[Federal Register Volume 85, Number 105 (Monday, June 1, 2020)]
[Notices]
[Pages 33199-33200]
[FR Doc No: 2020-11659]

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DEPARTMENT OF LABOR

Occupational Safety and Health Administration

[Docket No. OSHA-2020-0003]

Advisory Committee on Construction Safety and Health (ACCSH):
Notice of Meetings

AGENCY: Occupational Safety and Health Administration (OSHA), Labor.

ACTION: Notice of ACCSH and ACCSH Workgroup meetings.

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SUMMARY: The Advisory Committee on Construction Safety and Health
(ACCSH) will meet July 1, 2020, by teleconference and WebEx. In
conjunction with the ACCSH meeting, ACCSH Workgroups will also meet by
teleconference and WebEx on June 30, 2020.

DATES:
    ACCSH meeting: ACCSH will meet from 12:00 p.m. to 5:00 p.m., ET,
Wednesday, July 1, 2020.
    ACCSH Workgroup meetings: Prior to the full Committee meeting,
ACCSH Workgroups will meet Tuesday, June 30, 2020. (For Workgroup
meeting times, see the schedule under ``Workgroup Meetings'' in the
SUPPLEMENTARY INFORMATION section of this notice).

ADDRESSES:
    Submission of comments and requests to speak: Submit comments and
requests to speak at the ACCSH and ACCSH Workgroup meetings by
Thursday, June 25, 2020, identified by the docket number for this
Federal Register notice (Docket No. OSHA-2020-0003), using of the
following method:
    Electronically: Comments and request to speak, including
attachments, must be submitted electronically at: http://www.regulations.gov, the Federal eRulemaking Portal. Follow the online
instructions for submitting comments.
    Requests for special accommodations: Please submit requests for
special accommodations for this ACCSH meeting by Thursday, June 25,
2020, to Ms. Gretta Jameson, OSHA, Directorate of Construction, U.S.
Department of Labor; telephone:<PHONE_NUMBER>; email:
<EMAIL_ADDRESS>
FOR FURTHER INFORMATION CONTACT:
    For press inquiries: Mr. Frank Meilinger, Director, OSHA Office of
Communications, U.S. Department of Labor; telephone<PHONE_NUMBER>;
email<EMAIL_ADDRESS>    For general information about ACCSH: Mr. Damon Bonneau, OSHA,
Directorate of Construction, U.S. Department of Labor; telephone (202)
693-2183; email<EMAIL_ADDRESS>    Telecommunication requirements: For additional information about
the telecommunication requirements for the meeting, please contact Ms.
Veneta Chatmon, OSHA, Directorate of Construction, U.S. Department of
Labor; telephone<PHONE_NUMBER>; email<EMAIL_ADDRESS>    For copies of this Federal Register Notice: Electronic copies of
this Federal Register Notice are available at: http://www.regulations.gov. This notice, as well as news releases and other
relevant

information, are also available at OSHA's web page at www.osha.gov.

SUPPLEMENTARY INFORMATION:

I. Background

    ACCSH advises the Secretary of Labor and the Assistant Secretary of
Labor for Occupational Safety and Health (Assistant Secretary) in the
formulation of standards affecting the construction industry, and on
policy matters arising in the administration of the safety and health
provisions under the Contract Work Hours and Safety Standards Act
(Construction Safety Act (CSA)) (40 U.S.C. 3701 et seq.) and the
Occupational Safety and Health Act of 1970 (OSH Act) (29 U.S.C. 651 et
seq.) (29 CFR 1911.10 and 1912.3). In addition, the CSA requires the
Assistant Secretary to consult with ACCSH before the agency proposes
any occupational safety and health standard affecting construction
activities (40 U.S.C. 3704).
    ACCSH operates in accordance with the CSA, the OSH Act, the Federal
Advisory Committee Act (FACA) (5 U.S.C. App. 2), and regulations issued
pursuant to those statutes (29 CFR part 1912, 41 CFR part 102-3). ACCSH
generally meets two times a year.

II. Meeting Information

Workgroup Meetings

    Attending the meetings: Attendance at the ACCSH Workgroup meetings
will be by teleconference and WebEx only. The dial-in number and
passcode for the meeting are as follows: Dial-in number: 1-888-658-
5408; Passcode: 2597686. Directions for signing into the WebEx portion
of the meetings will be posted in the Docket and on the ACCSH web page,
https://www.osha.gov/advisorycommittee/accsh, prior to the meeting.

 Education, Training, and Outreach Workgroup: 12:00 p.m. to
2:30 p.m., ET
    Meeting agenda:
    1. Trench Safety.
    2. Fall Prevention.
 Emerging and Current Issues Workgroup: 3:00 to 5:30 p.m., ET
    Meeting agenda:
    1. Opioids.
    2. Suicides in construction.
    ACCSH workgroup meetings are open to the public. For additional
information on ACCSH workgroup meetings or participating in them,
please contact Mr. Bonneau (see ``For general information about ACCSH''
in the FOR FURTHER INFORMATION CONTACT section of this notice).

ACCSH Full Committee Meeting

    Attending the meeting: Attendance at the ACCSH Workgroup meetings
will be by teleconference and WebEx only. The dial-in number and
passcode for the meeting are as follows: Dial-in number: 1-888-324-
3487; Passcode: 9671553. Directions for signing into the WebEx portion
of the meetings will be posted in the Docket and on the ACCSH web page,
https://www.osha.gov/advisorycommittee/accsh, prior to the meeting.
    Meeting agenda: The tentative agenda for this meeting includes:
     Principal Deputy Assistant Secretary's agency update and
remarks;
     ACCSH's consideration of, and recommendation on, the
following proposals:
    --Updating the design and construction requirements of the powered
industrial trucks standards by adding an incorporation by reference to
the applicable provisions of the most recent ANSI/ITSDF consensus
standards;
    --Updating the Hazard Communication Standard to maintain alignment
with the Globally Harmonized System of Classification and Labelling of
Chemicals (GHS);
     Silica in construction update;
     ACCSH workgroup reports; and,
     Public comment period.
    Requests to speak and speaker presentations: Attendees who wish to
address ACCSH at either the full committee meeting or the workgroup
meetings must submit a request to speak, as well as any written or
electronic presentation, by Thursday, June 25, 2020, using one of the
methods listed in the ADDRESSES section of this notice. The request
must state:
     The amount of time requested to speak;
     The interest you represent (e.g., business, organization,
affiliation), if any; and
     A brief outline of your presentation.
    PowerPoint presentations and other electronic materials must be
compatible with PowerPoint 2010 and other Microsoft Office 2010
formats.
    Alternately, you may request to address ACCSH briefly during the
public-comment period. At his discretion, the ACCSH Chair may grant
requests to address ACCSH as time and circumstances permit.
    Docket: OSHA will place comments, requests to speak, and speaker
presentations, including any personal information you provide, in the
public docket without change, and those documents may be available
online at: http://www.regulations.gov. Therefore, OSHA cautions
interested parties about submitting personal information such as Social
Security Numbers and birthdates. OSHA also places in the public docket
the meeting transcript, meeting minutes, documents presented at the
meeting, and other documents pertaining to the ACCSH and ACCSH
Workgroup meetings. These documents are available online at: http://www.regulations.gov. To read or download documents in the public docket
for these ACCSH and ACCSH Workgroup meetings, go to Docket No. OSHA-
2020-0003 at: http://www.regulations.gov. All documents in the public
docket are listed in the index; however, some documents (e.g.,
copyrighted material) are not publicly available to read or download
through http://www.regulations.gov. All submissions are available for
inspection and, when permitted, copying at the OSHA Docket Office at
the above address. For information on using http://www.regulations.gov
to make submissions or to access the docket, click on the ``Help'' tab
at the top of the homepage. Contact the OSHA Docket Office for
information about materials not available through that website and for
assistance in using the internet to locate submissions and other
documents in the docket.

Authority and Signature

    Loren Sweatt, Principal Deputy Assistant Secretary of Labor for
Occupational Safety and Health, authorized the preparation of this
notice under the authority granted by 29 U.S.C. 655(b)(1) and 656(b),
40 U.S.C. 3704(a)(2), 5 U.S.C. App. 2, Secretary of Labor's Order No.
1-2012 (77 FR 3912), and 29 CFR part 1912.

    Signed at Washington, DC, on May 26, 2020.
Loren Sweatt,
Principal Deputy Assistant Secretary of Labor for Occupational Safety
and Health.
[FR Doc. 2020-11659 Filed 5-29-20; 8:45 am]
 BILLING CODE 4510-26-P


[Federal Register Volume 81, Number 232 (Friday, December 2, 2016)]
[Proposed Rules]
[Pages 87003-87016]
[FR Doc No: 2016-27544]

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 63

[EPA-HQ-OAR-2016-0069; FRL-9955-22-OAR]
RIN 2060-AT17

Revisions to Method 301: Field Validation of Pollutant
Measurement Methods From Various Waste Media

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: In this action, the Environmental Protection Agency (EPA)
proposes editorial and technical revisions to the EPA's Method 301
``Field Validation of Pollutant Measurement Methods from Various Waste
Media'' in order to correct and update the method. In addition, the EPA
is clarifying the applicability of Method 301 as well as its utility to
other regulatory provisions. The proposed revisions include ruggedness
testing for validation of test methods for application at multiple
sources, determination of limit of detection for all method
validations, incorporating procedures for determining the limit of
detection, revising the sampling requirements for the comparison
procedure, adding storage and sampling procedures for sorbent sampling
systems, and clarifying acceptable statistical results for candidate
test methods. We also propose to clarify the applicability of Method
301 to our regulations and to add equations to clarify calculation of
the correction factor, standard deviation, estimated variance of a
validated test method, standard deviation of differences, and t-
statistic for all validation approaches.
    Changes made to the Method 301 field validation protocol under this
proposed action would apply only to methods submitted to the EPA for
approval after the effective date of this action.

DATES: Comments. Comments must be received on or before January 31,
2017.
    Public Hearing. If anyone contacts the EPA requesting a public
hearing by December 12, 2016, the EPA will hold a public hearing on
January 3, 2017 from 1:00 p.m. (Eastern Standard Time) to 5:00 p.m.
(Eastern Standard Time) at the U.S. Environmental Protection Agency
building located at 109 T.W. Alexander Drive, Research Triangle Park,
NC 27711. Information regarding a hearing will be posted at http://www3.epa.gov/ttn/emc/methods/.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
OAR-2016-0069, to the Federal eRulemaking Portal: http://www.regulations.gov. Follow the online instructions for submitting
comments. Once submitted, comments cannot be edited or withdrawn. The
EPA may publish any comment received to its public docket. Do not
submit electronically any information you consider to be Confidential
Business Information (CBI) or other information whose disclosure is
restricted by statute.
    Multimedia submissions (audio, video, etc.) must be accompanied by
a written comment. The written comment is considered the official
comment and should include discussion of all points you wish to make.
The EPA will generally not consider comments or comment contents
located outside of the primary submission (i.e., on the Web, Cloud, or
other file sharing system). For additional submission methods, the full
EPA public comment policy, information about CBI or multimedia
submissions, and general guidance on making effective comments, please
visit http://www2.epa.gov/dockets/commenting-epa-dockets.

FOR FURTHER INFORMATION CONTACT: For information concerning this
proposal, contact Ms. Kristen J. Benedict, Office of Air Quality
Planning and Standards, Air Quality Assessment Division (E143-02),
Environmental Protection Agency, Research Triangle Park, NC 27711;
telephone number:<PHONE_NUMBER>; fax number:<PHONE_NUMBER>; email
address<EMAIL_ADDRESS>
SUPPLEMENTARY INFORMATION:

Table of Contents

I. General Information
    A. Does this action apply to me?
    B. What should I consider as I prepare my comments?
    C. Where can I get a copy of this document and other related
information?
II. Background
III. Summary of Proposed Revisions
    A. Technical Revisions
    B. Clarifying and Editorial Changes
IV. Request for Comments
V. Statutory and Executive Order Reviews
    A. Executive Order 12866: Regulatory Planning and Review and
Executive Order 13563: Improving Regulation and Regulatory Review
    B. Paperwork Reduction Act (PRA)
    C. Regulatory Flexibility Act (RFA)
    D. Unfunded Mandates Reform Act (UMRA)
    E. Executive Order 13132: Federalism
    F. Executive Order 13175: Consultation and Coordination With
Indian Tribal Governments
    G. Executive Order 13045: Protection of Children From
Environmental Health Risks and Safety Risks
    H. Executive Order 13211: Actions That Significantly Affect
Energy Supply, Distribution, or Use

    I. National Technology Transfer and Advancement Act (NTTAA)
    J. Executive Order 12898: Federal Actions To Address
Environmental Justice in Minority Populations and Low-Income
Populations

I. General Information

A. Does this action apply to me?

    Method 301 affects/applies to you, under 40 CFR 63.7(f) or 40 CFR
65.158(a)(2)(iii), when you want to use an alternative to a required
test method to meet an applicable requirement or when there is no
required or validated test method. In addition, the validation
procedures of Method 301 are an appropriate tool for demonstration of
the suitability of alternative test methods under 40 CFR 59.104 and
59.406, 40 CFR 60.8(b), and 40 CFR 61.13(h)(1)(ii). If you have any
questions regarding the applicability of the proposed changes to Method
301, contact the person listed in the preceding FOR FURTHER INFORMATION
CONTACT section.

B. What should I consider as I prepare my comments?

    Submitting CBI: Clearly mark the part or all of the information
that you claim to be CBI. For CBI information in a disk or CD-ROM that
you mail to the EPA, mark the outside of the disk or CD-ROM as CBI and
then identify electronically within the disk or CD-ROM the specific
information that is claimed as CBI. In addition to one complete version
of the comment that includes information claimed as CBI, a copy of the
comment that does not contain the information claimed as CBI must be
submitted for inclusion in the public docket. Information marked as CBI
will not be disclosed except in accordance with procedures set forth in
title 40 CFR part 2.
    Do not submit information that you consider to be CBI or otherwise
protected through http://www.regulations.gov or email. Send or deliver
information identified as CBI to: OAQPS Document Control Officer (Room
C404-02), U.S. EPA, Research Triangle Park, NC 27711, Attention Docket
ID No. EPA-HQ-OAR-2016-0069.
    If you have any questions about CBI or the procedures for claiming
CBI, please consult the person identified in the FOR FURTHER
INFORMATION CONTACT section.
    Docket: All documents in the docket are listed in the http://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, will be publicly available only in hard copy.
Publicly available docket materials are available either electronically
in http://www.regulations.gov or in hard copy at the EPA Docket Center,
EPA/DC, EPA WJC West Building, Room 3334, 1301 Constitution Ave. NW.,
Washington, DC. This Docket Facility is open from 8:30 a.m. to 4:30
p.m., Monday through Friday, excluding legal holidays. The telephone
number for the Public Reading Room is<PHONE_NUMBER>, and the telephone
number for the Air Docket is<PHONE_NUMBER>.

C. Where can I get a copy of this document and other related
information?

    In addition to being available in the docket, an electronic copy of
the proposed method revisions is available on the Technology Transfer
Network (TTN) Web site at http://www3.epa.gov/ttn/emc/methods/. The TTN
provides information and technology exchange in various areas of air
pollution control.

II. Background

    The EPA originally published Method 301 (appendix A to 40 CFR part
63, Test Methods) on December 29, 1992 (57 FR 61970), as a field
validation protocol method to be used to validate new test methods for
hazardous air pollutants in support of the Early Reductions Program of
Part 63 when test methods were unavailable. On March 16, 1994, the EPA
incorporated Method 301 into 40 CFR 63.7 (59 FR 12430) as a means to
validate a candidate test method as an alternative to a test method
specified in a standard or for use where no test method is provided in
a standard. To date, subsequent revisions of Method 301 have not
distinguished requirements for source-specific applications of a
candidate method versus application of a candidate test method at
multiple sources. The EPA's Method 301 specifies procedures for
determining and documenting the bias and precision of a test method
that is a candidate for use as an alternative to a test method
specified in an applicable regulation, or for use as a means for
showing compliance with a regulatory standard in absence of a validated
test method. Method 301 is required for these purposes under 40 CFR
63.7(f) and 40 CFR 65.158(a)(2)(iii), and would be considered an
appropriate tool for demonstration and validation of alternative
methods under 40 CFR 59.104 and 59.406, 40 CFR 60.8(b), and 40 CFR
61.13(h)(1)(ii). The procedures specified in Method 301 are applicable
to various media types (e.g., sludge, exhaust gas, wastewater).
    Bias (or systemic error) is established by comparing measurements
made using a candidate test method against reference values, either
reference materials or a validated test method. Where needed, a
correction factor for source-specific application of the method is
employed to eliminate/minimize bias. This correction factor is
established from data obtained during the validation test. Methods that
have bias correction factors outside a specified range are considered
unacceptable. Method precision (or random error) must be demonstrated
to be as precise as the validated method for acceptance or less than or
equal to 20 percent when the candidate method is being evaluated using
reference materials.
    Additionally, the EPA recognized that there were a number of ways
Method 301 could be clarified while reviewing submitted data and
answering questions from facilities, environmental labs, and technology
vendors on the application and requirements of the method.

III. Summary of Proposed Revisions

    In this action, we propose clarifications to the applicability and
utility of Method 301 to additional regulatory provisions, and propose
technical revisions and editorial changes intended to clarify and
update the requirements and procedures specified in Method 301.

A. Technical Revisions

1. Applicability of Ruggedness Testing and Limit of Detection
Determination
    In the current version of Method 301, the procedures for conducting
ruggedness testing in sections 3.1 and 14.0, and for determining the
limit of detection (LOD) in sections 3.1 and 15.0, are optional
procedures that are not required for validation of a candidate test
method. In this action, we propose to amend sections 3.1 and 14.0 to
require ruggedness testing when using Method 301 to validate a
candidate test method intended for application to multiple sources.
Ruggedness testing would continue to be optional for validation of
methods intended for source-specific applications. We also propose to
amend sections 3.1 and 15.0 to require determination of the LOD for
validation of all methods (i.e., those intended for both source and
multi-source application). Additionally, we propose clarifications to
the LOD definition in section 15.1.

    Ruggedness testing of a test method is a laboratory study to
determine the sensitivity of the method by measuring its capacity to
remain unaffected by small, but deliberate variations in method
parameters such as sample collection rate and sample recovery
temperature to provide an indication of its reliability during normal
usage. Requiring ruggedness testing and determination of the LOD for
validation of a candidate test method that is intended for use at
multiple sources will further inform the EPA's determination of whether
the candidate test method is valid across a range of source emission
matrices, varying method parameters, and conditions. Additionally,
conducting an LOD determination for source-specific validations will
account for the sensitivity of the candidate test method to ensure it
meets applicable regulatory requirements.
2. Limit of Detection Procedures
    The EPA proposes revisions to the requirements for determining the
LOD specified in section 15.2 and Table 301-5 (Procedure I) to
incorporate procedures of the EPA's proposed revisions to 40 CFR part
136, appendix B (80 FR 8955). The proposed revisions address laboratory
blank contamination and account for intra-laboratory variability,
consistent with the proposed changes to 40 CFR part 136. We propose to
require Procedure I of Table 301-5 for determining an LOD when an
analyte in a sample matrix is collected prior to an analytical
measurement or the estimated LOD is no more than twice the calculated
LOD.
    For the purposes of this proposed rule, LOD would be equivalent to
the calculated method detection limit (MDL) determined using the
procedures specified in proposed 40 CFR part 136, appendix B. Through
this proposed change, laboratories would be required to consider media
blanks when performing LOD calculations. If the revisions to 40 CFR
part 136, appendix B are finalized as proposed prior to a final action
on this proposal, we will cross-reference appendix B. If appendix B is
finalized before this action and the revisions do not incorporate the
procedures as described above, the EPA intends to incorporate the
specific procedures for determining the LOD in the final version of
Method 301 consistent with this proposal. If appendix B is not
finalized before these proposed revisions, the EPA also intends to
incorporate the specific procedures directly into Method 301. Other
than the proposed revisions to 40 CFR part 136, appendix B, as
discussed above, changes addressed under that rulemaking are outside
the scope of this proposed action.
3. Storage and Sampling Procedures
    Currently, the number of samples required by Method 301 when using
a quadruplicate sampling system for conducting the analyte spiking
procedure and for conducting the comparison procedure is not
consistent. In this action, we propose revisions to section 11.1.3 and
Table 301-1 to require six sets of quadruplicate samples (a total of 24
samples for the analyte spiking or comparison procedures) rather than
four sets. This proposed revision will ensure the bias and precision
requirements are consistent in the method and decrease the amount of
uncertainty in the calculations for bias and precision when comparing
an alternative test method with a validated method. Bias and precision
(standard deviation and variance) are all inversely related to the
number of sampling trains (sample results) used to estimate the
difference between the alternative test method and the validated
method. As the number of trains goes up, the bias and precision
estimates go down. Larger data sets provide better estimates of the
standard deviation or variance and the distribution of the data. The
proposed revision to collect a total of 24 samples when using the
analyte spiking approach is also consistent with the number of samples
required for the isotopic spiking approach. The 12 samples collected
when conducting the isotopic spiking approach are equivalent to the 24
samples collected using the analyte spiking approach because the
isotopic labelling of the spike allows each of the 12 samples to yield
two results, one for an unspiked sample and one for a spiked sample.
    In this action, we also propose revisions to section 9.0 to specify
that either paired sampling or quadruplicate sampling systems may be
used for isotopic spiking, while only quadruplicate sampling systems
may be used to establish precision for analyte spiking or when
comparing an alternative method to a validated method.
    For validations conducted by comparing the candidate test method to
a validated test method, we propose to add: (1) Storage and sampling
procedures for sorbent systems requiring thermal desorption to Table
301-2; and (2) a new Table 301-4 to provide a look-up table of F values
for the one-sided confidence level used in assessing the precision of
the candidate test method. We also propose an amendment to the
reference list in section 18.0 to include the source of the F values.
4. Bias Criteria for Multi-Source Versus Source-Specific Validation
    In this action, we propose clarification to sections 8.0, 10.3, and
11.1.3 to specify that candidate test methods intended for use at
multiple sources must have a bias less than or equal to 10 percent. We
propose that candidate test methods with a bias greater than 10
percent, but less than 30 percent, apply only at the source at which
the validation testing was conducted and that data collected in the
future be adjusted for bias using a source-specific correction factor.
A source-specific correction factor is not necessarily appropriate for
use at multiple sources. This proposed change provides flexibility for
source-specific Method 301 application while limiting the acceptance
criteria for use of the method at multiple sources. We believe that the
Method 301 results from a single source are not sufficient to allow us
to establish a correction factor that can be applied at multiple
sources.
5. Relative Standard Deviation Assessment
    In this action, we propose amendments to sections 9.0 and 12.2 to
clarify the interpretation of the relative standard deviation (RSD)
when determining the precision of a candidate test method using the
analyte spiking or isotopic spiking procedures. For a test method to be
acceptable, we propose that the RSD of a candidate test method must be
less than or equal to 20 percent. Accordingly, we propose to remove the
sampling provisions for cases where the RSD is greater than 20 percent,
but less than 50 percent. Poor precision makes it difficult to detect
potential bias in a test method. For this reason, we are proposing an
acceptance criteria of less than or equal to 20 percent for analyte and
isotopic spiking sampling procedures.
6. Applicability of Method 301
    Currently, Method 301 states that it is applicable for determining
alternative test methods for standards under 40 CFR part 63 (National
Emission Standards for Hazardous Air Pollutants for Source Categories).
Although 40 CFR 65.158(a)(2)(iii) specifically cross-references Method
301, Method 301 has not previously been revised to reference Part 65.
For parts 63 and 65, Method 301 must be used for establishing an
alternative test method. In this action, we propose revisions
clarifying that Method 301 is applicable to both parts 63 and 65 and
that Method 301 is also

appropriate for validating alternative test methods for use under the
following parts under title 40 of the Clean Air Act:

 Part 59 (National Volatile Organic Compound Emission Standards
for Consumer and Commercial Products)
 Part 60 (Standards of Performance for New Stationary Sources)
 Part 61 (National Emission Standards for Hazardous Air
Pollutants)

    We believe that the Method 301 procedures for determining bias and
precision provide a suitable technical approach for assessing candidate
or alternative test methods for use under these regulatory parts as the
testing provisions are very similar to those under parts 63 and 65. To
accommodate the expanded applicability and suitability, we propose to
revise the references in sections 2.0, 3.2, 5.0, 13.0, 14.0, and 16.1
to refer to all five regulatory parts.
7. Equation Additions
    In this action, we propose to clarify the procedures in Method 301
by adding the following equations:

 Equation 301-8 in section 10.3 for calculating the correction
factor
 Equation 301-11 in section 11.1.1 and Equation 301-19 in
section 12.1.1 for calculating the numerical bias
 Equation 301-12 in section 11.1.2 and Equation 301-20 in
section 12.1.2 for determining the standard deviation of differences
 Equation 301-13 in section 11.1.3 and Equation 301-21 in
section 12.1.3 for calculating the t-statistic
 Equation 301-15 in section 11.2.1 to estimate the variance of
the validated test method
 Equation 301-23 in section 12.2 for calculating the standard
deviation

    We also propose revisions to the denominator of Equation 22 to use
the variable ``CS'' rather than ``VS.'' Additionally, we propose
revisions to the text of Method 301, where needed, to list and define
all variables used in the method equations. These proposed changes are
intended to improve the readability of the method and ensure that
required calculations and acceptance criteria for each of Method 301's
three validation approaches are clear.

B. Clarifying and Editorial Changes

    In this action, we propose minor edits throughout the text of
Method 301 to clarify the descriptions and requirements for assessing
bias and precision, to ensure consistency when referring to citations
within the method, to renumber equations and tables (where necessary),
and to remove passive voice.
    We propose edits to clarify several definitions in section 3.2. In
the definition of ``Paired sampling system,'' we propose a minor edit
to note that the system is collocated. For the definition of
``Quadruplet sampling system,'' we propose to replace the term
``Quadruplet'' with ``Quadruplicate'' and to add descriptive text to
the definition to provide examples of replicate samples. We are also
proposing companion edits throughout the method text to reflect the
change in terminology from ``quadruplet'' to ``quadruplicate.''
Additionally, we propose clarifying edits to the definition of
``surrogate compound.''
    We also propose replacing the term ``alternative test method'' with
``candidate test method'' in section 3.2 and throughout Method 301 to
maintain consistency when referring to a test method that is subject to
the validation procedures specified in Method 301.
    Additionally, the EPA proposes the following updates and
corrections by:
     Updating the address for submitting waivers in section
17.2.
     Adding the t-value for 11 degrees of freedom to Table 301-
2.
     Correcting the t-value for four degrees of freedom in
Table 301-2.

IV. Request for Comments

    The EPA specifically requests public comments on the expanded
applicability of Method 301 to 40 CFR part 59 and to note the
suitability of Method 301 for validation of alternative test methods
under 40 CFR parts 60 and 61. In addition, we specifically request
comment on the following proposed technical amendments to Method 301:
    (A) Requiring ruggedness testing and determination of LOD for
validation of test methods intended for multi-source and source-
specific applications.
    (B) Incorporating the procedures specified in the proposed
revisions to 40 CFR part 136, appendix B, into the Method 301
procedures for determining LOD.
    (C) Revising the sampling requirements for the method comparison
procedure to require six sets of quadruplicate samples rather than four
sets, and adding storage and sampling procedures for sorbent systems
that require thermal desorption.
    (D) Clarifying that candidate test methods that are intended for
use at multiple sources must have a bias less than or equal to 10
percent and that test methods, where the bias is greater than 10
percent but less than to 30 percent, are applicable only on a source-
specific basis with the use of a correction factor.
    (E) Clarifying that the RSD of a candidate test method validated
using the analyte spiking or isotopic spiking procedure must be less
than or equal to 20 percent for the method to be acceptable.
    (F) Adding equations to calculate the: (1) Correction factor (if
required) when using isotopic spiking; (2) standard deviation when
using the analyte spiking procedure; (3) estimated variance of
validated test method when using the comparison procedure; and (4)
standard deviation of differences and t-statistic when using the
analyte spiking or comparison procedures.

V. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review and Executive
Order 13563: Improving Regulation and Regulatory Review

    This proposed action is not a significant regulatory action and
was, therefore, not submitted to the Office of Management and Budget
(OMB) for review.

B. Paperwork Reduction Act (PRA)

    This proposed action does not impose an information collection
burden under the PRA. The revisions being proposed in this action to
Method 301 do not add information collection requirements, but make
corrections and updates to existing testing methodology.

C. Regulatory Flexibility Act (RFA)

    I certify that this proposed action will not have a significant
economic impact on a substantial number of small entities under the
RFA. This action will not impose any requirements on small entities.
The proposed revisions to Method 301 do not impose any requirements on
regulated entities beyond those specified in the current regulations,
nor do they change any emission standard. We have therefore concluded
that this proposed action will have no net regulatory burden for all
directly regulated small entities.

D. Unfunded Mandates Reform Act (UMRA)

    This proposed action does not contain any unfunded mandate of $100
million or more as described in UMRA, 2 U.S.C. 1531-1538. The proposed
action imposes no enforceable duty on any state, local or tribal
governments or the private sector.

E. Executive Order 13132: Federalism

    This proposed action does not have federalism implications. It will
not have substantial direct effects on the states, on the relationship
between the national government and the states, or on the distribution
of power and

responsibilities among the various levels of government.

F. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments

    This proposed action does not have tribal implications, as
specified in Executive Order 13175. This proposed action would correct
and update the existing procedures specified in Method 301. Thus,
Executive Order 13175 does not apply to this proposed action.

G. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks

    The EPA interprets Executive Order 13045 as applying only to those
regulatory actions that concern environmental health or safety risks
that the EPA has reason to believe may disproportionately affect
children, per the definition of ``covered regulatory action'' in
section 2-202 of the Executive Order. This proposed action is not
subject to Executive Order 13045 because it does not concern an
environmental health risk or safety risk.

H. Executive Order 13211: Actions That Significantly Affect Energy
Supply, Distribution, or Use

    This proposed action is not subject to Executive Order 13211,
because it is not a significant regulatory action under Executive Order
12866.

I. National Technology Transfer and Advancement Act (NTTAA)

    This proposed action involves technical standards. The agency
previously identified ASTM D4855-97 (Standard Practice for Comparing
Test Methods) as being potentially applicable in previous revisions of
Method 301, but determined that the use of ASTM D4855-97 was
impractical (Section V in 76 FR 28664).

J. Executive Order 12898: Federal Actions To Address Environmental
Justice in Minority Populations and Low-Income Populations

    The EPA believes that this action is not subject to Executive Order
12898 (59 FR 7629, February 16, 1994) because it does not establish an
environmental health or safety standard. This action would make
corrections and updates to an existing protocol for assessing the
precision and accuracy of alternative test methods to ensure they are
comparable to the methods otherwise required; thus, it does not modify
or affect the impacts to human health or the environment of any
standards for which it may be used.

List of Subjects in 40 CFR Part 63

    Environmental protection, Air pollution control, Alternative test
method, EPA Method 301, Field validation, Hazardous air pollutants.

    Dated: November 8, 2016.
Gina McCarthy,
Administrator.

    For the reasons stated in the preamble, the EPA proposes to amend
title 40, chapter I of the Code of the Federal Regulations as follows:

PART 63--[AMENDED]

0
1. The authority citation for part 63 continues to read as follows:

    Authority: 42 U.S.C. 7401 et seq.

0
2. Appendix A to part 63 is amended by revising Method 301 to read as
follows:

Appendix A to Part 63--Test Methods Pollutant Measurement Methods From
Various Waste Media

Method 301--Field Validation of Pollutant Measurement Methods From
Various Waste Media

Sec.

Using Method 301

1.0 What is the purpose of Method 301?
2.0 When must I use Method 301?
3.0 What does Method 301 include?
4.0 How do I perform Method 301?

Reference Materials

5.0 What reference materials must I use?

Sampling Procedures

6.0 What sampling procedures must I use?
7.0 How do I ensure sample stability?

Bias and Precision

8.0 What are the requirements for bias?
9.0 What are the requirements for precision?
10.0 What calculations must I perform for isotopic spiking?
11.0 What calculations must I perform for comparison with a
validated method if I am using quadruplicate replicate sampling
systems?
12.0 What calculations must I perform for analyte spiking?
13.0 How do I conduct tests at similar sources?

Optional Requirements

14.0 How do I use and conduct ruggedness testing?
15.0 How do I determine the Limit of Detection for the candidate
test method?

Other Requirements and Information

16.0 How do I apply for approval to use a candidate test method?
17.0 How do I request a waiver?
18.0 Where can I find additional information?

Using Method 301

1.0 What is the purpose of Method 301?

    Method 301 provides a set of procedures for the owner or
operator of an affected source, to validate a candidate test method
as an alternative to a required test method based on established
precision and bias criteria. These validation procedures are
applicable under 40 CFR part 63 or 65 when a test method is proposed
as an alternative test method to meet an applicable requirement or
in the absence of a validated method. Additionally, the validation
procedures of Method 301 are appropriate for demonstration of the
suitability of alternative test methods under 40 CFR parts 59, 60,
and 61. If, under 40 CFR part 63 or 60, you choose to propose a
validation method other than Method 301, you must submit and obtain
the Administrator's approval for the candidate validation method.

2.0 What approval must I have to use Method 301?

    If you want to use a candidate test method to meet requirements
in a subpart of 40 CFR part 59, 60, 61, 63, or 65, you must also
request approval to use the candidate test method according to the
procedures in Section 16 of this method and the appropriate section
of the part (Sec.  59.104, Sec.  59.406, Sec.  60.8(b), Sec.
61.13(h)(ii), Sec.  63.7(f), or Sec.  65.158(a)(2)(iii)). You must
receive the Administrator's written approval to use the candidate
test method before you use the candidate test method to meet the
applicable federal requirements. In some cases, the Administrator
may decide to waive the requirement to use Method 301 for a
candidate test method to be used to meet a requirement under 40 CFR
part 59, 60, 61, 63, or 65 in absence of a validated test method.
Section 17 of this method describes the requirements for obtaining a
waiver.

3.0 What does Method 301 include?

    3.1 Procedures. Method 301 includes minimum procedures to
determine and document systematic error (bias) and random error
(precision) of measured concentrations from exhaust gases,
wastewater, sludge, and other media. Bias is established by
comparing the results of sampling and analysis against a reference
value. Bias may be adjusted on a source-specific basis using a
correction factor and data obtained during the validation test.
Precision may be determined using a paired sampling system or
quadruplicate sampling system for isotopic spiking. A quadruplicate
sampling system is required when establishing precision for analyte
spiking or when comparing a candidate test method to a validated
method. If such procedures have not been established and verified
for the candidate test method, Method 301 contains procedures for
ensuring sample stability by developing sample storage procedures
and limitations and then testing them. Method 301 also includes
procedures for ruggedness testing and determining detection limits.
The procedures for ruggedness testing and determining detection
limits are required for candidate test methods that are to be
applied to multiple sources and optional for

candidate test methods that are to be applied at a single source.
    3.2 Definitions.
    Affected source means an affected source as defined in the
relevant part and subpart under title 40 (e.g., 40 CFR parts 59, 60,
61, 63, and 65).
    Candidate test method means the sampling and analytical
methodology selected for field validation using the procedures
described in Method 301. The candidate test method may be an
alternative test method under 40 CFR part 59, 60, 61, 63, or 65.
    Paired sampling system means a sampling system capable of
obtaining two replicate samples that are collected as closely as
possible in sampling time and sampling location (collocated).
    Quadruplicate sampling system means a sampling system capable of
obtaining four replicate samples (e.g., two pairs of measured data,
one pair from each method when comparing a candidate test method
against a validated test method, or analyte spiking with two spiked
and two unspiked samples) that are collected as close as possible in
sampling time and sampling location.
    Surrogate compound means a compound that serves as a model for
the target compound(s) being measured (i.e., similar chemical
structure, properties, behavior). The surrogate compound can be
distinguished by the candidate test method from the compounds being
analyzed.

4.0 How do I perform Method 301?

    First, you use a known concentration of an analyte or compare
the candidate test method against a validated test method to
determine the bias of the candidate test method. Then, you collect
multiple, collocated simultaneous samples to determine the precision
of the candidate test method. Additional procedures, including
validation testing over a broad range of concentrations over an
extended time period are used to expand the applicability of a
candidate test method to multiple sources. Sections 5.0 through 17.0
of this method describe the procedures in detail.

Reference Materials

5.0 What reference materials must I use?

    You must use reference materials (a material or substance with
one or more properties that are sufficiently homogenous to the
analyte) that are traceable to a national standards body (e.g.,
National Institute of Standards and Technology (NIST)) at the level
of the applicable emission limitation or standard that the subpart
in 40 CFR part 59, 60, 61, 63, or 65 requires. If you want to expand
the applicable range of the candidate test method, you must conduct
additional test runs using analyte concentrations higher and lower
than the applicable emission limitation or the anticipated level of
the target analyte. You must obtain information about your analyte
according to the procedures in Sections 5.1 through 5.4 of this
method.
    5.1 Exhaust Gas Test Concentration. You must obtain a known
concentration of each analyte from an independent source such as a
specialty gas manufacturer, specialty chemical company, or chemical
laboratory. You must also obtain the manufacturer's certification of
traceability, uncertainty, and stability for the analyte
concentration.
    5.2 Tests for Other Waste Media. You must obtain the pure liquid
components of each analyte from an independent manufacturer. The
manufacturer must certify the purity, traceability, uncertainty, and
shelf life of the pure liquid components. You must dilute the pure
liquid components in the same type medium or matrix as the waste
from the affected source.
    5.3 Surrogate Analytes. If you demonstrate to the
Administrator's satisfaction that a surrogate compound behaves as
the analyte does, then you may use surrogate compounds for highly
toxic or reactive compounds. A surrogate may be an isotope or
compound that contains a unique element (e.g., chlorine) that is not
present in the source or a derivation of the toxic or reactive
compound if the derivative formation is part of the method's
procedure. You may use laboratory experiments or literature data to
show behavioral acceptability.
    5.4 Isotopically-Labeled Materials. Isotope mixtures may contain
the isotope and the natural analyte. The concentration of the
isotopically-labeled analyte must be more than five times the
concentration of the naturally-occurring analyte.

Sampling Procedures

6.0 What sampling procedures must I use?

    You must determine bias and precision by comparison against a
validated test method, using isotopic spiking, or using analyte
spiking (or the equivalent). Isotopic spiking can only be used with
candidate test methods capable of measuring multiple isotopes
simultaneously such as test methods using mass spectrometry or
radiological procedures. You must collect samples according to the
requirements specified in Table 301-1 of this method. You must
perform the sampling according to the procedures in Sections 6.1
through 6.4 of this method.
    6.1 Isotopic Spiking. Spike all 12 samples with isotopically-
labelled analyte at an analyte mass or concentration level
equivalent to the emission limitation or standard specified in the
applicable regulation. If there is no applicable emission limitation
or standard, spike the analyte at the expected level of the samples.
Follow the applicable spiking procedures in Section 6.3 of this
method.
    6.2 Analyte Spiking. In each quadruplicate set, spike half of
the samples (two out of the four samples) with the analyte according
to the applicable procedure in Section 6.3 of this method. You
should spike at an analyte mass or concentration level equivalent to
the emission limitation or standard specified in the applicable
regulation. If there is no applicable emission limitation or
standard, spike the analyte at the expected level of the samples.
Follow the applicable spiking procedures in Section 6.3 of this
method.
    6.3 Spiking Procedure.
    6.3.1 Gaseous Analyte With Sorbent or Impinger Sampling Train.
Sample the analyte being spiked (in the laboratory or preferably in
the field) at a mass or concentration that is approximately
equivalent to the applicable emission limitation or standard (or the
expected sample concentration or mass where there is no standard)
for the time required by the candidate test method, and then sample
the stack gas stream for an equal amount of time. The time for
sampling both the analyte and stack gas stream should be equal;
however, you must adjust the sampling time to avoid sorbent
breakthrough. You may sample the stack gas and the gaseous analyte
at the same time. You must introduce the analyte as close to the tip
of the sampling probe as possible.
    6.3.2 Gaseous Analyte With Sample Container (Bag or Canister).
Spike the sample containers after completion of each test run with
an analyte mass or concentration to yield a concentration
approximately equivalent to the applicable emission limitation or
standard (or the expected sample concentration or mass where there
is no standard). Thus, the final concentration of the analyte in the
sample container would be approximately equal to the analyte
concentration in the stack gas plus the equivalent of the applicable
emission standard (corrected for spike volume). The volume amount of
spiked gas must be less than 10 percent of the sample volume of the
container.
    6.3.3 Liquid or Solid Analyte With Sorbent or Impinger Trains.
Spike the sampling trains with an amount approximately equivalent to
the mass or concentration in the applicable emission limitation or
standard (or the expected sample concentration or mass where there
is no standard) before sampling the stack gas. If possible, do the
spiking in the field. If it is not possible to do the spiking in the
field, you must spike the sampling trains in the laboratory.
    6.3.4 Liquid and Solid Analyte With Sample Container (Bag or
Canister). Spike the containers at the completion of each test run
with an analyte mass or concentration approximately equivalent to
the applicable emission limitation or standard in the subpart (or
the expected sample concentration or mass where there is no
standard).
    6.4 Probe Placement and Arrangement for Stationary Source Stack
or Duct Sampling. To sample a stationary source, you must place the
paired or quadruplicate probes according to the procedures in this
subsection. You must place the probe tips in the same horizontal
plane.
    6.4.1 Paired Sampling Probes. For paired sampling probes, the
first probe tip should be 2.5 centimeters (cm) from the outside edge
of the second probe tip, with a pitot tube on the outside of each
probe. Section 17.1 of Method 301 describes conditions for waivers.
For example, the Administrator may approve a validation request
where other paired arrangements for the pitot tubes (where required)
are used.
    6.4.2 Quadruplicate Sampling Probes. For quadruplicate sampling
probes, the tips should be in a 6.0 cm x 6.0 cm square area measured
from the center line of the opening of the probe tip with a single
pitot tube, where required, in the center of the probe

tips or two pitot tubes, where required, with their location on
either side of the probe tip configuration. Section 17.1 of Method
301 describes conditions for waivers. For example, you must propose
an alternative arrangement whenever the cross-sectional area of the
probe tip configuration is approximately five percent or more of the
stack or duct cross-sectional area.

7.0 How do I ensure sample stability?

    7.1 Developing Sample Storage and Threshold Procedures. If the
candidate test method includes well-established procedures supported
by experimental data for sample storage and the time within which
the collected samples must be analyzed, you must store the samples
according to the procedures in the candidate test method and you are
not required to conduct the procedures specified in Section 7.2 or
7.3 of this method. If the candidate test method does not include
such procedures, your candidate method must include procedures for
storing and analyzing samples to ensure sample stability. At a
minimum, your proposed procedures must meet the requirements in
Section 7.2 or 7.3 of this method. The minimum time period between
collection and storage must be as soon as possible, but no longer
than 72 hours after collection of the sample. The maximum storage
duration must not be longer than 2 weeks.
    7.2 Storage and Sampling Procedures for Stack Test Emissions.
You must store and analyze samples of stack test emissions according
to Table 301-2 of this method. You may reanalyze the same sample at
both the minimum and maximum storage durations for: (1) Samples
collected in containers such as bags or canisters that are not
subject to dilution or other preparation steps, or (2) impinger
samples not subjected to preparation steps that would affect
stability of the sample such as extraction or digestion. For
candidate test method samples that do not meet either of these
criteria, you must analyze one of a pair of replicate samples at the
minimum storage duration and the other replicate at the proposed
storage duration but no later than 2 weeks of the initial analysis
to identify the effect of storage duration on analyte samples. If
you are using the isotopic spiking procedure, then you must analyze
each sample for the spiked analyte and the native analyte.
    7.3 Storage and Sampling Procedures for Testing Other Waste
Media (e.g., Soil/Sediment, Solid Waste, Water/Liquid). You must
analyze one of each pair of replicate samples (half the total
samples) at the minimum storage duration and the other replicate
(other half of samples) at the maximum storage duration or within
two weeks of the initial analysis to identify the effect of storage
duration on analyte samples. The minimum time period between
collection and storage should be as soon as possible, but no longer
than 72 hours after collection of the sample.
    7.4 Sample Stability. After you have conducted sampling and
analysis according to Section 7.2 or 7.3 of this method, compare the
results at the minimum and maximum storage durations. Calculate the
difference in the results using Equation 301-1 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.000

Where:

di = Difference between the results of the ith
replicate pair of samples.
Rmini = Results from the ith replicate sample
pair at the minimum storage duration.
Rmaxi = Results from the ith replicate sample
pair at the maximum storage duration.

    For single samples that can be reanalyzed for sample stability
assessment (e.g., bag or canister samples and impinger samples that
do not require digestion or extraction), the values for
Rmini and Rmaxi will be obtained from the same
sample rather than replicate samples.
    7.4.1 Standard Deviation. Determine the standard deviation of
the paired samples using Equation 301-2 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.001

Where:

SDd = Standard deviation of the differences of the paired
samples.
di = Difference between the results of the ith
replicate pair of samples.
dm = Mean of the paired sample differences.
n = Total number of paired samples.

    7.4.2 T Test. Test the difference in the results for statistical
significance by calculating the t-statistic and determining if the
mean of the differences between the results at the minimum storage
duration and the results after the maximum storage duration is
significant at the 95 percent confidence level and n-1 degrees of
freedom. Calculate the value of the t-statistic using Equation 301-3
of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.002

Where:

t = t-statistic.
dm = The mean of the paired sample differences.
SDd = Standard deviation of the differences of the paired
samples.
n = Total number of paired samples.

    Compare the calculated t-statistic with the critical value of
the t-statistic from Table 301-3 of this method. If the calculated
t-value is less than the critical value, the difference is not
statistically significant. Therefore, the sampling, analysis, and
sample storage procedures ensure stability, and you may submit a
request for validation of the candidate test method. If the
calculated t-value is greater than the critical value, the
difference is statistically significant, and you must repeat the
procedures in Section 7.2 or 7.3 of this method with new samples
using a shorter proposed maximum storage duration or improved
handling and storage procedures.

Bias and Precision

8.0 What are the requirements for bias?

    You must determine bias by comparing the results of sampling and
analysis using the candidate test method against a reference value.
The bias must be no more than 10 percent for the
candidate test method to be considered for application to multiple
sources. A candidate test method with a bias greater than 10 percent and less than or equal to 30 percent
can only be applied on

a source-specific basis at the facility at which the validation
testing was conducted. In this case, you must use a correction
factor for all data collected in the future using the candidate test
method. If the bias is more than 30 percent, the
candidate test method is unacceptable.

9.0 What are the requirements for precision?

    You may use a paired sampling system or a quadruplicate sampling
system to establish precision for isotopic spiking. You must use a
quadruplicate sampling system to establish precision for analyte
spiking or when comparing a candidate test method to a validated
method. If you are using analyte spiking or isotopic spiking, the
precision, expressed as the relative standard deviation (RSD) of the
candidate test method, must be less than or equal to 20 percent. If
you are comparing the candidate test method to a validated test
method, the candidate test method must be at least as precise as the
validated method as determined by an F test (see Section 11.2.2 of
this method).

10.0 What calculations must I perform for isotopic spiking?

    You must analyze the bias, RSD, precision, and data acceptance
for isotopic spiking tests according to the provisions in Sections
10.1 through 10.4 of this method.
    10.1 Numerical Bias. Calculate the numerical value of the bias
using the results from the analysis of the isotopic spike in the
field samples and the calculated value of the spike according to
Equation 301-4 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.003

Where:

B = Bias at the spike level.
Sm = Mean of the measured values of the isotopically-
labeled analyte in the samples.
CS = Calculated value of the isotopically-labeled spike level.

    10.2 Standard Deviation. Calculate the standard deviation of the
Si values according to Equation 301-5 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.004

Where:

SD = Standard deviation of the candidate test method.
Si = Measured value of the isotopically-labeled analyte
in the i\th\ field sample.
Sm = Mean of the measured values of the isotopically-
labeled analyte in the samples.
n = Number of isotopically-spiked samples.

    10.3 T Test. Test the bias for statistical significance by
calculating the t-statistic using Equation 301-6 of this method. Use
the standard deviation determined in Section 10.2 of this method and
the numerical bias determined in Section 10.1 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.005

Where:

t = Calculated t-statistic.
B = Bias at the spike level.
SD = Standard deviation of the candidate test method.
n = Number of isotopically spike samples.

    Compare the calculated t-value with the critical value of the
two-sided t-distribution at the 95 percent confidence level and n-1
degrees of freedom (see Table 301-3 of this method). When you
conduct isotopic spiking according to the procedures specified in
Sections 6.1 and 6.3 of this method as required, this critical value
is 2.201 for 11 degrees of freedom. If the calculated t-value is
less than or equal to the critical value, the bias is not
statistically significant, and the bias of the candidate test method
is acceptable. If the calculated t-value is greater than the
critical value, the bias is statistically significant, and you must
evaluate the relative magnitude of the bias using Equation 301-7 of
this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.006

Where:

BR = Relative bias.
B = Bias at the spike level.
CS = Calculated value of the spike level.

    If the relative bias is less than or equal to 10 percent, the
bias of the candidate test method is acceptable for use at multiple
sources. If the relative bias is greater than 10 percent but less
than or equal to 30 percent, and if you correct all data collected
with the candidate test method in the future for bias using the
source-specific correction factor determined in Equation 301-8 of
this method, the candidate test method is acceptable only for
application to the source at which the validation testing was
conducted and may not be applied to any other sites. If either of
the preceding two cases applies, you may continue to evaluate the
candidate test method by calculating its precision. If not, the
candidate test method does not meet the requirements of Method 301.

[GRAPHIC] [TIFF OMITTED] TP02DE16.007

Where:

CF = Source-specific bias correction factor.
B = Bias at the spike level.
CS = Calculated value of the spike level.

    If the CF is outside the range of 0.70 to 1.30, the data and
method are considered unacceptable.
    10.4 Precision. Calculate the RSD according to Equation 301-9 of
this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.008

Where:

RSD = Relative standard deviation of the candidate test method.
SD = Standard deviation of the candidate test method calculated in
Equation 301-5 of this method.
Sm = Mean of the measured values of the spike samples.

    The data and candidate test method are unacceptable if the RSD
is greater than 20 percent.

11.0 What calculations must I perform for comparison with a
validated method if I am using quadruplicate replicate sampling
systems?

    If you are comparing a candidate test method to a validated
method, then you must analyze the data according to the provisions
in this section. If the data from the candidate test method fail
either the bias or precision test, the data and the candidate test
method are unacceptable. If the Administrator determines that the
affected source has highly variable emission rates, the
Administrator may require additional precision checks.
    11.1 Bias Analysis. Test the bias for statistical significance
at the 95 percent confidence level by calculating the t-statistic.
    11.1.1 Bias. Determine the bias, which is defined as the mean of
the differences between the candidate test method and the validated
method (dm). Calculate di according to
Equation 301-10 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.009

Where:

di = Difference in measured value between the candidate
test method and the validated method for each quadruplicate sampling
train.
V1i = First measured value with the validated method in
the i\th\ quadruplicate sampling train.
V2i = Second measured value with the validated method in
the i\th\ quadruplicate sampling train.
P1i = First measured value with the candidate test method
in the i\th\ quadruplicate sampling train.
P2i = Second measured value with the candidate test
method in the i\th\ quadruplicate sampling train.

    Calculate the numerical value of the bias using Equation 301-11
of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.010

Where:

B = Numerical bias.
di = Difference between the candidate test method and the
validated method for the i\th\ quadruplicate sampling train.
n = Number of quadruplicate sampling trains.

    11.1.2 Standard Deviation of the Differences. Calculate the
standard deviation of the differences, SDd, using
Equation 301-12 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.011

Where:

SDd = Standard deviation of the differences between the
candidate test method and the validated method.
di = Difference in measured value between the candidate
test method and the validated method for each quadruplicate sampling
train.
dm = Mean of the differences, di, between the
candidate test method and the validated method.
n = Number of quadruplicate sampling trains.

    11.1.3 T Test. Calculate the t-statistic using Equation 301-13
of this method.

[GRAPHIC] [TIFF OMITTED] TP02DE16.012

Where:

t = Calculated t-statistic.
dm = The mean of the differences, di, between
the candidate test method and the validated method.
SDd = Standard deviation of the differences between the
candidate test method and the validated method.
n = Number of quadruplicate sampling trains.

    For the procedure comparing a candidate test method to a
validated test method listed in Table 301-1 of this method, n equals
six. Compare the calculated t-statistic with the critical value of
the t-statistic, and determine if the bias is significant at the 95
percent confidence level (see Table 301-3 of this method). When six
runs are conducted, as specified in Table 301-1 of this method, the
critical value of the t-statistic is 2.571 for five degrees of
freedom. If the calculated t-value is less than or equal to the
critical value, the bias is not statistically significant and the
data are acceptable. If the calculated t-value is greater than the
critical value, the bias is statistically significant, and you must
evaluate the magnitude of the relative bias using Equation 301-14 of
this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.013

Where:

BR = Relative bias.
B = Bias as calculated in Equation 301-11 of this method.
VS = Mean of measured values from the validated method.

    If the relative bias is less than or equal to 10 percent, the
bias of the candidate test method is acceptable. On a source-
specific basis, if the relative bias is greater than 10 percent but
less than or equal to 30 percent, and if you correct all data
collected in the future with the candidate test method for the bias
using the correction factor, CF, determined in Equation 301-8 of
this method (using VS for CS), the bias of the candidate test method
is acceptable for application to the source at which the validation
testing was conducted. If either of the preceding two cases applies,
you may continue to evaluate the candidate test method by
calculating its precision. If not, the candidate test method does
not meet the requirements of Method 301.
    11.2 Precision. Compare the estimated variance (or standard
deviation) of the candidate test method to that of the validated
test method according to Sections 11.2.1 and 11.2.2 of this method.
If a significant difference is determined using the F test, the
candidate test method and the results are rejected. If the F test
does not show a significant difference, then the candidate test
method has acceptable precision.
    11.2.1 Candidate Test Method Variance. Calculate the estimated
variance of the candidate test method according to Equation 301-15
of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.014

Where:

Sp\2\ = Estimated variance of the candidate test method.
di = The difference between the i\th\ pair of samples
collected with the candidate test method in a single quadruplicate
train.
n = Total number of paired samples (quadruplicate trains).

    Calculate the estimated variance of the validated test method
according to Equation 301-16 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.015

Where:

Sv\2\ = Estimated variance of the validated test method.
di = The difference between the i\th\ pair of samples
collected with the validated test method in a single quadruplicate
train.
n = Total number of paired samples (quadruplicate trains).

    11.2.2 The F test. Determine if the estimated variance of the
candidate test method is greater than that of the validated method
by calculating the F-value using Equation 301-17 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.016

Where:

F = Calculated F value.
Sp\2\ = The estimated variance of the candidate test method.
Sv\2\ = The estimated variance of the validated method.

    Compare the calculated F value with the one-sided confidence
level for F from Table 301-4 of this method. The upper one-sided
confidence level of 95 percent for F(6,6) is 4.28 when
the procedure specified in Table 301-1 of this method for
quadruplicate

sampling trains is followed. If the calculated F value is greater
than the critical F value, the difference in precision is
significant, and the data and the candidate test method are
unacceptable.

12.0 What calculations must I perform for analyte spiking?

    You must analyze the data for analyte spike testing according to
this section.
    12.1 Bias Analysis. Test the bias for statistical significance
at the 95 percent confidence level by calculating the t-statistic.
    12.1.1 Bias. Determine the bias, which is defined as the mean of
the differences between the spiked samples and the unspiked samples
in each quadruplicate sampling train minus the spiked amount, using
Equation 301-18 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.017

Where:

di = Difference between the spiked samples and unspiked
samples in each quadruplicate sampling train minus the spiked
amount.
S1i = Measured value of the first spiked sample in the
ith quadruplicate sampling train.
S2i = Measured value of the second spiked sample in the
ith quadruplicate sampling train.
M1i = Measured value of the first unspiked sample in the
ith quadruplicate sampling train.
M2i = Measured value of the second unspiked sample in the
ith quadruplicate sampling train.
CS = Calculated value of the spike level.

    Calculate the numerical value of the bias using Equation 301-19
of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.018

Where:

B = Numerical value of the bias.
di = Difference between the spiked samples and unspiked
samples in each quadruplicate sampling train minus the spiked
amount.
n = Number of quadruplicate sampling trains.

    12.1.2 Standard Deviation of the Differences. Calculate the
standard deviation of the differences using Equation 301-20 of this
method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.019

Where:

SDd = Standard deviation of the differences of paired
samples.
di = Difference between the spiked samples and unspiked
samples in each quadruplicate sampling train minus the spiked
amount.
dm = The mean of the differences, di, between
the spiked samples and unspiked samples.
n = Total number of quadruplicate sampling trains.

    12.1.3 T Test. Calculate the t-statistic using Equation 301-21
of this method, where n is the total number of test sample
differences (di). For the quadruplicate sampling system
procedure in Table 301-1 of this method, n equals six.
[GRAPHIC] [TIFF OMITTED] TP02DE16.020

Where:

t = Calculated t-statistic.
dm = Mean of the difference, di, between the spiked
samples and unspiked samples.
SDd = Standard deviation of the differences of paired
samples.
n = Number of quadruplicate sampling trains.

    Compare the calculated t-statistic with the critical value of
the t-statistic, and determine if the bias is significant at the 95
percent confidence level. When six quadruplicate runs are conducted,
as specified in Table 301-1 of this method, the 2-sided confidence
level critical value is 2.571 for the five degrees of freedom. If
the calculated t-value is less than the critical value, the bias is
not statistically significant and the data are acceptable. If the
calculated t-value is greater than the critical value, the bias is
statistically significant and you must evaluate the magnitude of the
relative bias using Equation 301-22 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.021

Where:

BR = Relative bias.
B = Bias at the spike level from Equation 301-19 of this method.
CS = Calculated value at the spike level.

    If the relative bias is less than or equal to 10 percent, the
bias of the candidate test method is acceptable. On a source-
specific basis, if the relative bias is greater than 10 percent but
less than or equal to 30 percent, and if you correct all data
collected with the candidate test method in the future for the
magnitude of the bias using Equation 301-8, the bias of the
candidate test method is acceptable for application to the tested
source at which the validation testing was conducted. Proceed to
evaluate precision of the candidate test method.
    12.2 Precision. Calculate the standard deviation using Equation
301-23 of this method.
[GRAPHIC] [TIFF OMITTED] TP02DE16.022

Where:

SD = Standard deviation of the candidate test method.
Si = Measured value of the analyte in the ith spiked
sample.
Sm = Mean of the measured values of the analyte in all
the spiked samples.
n = Number of spiked samples.

    Calculate the RSD of the candidate test method using Equation
301-9 of this method, where SD and Sm are the values from
Equation 301-23 of this method. The data and candidate test method
are unacceptable if the RSD is greater than 20 percent.

13.0 How do I conduct tests at similar sources?

    If the Administrator has approved the use of an alternative test
method to a test method required in 40 CFR part 59, 60, 61, 63, or
65 for an affected source, and you would like to apply the
alternative test method to a similar source, then you must petition
the Administrator as described in Section 17.1.1 of this method.

Optional Requirements

14.0 How do I use and conduct ruggedness testing?

    Ruggedness testing is an optional requirement for validation of
a candidate test method that is intended for the source where the
validation testing was conducted. Ruggedness testing is required for
validation of a candidate test method intended to be used at
multiple sources. If you want to use a validated test method at a
concentration that is different from the concentration in the
applicable emission limitation under 40 CFR part 59, 60, 61, 63, or
65, or for a source category that is different from the source
category that the test method specifies, then you must conduct
ruggedness testing according to the procedures in Reference 18.16 of
Section 18.0 of this method and submit a request for a waiver for
conducting Method 301 at that different source category according to
Section 17.1.1 of this method.
    Ruggedness testing is a study that can be conducted in the
laboratory or the field to determine the sensitivity of a method to
parameters such as analyte concentration, sample collection rate,
interferent concentration, collection medium temperature, and sample
recovery temperature. You conduct ruggedness testing by changing
several variables simultaneously instead of changing one variable at
a time. For example, you can determine the effect of seven variables
in only eight experiments. (W.J. Youden, Statistical Manual of the
Association of Official Analytical Chemists, Association of Official
Analytical Chemists, Washington, DC, 1975, pp. 33-36).

15.0 How do I determine the Limit of Detection for the candidate
test method?

    Determination of the Limit of Detection (LOD) as specified in
Sections 15.1 and 15.2 of this method is required for source-
specific method validation and validation of a candidate test method
intended to be used for multiple sources.

15.1 Limit of Detection. The LOD is the minimum concentration of a
substance that can be measured and reported with 99 percent confidence
that the analyte concentration is greater than zero. For this protocol,
the LOD is defined as three times the standard deviation,
So, at the blank level.

    15.2 Purpose. The LOD establishes the lower detection limit of
the candidate test method. You must calculate the LOD using the
applicable procedures found in Table 301-5 of this method. For
candidate test methods that collect the analyte in a sample matrix
prior to an analytical measurement, you must determine the LOD using
Procedure I in Table 301-5 of this method by calculating a method
detection limit (MDL) as described in proposed 40 CFR part 136,
appendix B. For the purposes of this section, the LOD is equivalent
to the calculated MDL. For radiochemical methods, use the Multi-
Agency Radiological Laboratory Analytical Protocols (MARLAP) Manual
(i.e., use the minimum detectable concentration (MDC) and not the
LOD) available at http://www2.epa.gov/radiation/marlap-manual-and-supporting-documents.

Other Requirements and Information

16.0 How do I apply for approval to use a candidate test method?

    16.1 Submitting Requests. You must request to use a candidate
test method according to the procedures in Sec.  63.7(f) or similar
sections of 40 CFR parts 59, 60, 61, and 65 (Sec.  59.104, Sec.
59.406, Sec.  60.8(b), Sec.  61.13(h)(ii), or Sec.
65.158(a)(2)(iii)). You cannot use a candidate test method to meet
any requirement under these parts until the Administrator has
approved your request. The request must include a field validation
report containing the information in Section 16.2 of this method.
You must submit the request to the Group Leader, Measurement
Technology Group, U.S. Environmental Protection Agency, E143-02,
Research Triangle Park, NC 27711.
    16.2 Field Validation Report. The field validation report must
contain the information in Sections 16.2.1 through 16.2.8 of this
method.
    16.2.1 Regulatory Objectives for the Testing, Including a
Description of the Reasons for the Test, Applicable Emission Limits,
and a Description of the Source.
    16.2.2 Summary of the Results and Calculations Shown in Sections
6.0 Through 16.0 of This Method, as Applicable.
    16.2.3 Reference Material Certification and Value(s).
    16.2.4 Discussion of Laboratory Evaluations.
    16.2.5 Discussion of Field Sampling.
    16.2.6 Discussion of Sample Preparation and Analysis.
    16.2.7 Storage Times of Samples (and Extracts, if Applicable).
    16.2.8 Reasons for Eliminating Any Results.

17.0 How do I request a waiver?

    17.1 Conditions for Waivers. If you meet one of the criteria in
Section 17.1.1 or 17.1.2 of this method, the Administrator may waive
the requirement to use the procedures in this method to validate an
alternative or other candidate test method. In addition, if the EPA
currently recognizes an appropriate test method or considers the
candidate test method to be satisfactory for a particular source,
the Administrator may waive the use of this protocol or may specify
a less rigorous validation procedure.
    17.1.1 Similar Sources. If the alternative or other candidate
test method that you want to use was validated for source-specific
application at another source and you can demonstrate to the
Administrator's satisfaction that your affected source is similar to
that validated source, then the Administrator may waive the
requirement for you to validate the alternative or other candidate
test method. One procedure you may use to demonstrate the
applicability of the method to your affected source is to conduct a
ruggedness test as described in Section 14.0 of this method.
    17.1.2 Documented Methods. If the bias and precision of the
alternative or other candidate test method that you are proposing
have been demonstrated through laboratory tests or protocols
different from this method, and you can demonstrate to the
Administrator's satisfaction that the bias and

precision apply to your application, then the Administrator may
waive the requirement to use this method or to use part of this
method.
    17.2 Submitting Applications for Waivers. You must sign and
submit each request for a waiver from the requirements in this
method in writing. The request must be submitted to the Group
Leader, Measurement Technology Group, U.S. Environmental Protection
Agency, E143-02, Research Triangle Park, NC 27711.
    17.3 Information Application for Waiver. The request for a
waiver must contain a thorough description of the candidate test
method, the intended application, and results of any validation or
other supporting documents. The request for a waiver must contain,
at a minimum, the information in Sections 17.3.1 through 17.3.4 of
this method. The Administrator may request additional information if
necessary to determine whether this method can be waived for a
particular application.
    17.3.1 A Clearly Written Test Method. The candidate test method
should be written preferably in the format of 40 CFR part 60,
appendix A, Test Methods. Additionally, the candidate test must
include an applicability statement, concentration range, precision,
bias (accuracy), and minimum and maximum storage durations in which
samples must be analyzed.
    17.3.2 Summaries of Previous Validation Tests or Other
Supporting Documents. If you use a different procedure from that
described in this method, you must submit documents substantiating
the bias and precision values to the Administrator's satisfaction.
    17.3.3 Ruggedness Testing Results. You must submit results of
ruggedness testing conducted according to Section 14.0 of this
method, sample stability conducted according to Section 7.0 of this
method, and detection limits conducted according to Section 15.0 of
this method, as applicable. For example, you would not need to
submit ruggedness testing results if you will be using the method at
the same affected source and level at which it was validated.
    17.3.4 Applicability Statement and Basis for Waiver Approval.
Discussion of the applicability statement and basis for approval of
the waiver. This discussion should address as applicable the
following: Applicable regulation, emission standards, effluent
characteristics, and process operations.

18.0 Where can I find additional information?

    You can find additional information in the references in
Sections 18.1 through 18.17 of this method.
    18.1 Albritton, J.R., G.B. Howe, S.B. Tompkins, R.K.M. Jayanty,
and C.E. Decker. 1989. Stability of Parts-Per-Million Organic
Cylinder Gases and Results of Source Test Analysis Audits, Status
Report No. 11. Environmental Protection Agency Contract 68-02-4125.
Research Triangle Institute, Research Triangle Park, NC. September.
    18.2 ASTM Standard E 1169-89 (current version), ``Standard Guide
for Conducting Ruggedness Tests,'' available from ASTM, 100 Barr
Harbor Drive, West Conshohoken, PA 19428.
    18.3 DeWees, W.G., P.M. Grohse, K.K. Luk, and F.E. Butler. 1989.
Laboratory and Field Evaluation of a Methodology for Speciating
Nickel Emissions from Stationary Sources. EPA Contract 68-02-4442.
Prepared for Atmospheric Research and Environmental Assessment
Laboratory, Office of Research and Development, U.S. Environmental
Protection Agency, Research Triangle Park, NC 27711. January.
    18.4 International Conference on Harmonization of Technical
Requirements for the Registration of Pharmaceuticals for Human Use,
ICH-Q2A, ``Text on Validation of Analytical Procedures,'' 60 FR
11260 (March 1995).
    18.5 International Conference on Harmonization of Technical
Requirements for the Registration of Pharmaceuticals for Human Use,
ICH-Q2b, ``Validation of Analytical Procedures: Methodology,'' 62 FR
27464 (May 1997).
    18.6 Keith, L.H., W. Crummer, J. Deegan Jr., R.A. Libby, J.K.
Taylor, and G. Wentler. 1983. Principles of Environmental Analysis.
American Chemical Society, Washington, DC.
    18.7 Maxwell, E.A. 1974. Estimating variances from one or two
measurements on each sample. Amer. Statistician 28:96-97.
    18.8 Midgett, M.R. 1977. How EPA Validates NSPS Methodology.
Environ. Sci. & Technol. 11(7):655-659.
    18.9 Mitchell, W.J., and M.R. Midgett. 1976. Means to evaluate
performance of stationary source test methods. Environ. Sci. &
Technol. 10:85-88.
    18.10 Plackett, R.L., and J.P. Burman. 1946. The design of
optimum multifactorial experiments. Biometrika, 33:305.
    18.11 Taylor, J.K. 1987. Quality Assurance of Chemical
Measurements. Lewis Publishers, Inc., pp. 79-81.
    18.12 U.S. Environmental Protection Agency. 1978. Quality
Assurance Handbook for Air Pollution Measurement Systems: Volume
III. Stationary Source Specific Methods. Publication No. EPA-600/4-
77-027b. Office of Research and Development Publications, 26 West
St. Clair St., Cincinnati, OH 45268.
    18.13 U.S. Environmental Protection Agency. 1981. A Procedure
for Establishing Traceability of Gas Mixtures to Certain National
Bureau of Standards Standard Reference Materials. Publication No.
EPA-600/7-81-010. Available from the U.S. EPA, Quality Assurance
Division (MD-77), Research Triangle Park, NC 27711.
    18.14 U.S. Environmental Protection Agency. 1991. Protocol for
The Field Validation of Emission Concentrations from Stationary
Sources. Publication No. 450/4-90-015. Available from the U.S. EPA,
Emission Measurement Technical Information Center, Technical Support
Division (MD-14), Research Triangle Park, NC 27711.
    18.15 Wernimont, G.T., ``Use of Statistics to Develop and
Evaluate Analytical Methods,'' AOAC, 1111 North 19th Street, Suite
210, Arlington, VA 22209. USA, 78-82 (1987).
    18.16 Youden, W.J. Statistical techniques for collaborative
tests. In: Statistical Manual of the Association of Official
Analytical Chemists, Association of Official Analytical Chemists,
Washington, DC, 1975, pp. 33-36.
    18.17 NIST/SEMATECH (current version), ``e-Handbook of
Statistical Methods,'' available from NIST, http://www.itl.nist.gov/div898/handbook/.

                    Table 301-1--Sampling Procedures
------------------------------------------------------------------------
            If you are . . .                  You must collect . . .
------------------------------------------------------------------------
Comparing the candidate test method      A total of 24 samples using a
 against a validated method.              quadruplicate sampling system
                                          (a total of six sets of
                                          replicate samples). In each
                                          quadruplicate sample set, you
                                          must use the validated test
                                          method to collect and analyze
                                          half of the samples.
Using isotopic spiking (can only be      A total of 12 samples, all of
 used with methods capable of             which are spiked with
 measurement of multiple isotopes         isotopically-labeled analyte.
 simultaneously).                         You may collect the samples
                                          either by obtaining six sets
                                          of paired samples or three
                                          sets of quadruplicate samples.
Using analyte spiking..................  A total of 24 samples using the
                                          quadruplicate sampling system
                                          (a total of six sets of
                                          replicate samples--two spiked
                                          and two unspiked).
------------------------------------------------------------------------

  Table 301-2--Storage and Sampling Procedures for Stack Test Emissions
------------------------------------------------------------------------
       If you are . . .             With . . .      Then you must . . .
------------------------------------------------------------------------
Using isotopic or analyte       Sample container   Analyze six of the
 spiking procedures.             (bag or            samples within 7
                                 canister) or       days and then
                                 impinger           analyze the same six
                                 sampling systems   samples at the
                                 that are not       proposed maximum
                                 subject to         storage duration or
                                 dilution or        2 weeks after the
                                 other              initial analysis.
                                 preparation
                                 steps.
                                Sorbent and        Extract or digest six
                                 impinger           of the samples
                                 sampling systems   within 7 days and
                                 that require       extract or digest
                                 extraction or      six other samples at
                                 digestion.         the proposed maximum
                                                    storage duration or
                                                    2 weeks after the
                                                    first extraction or
                                                    digestion. Analyze
                                                    an aliquot of the
                                                    first six extracts
                                                    (digestates) within
                                                    7 days and proposed
                                                    maximum storage
                                                    duration or 2 weeks
                                                    after the initial
                                                    analysis. This will
                                                    allow analysis of
                                                    extract storage
                                                    impacts.
                                Sorbent sampling   Analyze six samples
                                 systems that       within 7 days.
                                 require thermal    Analyze another set
                                 desorption.        of six samples at
                                                    the proposed maximum
                                                    storage time or
                                                    within 2 weeks of
                                                    the initial
                                                    analysis.
Comparing a candidate test      Sample container   Analyze at least six
 method against a validated      (bag or            of the candidate
 test method.                    canister) or       test method samples
                                 impinger           within 7 days and
                                 sampling systems   then analyze the
                                 that are not       same six samples at
                                 subject to         the proposed maximum
                                 dilution or        storage duration or
                                 other              within 2 weeks of
                                 preparation        the initial
                                 steps.             analysis.
                                Sorbent and        Extract or digest six
                                 impinger           of the candidate
                                 sampling systems   test method samples
                                 that require       within 7 days and
                                 extraction or      extract or digest
                                 digestion.         six other samples at
                                                    the proposed maximum
                                                    storage duration or
                                                    within 2 weeks of
                                                    the first extraction
                                                    or digestion.
                                                    Analyze an aliquot
                                                    of the first six
                                                    extracts
                                                    (digestates) within
                                                    7 days and an
                                                    aliquot at the
                                                    proposed maximum
                                                    storage durations or
                                                    within 2 weeks of
                                                    the initial
                                                    analysis. This will
                                                    allow analysis of
                                                    extract storage
                                                    impacts.
                                Sorbent systems    Analyze six samples
                                 that require       within 7 days.
                                 thermal            Analyze another set
                                 desorption.        of six samples at
                                                    the proposed maximum
                                                    storage duration or
                                                    within 2 weeks of
                                                    the initial
                                                    analysis.
------------------------------------------------------------------------

     Table 301-3--Critical Values of t for the Two-Tailed 95 Percent
                            Confidence Limit
------------------------------------------------------------------------
                   Degrees of freedom                           t95
------------------------------------------------------------------------
1.......................................................          12.706
2.......................................................           4.303
3.......................................................           3.182
4.......................................................           2.777
5.......................................................           2.571
6.......................................................           2.447
7.......................................................           2.365
8.......................................................           2.306
9.......................................................           2.262
10......................................................           2.228
11......................................................           2.201
------------------------------------------------------------------------

   Table 301-4--Upper Critical Values of the F Distribution for the 95
                        Percent Confidence Limit
------------------------------------------------------------------------
 Numerator (k1) and  denominator (k2) degrees of
                     freedom                      F{F>F.05(k1,k2){time}
------------------------------------------------------------------------
1,1.............................................                 161.4
2,2.............................................                  19.0
3,3.............................................                   9.3
4,4.............................................                  6.39
5,5.............................................                  5.05
6,6.............................................                  4.28
7,7.............................................                  3.79
8,8.............................................                  3.44
9,9.............................................                  3.18
10,10...........................................                  2.98
------------------------------------------------------------------------

                Table 301-5--Procedures for Estimating So
------------------------------------------------------------------------

------------------------------------------------------------------------
If the estimated LOD (LOD1, expected    If the estimated LOD (LOD1,
 approximate LOD concentration level)    expected approximate LOD
 is no more than twice the calculated    concentration level) is greater
 LOD or an analyte in a sample matrix    than twice the calculated LOD,
 was collected prior to an analytical    use Procedure II as follows
 measurement, use Procedure I as
 follows..
Procedure I                             Procedure II
Determine the LOD by calculating a      Prepare two additional standards
 method detection limit (MDL) as         (LOD2 and LOD3) at
 described in proposed 40 CFR part       concentration levels lower than
 136, appendix B.                        the standard used in Procedure
                                         I (LOD1).
                                        Sample and analyze each of these
                                         standards (LOD2 and LOD3) at
                                         least seven times.
                                        Calculate the standard deviation
                                         (S2 and S3) for each
                                         concentration level.
                                        Plot the standard deviations of
                                         the three test standards (S1,
                                         S2 and S3) as a function of
                                         concentration.
                                        Draw a best-fit straight line
                                         through the data points and
                                         extrapolate to zero
                                         concentration. The standard
                                         deviation at zero concentration
                                         is So.
                                        Calculate the LOD0 (referred to
                                         as the calculated LOD) as 3
                                         times So.
------------------------------------------------------------------------

[FR Doc. 2016-27544 Filed 12-1-16; 8:45 am]
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