior to direct analysis and
that pH alone is not sufficient for determination of complete
oxidation.
L. Adjustment for Amount of Bromine Monochloride to Blanks
Section 9.4.2.2 of EPA Method 1631 currently requires that the
amount of reagent that is added to a reagent blank must be the same as
the amount of reagent that is added to the samples. One of the
laboratories responsible for the development of EPA Method 1631
commented that this requirement is inconsistent with Section 12.3 which
allows adjustment during calculation of reagent blanks for greater
amounts of reagent that may be added to samples requiring increased
oxidation. Users also have commented that, although the correction
allowed in Section 12.3 is appropriate for volume adjustment, it is not
necessarily appropriate for adjustment of increased reagent
concentration.
In draft Method 1631D, EPA has clarified that a sample requiring
increased oxidation via an increased amount of reagents must be
associated with at least one blank sample that has been analyzed using
procedures identical to those used to prepare and analyze the sample.
This requirement is included with the requirements for method blanks
(draft Method 1631D, Section 9.4.4.3).
M. Addition of Method 1631 Guidance as a Reference
On March 2001, EPA published guidance to assist users with the
implementation and use of EPA Method 1631. This guidance, Guidance for
Implementation and Use of EPA Method 1631 for the Determination of Low-
Level Mercury (40 CFR Part 136) (EPA 821-R-01-023, March 2001), was
developed and published largely in response to the October 19, 2000
Settlement Agreement. EPA has added a reference for this guidance to
draft Method 1631D (Section 16.22).
VI. Proposed Amendment to 40 CFR 136.3(e) Table II
EPA is today proposing to amend Table II at 40 CFR 136.3(e), which
lists required containers, preservation techniques, and maximum holding
times for biological and chemical parameters. This amendment provides
consistency with previously approved requirements in EPA Method 1631
and with requirements proposed today (see Section V of this preamble).
This proposal would add a footnote (17) to Table II to include
requirements for collection, filtration, preservation, and maximum
holding times that are specific to samples collected for determination
of mercury using EPA Method 1631. This footnote would include the
following requirements for mercury samples: samples must be collected
using either fluoropolymer or glass containers, samples must be
preserved with either HCl or BrCl within 48 hours of collection,
preserved samples have a maximum holding time of 90 days, and samples
must be filtered in a clean area in the laboratory or in the field
prior to sample preservation. EPA invites comment on the proposed text
to be added to Table II at 40 CFR 136.3(e).
VII. Administrative Requirements
A. Executive Order 12866--Regulatory Planning and Review
Under Executive Order 12866 [58 FR 51735 (October 4, 1993)], the
Agency must determine whether the regulatory
[[Page 51526]]
action is ``significant'' and therefore subject to Office of Management
and Budget (OMB) review and the requirements of the Executive Order.
The Executive 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. 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, small entity is defined as: (1) A small business as defined
by the U.S. Small Business Administration definitions at 13 CFR
121.201; (2) a small governmental jurisdiction that is a government of
a city, county, town, school district or special district with a
population of less that 50,000; and (3) a small organization that is
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 proposed rule on
small entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. Today's rule
proposes a revised version of a currently approved EPA Method to
include additional requirements for clean techniques and quality
control and to improve and clarify method procedures. Today's rule also
proposes an amendment to Table II at 40 CFR 136.3(e) to provide
consistency with previously approved requirements in Method 1631 and
with revisions proposed today for collection, preservation, and storage
of samples collected for determination of mercury using Method 1631
procedures.
Overall, the cost of these revisions are minimal. While some of the
revisions may increase cost (e.g., clean technique and quality control
requirements), others will provide flexibility and actually lower the
overall analytical costs (e.g., use of new, less expensive equipment).
Only NPDES permitting authorities must use the clean techniques.
Permittees, including small entities, are not required to use them
unless required to do so by their permitting authority. Many of the
laboratories that analyze for mercury are already using the clean
techniques, further minimizing any potential cost increases. EPA
estimates that any costs associated with clean techniques would be
alleviated or eliminated by the additional flexibility resulting from
some of the proposed revisions to the Method that are discussed in
Section V. Therefore, EPA believes that this proposed rule will not
have a significant economic impact on a substantial number of small
entities. We continue to be interested in the potential impacts of the
proposed rule on small entities and welcome comments on issues related
to such impacts.
C. 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, Tribal, and local
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, Tribal, and local 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 of 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 the UMRA a small government agency plan. The plan must
provide for the notification of 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.
EPA has determined that today's proposed rule does not contain a
Federal mandate that may result in expenditures of $100 million or more
for State, Tribal, and local governments, in the aggregate, or the
private sector in any one year. This rule proposes revisions to a
previously approved method for measuring mercury in wastewater. This
rule also proposes to revise Table II at 40 CFR 136.3(e) to clarify
requirements for sample collection, preservation, and storage, and to
make these requirements consistent with previously approved
requirements in EPA Method 1631 and with today's proposed method
revisions. As discussed in Section VII.B regarding RFA analysis, EPA
expects the cost of these revisions to Method 1631 to be minimal. Thus,
today's rule is not subject to sections 202 and 205 of the UMRA. For
the same reasons, EPA has also determined that this rule contains no
regulatory requirements that might significantly or uniquely affect
small governments. Thus, today's rule is not subject to the
requirements of section 203 of the UMRA.
D. Paperwork Reduction Act
This action does not impose an information collection burden under
the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq.
This rule proposes to revise a currently approved test method for use
in water monitoring programs but does not require the use of the test
method.
Burden means the total time, effort, or financial resources
expended by persons to generate, maintain, retain, or disclose or
provide information to or for a Federal agency. This includes the time
needed to review instructions; develop,
[[Page 51527]]
acquire, install, and utilize technology and systems for the purposes
of collecting, validating, and verifying information, processing and
maintaining information, and disclosing and providing information;
adjust the existing ways to comply with any previously applicable
instructions and requirements; train personnel to be able to respond to
a collection of information; search data sources; complete and review
the collection of information; and transmit or otherwise disclose the
information.
An Agency may not conduct or sponsor, and a person is not required
to respond to a collection of information unless it displays a
currently valid OMB control number. The OMB control numbers for EPA's
regulations are listed in 40 CFR Part 9 and 48 CFR Chapter 15.
E. National Technology Transfer and Advancement Act
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., material specifications, test methods,
sampling procedures, business practices) that are developed or adopted
by voluntary consensus standard bodies (VCSBs). 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 proposed rulemaking involves technical standards. Therefore,
the Agency conducted a search to identify potentially applicable
voluntary consensus standards. However, we identified no standard for
the measurement of mercury at low water quality criteria levels or for
the use of ``clean techniques.'' Therefore, EPA proposes to use EPA
Method 1631, Revision D: Mercury in Water by Oxidation, Purge and Trap,
and Cold Vapor Atomic Fluorescence Spectrometry. EPA welcomes comments
on this aspect of the proposed rulemaking and, specifically, invites
the public to identify potentially applicable voluntary consensus
standards for measuring low levels of mercury and for ``clean
techniques'' and to explain why such standards should be used in this
regulation.
F. Executive Order 13045--Protection of Children From Environmental
Health Risks and Safety Risks
Executive Order 13045 (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
proposed rule is not subject to the Executive Order because it is not
economically significant as defined in Executive Order 12866, nor does
it concern an environmental health or safety risk that EPA has reason
to believe may have a disproportionate effect on children.
G. Executive Order 13132--Federalism
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.''
This proposed rule does not have federalism implications. It 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 proposes revisions
to EPA's Method 1631, Revision C, for measuring mercury at low levels
for compliance monitoring under the Clean Water Act. As discussed in
Section VII.B regarding RFA analysis, EPA expects the cost of these
revisions to Method 1631 to be minimal. Thus, Executive Order 13132
does not apply to this rule.
In the spirit of Executive Order 13132, and consistent with EPA
policy to promote communications between EPA and State and local
governments, EPA specifically solicits comment on this proposed rule
from State and local officials.
H. Executive Order 13175--Consultation and Coordination With Indian
Tribal Governments
Executive Order 13175, entitled ``Consultation and Coordination
With Indian Tribal Governments'' (65 FR 67249, November 6, 2000),
requires EPA to develop an accountable process to ensure ``meaningful
and timely input by tribal officials in the development of regulatory
policies that have tribal implications.'' ``Policies that have tribal
implications'' is defined in the Executive Order to include regulations
that have ``substantial direct effects on one or more Indian tribes, on
the relationship between the Federal government and the Indian tribes,
or on the distribution of power and responsibilities between the
Federal government and Indian tribes.''
This proposed rule does not have tribal implications. It will not
have substantial direct effects on tribal governments, on the
relationship between the Federal government and Indian tribes, or on
the distribution of power and responsibilities between the Federal
government and Indian tribes, as specified in Executive Order 13175. As
discussed in Section VII.B regarding RFA analysis, EPA expects the cost
of these revisions to Method 1631 to be minimal. Thus, Executive Order
13175 does not apply to this rule.
In the spirit of Executive Order 13175, and consistent with EPA
policy to promote communications between EPA and tribal governments,
EPA specifically solicits comment on this proposed rule from tribal
officials.
I. Executive Order 13211: Actions Concerning Regulations That
Significantly Affect Energy Supply, Distribution, or Use
This rule is not subject to Executive Order 13211, ``Actions
Concerning Regulations That Significantly Affect Energy Supply,
Distribution, or Use'' (66 FR 28355 (May 22, 2001)) because it is not a
significant regulatory action under Executive Order 12866.
J. Plain Language Directive
Executive Order 12866 requires each agency to write all rules in
plain language. We invite your comments on how to make this proposed
rule easier to understand. For example, have we organized the material
to suit your needs? Are the requirements in the rule clearly stated?
Does the rule contain technical language or jargon that isn't clear?
Would a different format (grouping and order of sections, use of
[[Page 51528]]
headings, paragraphing) make the rule easier to understand? Would more
(but shorter) sections be better? Could we improve clarity by adding
tables, lists, or diagrams? What else could we do to make the rule
easier to understand?
VIII. Request for Comments
EPA encourages public participation in this rulemaking and is
requesting comments on the various EPA Method 1631 revisions detailed
in the proposal. EPA is also requesting data supporting comments, if
available. Specifically, EPA is soliciting comments on: the proposed
requirements for certain quality control and clean techniques that are
currently recommended in the method and that are detailed in Section
IVA of this preamble; the proposal to allow a discharger to elect not
to implement the requirements at Section IVA; the proposed revisions to
Method 1631 that address stakeholder comments and are detailed in
Section V of this preamble; the proposed amendment to 40 CFR 136.3(e)
Table II to include requirements for preservation and storage that are
specific to aqueous samples collected for measurement of mercury using
Method 1631; and the testing costs that may be associated with any of
the proposed method modifications.
To ensure that EPA can properly respond to comments, commenters
should cite, where possible, the paragraph(s) or section(s) in this
proposal or in Method EPA 1631 to which each comment refers.
List of Subjects at 40 CFR Part 136
Environmental protection, Reporting and recordkeeping requirements,
Water pollution control.
Dated: September 28, 2001
Christine Todd Whitman,
Administrator.
For the reasons set out in the preamble, title 40, Chapter I of the
Code of Federal Regulations, is proposed to be amended as follows:
PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS
1. The authority citation for 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 by revising paragraph (b) (41) and by
revising the ``Metals'' entry in Table II of paragraph (e) to read as
follows:
Sec. 136.3 Identification of test procedures.
* * * * *
(b) * * *
(41) USEPA. 2001. Method 1631, Revision D, ``Mercury in Water by
Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence
Spectrometry.'' September 2002. Office of Water, U.S. Environmental
Protection Agency (EPA-821-R-xx-xxx). Available from: National
Technical Information Service, 5285 Port Royal Road, Springfield,
Virginia 22161. Publication No. PB2001-xxxxxx. Cost: $25.50 (subject to
change). Table IB, Note 43.
* * * * *
----------------------------------------------------------------------------------------------------------------
Parameter No./name Container \1\ Preservation 2, 3 Maximum holding time
---------------------------------------------------------------------------------------------------\4\----------
* * * * * *
*
Metals
18. Chromium VI \7\.............. P, G................... Cool, 4 deg.C.......... 24 hours.
35. Mercury \17\................. P, G................... HNO3 to pH2............ 28 days.
3, 5-8, 12,13, 19, 20, 22, 26, P, G................... ......do............... 6 months.
29, 30, 32-34, 36, 37, 45, 47,
51, 52, 58-60, 62, 63, 70-72,
74, 75. Metals except boron,
chromium VI and mercury \7\.
* * * * * *
*
----------------------------------------------------------------------------------------------------------------
\1\ Polyethylene (P) or glass (G). For microbiology, plastic sample containers must be made of sterilizable
materials (polypropylene or other autoclavable plastic), except for samples collected for trace-level mercury
(see footnote 17).
\2\ Sample preservation should be performed immediately upon sample collection. For composite chemical samples
each aliquot should be preserved at the time of collection. When use of an automated sampler makes it
impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4 deg.C until
compositing and sample splitting is completed, except for samples collected for trace-level mercury (see
footnote 17).
\3\ When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply
with the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering
such material for transportation is responsible for ensuring such compliance. For the preservation
requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of
Transportation has determined that the Hazardous Materials Regulations do not apply to the following
materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about
1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about
1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH
about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight
or less (pH about 12.30 or less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before analysis and still be considered valid. (See footnote 17 for samples collected for
trace level mercury). Samples may be held for longer periods only if the permittee, or monitoring laboratory,
has data on file to show that for the specific types of samples under study, the analytes are stable for the
longer time, and has received a variance from the Regional Administrator under Sec. 136.3(e). Some samples
may not be stable for the maximum time period given in the table. A permittee, or monitoring laboratory , is
obligated to hold the sample for a shorter time if knowledge exists to show that this is necessary to maintain
sample stability. See Sec. 136.3(e) for details. The term ``analyze immediately'' usually means within 15
minutes or less of sample collection.
* * * * *
\7\ Samples should be filtered immediately on site before adding preservative for dissolved metals, except for
samples collected for trace-level mercury (see footnote 17).
* * * * *
\17\ Samples collected for the determination of trace level mercury using EPA Method 1631, must be collected in
tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48 hours of
sample collection. Samples for dissolved trace level mercury must be filtered in a clean area in the field or
the laboratory prior to sample preservation. Samples that have been preserved for determination of total or
dissolved trace level mercury must be analyzed within 90 days of sample collection.
[FR Doc. 01-24886 Filed 10-5-01; 8:45 am]
BILLING CODE 6560-50-P