Guidelines Establishing Test Procedures for the Analysis of Pollutants and National Primary Drinking Water Regulations; Flexibility in Existing Test Procedures and Streamlined Proposal of New Test Procedures
Federal RegisterMar 28, 1997
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SUMMARY: The Environmental Protection Agency (EPA) proposes to
streamline the process for EPA approval of analytical methods (and
modifications thereof) under the Clean Water Act (CWA) and the Safe
Drinking Water Act (SDWA). The current methods approval process applies
to and is used by public and private laboratories, manufacturers of
analytical equipment and analysts who modify analytical methods or who
develop new methods for use in compliance monitoring under the CWA and
SDWA. The proposed rule only affects states if they choose to adopt the
proposed streamlined process as part of their laboratory auditing
programs. Under the streamlined methods approval system, EPA would
increase the analyst's flexibility to modify existing test procedures,
expedite approval of new and modified test procedures, establish and
require the use of standardized quality control (QC) and QC acceptance
criteria in existing and new test procedures, and recommend use of
standard data elements for reporting test results. Today's action
responds to the Administration's Environmental Technology and
Reinventing Government Initiatives and the National Technology Transfer
and Advancement Act by promoting use of emerging technologies and
encouraging participation of consensus standards organizations and
other organizations in developing test procedures (analytical methods).
The action proposed in today's rule would increase the options
available to the regulated community in complying with EPA regulations
under the CWA and SDWA. These actions are only an initial and interim
step in the Agency's pursuit of a performance-based approach to
environmental measurements, and are not meant to define or limit the
Agency's ultimate implementation of a ``pure'' performance-based
measurement system. The increased flexibility provided by this proposed
action should significantly reduce the need for Agency review of
alternate test procedures and make it easier for the analyst to select
analytical methods that are most suited to specific regulatory
measurement needs.
DATES: Comments on this proposed rule will be accepted until June 26,
1997.
ADDRESSES: Send written comments to the Streamlining Methods Docket
Clerk, Water Docket (MC-4101), USEPA, 401 M Street, SW., Washington, DC
20460. Please submit an original and three copies of your comments and
enclosures (including references). To ensure that EPA can read,
understand and therefore properly respond to comments, the Agency would
prefer that commenters cite, where possible, the paragraph(s) or
sections in the proposed regulation or in the supporting documents to
which each comment refers. Commenters should use a separate paragraph
for each issue discussed. Commenters who want EPA to acknowledge
receipt of their comments should enclose a self-addressed, stamped
envelope. No facsimiles (faxes) or electronic mail (email) will be
accepted because EPA cannot ensure that they will be submitted to the
Water Docket. A copy of the supporting documents cited in this proposal
are available for review at EPA's Water Docket, 401 M Street, SW.,
Washington, DC 20460. For access to docket materials, call 202/260-3027
between 9:00 a.m. and 3:30 p.m. for an appointment.
FOR FURTHER INFORMATION CONTACT: Dr. Richard Reding, USEPA, Office of
Ground Water and Drinking Water (MS-140), 26 W. Martin Luther King
Drive, Cincinnati, OH 45268, 513/569-7961.
SUPPLEMENTARY INFORMATION: The supporting documents that are a part of
the administrative record for this proposal may be obtained from the
National Center for Environmental Publications and Information (NCEPI)
(513/489-8190), from the National Technical Information Service (NTIS)
(703/487-4650), from the Educational Resources Information Center
(ERIC) (800/276-0462), and via the Internet on the EPA Office of Water
home page at http://www.epa.gov/watrhome. These documents are titled,
Guide to Method Flexibility and Approval of EPA Water Methods, December
1996 Draft, EPA-821-D-96-004, NTIS PB97-117766, ERIC D-A43 or D-A46
(diskette) (Streamlining Guide, EPA 1996a), Methods for Organic
Chemical Analysis of Municipal and Industrial Wastewater, December
1996, EPA-821-B-96-005, NTIS PB97-125298, ERIC D-A44 or D-A47
(diskette) (Organic Methods, EPA 1996b), and Guidelines and Format for
Methods to Be Proposed at 40 CFR Part 136 or Part 141, July 1996, EPA-
821-B-96-003, NTIS PB96-210448, ERIC D-A42 or D-A45 (diskette) (Method
Guidelines and Format, EPA 1996c).
Regulated Entities
Entities potentially regulated by this action are those who seek
EPA approval of analytical technologies for monitoring under the
provisions of the CWA and SDWA. Entities potentially regulated by this
action are listed in the table below. These entities potentially
include consensus methods organizations that publish compendiums of
analytical methods for water, and equipment manufacturers, instrument
manufacturers and laboratories that modify compliance methods or seek
approval of new methods for compliance monitoring.
------------------------------------------------------------------------
Category Examples of regulated entities
------------------------------------------------------------------------
Public............................ Government laboratories that develop
analytical methods for compliance
with the CWA and the SDWA.
Private........................... Commercial laboratories, consensus
methods organizations, instrument
manufacturers, vendors, and other
entities that develop or publish
analytical methods for compliance
with the CWA and the SDWA.
------------------------------------------------------------------------
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. To determine whether
your organization is likely to be regulated by this action, you should
carefully read the applicability language of today's rule at
Secs. 136.4, 136.5 and 141.27. If you have questions regarding the
applicability of this action to a particular entity, consult the
individual listed in the preceding FOR FURTHER INFORMATION CONTACT
section.
Table of Contents
I. Authority
A. Clean Water Act
B. Safe Drinking Water Act
II. Background and History
A. Introduction
B. Current Office of Water Methods Approval Programs
C. Streamlining Initiative
D. Streamlining Objectives
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E. Public Meetings and Stakeholder Participation in Streamlining
Development
F. Preamble Structure
III. Summary of Proposed Rule
A. Method Flexibility
1. Reference Method
2. Method Modifications
B. Quality Control
1. Standardized Quality Control Elements
2. Development of QC Acceptance Criteria
C. Method Validation for Modified or New Methods
1. Validation Study Plan
2. Testing
Table I. Summary of Validation Requirements for New Methods and
Method Modifications
3. Validation Study Report
4. Further Validation of a New Method
5. Approval of a Screening Method as a New Method
D. Method Review and Approval
Table II. EPA Review and Action for New and Modified Methods
1. Review and Approval of New Methods
2. Review and Approval of Modified Methods
3. Submission Package
4. Regulatory Assistance Provided by Submitter
5. EPA Review of Submission Package
6. Proposal of Methods
E. Other Issues
1. Legal Impacts
2. Method-defined Analytes
3. Biological Methods
4. Proprietary Reagents, Instruments, and Methods
5. Restrictions by Consensus Standards Organizations
6. Standard Data Format
7. Withdrawal of Outdated Methods
8. Administrative Record: Organic Methods, Streamlining Guide,
and Method Guidelines and Format
9. Coordination with Other Federal Register Proposals
IV. Regulatory Analysis
A. Executive Order 12866
B. Unfunded Mandates
C. Regulatory Flexibility Act
D. Paperwork Reduction Act
V. Request for Comments
A. General
B. Specific
VI. References
I. Authority
A. Clean Water Act
The Clean Water Act (CWA) requires the U.S. Environmental
Protection Agency (EPA) Administrator to promulgate effluent
limitations guidelines for specified categories and classes of point
sources. Section 301 of CWA prohibits the discharge of any pollutant
into navigable waters unless the discharge complies with a National
Pollutant Discharge Elimination System (NPDES) permit issued under CWA
section 402. Section 307 requires the EPA Administrator to publish
regulations establishing pretreatment standards for introduction of
pollutants into publicly owned treatment works (POTWs). Section 401
requires State and Tribal certification of a federal license that may
result in any discharge into the navigable waters.
Section 304(h) of CWA requires the EPA Administrator to promulgate
guidelines establishing test procedures for data gathering and for
monitoring compliance with published guidelines. EPA's promulgation of
analytical methods is authorized under this section of CWA, as well as
the general rulemaking authority in CWA section 501(a). The section
304(h) test procedures (analytical methods) are published or
incorporated by reference at 40 CFR part 136. They include Methods for
Chemical Analysis of Water and Wastes (MCAWW); the EPA 200-, 600-, and
1600-series methods; methods published by consensus standards
organizations such as ASTM, AOAC-International, and Standard Methods
for the Examination of Water and Wastewater (Standard Methods)
published jointly by the American Public Health Association (APHA), the
American Water Works Association (AWWA), and the Water Environment
Federation (WEF); methods used by the U.S. Geological Survey; methods
developed by third parties; and other methods referenced in CWA
regulations. These methods support development of effluent limitations
guidelines and standards promulgated at 40 CFR parts 405-503, establish
compliance with NPDES permits issued under CWA section 402, allow
implementation of the pretreatment standards issued under CWA section
307, and apply to the certification of compliance with State water
quality standards under CWA section 401.
B. Safe Drinking Water Act
The Safe Drinking Water Act (SDWA) requires the EPA Administrator
to promulgate national primary drinking water regulations (NPDWRs) that
specify maximum contaminant levels (MCLs) or treatment techniques for
listed drinking water contaminants (section 1412). Section 1445(a)
authorizes the Administrator to establish regulations for monitoring to
assist in determining whether persons comply with the requirements of
SDWA. EPA's promulgation of analytical methods is authorized under
these sections of SDWA, as well as the general rulemaking authority in
SDWA section 1450(a).
SDWA section 1401(1)(D) specifies that NPDWRs contain criteria and
procedures to ensure a supply of drinking water that dependably
complies with MCLs, including quality control (QC) and testing
procedures to ensure compliance with such levels and to ensure proper
operation and maintenance of drinking water supply and distribution
systems. These test procedures are promulgated at 40 CFR part 141 and
include three MCAWW methods, the 200-, 300-, and 500-series EPA
methods, methods published by consensus standards organizations, and
other methods referenced in SDWA regulations. EPA uses these test
procedures to establish MCLs under SDWA section 1412 and to establish
monitoring requirements under SDWA section 1445(a).
II. Background and History
A. Introduction
Within EPA, the Office of Water (OW) publishes analytical methods
for use in data gathering and environmental monitoring under the Clean
Water Act (CWA) and the Safe Drinking Water Act (SDWA). These methods
have been developed by EPA, by consensus standards organizations, and
by others. Many of these methods, especially those published before
1988, are prescriptive, with limited flexibility to change technologies
to respond to specific situations or to incorporate advances in
measurement technology. There has been a growing awareness, both within
EPA and in the analytical community, that the requirement to use
prescriptive measurement methods to comply with Agency regulations has
imposed an unintended regulatory burden and potentially created a
barrier to innovation in environmental monitoring.
To reduce this regulatory burden and to lower the barriers to
innovation, the Agency in a future rulemaking may propose to adopt a
completely performance-based approach to environmental measurements. As
envisioned under such an approach, the Agency would specify the
question(s) to be answered by the measurement, the decision(s) to be
supported by the data, and the level of uncertainty that is acceptable.
EPA would specify performance criteria for the measurement and data
producers would be required to demonstrate that their proposed
measurement system (i.e., methods, sample handling procedures) meets
these specific performance criteria. Data producers would be required
to document performance and certify that they have used appropriate
quality assurance and QC procedures. The system would apply to
physical, chemical, and biological measurements
[[Page 14978]]
conducted either in laboratories or in the field (EPA 1996d).
In a series of steps designed to adopt the performance-based
approach, each program office in the Agency has developed (or will
develop) an implementation plan that describes how the performance-
based approach would be put into practice. The Agency's goal is to have
these implementation plans as consistent as possible (i.e.,
``harmonized'') from program to program (EPA 1996e). The streamlining
initiative proposed in today's notice describes how EPA's Office of
Water is taking immediate steps to remove some of the regulatory
barriers to the use of new technologies for environmental measurements
of chemical analytes under the CWA and SDWA. This initiative would use
reference chemical methods that contain performance criteria and
methods that are already approved at 40 CFR parts 136 and 141. Other
implementation approaches to a performance-based measurement system,
such as listing in the CFR only the required performance criteria for
the measurement, are also possible; these approaches, which are not the
subject of today's proposal, may be the subject of future rulemakings.
Today's rule proposes a process that would use standardized QC, QC
acceptance criteria, and method validation procedures for stakeholders
to gain approval of new and modified methods for compliance monitoring
under the SDWA and CWA. Today's rule also proposes to designate certain
approved drinking water and wastewater methods as reference methods.
The approved reference methods either presently contain QC acceptance
criteria, are supplemented with these criteria in today's proposal, or
would be supplemented with these criteria in a future rulemaking. In
subsequent rulemakings, EPA intends to extend the streamlined method
approval process to physical and biological (including microbiological)
measurements in the water programs.
Through public meetings, announcements, and technical
presentations, EPA's Office of Water has coordinated this streamlining
initiative with various EPA Headquarters offices, EPA Regions, the
States, other governmental agencies, industry, consensus standards
organizations, environmental laboratories, and other interested
parties. With today's proposal, EPA attempts to define a comprehensive
program to increase analytical choices in selection of compliance
monitoring methods and to streamline the procedures for approval of
water methods. In this initiative, EPA seeks to promote rapid
introduction of innovative technologies, to encourage non-EPA
organizations to participate in the method development and approval
process, and to implement procedures to expedite the review and
approval of new and modified methods. Most importantly, EPA believes
that this initiative also offers the opportunity to improve the quality
of environmental monitoring.
The proposed streamlined procedures for approval of water methods
would allow analysts to use professional judgement to modify and
develop alternatives to established Agency methods and to take
advantage of emerging technologies that reduce costs, overcome
analytical difficulties, and enhance data quality. The proposal to
increase the flexibility to modify reference methods would be governed
by QC acceptance criteria designed to ensure that the quality of the
environmental data would not be compromised. These criteria would be
used to demonstrate that a modified method produces results equal or
superior to results produced by the reference method. EPA also proposes
to require that all new methods contain such QC acceptance criteria so
that modifications could be made to new methods.
EPA believes that allowing reference method modifications and
providing rapid approval of new methods would yield several benefits.
On behalf of regulated entities, analysts could select the analytical
method that yields the best performance in a specific situation. The QC
acceptance criteria in the reference method would enable the analyst to
document equivalent or superior performance to the satisfaction of
reviewing authorities. New technologies could be utilized to overcome
matrix interference problems, lower detection limits, improve
laboratory productivity, or reduce the amount of hazardous materials
used and hazardous wastes produced in the laboratory.
A more flexible method approval program is consistent with the
Administration's Environmental Technology and Reinventing Government
initiatives and the National Technology Transfer and Advancement Act of
1995 (NTTAA). The proposed program would empower stakeholders while
decreasing demands on Agency resources and is intended to accelerate
environmental technological innovation while enhancing and maintaining
environmental protection. EPA believes that the incentives provided by
a more flexible water test methods approval program would spur the
development of new technologies and, with them, new jobs. EPA also
anticipates that the use of new technologies may lower the cost of
environmental measurements, thereby reducing costs of environmental
compliance for American industries and municipalities.
B. Current Office of Water Methods Approval Programs
Requirements for approval of alternate analytical techniques
(methods) are specified at 40 CFR 136.4 and 136.5 for wastewater and at
40 CFR 141.27 for drinking water methods. These requirements are the
basis for the Agency's alternative test procedures (ATP) program for
water methods. Under the ATP program, persons may request approval to
modify steps in a reference method or approval to use a new method. The
person that submits the ATP application is responsible for validating
the new or modified method. Agency staff review the ATP validation
package and, if required, successful applications undergo formal
rulemaking. Rulemaking is required when a new or revised method is to
be added to the list of approved methods in the CFR. The ATP and
rulemaking processes make heavy demands on stakeholder, contractor,
EPA, and Office of Federal Register resources. The process can require
one to two years to gain approval of a method. Because advances in
analytical technology continue to outpace the capacity of OW's methods
approval program, the program is slow to respond to emerging
technologies and has been under-utilized. Under the streamlining
initiative described below, EPA proposes to increase method flexibility
by amending the procedures at 40 CFR 136.4, 136.5 and 141.27 to specify
a more rapid and less resource intensive process for approval of new
technologies.
C. Streamlining Initiative
The proposed streamlining initiative is designed to improve overall
resource use while making the method development process more efficient
and accessible to non-EPA organizations. The goals of the initiative
are to decrease the need for developers of modified methods to use the
ATP program and to speed up the approval (or disapproval) of methods
subject to ATP review. EPA believes the streamlining initiative would
(1) encourage the use of emerging technologies by increasing the
flexibility to modify approved methods without formal EPA approval, (2)
provide a mechanism for non-EPA organizations to develop and submit new
methods for
[[Page 14979]]
approval, and (3) expedite the approval of new and modified methods by
improving the current ATP program. This initiative applies to approval
of wastewater and drinking water methods. Because of current emphases
on decreasing redundant activities, forming partnerships with
stakeholders, and more quickly adopting advances in technology, EPA
believes this is an appropriate time to look to organizations outside
of EPA for assistance in developing new methods that take advantage of
emerging technologies that reduce costs, overcome analytical
difficulties, and enhance data quality. Once the streamlining
initiative is in place, EPA expects to increase its reliance on outside
organizations as the developers of many new methods. EPA would focus
its method development activities on specialized or esoteric methods
needed to support regulation development or compliance monitoring.
OW has coordinated the development of the streamlining initiative
with various governmental entities, industry, consensus standards
organizations, environmental laboratories, and other interested
parties. These organizations include the National Environmental
Laboratory Accreditation Committee (NELAC), and the Interagency
Steering Committee for Quality Assurance for Environmental
Measurements, which includes representatives from the Department of
Energy, Department of Defense, EPA, Air Force, U.S. Army Corps of
Engineers, U.S. Geological Survey (USGS), Bureau of Reclamation, and
other organizations.
D. Streamlining Objectives
The purpose of the streamlining initiative is to implement a more
performance-based approach to environmental measurements under the SDWA
and CWA. The proposed streamlined methods approval procedures would
revolutionize the water methods approval program to expand the
flexibility to modify existing methods, provide a mechanism for non-EPA
organizations to gain approval of new methods, and expedite the
approval of new and modified methods. EPA has defined several specific
streamlining objectives:
Increase the current flexibility to modify approved
chemical test procedures (methods) without formal EPA approval; this
would allow laboratories to overcome matrix interferences and would
facilitate early introduction of innovative technologies.
Designate a reference method for each unique
combination of analyte and determinative technique and establish
standardized QC tests for approved methods to ensure data quality.
Develop and publish QC acceptance criteria for any
reference method that does not have these criteria so that
laboratories can demonstrate equivalent or superior performance of a
modified method.
Provide a standard method format and mechanism for
validation and approval of new methods to expedite method approval
and to increase confidence in the validity of the methods and
resulting data.
Encourage stakeholder participation in method
development to keep pace with emerging technologies.
Harmonize the wastewater and drinking water test
procedures to eliminate unnecessary inconsistencies.
Increase standardized data reporting by recommending
use of standard data elements for reporting analytical results for
environmental and QC samples.
Identify and propose withdrawal of outdated or obsolete
methods from 40 CFR parts 136 and 141 to modernize approved test
methods and to eliminate methods that are no longer published by the
issuing government agency, consensus methods organization, or
vendor.
Work with the Office of Federal Register to incorporate
more methods by reference to reduce the volume of material published
in the CFR while ensuring and improving access to those methods by
all interested parties.
E. Public Meetings and Stakeholder Participation in Streamlining
Development
EPA conducted four public meetings to develop a streamlined water
test methods approval program. EPA held the meetings in Seattle,
Washington, on September 28, 1995; in Boston, Massachusetts, on January
25, 1996; in Chicago, Illinois, on February 14, 1996; and in Denver,
Colorado, on July 24, 1996. The purpose of the meetings was to present
and discuss EPA's draft of the streamlining initiative and obtain
stakeholder advice for refining the streamlining approach prior to
proposal.
All meetings were announced in the Federal Register in advance. The
first meeting, held in Seattle, was announced on September 12, 1995, in
a Federal Register notice titled, ``A Public Meeting and Availability
of Documents on Streamlining Approval of Analytical Methods at 40 CFR
part 136 and Flexibility in Existing Test Methods'' (60 FR 47325). This
Federal Register notice provided supplementary information regarding
the streamlining effort and made available several supporting
documents. Subsequent public meetings in Boston and Chicago were
announced on December 18, 1995 (60 FR 65207), and the fourth public
meeting in Denver was announced on July 10, 1996 (61 FR 36328). The
supporting documents and summaries of the four public meetings are in
the rule docket.
In addition to the public meetings, EPA solicited support and
expertise from each of the consensus standards organizations and
government agencies that developed the methods already approved for use
under the wastewater and drinking water programs. These groups include
the American Public Health Association (APHA), American Water Works
Association (AWWA), and Water Environment Federation (WEF) as
publishers of Standard Methods for the Examination of Water and
Wastewater (Standard Methods); ASTM (formerly, American Society for
Testing and Materials); AOAC-International (formerly, the Association
of Official Analytical Chemists); and the USGS. EPA also provided the
opportunity for individuals, the regulated industry, the States, local
permitting authorities, vendors, laboratories, and laboratory
organizations such as the International Association of Environmental
Testing Laboratories (IAETL), to voice opinions at the meetings. The
groups offered valuable insight concerning problems with the current
program and recommended areas of improvement.
Through the public meeting process and through individual meetings
with key stakeholder organizations, EPA received input from more than
400 stakeholders, including all major stakeholder organizations.
Following the first three public meetings, EPA compiled and
reviewed preliminary stakeholder advice to assess the initial response
to streamlining and revise the approach accordingly. In response to
stakeholder suggestions, EPA made the following changes to the
streamlining initiative:
Included drinking water methods (40 CFR part 141);
Expanded flexibility to allow changes to the
determinative technique;
Qualified flexibility to clarify that flexibility in
front-end techniques does not apply to sample collection and
preservation;
Expanded Tier 1 validation to allow single-laboratory
application of a method modification to multiple matrix types;
Added an option to have EPA review Tier 2 and Tier 3
method modifications upon request;
Added an option to have EPA formally approve, upon
request, Tier 2 and Tier 3 method modifications through rulemaking;
and
Added an option to submit screening methods to EPA for
approval.
The Streamlining Guide (EPA 1996a) and Method Guidelines and Format
(EPA 1996c) served as the revised draft of the streamlining initiative
that was discussed at the final public meeting on streamlining held in
Denver. This
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proposed rule incorporates suggestions received at the Denver public
meeting, at previous public meetings, by mail, by electronic mail, and
in informal discussions with and among EPA personnel, EPA contractors,
and stakeholders.
Based upon the extensive involvement of internal and external
parties, and the generally favorable response, EPA anticipates that the
proposed regulations will be well received by regulatory authorities,
the regulated community, the technology development community, and the
laboratory service community.
F. Preamble Structure
Section III of this preamble outlines the key elements of
streamlining. Section III.A describes EPA's proposal for increased
flexibility within the method approval program and increased
flexibility for modifications to existing methods. Section III.B
describes the standardized QC requirements and QC acceptance criteria
associated with implementation of flexibility. Section III.C describes
the requirements for validating new methods and method modifications,
using a system based on the intended application of the method or
modification. Section III.D describes the expedited method approval
process and includes procedures for submitting validated methods to EPA
for approval. Section III.E describes other issues associated with the
streamlining initiative. The descriptions in Section III delineate the
framework of EPA's method flexibility and methods approval streamlining
initiative. The Streamlining Guide (EPA 1996a) and other supporting
documents cited in this notice contain specifics about the start-up and
operation of the proposed streamlining initiative.
III. Summary of Proposed Rule
A. Method Flexibility
In developing plans to improve the method approval program for
drinking water and wastewater methods, EPA concluded that the program's
success would depend largely on its ability to reflect the latest
advances in technology. This required, in turn, that the program be
efficient and flexible enough to encourage the development and use of
new measurement techniques. To meet these objectives, EPA determined
that the improved program would have two types of flexibility:
(1) Flexibility to modify reference methods without seeking formal
approval through the regulatory process, and
(2) Flexibility to develop and submit for approval entirely new
methods.
The first type of flexibility is primarily an expansion of the
flexibility already provided in some approved water methods. Under the
streamlining program, it would no longer be necessary to apply for ATP
approval of a method modification, because an analyst would only need
to demonstrate and document that the modified method produces results
equal or superior to results produced by an EPA-designated reference
method. A designated reference method that contains QC acceptance
criteria against which performance of a method modification could be
measured would be the primary control to ensure data quality. Other
controls would include specific multi-laboratory and multi-matrix
requirements for validating modified methods and checklists for
documenting equivalency.
The second type of flexibility would expand the ATP concept by
providing a mechanism whereby entirely new techniques would be
submitted to the Agency for approval, even when these techniques would
not serve as alternates to currently approved methods.
In designing a framework through which this flexibility could be
implemented, EPA sought to balance the advantages of increased
flexibility against the concern that results produced by modifications
would be inferior to results produced by approved methods. To ensure
that these competing objectives could be met, EPA has devised a
framework that is based on:
(1) Use of a standardized QC program with elements that could be
applied to all new and existing methods, and that is stringent enough
to meet compliance monitoring objectives, extensive enough to be
applied to a wide variety of analytical procedures, and yet simple
enough to avoid unwieldy or unnecessary restrictions;
(2) Development and application of QC acceptance criteria for each
QC element against which method modifications could be assessed and
documented; and
(3) Designation of a single reference method for each unique
combination of analyte and determinative technique. This reference
method would contain the QC acceptance criteria used to assess each QC
element for method equivalency.
In today's proposed revisions to 40 CFR parts 136 and 141, EPA
would define the QC elements and associated acceptance criteria (e.g.,
calibration, sensitivity, accuracy, precision) necessary to demonstrate
the equivalency of a modified method to a reference method. These
proposed QC requirements are based on the three components outlined
above. Once equivalency was demonstrated, a modified method could be
used immediately without review by EPA because EPA would have
``preapproved'' the modified method.
EPA believes that incorporating method flexibility into approved
analytical methods would improve laboratory operations by allowing
analysts to rely on professional judgement to ascertain the procedures
and protocols necessary to obtain the best results. Analysts could
employ new technologies to overcome matrix interferences, lower
detection limits, improve the reliability of results, reduce the
generation of hazardous wastes, improve laboratory productivity, and
reduce analytical costs.
1. Reference Method
The foundation of the flexibility concept is the use of a reference
method. For each unique combination of analyte and determinative
technique, EPA has identified or would designate one approved method as
the reference method. If the performance of the modified method is
equal or superior to the performance of the reference method, the
method modification would be allowed. EPA believes that the use of a
reference method with defined QC acceptance criteria as the performance
measure provides a means for implementing the streamlining initiative.
This approach would clarify and reduce the effort required to
demonstrate the equivalency of method modifications.
To implement the streamlining initiative, all reference methods
would need to specify standardized QC and QC acceptance criteria. The
QC and QC acceptance criteria would be necessary to demonstrate method
equivalency. Some methods, such as those approved at 40 CFR part 136,
Appendix A, already contain the necessary standardized QC and QC
acceptance criteria. Some other methods do not specifically identify
acceptance criteria for all of the standardized QC elements, but EPA
has the data from which such criteria could be developed. For this
proposed rule, selection of reference methods was based either on the
existence of QC acceptance criteria in the method or the availability
of data from which QC acceptance criteria could be developed. EPA is
proposing QC acceptance criteria for some inorganic analytes and
reference methods. These criteria are specified at 40 CFR 136.3 Table
IF and at 141.27(d) in the proposed rule text.
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The remaining criteria for other analytes and reference methods would
be developed and proposed in subsequent rulemaking(s).
For some determinative techniques, no currently approved method
contained either all of the QC acceptance criteria proposed in today's
rule (e.g., Table ID in 40 CFR part 136) or sufficient data from which
to develop such criteria. In these cases, no reference method has been
proposed; therefore, all of those methods would be classified as other
approved methods. Without a reference method, users would not be able
to implement the method flexibility proposed in this streamlining
initiative.
EPA plans to include standardized QC with QC acceptance criteria in
all water methods under development and for all future water methods.
However, for drinking water methods, some of the QC acceptance criteria
(e.g., laboratory certification criteria) are currently (and may
continue to be) specified in drinking water regulations because these
criteria are an integral part of EPA's compliance monitoring
requirements.
In the future, the selection of a new reference method would depend
upon requirements imposed by the submitting organization, the
availability of standardized QC and QC acceptance criteria in the
method, and the timing of the selection. EPA intends to rely on outside
organizations to develop the majority of the new methods. Therefore, it
is anticipated that new reference methods for a particular
determinative technique would be designated by being the first method
approved for the given combination of analyte and determinative
technique. To become a reference method, the new method would need to
contain standardized QC and QC acceptance criteria, and be approved
through an Agency rulemaking.
The purpose of specifying a single reference method for a specific
combination of analyte and determinative technique is to avoid the
possible confusion that could be created if two or more reference
methods contained differing QC acceptance criteria. The QC acceptance
criteria associated with the single reference method would be the sole
criteria against which a method modification would be tested.
In today's action, EPA proposes to retain all methods approved for
use at 40 CFR parts 136 or 141, but would re-categorize each of these
methods as either a ``reference method'' or an ``other approved
method.'' Both types of methods would carry equal regulatory status.
The difference between the methods would be that the reference method
would contain (or would be supplemented with) detailed QC acceptance
criteria that would need to be used to assess the equivalency of a
method modification.
2. Method Modifications
Currently, explicit flexibility to modify a method is provided in
some of the approved 200-, 300-, 500-, 600-, and 1600-series methods
published by EPA. The allowed flexibility is typically specified
through use of the term ``should'' or the words ``or equivalent.''
Substitution of a 500-mL beaker for a 250-mL beaker or use of an
``equivalent'' chromatographic column are examples of such explicit
flexibility. The EPA 600- and 1600-series wastewater methods approved
at 40 CFR part 136, Appendix A, also provide limited flexibility to
improve separations and reduce the cost of measurements as long as
method performance is not sacrificed. As specified in those methods,
analysts who choose to exercise explicit flexibility are required to
meet the QC acceptance criteria of the approved method and to maintain
a record of the performance of the modified method for review at the
request of an auditor. In the development of more recent methods (e.g.,
Method 1664 and Method 1613), EPA expanded its definition of ``allowed
flexibility'' to further encourage use of new techniques that provide
equal or better performance at lower costs. However, no approved
methods provide unlimited flexibility and few provide the extensive
flexibility that EPA proposes in this initiative.
The categories of method modifications considered in this proposal
are: (1) Sample collection and holding procedures, (2) front-end
techniques, (3) determinative techniques, and (4) analyte addition.
These categories are defined below and described in terms of present
and proposed flexibility to modify the procedures or techniques
included in each category.
The first category, sample collection and holding procedures,
includes procedures and reagents used in the field, in transit, and at
the laboratory. This category includes sample containers, sample
holding times, preservation reagents and procedures, and shipping and
storage procedures and conditions. Currently, the Regional
Administrator may approve modifications to these procedures for
wastewater methods if the submitter so requests as specified at 40 CFR
136.3(c). In the drinking water program, except as explicitly allowed
in the compliance method, modifications of sample collection and
holding procedures would be approved through the ATP specification at
40 CFR 141.27.
The flexibility proposed in today's rule would not extend to sample
collection or holding procedures. Upon implementation of streamlining,
modifications to sample collection and preservation conditions would
continue to require EPA approval as specified at 40 CFR 136.3(c) and
141.27(b). The latter section, 141.27(b), is a proposed amendment of 40
CFR 141.27 that was written to conform more closely with the
modification provisions at 40 CFR 136.3.
Front-end techniques, the second category of method modifications,
are steps in the analytical process used at the laboratory that precede
the determinative technique and include all procedures, equipment,
solvents, etc., that are used to prepare a sample for analysis. The
third category is the determinative technique, which is defined as the
physical and/or chemical process by which an analyte is identified and
its concentration measured. For most methods, the determinative
technique consists of an instrumental measurement (e.g., a detector).
The fourth category covers increasing the analytical scope of a
reference method to include additional analytes.
Historically, the wastewater program has allowed some changes to
front-end techniques, but only a few methods allow changes to the
determinative step. The drinking water program has allowed similar
changes provided the chemistry of the method is not changed. This means
that some modifications, such as changing the extraction solvent, are
not allowed in drinking water methods unless they receive formal EPA
approval.
This proposed rule expands and more clearly defines proposed
modifications to approved methods. EPA proposes to allow the laboratory
analyst the flexibility to modify any and all front-end techniques,
provided the modification is not explicitly prohibited in the reference
method and provided the analyst demonstrates and documents that the
modification produces results equal or superior to results produced by
the reference method. The laboratory analyst would keep on file the
documents that demonstrate equivalency. Readers are referred to the
Streamlining Guide (EPA 1996a) for more guidance on this subject.
EPA considered restricting the flexibility to change front-end
procedures, such as extraction solvents,
[[Page 14982]]
solvent-to-sample volumes, extraction media, and pH, because such
changes require a deeper understanding of the measurement science than
some users may have. However, EPA is not proposing to restrict front-
end flexibility because EPA believes it is appropriate to allow the
method development and auditing communities an opportunity to comment
on a far-reaching change to the current system. The developer of a
modified method always would have the option to ask EPA or another
regulatory authority for a technical opinion on the acceptability of
the validation data that supports the method. In the list of questions
at the end of this preamble, EPA invites public comment on what, if
any, additional QC would be needed to document the acceptability of
front-end modifications to a reference method.
EPA proposes to allow use of an alternate determinative technique
that is not explicitly prohibited in the reference method, provided
that the analyst could demonstrate and document equivalency as outlined
above, and provided that four conditions could be met: (1) The
alternate determinative technique measures a property similar to the
prescribed technique, (2) the alternate technique is demonstrated to be
more specific (i.e., provides better separation of the analyte from
interferences) and/or more sensitive (i.e., produces a lower detection
limit) for the analyte of concern than the determinative technique in
the reference method, (3) there is not another approved method that
uses the alternate determinative technique for the determination of
that analyte, and (4) use of the alternate determinative technique
would not result in a nonsensical combination of analyte, front-end
technique, and determinative technique.
Examples of allowed changes to a determinative technique would be
substitution of a photoionization detector for a flame ionization
detector for determination of polynuclear aromatic hydrocarbons,
substitution of a nitrogen-phosphorous detector for an electron capture
detector (ECD) for determination of analytes containing nitrogen or
phosphorous, and substitution of a fluorescence detector for an
ultraviolet or visible wavelength detector. Substitution of a mass
spectrometer (MS) for an ECD would not be allowed if there is an
approved MS method that measures the analyte of concern. Readers are
referred to the Streamlining Guide (EPA 1996a) for more guidance on
this subject.
EPA proposes to limit changes to a determinative technique by the
four conditions described above to preclude nonsensical combinations of
analyte and determinative technique, to encourage a net benefit
(increased sensitivity and/or specificity), and to preclude multiple
reference methods with the same determinative technique but with
different QC acceptance criteria for the same analyte(s) of concern.
For example, if a mass spectrometer were substituted for the
conventional detectors in EPA methods 601-612, all of these methods
would become GC/MS methods, but all would contain different QC
acceptance criteria. Further, they would all conflict with approved GC/
MS Methods 625 and 1625. The proposed criteria for detector
substitution also would be consistent with EPA's decision in the
December 5, 1994, drinking water methods final rule (59 FR 62456) not
to allow substitution of MS in methods that specify conventional GC
detectors.
Another reason for proposing to limit changes to the determinative
technique is that there are techniques, such as immunoassay, for which
EPA has no reference method and therefore no history to ensure that the
standardized QC proposed in today's rule would be germane to, or
adequate for, assurance of the quality of data produced by the novel
determinative technique. EPA would prefer that a new method be written
and submitted for approval when a novel determinative technique is
developed. EPA invites public comment on the suitability of the
conditions EPA proposes to place on the flexibility to modify
determinative techniques in EPA reference methods.
In today's proposed rule, EPA also has specified how the analyst
would modify the analytical scope of a reference method to add
additional analytes. This option is proposed in response to public
comment on previous rules (59 FR 62456, December 5, 1994; 58 FR 65622,
December 15, 1993) to extend the scope of a reference method to the
determination of other analytes. Method developers seek this approval
when they want to adapt an existing method rather than develop a new
one to obtain occurrence data for a new analyte. EPA believes these
requests would have merit when there is a potential for new regulatory
requirements and historical monitoring data would be useful in making
process, treatment, or regulatory decisions. Examples of monitoring for
a new analyte would include industrial or POTW monitoring for ethers in
a discharge, public water system (PWS) monitoring for unregulated
pesticides or pesticide metabolites, and PWS monitoring for analytes on
the drinking water priority list. EPA also believes these requests
would have merit when technological advances would make the measurement
of additional analytes feasible (e.g., adding lead to the scope of EPA
Method 200.7). Under the proposed flexibility procedures for modified
and new methods, developers would obtain approval for the addition of
analytes to a reference method as an allowed method modification if the
conditions below would be met.
An analyst may add a new target analyte to a reference method
provided (1) it could be demonstrated that the analyte would not
interfere with determination of the analytes of concern in that method,
(2) QC acceptance criteria were developed and employed for
determination of the target analyte, (3) there would not be another
approved method that uses the same determinative technique for that
analyte, and (4) that the reason for adding the analyte would not be to
avoid the sample preservation or sample (or extract) holding time
conditions that are already required for that analyte in another
approved method. The third and fourth criteria would preclude method
shopping whereby an analyst might add analytes to a reference method
with less rigid QC acceptance, sample collection or holding time
criteria. Under the criteria proposed above, if a reference method for
an analyte of concern required acidification of the sample, an analyst
would not have the flexibility to modify a method that does not require
sample acidification to include analysis of the analyte of concern.
Modifications of this type would require EPA approval as a new method.
If QC acceptance criteria do not exist to allow addition of a new
analyte, the guidelines specified at 40 CFR part 136 Appendix E, at 40
CFR 136.4, 136.5 and 141.27 would be followed to develop and obtain
approval for these criteria. Alternatively, QC acceptance criteria for
the new analyte could be transferred from the criteria for an analyte
with similar chemical characteristics in the same method or from the
criteria for the analyte in another approved method. EPA provides
additional guidance on developing QC acceptance criteria in Chapter 3
of the Streamlining Guide (EPA 1996a).
B. Quality Control
In order to establish that method modifications do not degrade
method performance, a standard would be required against which changes
could be compared. This standard would consist of standardized QC
elements and QC acceptance criteria that would be listed in the
reference method and/
[[Page 14983]]
or in the regulations at 40 CFR parts 136 and 141. These criteria
would serve as definitive test criteria for evaluating the performance
of a method modification. As proposed, new methods would be required to
include QC acceptance criteria that were developed from a method
validation study according to procedures specified at 40 CFR 136.5,
141.27(c) and (e).
1. Standardized Quality Control Elements
The standardized QC elements, described below, when paired with the
relevant QC acceptance criteria for each element, would allow analysts
to establish and document method performance. These elements would be
specified at 40 CFR part 136 Appendix E and at 40 CFR 136.4, 136.5 and
141.27. Additional guidance on procedures and requirements for these QC
elements are provided in the Streamlining Guide (EPA 1996a).
Calibration--the process of establishing the
relationship between the concentration or amount of material
introduced into an instrument or measurement process and the output
signal.
Calibration Verification--the means of establishing
that instrument performance remains within pre-established limits.
Initial Precision and Recovery (IPR)--the mechanism to
demonstrate that a laboratory would produce reliable results with
the method prior to analysis of environmental samples. IPRs also
would demonstrate that a method modification produces results equal
or superior to those produced by a reference method.
Ongoing Precision and Recovery--a process that
demonstrates that a laboratory is able to produce reliable results
continuously.
Matrix Spike (MS)--a means to assess method performance
(especially analyte recovery) on a sample by adding a known amount
of the tested analyte.
Matrix Spike Duplicate--a process to test the precision
of an analysis by repeating the MS test.
Method Blank--a test that checks for laboratory
contamination.
Method Detection Limit (MDL)--the MDL test, as
specified at Appendix B of 40 CFR part 136, is used to confirm that
a laboratory is capable of detecting an analyte of concern at the
level specified in the method or at an acceptable level for
regulatory compliance monitoring.
Reference Sample--a test that serves as an external
check on method accuracy.
Retention Time and Relative Retention Time Precision--a
means to assess the performance of a chromatographic separation
system; used to aid in the identification of each target analyte in
a complex mixture.
Surrogate--a means to assess the performance of the
method within the given sample matrix by adding a known amount of a
different but chemically similar analyte. The results of these tests
would be used to assess method and laboratory performance.
For each reference method, each QC test would have acceptance
criteria that define data acceptability.
2. Development of QC Acceptance Criteria
QC acceptance criteria would be used to ensure that a modified
method produces results that are reliable, defensible and suitable for
regulatory decisions. QC acceptance criteria would be specified as
numeric limits. For example, the QC acceptance criteria for a MS/MSD
test may be 75-125 percent recovery with a relative percent difference
(RPD) of 20 or less. If these criteria were met for the MS/MSD test,
and all other QC acceptance criteria were met, results produced using
the modified method could be used for regulatory compliance purposes;
if not, corrective action would need to be taken and the sample
reanalyzed.
Some methods currently approved at 40 CFR parts 136 and 141
explicitly specify QC acceptance criteria for all of the standardized
QC elements outlined in today's proposal, but many do not. In selecting
reference methods for today's proposal, EPA chose those methods that
contained QC acceptance criteria or data from which QC acceptance
criteria could be developed. For those methods that did not contain QC
acceptance criteria, QC acceptance criteria were developed from results
of single-laboratory or interlaboratory study data contained in the
method or from criteria contained in Appendix D of 40 CFR part 136.
These criteria are provided at 40 CFR 141.27(d) and 136.3 Table IF for
drinking water and wastewater reference methods, respectively. EPA
would develop QC acceptance criteria for certain approved methods that
do not presently contain these criteria. EPA would propose to designate
these approved methods as reference methods in a future rulemaking.
C. Method Validation for Modified or New Methods
Method validation is the process by which an analyst or vendor
would establish the performance of a new method or would substantiate
the performance of a method modification to a reference method.
Validation would be necessary to demonstrate and document that the new
or modified method could yield reliable data for compliance monitoring
and other purposes. The party who developed the method or method
modification would be responsible for validating the method or method
modification.
The requirements for validation would depend on the level of
intended use for the method modification or new method, and the
characteristics of the sample to which the method modification or new
method would be applied. Based on interactions with stakeholders, EPA
proposes to establish three levels of validation:
Tier 1 methods would be used in a single laboratory in
a single matrix type from one industrial category or subcategory, or
in additional matrix types from any industrial category or
subcategory.
Tier 2 methods would be used by all laboratories in one
or more matrix types within one industrial category or subcategory.
Tier 3 methods would be used by all laboratories in
matrix types from all industrial categories or subcategories.
Proposed definitions of the terms laboratory, matrix type, medium,
and tier are in the definitions sections at 40 CFR 136.2 and 141.2. In
the streamlining initiative, the term matrix type would be defined and
used to identify a sample medium with common characteristics across a
given industrial category or subcategory. The terms facility or system
would identify places where an industrial discharge activity occurs or
where a water source is treated and distributed as drinking (potable)
water. For example, all POTWs that comprise the municipal wastewater
treatment industry would be considered to be in one industrial
category. A typical municipal POTW has three matrix types: untreated
wastewater, treated wastewater, and sludge. All PWSs that comprise the
drinking water industry would be considered to be in one industrial
category and to be one matrix type--potable water. Similar definitions
would apply to matrix types in other industrial categories and
subcategories. EPA invites public comment on these definitions and
seeks suggestions on additional terms or concepts for which the public
believes a regulatory definition would be useful in implementing and
administering EPA's methods approval system.
Method validation would comprise three steps: (1) development of a
validation study plan, (2) testing, and (3) preparation of a validation
study report.
1. Validation Study Plan
A validation study plan would be required for development of a new
method at any tier or for modification of a reference method at Tiers 2
and 3. The organization responsible for conducting the study would
prepare the validation study plan. Requirements for method validation
would be specified at 40 CFR 136.4, 136.5 and 141.27 and at 40 CFR part
136 Appendix E. Additional guidance on suggested validation study
[[Page 14984]]
plans is available in the Streamlining Guide (EPA 1996a).
A validation study plan would not be required for Tier 1 method
modifications, because EPA would expect that single-laboratory use
modifications would be simple and straightforward, and that requiring a
validation study plan for single-laboratory modifications would impose
an unnecessary regulatory burden on small laboratories.
2. Testing
The number of testing laboratories, matrices, and replicate QC
tests for the method validation would depend on the tier at which the
new or modified method would be validated, as indicated in Table I
below. The specific requirements and procedures for performing QC
validation testing are specified at 40 CFR 136.4, 136.5 and at 141.27;
additional guidance is available in the Streamlining Guide (EPA 1996a).
Table I, which is taken from 40 CFR 136.5(d), summarizes validation
requirements at each tier.
Table I.--Summary of Validation Requirements for New Methods and Method Modifications 1
--------------------------------------------------------------------------------------------------------------------------------------------------------
Number of Number of analyses required
------------------------------------------------------------------------------------------
Method application Matrix Facilities/ IPR-reagent IPR-sample
Labs types PWSs water 2 matrix 3 MS/MSD MDL \4\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Tier 1-Single-lab WW/DW--First matrix type or first PWS...... 1 1 1 4 4 5 2 7
WW--Each addt'l matrix type (8 max.) from any industrial
category.................................................... 1 1 1 6 0 6 0 5 2 6 0
DW--Each addt'l PWS (2 max.)................................. 1 1 1 6 0 6 0 5 2 6 0
Tier 2-Multi-lab, single matrix type WW/DW--Each matrix type
in a single industrial category............................. 3 1 3 12 0 7 6 21
Tier 3-Multi-lab, multiple matrix types WW only--All matrix
types, all industrial categories............................ 8 9 9 9 36 0 7 18 63
--------------------------------------------------------------------------------------------------------------------------------------------------------
1 Numbers of analyses in this table do not include background analyses or additional QC tests such as calibration, blanks, etc. Validation requirements
are based on the intended application of the method. Method application would be designated by tier for wastewater (WW) and drinking water (DW)
programs. Three would be the maximum number of public water systems (PWSs) that would be required to validate a new or modified drinking water method
at Tier 1 or 2. Nine would be the maximum number of matrix types (or facilities) that would be required to validate a new or modified wastewater
method at Tier 1 or 3; at Tier 2 the number would be three matrix types.
2 IPR reagent water analyses would be used to validate a method modification and to establish QC acceptance criteria for initial precision and recovery
(IPR) and ongoing precision and recovery (OPR) for a new method. The required number of IPR analyses, except as noted under footnote 7, would be four
times the number of laboratories required to validate a method modification or new method because each laboratory would perform a 4-replicate IPR
test.
3 IPR sample matrix analyses would be used to establish QC acceptance criteria for matrix spike/matrix spike duplicate (MS/MSD) recovery and precision
for a Tier 1 new method only. Would not be required for validation of Tier 2 or 3 new methods because this variability data would be obtained from MS/
MSD tests. Would not be required for validation of a method modification because MS/MSD data from the reference method would be used.
4 A method detection limit (MDL) test would be performed in each laboratory using the new or modified method. 40 CFR part 136 Appendix B requires a
minimum of seven analyses per laboratory to determine an MDL. Each lab involved in validation of a wastewater modification would demonstrate that the
modified method would achieve the detection limits specified in the regulations at 40 CFR parts 136 and 141 and/or in chapter 6 of the Streamlining
Guide (EPA 1996a).
5 MS/MSD analyses would be required only for a method modification because, for new methods, the MS/MSD QC acceptance criteria would be established by
the 4-replicate sample matrix IPR test. For modified methods, the MS/MSD test would demonstrate that the reference method MS/MSD QC acceptance
criteria have been met.
6 The MDL, reagent water IPR, and sample matrix IPR tests would not have to be repeated after the first matrix type, facility, or PWS was validated.
7 For validation of a new method, the MS/MSD analyses would establish QC acceptance criteria for MS/MSD recovery and precision. For validation of a
method modification, the MS/MSD analyses would demonstrate that reference method MS/MSD recovery and precision have been met. The required number of
MS/MSD analyses would be two times the number of facilities, PWSs or matrix types tested.
8 The number of laboratories and samples would vary if a conventional interlaboratory study is used.
The tiered approach to validating new and modified methods would
accommodate variability in the analytical performance of a method that
can be attributed to the type of sample analyzed. This variability is
termed a matrix effect and can be observed in samples taken at
different locations in matrices of the same type (intramatrix) or in
samples from different locations and in different matrix types
(intermatrix). Under the streamlining initiative, each successive tier
addresses matrix effects to a greater degree through increasing levels
of sample matrix effect validation, broadly defined as a test of the
extent to which differences, if any, in method performance could be
attributed to variability between samples obtained from different
industrial matrices, facilities, or PWSs. Matrix effects would need to
be tested by the IPR sample matrix and MS/MSD analyses listed in Table
I. Intramatrix effects would need to be tested in water samples taken
from different PWSs or from different waste streams. Intermatrix
effects would need to be validated on a group of samples taken from
discharge samples collected from several different industrial
categories. In all cases, the laboratory would try to determine if the
measurement result for the target analyte using a new or modified
method differed from the result obtained in a reagent water matrix or
in a previously validated matrix type or PWS sample.
As indicated in Table I, a Tier 1 new or modified method would be
validated in a single laboratory on one or more matrix types obtained
from one or more facilities, or on samples obtained from one or more
PWSs. Validation of additional facilities or PWSs would require
analysis of MS/MSD samples for each additional facility or PWS.
However, in response to stakeholder requests that there should be some
maximum number of single-laboratory validations after which further
validation would be unnecessary because sample matrix effects would
have been sufficiently addressed, EPA
[[Page 14985]]
added a provision for a maximum number of matrix type, facility or PWS
analyses for Tier 1 methods. For a wastewater method, the maximum
number of matrix types or facilities tested under Tier 1 would be nine,
each from a different industrial category or subcategory. For a
drinking water method, the maximum number of PWS samples tested under
Tier 1 would be three samples, each from a PWS with different water
quality characteristics. EPA proposes to require validation in three
rather than nine PWSs, because three is consistent with the validation
data in many EPA drinking water methods and because the variability in
drinking water samples (and therefore the probability of matrix
effects) is usually less in drinking water samples than in wastewater
samples.
Tier 2 validation would be applicable to one or more matrix types
within a single industrial category or subcategory. Because Tier 2 new
and modified methods would apply to each matrix across all
laboratories, EPA developed Tier 2 validation requirements to
incorporate intramatrix variability. Tier 2 would require validation of
the method in drinking water samples obtained from three PWSs, or
wastewater samples of one or more matrix types obtained from three or
more facilities within a single industrial category or subcategory.
Tier 3 validation would be applicable to all matrix types in all
industrial categories. Consequently, Tier 3 validation requirements
would include provisions to account for both intramatrix and
intermatrix variability. However, Tier 3 validation would not apply to
the drinking water program because the program regulates only one
matrix type, drinking (potable) water. The wastewater program regulates
several industrial categories, each of which may contain more than one
matrix type. Tier 3 would require validation of the method in
wastewater samples of up to nine matrix types obtained from nine
different facilities.
For all multi-matrix tiers, it would be extremely important to
select suitable samples and matrix types for validation. The matrix
types, facilities, or PWSs selected for matrix effect validation would
need to have sufficiently different water quality characteristics so
that the matrix effects, if any, could be observed. Proposed criteria
for selecting matrix types, facilities, or PWSs from which to obtain
these samples is specified at 40 CFR 136.4(a)(2)(i) and 141.27(b)(iii).
Additional guidance on testing sample matrix effects is available in
the Streamlining Guide (EPA 1996a).
EPA invites public comment on the number of tests, laboratories,
matrix types, facilities, and PWSs that EPA is proposing for validation
of Tier 1, 2, or 3 methods. EPA is specifically interested in
suggestions for adding, deleting, or modifying the tests listed in
Table I. Commenters should provide EPA with reasons for (and preferably
data to support) any suggested changes.
3. Validation Study Report
A validation study report would be required for a new method or
method modification at all tiers to document successful validation. The
primary documents to be included in the report would be the Checklist
for Initial Demonstration of Method Performance, the Checklist for
Continuing Demonstration of Method Performance (collectively, the
``Checklists''), and a Certification Statement. The Checklists would
document that all requirements for establishing equivalency were met;
the certification statement would commit the persons involved in the
method development or modification effort to the statements made in the
Checklists and the supporting information provided. The proposed
Checklists would be specified at 40 CFR part 136 Appendix E. The
checklists also would be published in the Streamlining Guide (EPA
1996a) with additional guidance on how to complete a checklist for a
typical water method. This guidance would be provided to aid the method
modifier or developer in understanding the information and test data to
be provided. The Checklists and certification statement would be
required as part of the validation study report. For Tier 1 method
modifications, the Checklists and certification statement would
comprise the data validation report. For all tiers, each laboratory
involved in validation of a method modification would need to complete
the Checklists and Certification Statement. More extensive
documentation would be required for a modification at Tiers 2 and 3 and
for all new methods.
The validation study report for Tiers 2 and 3 would need to specify
the following information, as appropriate, for validation of a new or
modified method:
Narrative--includes (a) a description of the method
being validated and the matrices, matrix types, and media to which
the method is applicable; (b) an indication of whether the method is
a modification of an approved reference method or a new method; (c)
reason for and description of the modification, if applicable; and
(d) information on the organization responsible for developing the
new method or method modification.
Analyte(s)--name and Chemical Abstracts Service (CAS)
Registry Number or an EPA Environmental Monitoring Methods Index
(EMMI) Number. If a CAS Registry Number has not been assigned, the
submitter should attempt to obtain a number from the CAS Registry.
If the CAS Registry will not assign a number, the submitter should
contact the AMS Director for assignment of an EMMI Number. A report
for a modified method should indicate whether the modification
includes all forms of the analyte(s) in the scope of the reference
method. The definition of AMS Director is at 40 CFR parts 136.2 and
141.2.
Method or modified test procedure--prepared in a
standard format; modified test procedures would be prepared in the
format of the reference method.
Methodology and procedures--indicates the tier level at
which the new or modified method was tested, describes the approach
used to implement the study, describes the procedures used to report
and validate the data, and identifies the problems encountered
during implementation of the study.
Results--for modified methods, includes a summary of QC
results required by the reference method and corresponding QC
results obtained with the modified method.
Conclusions--describes the conclusions and limitations
of the study.
Discussion--critically examines the study results.
The following items would need to be included in appendixes to the
validation study report:
Calculations;
Raw data to allow an independent reviewer to verify
each determination and calculation performed by the laboratory;
For instruments involving data systems, raw data on
magnetic tape or disk (upon request only);
Names, titles, addresses, and phone numbers of analysts
who performed analyses and QA Officer who verified analyses; and
Completed Checklists and Certification Statement.
The validation study report for a new or modified method would need
to be retained on file by the organization responsible for developing
or applying the modification, and by regulated entities whose samples
are tested with the method modification. The party responsible for
developing and submitting the new method also would need to maintain on
file the complete records of all validation study tests including the
study plan, all laboratory results, the validation study report,
completed Checklists and Certification Statement, and other information
that supports the new method or method modification. All records would
need to be made available for review upon request to an auditor,
permitting authority, or other regulatory authority. These records
would need to be submitted to EPA if the method
[[Page 14986]]
developer elected to request formal approval of a method modification
at Tier 2 or 3.
4. Further Validation of a New Method
After completing a Tier 1, 2, or 3 validation study of a new
method, the organization responsible for developing the method would
need to document the study results in accordance with requirements
proposed at 40 CFR part 136 Appendixes E, F, and G and would need to
submit the results and the method to EPA for review and approval. If,
based on its review of the method, EPA concluded that the method was
not sufficiently rugged or reliable for its intended use, EPA would
require further method development and testing. The tests and studies
that would be performed would need to be determined on a case-by-case
basis as these situations arise and would depend on the analyte(s) and
the analytical system.
5. Approval of a Screening Method as a New Method
Methods currently approved for compliance monitoring at 40 CFR
parts 136 and 141 are considered to be confirmatory methods if the
method is sufficiently selective and quantitative so that most positive
results do not have to be verified by analysis with another method. The
term ``confirmatory'' is used to distinguish these methods from
screening methods. When using a screening method, all positive results
should be verified by re-analysis with a confirmatory method because
screening methods can be less selective and/or quantitative and,
therefore, more subject to false positives or imprecise results than
confirmatory methods. Characteristics of screening methods are
described in more detail in Chapter 2 of the Streamlining Guide (EPA
1996a).
EPA has been asked by many stakeholders to allow use of screening
methods for wastewater and drinking water analyses. Although screening
methods may be less selective and quantitative than confirmatory
methods, they also could be designed to serve meaningful uses under
those statutes. Screening methods could be especially useful when
measuring trends in the contamination of a water source or when
knowledge of the performance of a waste treatment process would be more
important than an exact knowledge of the absolute amount and identity
of the contaminant or pollutant.
Historically, EPA has not considered screening methods for approval
at 40 CFR part 136 or part 141. Under the streamlining initiative, EPA
proposes to consider the approval of screening methods for compliance
monitoring under the Safe Drinking Water Act provided that: (1) the
method would meet all the requirements specified in the regulations at
40 CFR 141.27, (2) all positive sample results obtained with the method
would be confirmed and reported using an approved confirmatory method,
and (3) the probability of the method producing a false negative result
at concentrations of regulatory interest would be no more than one
percent (1%). EPA has not yet specified how it intends to implement the
use of screening methods under the SDWA; the term was only recently
added in the 1996 SDWA amendments. Under the Clean Water Act, EPA is
considering the appropriateness of screening methods for use in NPDES
permit applications and ambient water quality monitoring by States. EPA
proposes to publish a separate table at 40 CFR parts 136 and 141 to
list approved screening methods. The Agency invites comment on the
approval criteria for screening methods for the uses described in the
SDWA, as well as for NPDES permit applications and ambient water
quality monitoring.
D. Method Review and Approval
Under this proposed rule, EPA expects to significantly reduce the
number of methods that would pass through the ATP review and rulemaking
processes. EPA has this expectation because, once implemented, the
streamlining initiative would make it easier for method modifications
to be judged as being ``within the flexibility allowed by the
streamlining initiative.'' Method modifications demonstrated and
documented to be within the flexibility allowed by the streamlining
initiative would be preapproved by EPA for use at the tier for which
the modification was validated. Stakeholder remarks suggest that most
laboratories and method development organizations would welcome and use
this allowed flexibility.
Stakeholders also have asked EPA to approve more quickly revised
versions of approved methods that are periodically published by EPA,
consensus standards organizations, and other government agencies. In
the past, EPA approved these revisions through a formal proposal and
public comment process. Using the flexibility provisions of today's
rule, users would be able to use a revised version of a reference
method as soon as it is published, provided that the results produced
were demonstrated to meet the QC acceptance criteria of the reference
method. This benefit alone would relieve much stakeholder frustration,
decrease the Agency's rulemaking burden, and improve EPA's partnership
with other government agencies and consensus standards organizations.
Table II summarizes EPA's review and rulemaking responsibilities
for new and modified methods by tier.
Table II.--EPA Review and Action for New and Modified Methods
------------------------------------------------------------------------
New Method Modified Method
------------------------------------------------------------------------
Tier 1, Single-lab.............. EPA review No EPA review.
required; EPA
issues a letter
of approval.
Tier 2, Multi-lab, single matrix EPA review If requested, EPA
type. required; reviews and
approved through --issues letter of
rulemaking. approval, or
--conducts
rulemaking.
Tier 3, Multi-lab, multiple EPA review If requested, EPA
matrix types. required; reviews and
approved through --issues letter of
rulemaking. approval, or
--conducts
rulemaking.
------------------------------------------------------------------------
1. Review and Approval of New Methods
Currently, all new methods must be approved by EPA through
``formal'' EPA approval including rulemaking and publication at 40 CFR
part 136 or 141 before use. In today's rule, EPA proposes to grant
letter approvals of new methods that would be submitted under Tier 1
(i.e., single-laboratory, limited-use methods). New methods developed
for use under Tiers 2 or 3 would still require rulemaking. The purpose
for not requiring formal rulemaking at Tier 1 would be to
[[Page 14987]]
provide the means by which (1) a new technology could be introduced,
(2) confidentiality of a new technology could be maintained if desired
by the user of the new method, and (3) specific matrix interference
problems could be overcome. Allowing use of Tier 1 new methods would
enable multiple single laboratories to use a new technology until a
sufficient number of devices were available for interlaboratory
validation as a Tier 2 or 3 new method.
EPA recognizes that allowing single-laboratory use of a new
technology for regulatory compliance carries with it the risk that
results produced with the new technology may not agree with results
produced by a reference method. However, EPA believes that sufficient
controls would be included in the streamlining program to ensure data
quality. EPA also believes that there would be a net benefit to the
regulated community by allowing new technologies that overcome matrix
interference problems. EPA solicits comment on this aspect of
streamlining, and is particularly interested in alternative ways EPA
might allow introduction of new technologies without rulemaking.
2. Review and Approval of Modified Methods
Under the streamlining initiative proposed in today's rule, method
modifications would not require formal EPA approval; they would be
preapproved provided the analyst demonstrates and documents equivalency
with or superiority to the reference method QC criteria. Although
formal approval of a modification would not be required under the
streamlining initiative, several stakeholders have commented that, in
practice, use of a method modification would require the consent of the
regulated entity and responsible regulatory authority. These
stakeholders also expressed concern that without formal EPA approval,
obtaining consent from the regulated entity and/or regulatory authority
would be difficult. In response to these comments, EPA proposes to
allow, but not require, laboratories, industry associations, consensus
standards organizations, instrument manufacturers, and others to submit
Tier 2 or Tier 3 method modifications for EPA review with the
anticipation of a letter from EPA documenting approval. Also, for those
seeking public recognition that their Tier 2 or 3 method modifications
have been demonstrated to be acceptable for use, EPA proposes to work
with the organization to approve the method at 40 CFR part 136 or 141.
EPA would not review, provide letters of approval, or conduct formal
rulemaking for Tier 1 method modifications.
EPA recognizes that preapproving method modifications poses
additional burdens for regulatory authorities, who may need to assess
the reasonableness and effectiveness of each modification. EPA
believes, however, that the Checklists, certification statement, and
accompanying instructions, which are proposed at 40 CFR part 136
Appendix E, and the validation report for the method modification,
which is proposed at 40 CFR part 136 Appendixes F and G, would provide
a regulatory authority the information necessary to make equivalency
assessments, and that this information would be presented in a
standardized and readily understandable format. To further assist
regulatory authorities in implementing this initiative, EPA has
included detailed guidance on assessing method modifications for
equivalency. This guidance is provided in Chapter 6 and in the
appendixes of the Streamlining Guide (EPA 1996a).
3. Submission Package
The items to be submitted to EPA for proposal of a new method at
Tier 2 or 3 would include the method validation study report, which
would include the method prepared in a standard format. If the
submitter requested formal rulemaking to propose the method for
publication in the CFR, information in a format suitable for inclusion
in a draft preamble would also be required. Additionally, the
submission packet would need to include all relevant supporting
documents.
To preclude a proliferation of potentially confusing formats, a
method should be submitted in a standard format. EPA recommends and
specifies the format that would be specified at 40 CFR part 136
Appendix F. This format is also detailed in Method Guidelines and
Format (EPA 1996c). Appendix F describes all elements of the format
prescribed by EPA's Environmental Monitoring Management Council (EMMC).
An objective of the EMMC format is to standardize all Agency analytical
methods. A standardized format used by a government agency such as the
U.S. Geological Survey or from a consensus standards organization such
as Standard Methods, ASTM, or AOAC-International could be used, but EPA
recommends that these formats be reserved for those organizations to
avoid the possible confusion over authorship. EPA would not accept
methods in non-standard formats because of the confusion that could be
created by a proliferation of method formats.
A new method would need to include the standardized QC elements and
QC acceptance criteria. The QC acceptance criteria would need to be
developed from data gathered in the method validation study. Chapter 3
of the Streamlining Guide (EPA 1996a) provides guidance on the detailed
technical requirements for developing criteria that meet the
requirements that would be specified at 40 CFR 136.4, 136.5 and 141.27
and at 40 CFR part 136 Appendix E.
4. Regulatory Assistance Provided by Submitter
Using procedures that would be specified at 40 CFR part 136
Appendix G, EPA would ask method submitters to assist EPA by providing,
as part of the submission package for methods to be proposed in the
Federal Register, information that would facilitate EPA's drafting of a
proposed rule. EPA would also ask submitters to provide technical
assistance, when necessary, in responding to public comments on the
submitter's method. Other assistance could be requested by EPA. The
information should be submitted in a format corresponding to the
preamble drafting conventions specified by the Office of the Federal
Register. Citations of examples for preambles are given in 40 CFR part
136 Appendix G and in the Streamlining Guide (EPA 1996a). Instructions
for drafting documents for the Office of the Federal Register are given
in the Document Drafting Handbook, for sale by the Superintendent of
Documents, Mail Stop: SSOP, Washington, DC 20402-9328 (Document 1993
O--351-677 QL3).
5. EPA Review of Submission Package
Upon receipt of a request for approval, EPA would first check the
submission packet for completeness. If all of the documentation was in
order, EPA would use an internal workgroup to assess the scientific
merit of the method or modification and to evaluate the validation
study for consistency and appropriateness. Should any problems be
identified, the workgroup would contact the submitter to resolve the
outstanding issues. If these issues could not be resolved, EPA would
take no further action on the submission. If all validation
requirements were met and the submission passed internal review, EPA
would either issue a letter of approval or begin the rulemaking
process. All method modifications are preapproved, but a submitter
would have the option to request an EPA letter of approval or to
request a formal rulemaking for Tier 2 and 3 method
[[Page 14988]]
modifications. All new methods would be subject to EPA review. For Tier
1 new methods, EPA would issue letter approvals; Tier 2 and 3 new
methods would require formal Agency rulemaking.
6. Proposal of Methods
For rulemaking, EPA would prepare the proposed rule based on the
draft preamble provided by the submitter. EPA would add the appropriate
updates to CFR tables or language and submit the proposed rule to the
Office of the Federal Register for publication. The proposed rule would
request public comment and allow a specified comment period (typically
60 days after publication in the Federal Register). At the end of the
comment period, EPA would forward significant public comments, if any,
to the method submitter. The submitter would need to provide technical
assistance to EPA in drafting responses to the comments. If the
comments could not be adequately addressed, EPA would not take final
action to approve the method. If all comments are addressed, EPA (with
assistance from the submitter) would need to complete a response-to-
comments document and prepare a final rule to approve the proposed
method. The final rule would state the date that the rule becomes
effective, typically 30 days after rule publication. As of this
effective date, the method would be approved (promulgated) and the
appropriate tables in the CFR would be updated.
To expedite approval of noncontroversial updates to methods, such
as revisions to the methods published by EPA, other government
organizations, and consensus standards organizations, EPA intends to
use ``direct final'' rulemaking. Direct final rules would be warranted
when the action would not be expected to elicit public comment to which
the Agency would normally respond (i.e., no adverse comment). In this
process, the final rule and the companion proposal would be published
simultaneously as a ``direct final rule'' in the Federal Register. In a
direct final rule, the proposed rule has a specific comment period and
the final rule has a later effective date. If no adverse public
comments are received during the comment period for the proposed rule,
the actions become effective on the effective date of the final rule.
If adverse comment is received, the companion final rule is withdrawn
and a second final rule that responds to the public comments is
prepared and published with a new effective date.
E. Other Issues
1. Legal Impacts
Stakeholders expressed concern regarding potential conflicts
between regulators and regulated entities when using modified methods.
For example, there was widespread concern over a situation in which a
discharger used a modified method and demonstrated compliance with a
regulatory concentration limit while a regulatory authority used the
unmodified reference method and obtained results suggesting that the
discharger was out of compliance.
Based on internal EPA discussions, it became apparent that the
streamlining initiative would work only if the modified method, once
demonstrated to be equivalent to the reference method, carried the same
legal force and effect as the reference method. Therefore, the
difference in results produced by the modified and unmodified methods
would be attributable not to the modification, but to differences in
results produced by two laboratories. This situation is no different
than the existing situation where two laboratories can produce
different results, one set of which is above and the other below, a
regulatory compliance limit. The legal resolution would therefore
remain the same as today--a decision would be made based on examination
of all the relevant data.
2. Method-Defined Analytes
The method flexibility introduced in today's proposal does not
extend to methods in which some part of the method ``defines'' the
analyte of concern. This type of analyte is termed a method-defined
analyte. Because method-defined analytes do not have a specific, known
composition, the result of the analytical measurement depends totally
on how the measurement is made. Examples of method-defined analytes
include adsorbable organic halides, biochemical oxygen demand, total
organic carbon, and whole effluent toxicity. Changes to the front-end
steps or the determinative techniques in these methods have the
potential of changing the result produced. EPA believes, however, that
certain parts of procedures for method-defined analytes could be
modified without adversely affecting method performance.
3. Biological Methods
EPA intends to expand method flexibility to include biological
methods, but not in today's proposal. Biological methods include both
the testing of an environmental sample for the presence of
microbiological material (e.g., bacteria, protozoa and viruses) and the
use of biological organisms to measure whole effluent toxicity (WET) of
an environmental sample. EPA believes that flexibility in testing for
biological material would be similar to the flexibility allowed in the
modification to chemical analytical methods. Both the front-end and
determinative techniques should be able to be modified when the
modifications produce equivalent or superior results. EPA has protocols
for some microbiological methods that are currently used in the ATP
program (EPA 1995a, b). In a future rulemaking, EPA may revise the
microbiology protocols to conform with streamlining and method
flexibility procedures. In keeping with Agency goals for a more
performance-based approach to all environmental measurements, EPA also
may develop and propose method flexibility and new method approval
procedures for biological methods and for microbiological parameters
not covered under current EPA protocols.
For WET methods, both new and modified methods are possible. New
methods may involve the use of a different taxonomic category other
than those currently listed at 40 CFR part 136. Method modifications
may be defined as the variation of one of the established summary test
conditions of the method, such as temperature or salinity. Method
modifications to the summary test conditions would not change the
acceptance criteria (e.g., control survival) which serve to identify
the standards of comparison of the ``reference method.'' EPA has not
sufficiently explored this issue to propose the specific requirements
to allow flexibility in all approved biological methods. Until EPA can
clarify the extent of acceptable flexibility, requests for changes in
biological methods would be reviewed and approved on an individual
basis.
4. Proprietary Reagents, Instruments, and Methods
Stakeholders expressed concern over the role of proprietary
components in the streamlined water method approval process. EPA
separates proprietary components into three categories: proprietary
reagents, proprietary instruments, and proprietary methods. EPA intends
to attempt to accommodate the inclusion of proprietary reagents and
instruments in the approval of analytic methods for compliance purposes
to the extent that such inclusion still provides an adequate
opportunity for public review and comment under the Administrative
Procedure Act. EPA does not anticipate,
[[Page 14989]]
however, that it could approve the use of proprietary methods for
determining compliance with regulatory requirements where the entire
method is claimed as ``confidential business information'' because the
opportunity for public review and comment might be restricted too
severely. If a proprietary method is patented, the method would be
considered for approval as a compliance method because the public would
be able to comment on the patented method. EPA believes the restriction
on approval of proprietary methods is not serious because reagents or
instruments, not complete methods, will continue to be the most common
proprietary components used in compliance methods.
Proprietary reagents and instruments are currently included for use
in approved methods and would continue to be allowed in approved
methods. The details of the proprietary elements would need to be
disclosed to EPA, but would be withheld from the public if the person
requesting protection for the confidential business information (CBI)
demonstrates that the information is entitled to confidential treatment
under 40 CFR part 2. Examples of proprietary components may include
immunoassay reagents and antibodies and liquid phases in GC columns;
e.g., DB-1, SPB-octyl, Dexsil'', etc. A new or
modified method submitted for EPA approval would need to include
language stating that the proprietary reagent or instrument could be
replaced by an equivalent. Changes made to the method after EPA
approval would require the manufacturer to demonstrate, through
supporting documentation, that the new proprietary equipment,
substance, or reagent would produce results equal or superior to
results produced with the material originally tested and on which the
method approval is based. Additionally, EPA would not propose a method
containing a proprietary reagent without accurate, specific
instructions for handling the reagent and for safe disposal of each
spent proprietary reagent and/or reaction product. When a material
safety data sheet (MSDS) would need to accompany the proprietary
material, the MSDS would be the appropriate vehicle to provide these
instructions. Submission of a complete MSDS with a new method would
satisfy EPA's need for instructions for safe handling and disposal of
the reagent.
5. Restrictions by Consensus Standards Organizations
As envisioned, this initiative allows modification to a reference
method, provided that the QC acceptance criteria are met. Many of the
methods approved at 40 CFR parts 136 and 141 were developed by
consensus standard organizations such as Standard Methods, ASTM, and
AOAC-International. EPA expects to rely on these and other consensus
standards organizations for future methods, as required by the National
Technology Transfer and Advancement Act of 1995 (NTTAA) and because of
limited Agency resources for method development.
Consensus standards organizations have expressed concern that a
modification to their methods would constitute a violation of the
method being considered a ``standard.'' Standard Methods, ASTM, and
AOAC-International have declined to allow unlimited modification of
their approved methods and, therefore, their methods could not serve as
reference methods nor be modified under the procedures outlined in this
initiative, as can be seen in the proposed CFR tables. This restriction
would not greatly affect the streamlining initiative because an EPA
method exists that would be used as a reference method for nearly all
analytes, and because most methods from consensus standards
organizations have sufficient internal flexibility to meet the
objectives of streamlining or are updated frequently to reflect recent
advances in technologies.
6. Standard Data Format
For this proposed rule, EPA would not establish a standard format
for the submission of analytical data because of the large variety of
formats currently in use. However, EPA strongly recommends the
Department of Energy's Environmental Management Electronic Data
Deliverable Master Specification (DEEMS) because it is comprehensive
and it would expedite processing of a submitter's request. DEEMS is a
list of data elements that laboratories should submit to document the
method modification process. A DEEMS data element dictionary is
provided in the Streamlining Guide (EPA 1996a).
7. Withdrawal of Outdated Methods
EPA also is considering withdrawal of methods that the Agency
believes are obsolete or are no longer used. For example, 40 CFR part
136, Table ID, footnote 3, references methods published in 1978 that
include thin-layer chromatography (TLC) methods. Because gas
chromatography and high performance liquid chromatography methods
provide better monitoring data and are more cost effective, most, if
not all, laboratories no longer use TLC methods. The TLC methods were
proposed for withdrawal in a previous notice (60 FR 53988, October 18,
1995), and EPA believes there may be similar outdated methods. EPA is
conducting a careful examination of Tables IA through IE of 40 CFR part
136 and of the tables at 40 CFR part 141, for obsolete or outdated
methods, and intends to propose withdrawal of those methods for which
newer methods are available.
8. Administrative Record: Organic Methods, Streamlining Guide, and
Method Guidelines and Format
EPA specifies several 600- and 1600-series analytical methods at 40
CFR part 136 Appendix A for analysis of organic chemicals. If the
Office of the Federal Register approves incorporation by reference of
the Appendix A methods, EPA will withdraw Appendix A and publish all of
these methods in the document Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, December 1996, EPA-821-B-96-005,
NTIS PB97-125298, ERIC D-A44/D-A47 (Organic Methods, EPA 1996b). This
document is part of the administrative record for this proposed rule;
copies can be inspected or obtained from NTIS or other sources as
described in the ADDRESSES section above.
EPA also has drafted two guidance documents that are an integral
part of the administrative record for this proposed rule. The first
document, Guide to Method Flexibility and Approval of EPA Water
Methods, December 1996 Draft, EPA-821-D-96-004, PB97-117766
(Streamlining Guide, EPA 1996a), provides detailed guidance on the
overall streamlining initiative. The second document, Guidelines and
Format for Methods to Be Proposed at 40 CFR Part 136 or Part 141, EPA-
821-B-96-003, PB96-210448, July 1996 (Method Guidelines and Format, EPA
1996c), specifies the content and format required for new methods
developed by outside organizations. These documents are readily and
widely available to the public through NTIS, online, and other sources
listed in the ADDRESSES section above.
The Streamlining Guide (EPA 1996a) in particular was drafted to
help method developers use the procedures proposed in today's rule to
validate and obtain approval of new or modified methods. The guidance
was written for use by laboratory auditors, permittees, water
utilities, regulatory authorities,
[[Page 14990]]
purveyors of new technology, and analytical laboratory personnel. The
document is organized into seven chapters, some of which are procedural
and others are descriptive, as appropriate to the topic. Chapter 1
summarizes the proposed streamlining initiative. Chapter 2 describes
the proposed expanded method flexibility. Chapter 3 describes the
proposed standard quality control tests and useful statistical
procedures for developing QC acceptance criteria for new methods.
Chapter 4 describes the proposed tiered system for validating a new
method or a method modification. Chapter 5 describes the proposed
method approval process, a standard method format, and procedures for
submitting validated methods to EPA for approval. Chapter 6 provides
guidance for assessing the method equivalency. Chapter 7 describes
possible future plans to extend method flexibility to microbiological
and macrobiological methods.
The Streamlining Guide (EPA 1996a) also includes eight appendixes.
Appendix A provides a list of acronyms and abbreviations. Appendix B
provides a glossary of terms used in the streamlining initiative.
Appendix C provides examples of currently allowed method modifications.
Appendix D contains a DEEMS data element dictionary, which is a
Department of Defense reporting format that EPA suggests would speed
review of method validation data. Appendix E provides the EMMC method
equivalency checklists and certification statement. Appendix F provides
an example of a completed Appendix E checklist. Appendix G contains
bibliographic references. Appendix H describes EPA derived the proposed
QC acceptance criteria for inorganic chemicals, which are proposed at
40 CFR 136.3 Table IF and 141.27(d)., were calculated.
EPA proposes to make some of the information in the Streamlining
Guide (EPA 1996a) and Method Guidelines and Format (EPA 1996c) a
regulatory requirement. Specifically, EPA proposes to include much of
the information in Chapter 2 (Method Flexibility), Chapter 6 (Assessing
Method Equivalency), Chapter 5 (Method Approval Process) and Appendix E
(Equivalency Checklists) as a requirement for approval of drinking and
wastewater methods. EPA proposes to accomplish this by designating the
excerpts from Chapters 2, 5 and 6 as 40 CFR part 136 Appendix G and the
equivalency checklists in Appendix E as 40 CFR part 136 Appendix E.
Other provisions of the Streamlining Guide (EPA 1996a), including, but
not limited to, Table 4-2, definitions of standardized QC elements, QC
acceptance criteria for inorganic chemicals, would also be included at
40 CFR 136.2, 136.3 Table IF, 136.4, 136.5, 141.2, and 141.27. EPA
would also adopt most of the provisions in Method Guidelines and Format
(EPA 1996c) as Appendix F at 40 CFR part 136. EPA invites public
comment on these two guidance documents and solicits comments on
whether additional guidance in these documents should be a regulatory
requirement.
9. Coordination with Other Federal Register Proposals
On October 18, 1995 (60 FR 53988), EPA proposed to amend the list
of approved methods at 40 CFR part 136 by adding new or revised methods
for certain metal and inorganic analytes and by adding method citations
to Table IB and amending the incorporation by reference section
accordingly. EPA also proposed to withdraw approval of certain outdated
or rarely used analytical methods, as well as certain methods that
require use of hazardous or toxic reagents. As of today, EPA has not
promulgated a final rule implementing the proposed actions.
The methods proposed for withdrawal that relate to this
streamlining initiative are primarily the EPA 200-series flame atomic
absorption spectrophotometry (FLAA) methods. Although approval of the
EPA FLAA methods is proposed to be withdrawn, FLAA methods published by
ASTM, Standard Methods, AOAC-International, and USGS would remain
approved and would remain listed in 40 CFR 136.3, Table IB. Withdrawal
of approval of EPA FLAA methods would remove these methods as reference
methods and would remove the QC acceptance criteria associated with
these methods. The net impact would be that there would be no FLAA
method against which modifications would be made. EPA does not consider
this a serious limitation because four FLAA methods (ASTM, Standard
Methods, AOAC-International, and USGS) would remain approved for nearly
all metals and the flexibility afforded by these methods should
adequately cover method modifications.
In 1997, EPA intends to amend the regulations at parts 136 and 141,
as appropriate, to update outdated versions of methods to versions
published in the 19th edition of Standard Methods (APHA 1995), the 1996
Annual Book of ASTM Standards, Vols. 11.01 and 11.02 (ASTM 1996), and
in EPA's August 1995 manual titled, Methods for the Determination of
Organic Compounds in Drinking Water--Supplement III (EPA 1995c). If and
when the provisions of today's rule are promulgated, EPA expects to be
able to list these 1995 and 1996 versions of the compliance methods as
approved methods in the tables listed at 40 CFR parts 136 and 141. If
inclusion of these more recent versions would provide a basis to change
any of the QC acceptance criteria for the reference methods, the public
would be notified and provided with the opportunity to comment on the
new criteria.
10. Laboratory Certification and Laboratory Auditing
Broad requirements for States to have an approved laboratory
certification program for analysis of drinking water samples are
specified at 40 CFR 142.10(b)(3). EPA provides more specific help to
State certification officers through written and verbal guidance. To
improve the uniformity of these certification programs, some laboratory
certification officers, method developers, and vendors have asked EPA
to provide more specific regulatory requirements. Today's rule responds
to these requests by proposing standardized QC elements for all water
compliance methods at 40 CFR 136.2 and 141.2, and at Appendix G of 40
CFR part 136. To standardize and facilitate laboratory audits, EPA also
would recommend use of several detailed checklists for auditing both
modified and unmodified methods. These standardized checklists would be
specified at Appendix E of 40 CFR part 136. EPA understands that
increasing the analyst's current flexibility to modify steps in a
compliance method could make the conduct of laboratory audits more
difficult. However, EPA believes that the proposal to specify
standardized QC elements for all methods and to require that
laboratories use standardized checklists to document and check method
performance will ameliorate these potential problems. EPA invites
public comment and is especially interested in what additional action,
if any, the Agency should take to facilitate the auditing of water
laboratories.
IV. Regulatory Analysis
A. Executive Order 12866
Under Executive Order 12866 [58 FR 51,735 (October 4, 1993)], the
Agency must determine whether the 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
[[Page 14991]]
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.
This regulation is not major because it is intended to reduce costs
through flexibility and innovation. Therefore, this regulation would
not result in a cost to the economy of $100 million or more; would not
result in a major increase in costs or prices for consumers or
individual industries; and would not have significant adverse effects
on competition, investment, innovation, or international trade.
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
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Pub.
L. 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 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 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.
EPA has determined that this rule does not contain a Federal
mandate that may result in expenditures of $100 million or more for
State, local, and tribal governments, in the aggregate, or the private
sector in any one year. EPA has further determined that this rule
contains no regulatory requirements that might significantly or
uniquely affect small governments. This rulemaking should have minimal
financial impact, if any, on the current regulatory burden imposed on
regulated entities and regulators because the rulemaking does not
establish any additional regulatory requirements. The proposed rule
simply provides the option to modify approved methods or propose new
methods, if desired. EPA believes that method modifications and new
methods would not be used if not cost effective. Thus, today's rule is
not subject to the requirements of sections 202, 203, and 205 of the
UMRA.
C. Regulatory Flexibility Act
The Regulatory Flexibility Act, 5 U.S.C. 601 et seq., requires EPA
and other agencies to prepare a final regulatory flexibility analysis
for regulations that have a significant impact on a substantial number
of small entities. This regulatory action does not have any adverse
impact on either small or large entities. Therefore, a regulatory
flexibility analysis is not required. Pursuant to section 605(b) of the
Regulatory Flexibility Act, 5 U.S.C. 605(b), the Administrator
certifies that this rule will not have a significant economic impact on
a substantial number of small entities.
D. Paperwork Reduction Act
The information collection requirements in this proposed rule will
be submitted for approval to the Office of Management and Budget (OMB)
under the Paperwork Reduction Act, 44 U.S.C. 3501 et seq. shortly. EPA
is preparing an information collection request (ICR) document for this
proposed rule and will solicit public comment on it prior to
promulgating a final regulation. Comments on the proposed rule,
preamble, and ICR will all be considered before a final rule is
promulgated. The information collection requirements in this proposal
are described in Parts III.A (Method Flexibility), III.B (Quality
Control), III.C (Method Validation), III.D (Method Review), and III.E.6
(Standard Data Format). The information collection requirements in this
proposal are specified in Appendix E (Equivalency Checklists), Appendix
F (Guidelines and Format for Methods) and Appendix G (Method
Flexibility, Equivalency, and Approval) of 40 CFR part 136 and at 40
CFR 136.3(d); 136.4 (b) and (c); 136.5 (a), (b), (c), and (d); and at
40 CFR 141.27 (a), (b), and (c).
The information requirements are not effective until OMB approves
them. 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.
V. Request for Comments
A. General
EPA is interested in eliciting constructive comments that would
allow the Agency to incorporate flexibility into existing methods and
to streamline the proposal and promulgation of new methods at 40 CFR
parts 136 and 141. On the other hand, EPA is interested in compelling
reasons why such a program may not work, even with extensive built-in
controls to ensure that the results produced by modified or new
analytical methods are reliable. EPA looks forward to working with all
interested and concerned parties to produce an improved system for
methods approval under the water methods program.
B. Specific
EPA is soliciting public comment on the following specific
questions and options that relate to technical and policy decisions
that EPA may need to make to implement the streamlining initiative.
1. As described in this preamble and the Streamlining Guide (EPA
1996a), the streamlining initiative would use a performance-based
approach in which a reference method that contains or is supplemented
with QC acceptance criteria is the standard against which a method
modification would be tested to demonstrate equivalency. In contrast to
the proposed performance-based reference-method approach, another
performance-based approach would be to specify only the QC acceptance
[[Page 14992]]
criteria without the need for a reference method. Should EPA retain the
proposed reference method approach with QC acceptance criteria? Or
should EPA change to a QC acceptance criteria approach only?
2. Regarding question number one above, for what analytes, methods
or monitoring situations, if any, do you believe EPA should allow use
of either the performance-based reference method approach or the QC
acceptance criteria only approach?
3. It may not be appropriate to develop QC acceptance criteria to
allow modification of methods for ``method-defined parameters,'' such
as biochemical oxygen demand or total suspended solids. What chemical,
microbiological, or biological analytes or analytical procedures do you
believe might not be amenable to streamlining or method flexibility
procedures?
4. Should EPA implement streamlining and method flexibility
procedures only for new regulatory actions? Should EPA apply these
procedures to existing regulatory requirements but only when these
requirements are updated for some other purpose? Or should EPA apply
these proposed procedures to existing regulations now?
5. EPA has undertaken several pilot studies of new methods to test
the streamlined method approval process, and expects the pilots to be
completed prior to promulgation of a final rule. Should EPA conduct
more extensive pilot studies, e.g., several pilots at each tier, or
should the changeover take place as soon as possible? If a pilot or
phase-in approach is adopted, should EPA phase-in by analyte group
(e.g., VOCs, metals, pesticides)? Or by the technologies employed by
the reference method (electron capture, mass spectrometry)?
6. Is the proposed flexibility to modify the front-end and
determinative steps in a reference method broad enough to be of value
to the methods development community? For what steps in a reference
method, if any, would you increase or decrease the flexibility to
modify a method? If method flexibility were broadened, what additional
standardized QC elements or checklist items should be added to ensure
and document acceptable performance of the modification?
7. If you believe that the proposed flexibility is too broad for
some methods, would you prefer that EPA limit flexibility by revising
approved methods to indicate the steps that could or could not be
changed? If yes, for which steps in a method (e.g., extraction/
digestion, concentration, determinative) or for which types of method
(e.g., those with method-defined analytes) should changes be allowed or
prohibited? If possible, please cite methods listed in 40 CFR part 136
or 141 as examples.
8. If method flexibility were implemented as proposed, are the
standardized QC elements (accuracy, precision, detection limit,
calibration, reference sample, matrix spikes, etc.) described in part
III.C of this proposal and in the Streamlining Guide (EPA 1996a)
adequate to validate the acceptability of a modification to a reference
method? If not, which QC elements should be added? On the other hand,
are the QC elements too extensive? If yes, which QC elements should be
deleted? And why?
9. There has been some concern about the effect that changes to the
chemistry of a method may have on a laboratory or method developer's
ability to validate the performance of a modified method using the
Checklists and other requirements in the Streamlining Guide (EPA
1996a). For example, what effect, if any, might changing the extraction
solvent have on extract holding times that would not be picked up by
the Checklists' criteria? What effect, if any, might use of a different
extraction technique or a different solvent-to-sample ratio have that
would not be picked up by the standardized QC? What, if any, QC
elements should be changed or added to mitigate these concerns?
10. Once EPA adopts streamlining and method flexibility procedures,
should EPA continue to develop and publish new methods or should EPA
rely on the private sector and consensus standards organizations? In
addressing this question, please consider the effect on small
laboratories, PWSs, and POTWs, if EPA discontinued providing EPA
methods.
11. EPA has determined that, for wastewater programs, a modified
method, once validated and documented in accordance with the details in
this proposal, would carry the same force and legal effect as a
reference method. Do stakeholders believe that a modified method should
have equal status with a reference method? Or should EPA require
different levels of documentation for data gathered with the modified
method? If a modified method had a different level of documentation,
would stakeholders accept that it has legal status equal to that of an
unmodified method?
12. Should EPA change the QC acceptance criteria in a reference
method when a significant technological advance or some other factor
demonstrates that the criteria could be made more rigorous? In your
response, you may assume that changing the criteria would not adversely
decrease the number of qualified laboratories needed to conduct
compliance monitoring with the more rigorous method.
13. EPA plans to implement streamlining and method flexibility for
water methods through informal gathering of public comment and through
rulemaking (Federal Register proposal, public comment, and final rule),
of which this proposal is a part. Are there additional measures needed
to ensure that all stakeholders would be aware of the initiative and,
if so, what additional steps should EPA take?
14. Given that a laboratory would be able to modify a method
without prior EPA approval, how would current EPA and state laboratory
auditing and certification programs continue to ensure that the
regulated community is properly conducting monitoring activities and
documenting monitoring system performance? Should documentation be
retained at the testing laboratory? At the facility? Or should EPA
require that the data be submitted to EPA or other regulatory authority
with each data package that results from use of the modification?
15. Adoption of streamlining and method flexibility procedures
would require a deeper understanding of the science behind measurement
methods. Consequently, ``first-line'' compliance and enforcement
efforts may require additional resources and training of auditors. What
training would EPA, the Regions, the States, laboratories, and the
regulated community need to employ to successfully implement
streamlining or method flexibility procedures? What courses could be
developed, and who should be responsible for their development?
16. Under the streamlining initiative, requests for approval of new
methods (i.e., new technologies or determinative techniques) would be
submitted to EPA under a streamlined ATP-type program. Should EPA
process these requests in the order received or should EPA have the
discretion to accelerate review of methods that provide the most
benefit to the Agency's regulatory program and/or to the needs of the
regulated community?
17. What additional steps, if any, should the Agency take to ensure
that the use of method flexibility does not compromise enforceability
of applicable statutes and regulatory requirements? Will additional
training be sufficient or will inspectors need additional
qualifications to be able to assess the
[[Page 14993]]
quality of CWA and SDWA compliance data produced by a modified or new
reference method? What resources would be required to mitigate concerns
about the need for appropriate training of inspectors?
18. EPA proposes to define several administrative (e.g., Assistant
Administrator, AMS Director) and technical (e.g. screening method,
standardized quality control) terms in the definitions at 40 CFR 136.2
and 141.2 and invites public comment on these definitions. Should EPA
omit any of the proposed definitions to avoid unnecessary confusion or
restrictions? Are there additional terms or concepts for which a
regulatory definition would be useful in implementing and administering
EPA's proposed methods approval system?
19. EPA invites public comment on the guidance contained in the
Streamlining Guide (EPA 1996a) and in Method Guidelines and Format (EPA
1996c). These documents, which are part of the administrative record
for this proposal, provide guidance on method flexibility and method
validation procedures under the proposed streamlining initiative. The
documents also provide examples of certification statements and
checklists that would satisfy EPA's proposed requirements for
documenting the performance and equivalency of a modified or new
method. Portions of these documents are proposed to be regulatory
requirements (for example, see the proposed Appendixes E, F, and G and
other amendments to 40 CFR parts 136 and 141). Which, if any, of the
proposed requirements should EPA remove from the regulations and only
keep as guidance?
20. In future rulemakings, EPA may propose to make more of the
information in the two documents described above regulatory
requirements. EPA would accomplish this by amending the wastewater and
drinking water regulations or, with the approval of the Office of the
Federal Register, incorporate by reference all or parts of the
Streamlining Guide (EPA 1996a) and Method Guidelines and Format (EPA
1996c) into the CFR. What, if any, additional guidance from these
documents should EPA propose as a regulatory requirement?
VI. References
APHA. 1995. Nineteenth edition of Standard Methods for
the Examination of Water and Wastewater, 1992, American Public
Health Association, 1015 Fifteenth Street NW, Washington, D.C.
20005.
ASTM. 1996. Annual Book of ASTM Methods, 1996, Vol.
11.01 and 11.02, American Society for Testing and Materials, 101
Barr Harbor Drive, West Conshohocken, PA 19428.
EPA. 1995a. Protocol for Alternate Test Procedures for
Coliform Bacteria in Compliance with Drinking Water Regulations:
Presence/Absence Liquid Culture Methods for Finished Waters, Ver.
1.2, December 1995, U.S. Environmental Protection Agency.
EPA. 1995b. Protocol for Alternate Test Procedures for
Coliform Bacteria in Compliance with Drinking Water Regulations:
Presence/Absence Membrane Filter Methods for Finished Waters, Ver.
1.2, December 1995, U.S. Environmental Protection Agency.
EPA. 1995c. Methods for the Determination of Organic
Compounds in Drinking Water--Supplement III, EPA-600/R-95-131,
August 1995, NTIS PB95-261616.
EPA. 1996a. Guide to Method Flexibility and Approval of
EPA Water Methods, December 1996 Draft, EPA-821-D-96-004, NTIS PB97-
117766, ERIC D-A43/D-A46 (Streamlining Guide, EPA 1996a).
EPA. 1996b. Methods for Organic Chemical Analysis of
Municipal and Industrial Wastewater, December 1996, EPA-821-B-96-
005, NTIS PB97-125298, ERIC D-A44/D-A47 (Organic Methods, EPA
1996b).
EPA. 1996c. Guidelines and Format for Methods to Be
Proposed at 40 CFR Part 136 or Part 141, EPA-821-B-96-003, NTIS
PB96-210448, ERIC D-A42/D-A45, July 1996 (Method Guidelines and
Format, EPA 1996c).
EPA. 1996d. Draft Memorandum from Assistant
Administrators, ``Implementation Plan for the Agency Performance-
Based Measurement System,'' October 25, 1996, U.S. Environmental
Protection Agency.
EPA. 1996e. Memorandum from Robert Perciasepe,
``Agency-wide Adoption of the Performance-Based Measurement System
Approach,'' November 1, 1996, U.S. Environmental Protection Agency.
List of Subjects
40 CFR Part 136
Environmental protection, Laboratories, Water pollution control,
Reporting and recordkeeping requirements.
40 CFR Part 141
Environmental protection, Laboratories, Water supply, Reporting and
recordkeeping requirements.
Dated: March 17, 1997.
Carol M. Browner,
Administrator.
For the reasons set out in the preamble, title 40 of the Code of
Federal Regulations is proposed to be amended as set forth below:
PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS
1. The authority for part 136 is proposed to be revised 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.).
* * * * *
2. Section 136.2 is proposed to be revised to read as follows:
Sec. 136.2 Definitions.
As used in this part, the term:
Accuracy means the degree of agreement between an observed value
and an accepted reference value. Accuracy includes random error
(precision) and systematic error (bias) that are caused by sampling and
analysis.
Act means the Clean Water Act.
Administrator means the Administrator of the U.S. Environmental
Protection Agency (EPA).
Analyte or Analyte of concern means a substance or property that is
to be measured by an analysis.
Approved method means a testing procedure or analytical method
promulgated at this part or at 40 CFR parts 405 through 500.
Assistant Administrator (AA) means the EPA Assistant Administrator
for Water.
Calibration (CAL) means the process of establishing the
relationship between the concentration or amount of material introduced
into an instrument or measurement process and the output signal.
Calibration linearity means the degree to which calibration points
lie along a straight line.
Calibration verification means the means of establishing that
instrument performance remains within pre-established limits.
Determinative technique means the process (physical or chemical or
both) to measure the identity and concentration of an analyte. In test
methods, the determinative technique follows the front-end techniques.
Director means the Director of the State Agency authorized to carry
out an approved National Pollutant Discharge Elimination System Program
under section 402 of the Act.
Front-end technique means any technique in the analytical process
that precedes the determinative technique, including all procedures,
equipment, solvents, etc. that are used in the laboratory in the
preparation and cleanup of a sample but this excludes conditions and/or
procedures for the collection, preservation, shipment and storage of
the sample.
Initial precision and recovery test (IPR) means analysis of a
minimum of four spiked replicate reference matrix samples under the
same conditions as
[[Page 14994]]
will be used for analysis of environmental samples. The IPR is used to
demonstrate that a laboratory is able to produce reliable results with
the method prior to analysis of environmental samples.
Interference means a positive or negative effect on a measurement
caused by a substance other than the analyte being determined.
Matrix means the component or substrate that contains the target
analyte.
Matrix spike (MS) means a sample prepared by adding a known
quantity of target analyte to a specified amount of a sample matrix for
which an independent estimate of target analyte concentration is
available.
Matrix spike duplicate (MSD) means a duplicate of the matrix spike.
The MS/MSD are used in combination to test the precision of an
analysis.
Matrix type means a sample medium with common characteristics
across a given industrial category or industrial subcategory. Examples
include: C-stage effluents from chlorine bleach mills in the Pulp,
Paper, and Paperboard industrial category; effluent from the continuous
casting subcategory of the Iron and Steel industrial category; publicly
owned treatment work (POTW) sludge; and in-process streams in the
Atlantic and Gulf Coast Hand-shucked Oyster Processing subcategory.
Medium means the physical phase of a sample matrix. Air, water,
soil, sediment, rock, and sludge are sample media.
Method means an orderly and systematic arrangement of procedures
and techniques for performing an analysis.
Method blank (or blank) means a sample absent the analytes of
interest and interferences, which is processed through all steps of a
method simultaneously with and under the same conditions as samples
that may contain an analyte of interest.
Method detection limit (MDL) means the minimum concentration of a
substance that can be measured and reported with 99% confidence that
the analyte concentration is greater than zero as determined by the
procedure set forth in appendix B of this part.
Method Guidelines and Format means the procedures set forth in
appendix F of this part.
Method modification means a change to a reference method. The
change may be to a front-end technique or to the determinative
technique.
Method validation means a process by which a laboratory or vendor
establishes the performance of a new method or substantiates the
performance of a method modification.
Minimum level (ML) means the lowest level at which an entire
analytical system gives a recognizable signal and acceptable
calibration point for an analyte. It is equivalent to the concentration
of the lowest calibration standard, assuming that all method-specified
sample weights, volumes, and clean-up procedures have been employed.
National Pollutant Discharge Elimination System (NPDES) means the
national system for the issuance of permits under section 402 of the
Clean Water Act and includes any State or interstate program which has
been approved by the Administrator, in whole or in part, pursuant to
section 402 of the Clean Water Act.
New method means a combination of analyte of concern and
determinative technique that is different from those in the approved
methods.
Ongoing precision and recovery sample (OPR) means a spiked
reference matrix sample that is processed through all steps of a method
simultaneously with and under the same conditions as samples that may
contain an analyte of interest. Also called a laboratory control sample
(LCS), the OPR/LCS is used to demonstrate that a laboratory is able to
produce reliable results continuously.
Organic Methods means the document titled: Methods for the
Determination of Organic Compounds in Drinking Water--Supplement III
(available from the National Technical Information Service (NTIS), U.S.
Department of Commerce, Springfield, Virginia, 22161, 703/487-4600, at
NTIS publication PB97-125298).
Other approved method means a promulgated method that is not
designated as a reference method.
Percent recovery means the recovery multiplied by one hundred.
Person means an individual; corporation; company; association;
partnership; municipality; or State, Federal, or tribal agency.
Precision means the degree to which a set of observations or
measurements of the same property, usually obtained under similar
conditions, conform. Precision is usually expressed as standard
deviation, variance, or range, in either absolute or relative terms.
Preparation means processing performed on a sample prior to
analysis, including extraction, concentration, and cleanup.
Procedure means a set of systematic instructions for performing an
activity.
Promulgated method means a method that has been published or
incorporated by reference into 40 CFR parts 136 or 405 through 500.
Quality assurance (QA) means an integrated system of activities
involving planning, quality control, quality assessment, reporting, and
quality improvement to ensure that a product or service meets defined
standards of quality with a stated level of confidence.
Quality control (QC) means the overall system of technical
activities conducted to measure and control the quality of a product or
service so that it meets the needs of a user. The purpose of QC is to
provide quality that is satisfactory, adequate, dependable, and
economical.
Quality control acceptance criteria (QC acceptance criteria) means
performance specifications developed from validation data and used to
control the limits within which an analytical method is operated.
Recovery means the total amount of analyte found divided by the
amount of analyte added as a spike.
Reference method means an approved method that is designated as a
standard to which a modified method can be compared. A reference method
includes standardized QC and QC acceptance criteria as well as sample
preparation, cleanup, and other procedures.
Regional Administrator means an EPA Regional Administrator.
Screening method means a method that employs a qualitative
determinative technique for an analyte of interest that is different
from the determinative techniques used in the approved methods for that
analyte. The screening method should produce a false negative
probability less than 1%.
Selectivity means the capability of a method or instrument to
respond to an analyte in the presence of interferences.
Sensitivity means the capability of a method or instrument to
differentiate between different amounts or concentrations of an
analyte.
Spike means the process of adding a known amount of an analyte to a
sample to determine the recovery.
Spike amount means a known quantity of analyte added to a sample
and used to determine the recovery of a method.
Standard deviation means the measure of the dispersion of observed
values expressed as the positive square root of the sum of the squares
of the difference between the individual values of a set and the
arithmetic mean of the set, divided by one less than the number of
values in the set.
Standardized quality control (standardized QC) means a uniform set
of performance testing procedures that ensure reliable results.
Depending on
[[Page 14995]]
the method, standardized QC procedures include, but are not limited to,
the following: calibration, calibration linearity, calibration
verification, absolute retention time, absolute and relative retention
time precision, initial precision and recovery, ongoing precision and
recovery (laboratory control sample), surrogate or labeled compound
recovery, analysis of blanks, matrix spike and matrix spike duplicate
recovery and precision, demonstration of method detection limit(s), and
analysis of a reference sample.
Surrogate means a substance with properties that mimic the behavior
of an analyte, that is unlikely to be found in an environmental sample,
and that is added to the sample for quality control purposes.
Tier 1 means the application of a new or modified method in a
single laboratory to one or more matrix types.
Tier 2 means the application of a new or modified method by all
laboratories to one or more matrix types within a single industrial
category or subcategory.
Tier 3 means the application of a new or modified method by all
laboratories to all matrix types in all industrial categories and
subcategories (nationwide use).
3. Section 136.3 is proposed to be amended by revising the last two
sentences and Tables IB, IC, and ID in paragraph (a); by adding Table
IF in paragraph (a); by revising paragraphs (c) and (d); and by
removing paragraph (e) (Table II following paragraph (e) is unchanged)
to read as follows:
Sec. 136.3 Identification of test procedures.
* * * * *
(a) * * *
The discharge parameter values for which reports are required must
be determined by one of the standard analytical test procedures
incorporated by reference and described in Tables IA, IB, IC, ID, and
IE, or by any alternate test procedure which has been approved by the
Administrator or Assistant Administrator under the provisions of
paragraph (d) of this section and Secs. 136.4 and 136.5. Under
paragraphs (b), (c) of this section and 40 CFR 401.13 alternate test
procedures may be used when such other test procedures have been
previously approved by the Administrator, Assistant Administrator, or
Regional Administrator of the Region in which the discharge will occur,
and providing the Director of the State in which such discharge will
occur does not object to the use of such alternate test procedure.
Standardized QC and QC acceptance criteria for modifications of the
inorganic contaminant reference methods in Table IB are specified in
Table IF.
* * * * *
Table IB.--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Other approved methods
Reference -----------------------------------------------------------------------------------------------------------
Parameter/methodology method 1, Standard methods 18th
35 Ed.39 ASTM 39 USGS 2, 39 AOAC--Intl.39 Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:
Electrometric endpoint or 305.1 2310 B(4a) D1067-92 ................. ................. .................
phenolphthalein endpoint.
2. Alkalinity, as CaCO3, mg/L:
Electrometric or 310.1 2320 B D1067-92 I-1030-85 973.43 3 .................
Colorimetric titration to 310.2 I-2030-85
pH 4.5, manual or
automated.
3. Aluminum--Total,4 mg/L;
Digestion 4 followed by:
AA direct aspiration 36.... 202.1 3111 D ...................... I-3051-85 ................. .................
AA furnace................. 202.2 3113 B ...................... ................. ................. .................
Inductively Coupled Plasma/ 5 200.7 3120 B ...................... ................. ................. .................
Atomic Emission
Spectrometry (ICP/AES).36.
Direct Current Plasma (DCP) ........... ......................... D4190-82(88) ................. ................. AES0029 34
36.
Colorimetric (Eriochrome ........... 3500-AI D ...................... ................. ................. .................
cyanine R).
4. Ammonia (as N), mg/L:
Manual, distillation (at pH 350.2 4500-NH3 B ...................... ................. 973.49 3 .................
9.5) 6 followed by:.
Nesslerization............. 350.2 4500-NH3 C D1426-93(A) I-3520-85 973.49 3 .................
Titration.................. 350.2 4500-NH3 E ...................... ................. ................. .................
Electrode.................. 350.3 4500-NH3 F or G D1426-93(B) ................. ................. .................
Automated phenate.......... 350.1 4500-NH3 H ...................... I-4523-85 ................. .................
Automated electrode........ ........... ......................... ...................... ................. ................. 379-75WE 7
5. Antimony--Total,4 mg/L;
Digestion 4 followed by:
AA direct aspiration 36.... 204.1 3111 B ...................... ................. ................. .................
AA furnace................. 204.2 3113 B ...................... ................. ................. .................
ICP/AES 36................. 5 200.7 3120 B ...................... ................. ................. .................
6. Arsenic--Total,4 mg/L:
Digestion 4 followed by.... 206.5 ......................... ...................... ................. ................. .................
AA gaseous hydride......... 206.3 3114 B 4.d D2972-93(B) I-3062-85 ................. .................
AA furnace................. 206.2 3113 B D2972-93(C) ................. ................. .................
ICP/AES 36................. 5 200.7 3120 B ...................... ................. ................. .................
Colorimetric (SDDC)........ 206.4 3500-As C D2972-93(A) I-3060-85 ................. .................
7. Barium--Total,4 mg/L;
Digestion 4 followed by:
AA direct aspiration 36.... 208.1 3111 D ...................... I-3084-85 ................. .................
AA furnace................. 208.2 3113 B D4382-91 ................. ................. .................
ICP/AES 36 ................ 5 200.7 3120 B ...................... ................. ................. .................
DCP 36..................... ........... ......................... ...................... ................. ................. AES0029 34
8. Beryllium--Total,4 mg/L;
Digestion 4 followed by:
[[Page 14996]]
AA direct aspiration....... 210.1 3111 D D3645-93(88)(A) I-3095-85 ................. .................
AA furnace................. 210.2 3113 B D3645-93(88)(B) ................. ................. .................
ICP/AES.................... 5 200.7 3120 B ...................... ................. ................. .................
DCP........................ ........... ......................... D4190-82(88) ................. ................. AES0029 34
Colorimetric (aluminon).... ........... 3500-Be D ...................... ................. ................. .................
9. Biochemical oxygen demand
(BOD5), mg/L:
Dissolved Oxygen Depletion. 405.1 5210 B ...................... I-1578-78 8 973.44 3 p. 17 9
10. Boron 37--Total, mg/L:
Colorimetric (curcumin).... 212.3 4500-B B ...................... I-3112-85 ................. .................
ICP/AES.................... 5 200.7 3120 B ...................... ................. ................. .................
DCP........................ ........... ......................... D4190-82(88) ................. ................. AES0029 34
11. Bromide, mg/L:
Titrimetric................ 320.1 ......................... D1246-82(88)(C) I-1125-85 ................. p. S44 10
12. Cadmium--Total,4 mg/L;
Digestion 4 followed by:
AA direct aspiration 36.... 213.1 3111 B or C D3557-90 I-3135-85 or 974.27 3 p. 37 9
(A or B) I-3136-85
AA furnace................. 213.2 3113 B D3557-90(C) ................. ................. .................
ICP/AES 36................. 5200.7 3120 B ...................... I-1472-85 ................. .................
DCP 36 .................... ........... ......................... D4190-82(88) ................. ................. AES0029 34
Voltametry 11.............. ........... ......................... D3557-90(C) ................. ................. .................
Colorimetric (Dithizone)... ........... 3500-Cd D ...................... ................. ................. .................
13. Calcium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration....... 215.1 3111B 511-93(B) I-3152-85 ................. .................
ICP/AES.................... \5\ 200,7 3120 B ...................... ................. ................. .................
DCP........................ ........... ......................... ...................... ................. ................. AES0029 \34\
Titrimetric (EDTA)......... 215.2 3500-Ca D 511-93(A) ................. ................. .................
14. Carbonaceous biochemical
oxygen demand (CBOD5), mg/
L\12\:
Dissolved Oxygen Depletion ........... 5210B ...................... ................. ................. .................
with nitrification
inhibitor.
15. Chemical oxygen demand
(COD), mg/L; Titrimetric
410.1 5220 C D1252-88(A) I-3560-85 973.46 \3\ p. 17 \9\
410.2 ......................... ...................... I-3562-85 ................. .................
410.3 ......................... ...................... ................. ................. .................
Spectrophotometric, manual 410.4 5220 D D1252-88(B) I-3561-85 ................. Notes 13 or 14
or automated.
16. Chloride, mg/L:
Titrimetric (silver ........... 4500-Cl-B D512-89(B) I-1183-85 .................
nitrate).
(Mercuric nitrate)......... 325.3 4500-Cl-C D512-89(A) I-1184-85 973.51 \3\
Colorimetric, manual....... ........... ......................... ...................... I-1187-85 ................. .................
Automated (Ferricyanide)... 325.1 or 4500-Cl-E ...................... I-2187-85 ................. .................
325.2
17. Chlorine-Total residual, mg/
L; Titrimetric:
Amperometric direct........ 330.1 4500-Cl D D1253-86(92) ................. ................. .................
Iodometric direct.......... 330.3 4500-Cl B ...................... ................. ................. .................
Back titration ether end- 330.2 4500-Cl C ...................... ................. ................. .................
point \15\.
DPD-FAS.................... 330.4 4500-Cl F ...................... ................. ................. .................
Spectrophotometric, DPD.... 330.5 4500-Cl G ...................... ................. ................. .................
or Electrode............... ........... ......................... ...................... ................. ................. Note 16
18. Chromium VI dissolved, mg/
L; 0.45 micron filtration
followed by:
AA chelation-extraction.... 218.4 3111 C ...................... I-1232-85 ................. .................
Colorimetric ........... 3500-Cr D D1687-92(A) I-1230-85 ................. .................
(Diphenylcarbazide).
19. Chromium-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.. 218.1 3111 B D1687-92(B) I-3236-85 974.27 \3\ .................
AA chelation-extraction.... 218.3 3111 C ...................... ................. ................. .................
AA furnace................. 218.2 3113 B D1687-92(C) ................. ................. .................
ICP/AES \36\............... \5\ 200.7 3120 B ...................... ................. ................. .................
DCP \36\................... ........... ......................... D4190-82(88) ................. ................. AES0029 \34\
Colorimetric ........... 3500-Cr D ...................... ................. ................. .................
(Diphenylcarbazide).
[[Page 14997]]
20. Cobalt-Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration....... 219.1 3111 B or C D3558-90(A or B) I-3239-85 ................. p. 37 \9\
AA furnace................. 219.2 3113 B D3558-90(C) ................. ................. .................
ICP/AES.................... \5\ 200.7 3120B ...................... ................. ................. .................
DCP........................ ........... ......................... D4190-82(88) ................. ................. AES0029 \34\
21. Color platinum cobalt units
or dominant wavelength, hue,
luminance purity:
Colorimetric (ADMI)........ 110.1 2120 E ...................... ................. ................. Note 18
(Platinum cobalt).......... 110.2 2120 B ...................... I-1250-85 ................. .................
Spectrophotometric......... 110.3 2120 C ...................... ................. ................. .................
22. Copper--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.. \5\ 220.1 3111 B or C D1688-90(A or B I-3270-85 or I- 974.27 \3\ p. 37 \9\
3271-85
AA furnace................. 220.2 3113 B D1688-90(C) ................. ................. .................
ICP/AES \36\............... \5\ 200.7 3120 B ...................... ................. ................. .................
DCP \36\................... ........... ......................... D4190-82(88) ................. ................. AES0029 \34\
Colorimetric (Neocuproine). ........... 3500-Cu D ...................... ................. ................. .................
(Bicinchoninate)........... ........... Or E ...................... ................. ................. 8506 \19\
23. Cyanide--Total, mg/L:
Manual distillation with ........... 4500-CN C D2036-91(A) ................. ................. .................
MgCl2 followed by.
Titrimetric................ ........... 4500-CN D ...................... ................. ................. p. 22 \9\
Spectrophotometric, manual. \31\335.2 4500-CN E D2036-91(A) I-3300-85 ................. .................
Automated \20\............. \31\335.3 ......................... ...................... ................. ................. .................
24. Cyanide amenable to
chlorination, mg/L:
Manual distillation with 335.1 4500-CN G D2036-91(B) ................. ................. .................
MgCl2 followed by
titrimetric or
Spectrophotometric.
25. Fluoride--Total, mg/L:
Manual distillation \6\ ........... 4500-F B ...................... ................. ................. .................
followed by.
Electrode, manual.......... 340.2 4500-F C D1179-93(B) ................. ................. .................
Automated.................. ........... ......................... ...................... I-4327-85 ................. .................
Colorimetric (SPADNS)...... 340.1 4500-F D D1179-93(A) ................. ................. .................
Automated complexone....... 340.3 4500-F E ...................... ................. ................. .................
26. Gold--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration....... 231.1 3111 B ...................... ................. ................. .................
AA furnace................. 231.2 ......................... ...................... ................. ................. .................
DCP........................ ........... ......................... ...................... ................. ................. AES0029 \34\
27. Hardness--Total, as CaCO3,
mg/L:
Automated colorimetric..... 130.1 ......................... ...................... ................. ................. .................
Titrimetric (EDTA), or Ca 130.2 2340 B or C D1126-86(92) I-1338-85 973.52B \3\ .................
plus Mg as their
carbonates, by inductively
coupled plasma or AA
direct aspiration. (See
Parameters 13 and 33)..
28. Hydrogen ion (pH), pH
units:
Electrometric measurement.. 150.1 4500-H+ B D1293-84(90) I-1586-85 973.41 \3\
(A or B)
Automated electrode........ ........... ......................... ...................... ................. ................. 378-75WA \21\
29. Iridium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration....... 235.1 3111 B ...................... ................. ................. .................
AA furnace................. 235.2 ......................... ...................... ................. ................. .................
30. Iron--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\.. 236.1 3111 B or C D1068-90 I-3381-85 974.27 \3\ .................
(A or B)
AA furnace................. 236.2 3113 B D1068-90(C) ................. ................. .................
ICP/AES \36\............... \5\ 200.7 3120 B ...................... ................. ................. .................
DCP \36\................... ........... ...
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