[Federal Register Volume 87, Number 136 (Monday, July 18, 2022)]
[Rules and Regulations]
[Pages 42647-42649]
[FR Doc No: 2022-15232]

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DEPARTMENT OF HOMELAND SECURITY

Coast Guard

33 CFR Part 117

[Docket No. USCG-2019-0910]
RIN 1625-AA09

Drawbridge Operation Regulation; Bayou Sara, Saraland, AL

AGENCY: Coast Guard, DHS.

ACTION: Final rule.

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SUMMARY: The Coast Guard is changing how the CSX Transportation
Railroad swing bridge across Bayou Sara, mile 0.1 near Saraland,
Alabama will be operated. The bridge will continue to open according to
the drawbridge regulations but the bridge tender will operate this
bridge from a remote location at the CSX railroad terminal in Mobile,
Alabama.

DATES: This rule is effective August 17, 2022.

ADDRESSES: To view documents mentioned in this preamble as being
available in the docket, go to https://www.regulations.gov. Type the
docket number USCG-2019-0910 in the ``SEARCH'' box and click
``SEARCH''. In the Document Type column, select ``Supporting & Related
Material.''

FOR FURTHER INFORMATION CONTACT: If you have questions on this rule,
call or email Doug Blakemore, Eighth Coast Guard Bridge Administrator
at<PHONE_NUMBER> or email [email protected].

SUPPLEMENTARY INFORMATION:

I. Table of Abbreviations

CFR Code of Federal Regulations
DHS Department of Homeland Security
FR Federal Register
OMB Office of Management and Budget
NPRM Notice of Proposed Rulemaking (Advance, Supplemental)
Sec.  Section
U.S.C. United States Code

II. Background Information and Regulatory History

    On January 22, 2020, the Coast Guard published a Test Deviation,
with a request for comments, entitled ``Drawbridge Operation
Regulation; Bayou Sara, Saraland, AL'' in the Federal Register (85 FR
3853), to seek your comments on whether the Coast Guard should consider
modifying the current operating schedule to test this operating
schedule for the CSX Railroad Bridge. Two comments were received during
the test period and those comments were addressed in the NPRM.
    On March 30, 2021, the Coast Guard published a Notice of Proposed
Rulemaking entitled ``Drawbridge Operation Regulation; Bayou Sara,
Saraland, AL'' in the Federal Register (86 FR 16680). There we stated
why we issued the NPRM, and invited comments on our proposed regulatory
action related to this regulatory change. No additional comments were
received during the NPRM comment period.

III. Legal Authority and Need for Rule

    The Coast Guard is issuing this rule under authority 33 U.S.C. 499.
    The CSX Railroad Company, the owner of the bridge requested to
change operation of the bridge from a tended drawbridge to a remotely
operated drawbridge. The CSX Transportation Railroad drawbridge has a
vertical clearance of 5' in the closed to navigation position and
operates in accordance with 33 CFR 117.105. This rule will not change
the operation schedule of the bridge. This bridge will be operated from
the CSX railroad yard located in Mobile, AL.
    The waterway users include recreational vessels and commercial
tows; which combined requires approximately six openings a day.

IV. Discussion of Comments, Changes and the Final Rule

    As mentioned above in Section II, two comments were received during
the test period Federal Register (85 FR 3853), and those comments were
addressed in the NPRM Federal Register (86 FR 16680). 33 CFR 117.42
sets Coast Guard drawbridge regulations to operate a bridge from a
remote location. This rule does not change the operating schedule nor
does it change the request to open the bridge. Mariners requiring an
opening may do so by contacting the CSX remote control center on
Channels 13/16 or by the phone number posted at the bridge. We note
that in the NPRM some language was removed from the regulatory text
found in 33 CFR 117.105. Specifically, language about notice for

openings between 6 p.m. and 10 a.m. and openings for severe storms or
hurricanes. We have reinserted that language here so that it will
remain in effect upon publication of this rule.
    This rule continues to allow opening on signal, except eight hours'
notice is required for openings between 6 p.m. and 10 a.m. The rule
also allows CSX to control the drawbridge from their remote control
center located in Mobile, AL and requires CSX to have the capability,
including resources and manpower to return the operator to the bridge
location within 3 hours following any of the below situations:
     Any component of the remote operations system fails and
prevents the remote operator from being able to visually identify
vessels, communicate with vessels, detect vessels immediately
underneath the bridge or visually identify trains approaching the
bridge.
     CSX fails to meet Federal Railway Administration (FRA) or
any other government agency safety requirements.
     At the direction of the District Commander.

V. Regulatory Analyses

    We developed this rule after considering numerous statutes and
Executive Orders related to rulemaking. Below we summarize our analyses
based on a number of these statutes and Executive Orders.

A. Regulatory Planning and Review

    Executive Orders 12866 and 13563 direct agencies to assess the
costs and benefits of available regulatory alternatives and, if
regulation is necessary, to select regulatory approaches that maximize
net benefits. This rule has not been designated a ``significant
regulatory action,'' under Executive Order 12866. Accordingly, it has
not been reviewed by the Office of Management and Budget (OMB).
    This regulatory action determination is based on the ability that
vessels can still transit the bridge given advanced notice.

B. Impact on Small Entities

    The Regulatory Flexibility Act of 1980 (RFA), 5 U.S.C. 601-612, as
amended, requires federal agencies to consider the potential impact of
regulations on small entities during rulemaking. The term ``small
entities'' comprises small businesses, not-for-profit organizations
that are independently owned and operated and are not dominant in their
fields, and governmental jurisdictions with populations of less than
50,000. The Coast Guard received 0 comments from the Small Business
Administration on this rule. The Coast Guard certifies under 5 U.S.C.
605(b) that this rule will not have a significant economic impact on a
substantial number of small entities.
    While some owners or operators of vessels intending to transit the
bridge may be small entities, for the reasons stated in section V. A
above, this rule will not have a significant economic impact on any
vessel owner or operator.
    Under section 213(a) of the Small Business Regulatory Enforcement
Fairness Act of 1996 (Pub. L. 104-121), we want to assist small
entities in understanding this rule. If the rule would affect your
small business, organization, or governmental jurisdiction and you have
questions concerning its provisions or options for compliance, please
contact the person listed in the FOR FURTHER INFORMATION CONTACT
section.
    Small businesses may send comments on the actions of Federal
employees who enforce, or otherwise determine compliance with, Federal
regulations to the Small Business and Agriculture Regulatory
Enforcement Ombudsman and the Regional Small Business Regulatory
Fairness Boards. The Ombudsman evaluates these actions annually and
rates each agency's responsiveness to small business. If you wish to
comment on actions by employees of the Coast Guard, call 1-888-REG-FAIR
(1-888-734-3247). The Coast Guard will not retaliate against small
entities that question or complain about this rule or any policy or
action of the Coast Guard.

C. Collection of Information

    This rule calls for no new collection of information under the
Paperwork Reduction Act of 1995 (44 U.S.C. 3501-3520).

D. Federalism and Indian Tribal Government

    A rule has implications for federalism under Executive Order 13132,
Federalism, if it has a substantial direct effect 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. We have analyzed this rule under that Order and have
determined that it is consistent with the fundamental federalism
principles and preemption requirements described in Executive Order
13132.
    Also, this rule does not have tribal implications under Executive
Order 13175, Consultation and Coordination with Indian Tribal
Governments, because it does not have a substantial direct effect on
one or more Indian tribes, on the relationship between the Federal
Government and Indian tribes, or on the distribution of power and
responsibilities between the Federal Government and Indian tribes.

E. Unfunded Mandates Reform Act

    The Unfunded Mandates Reform Act of 1995 (2 U.S.C. 1531-1538)
requires Federal agencies to assess the effects of their discretionary
regulatory actions. In particular, the Act addresses actions that may
result in the expenditure by a State, local, or tribal government, in
the aggregate, or by the private sector of $100,000,000 (adjusted for
inflation) or more in any one year. Though this rule will not result in
such an expenditure, we do discuss the effects of this rule elsewhere
in this preamble.

F. Environment

    We have analyzed this rule under Department of Homeland Security
Management Directive 023-01, Rev.1, associated implementing
instructions, and Environmental Planning Policy COMDTINST 5090.1
(series) which guide the Coast Guard in complying with the National
Environmental Policy Act of 1969 (NEPA)(42 U.S.C. 4321-4370f). The
Coast Guard has determined that this action is one of a category of
actions that do not individually or cumulatively have a significant
effect on the human environment. This rule promulgates the operating
regulations or procedures for drawbridges and is categorically excluded
from further review, under paragraph L49, of Chapter 3, Table 3-1 of
the U.S. Coast Guard Environmental Planning Implementation Procedures.
    Neither a Record of Environmental Consideration nor a Memorandum
for the Record are required for this rule.

List of Subjects in 33 CFR Part 117

    Bridges.

    For the reasons discussed in the preamble, the Coast Guard amends
33 CFR part 117 as follows:

PART 117--DRAWBRIDGE OPERATION REGULATIONS

0
1. The authority citation for part 117 continues to read as follows:

    Authority:  33 U.S.C. 499; 33 CFR 1.05-1; and Department of
Homeland Security Delegation No. 0170.1.

0
2. Revise Sec.  117.105 to read as follows:

Sec.  117.105   Bayou Sara.

    (a) The draw of the CSX Transportation Railroad bridge, mile 0.1
near Saraland, shall open on signal; except that, from 6 p.m. to 10
a.m. the draw shall open on signal if at least eight hours' notice is
given. During

periods of severe storms or hurricanes, from the time the National
Weather Service sounds an ``alert'' for the area until the ``all
clear'' is sounded, the draw shall open on signal.
    (b) The draw of the CSX Transportation Railroad bridge, mile 0.1
near Saraland, AL shall be remotely operated by the bridge tender at
CSX's bridge remote control center in Mobile, Alabama. Vessels can
contact the CSX bridge tender via VHF-FM channel 13 or by telephone at
the number displayed on the signs posted at the bridge to request an
opening of the draw.
    (c) CSX will return the tender to the bridge location within 3
hours following any of the below situations:
    (1) Any component of the remote operations system fails and
prevents the remote operator from being able to visually identify
vessels, communicate with vessels, detect vessels immediately
underneath the bridge or visually identify trains approaching the
bridge;
    (2) CSX fails to meet Federal Railway Administration (FRA) or any
other government agency safety requirements;
    (3) Anytime at the direction of the District Commander.

    Dated: June 28, 2022.
R.V. Timme,
Rear Admiral, U.S. Coast Guard, Commander, Eighth Coast Guard District.
[FR Doc. 2022-15232 Filed 7-15-22; 8:45 am]
BILLING CODE 9110-04-P


Comment Info: =================

General Comment:Supplemental Material Document Title:  CATEX (Categorical Exclusion Determination) and EAC (Environmental Analysis Checklist) 3 Pages


[Federal Register Volume 81, Number 129 (Wednesday, July 6, 2016)]
[Notices]
[Page 44088]
[FR Doc No: 2016-15948]

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DEPARTMENT OF TRANSPORTATION

Office of the Secretary

Application of Public Charters, Inc. for Commuter Authority

AGENCY: Department of Transportation.

ACTION: Notice of Order to Show Cause (Order 2016-6-14), Docket DOT-
OST-2015-0234.

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SUMMARY: The Department of Transportation is directing all interested
persons to show cause why it should not issue an order tentatively
finding Public Charters, Inc., fit, willing, and able to provide
scheduled passenger service as a commuter air carrier using small
aircraft pursuant to Part 135 of the Federal Aviation Regulations.

DATES: Persons wishing to file objections should do so no later than
July 11, 2016.

ADDRESSES: Objections and answers to objections should be filed in
Docket DOT-OST-2015-0234 and addressed to U.S. Department of
Transportation, Docket Operations, (M-30, Room W12-140), 1200 New
Jersey Avenue SE., West Building Ground Floor, Washington, DC 20590,
and should be served upon the parties listed in Attachment A to the
order.

FOR FURTHER INFORMATION CONTACT: Catherine J. O'Toole, Air Carrier
Fitness Division (X-56, Room W86-489), U.S. Department of
Transportation, 1200 New Jersey Avenue SE., Washington, DC 20590, (202)
366-9721.

    Dated: June 27, 2016.
Jenny T. Rosenberg,
Acting Assistant Secretary for Aviation and International Affairs.
[FR Doc. 2016-15948 Filed 7-5-16; 8:45 am]
 BILLING CODE 4910-9X-P


[Federal Register Volume 84, Number 123 (Wednesday, June 26, 2019)]
[Notices]
[Page 30102]
[FR Doc No: 2019-13580]

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DEPARTMENT OF ENERGY

Federal Energy Regulatory Commission

[Docket No. ER19-2190-000]

Cubico Palmetto Lessee, LLC.; Supplemental Notice That Initial
Market-Based Rate Filing Includes Request for Blanket Section 204
Authorization

    This is a supplemental notice in the above-referenced proceeding of
Cubico Palmetto Lessee, LLC's application for market-based rate
authority, with an accompanying rate tariff, noting that such
application includes a request for blanket authorization, under 18 CFR
part 34, of future issuances of securities and assumptions of
liability.
    Any person desiring to intervene or to protest should file with the
Federal Energy Regulatory Commission, 888 First Street NE, Washington,
DC 20426, in accordance with Rules 211 and 214 of the Commission's
Rules of Practice and Procedure (18 CFR 385.211 and 385.214). Anyone
filing a motion to intervene or protest must serve a copy of that
document on the Applicant.
    Notice is hereby given that the deadline for filing protests with
regard to the applicant's request for blanket authorization, under 18
CFR part 34, of future issuances of securities and assumptions of
liability, is July 10, 2019.
    The Commission encourages electronic submission of protests and
interventions in lieu of paper, using the FERC Online links at http://www.ferc.gov. To facilitate electronic service, persons with internet
access who will eFile a document and/or be listed as a contact for an
intervenor must create and validate an eRegistration account using the
eRegistration link. Select the eFiling link to log on and submit the
intervention or protests.
    Persons unable to file electronically should submit an original and
5 copies of the intervention or protest to the Federal Energy
Regulatory Commission, 888 First Street NE, Washington, DC 20426.
    The filings in the above-referenced proceeding are accessible in
the Commission's eLibrary system by clicking on the appropriate link in
the above list. They are also available for electronic review in the
Commission's Public Reference Room in Washington, DC. There is an
eSubscription link on the website that enables subscribers to receive
email notification when a document is added to a subscribed docket(s).
For assistance with any FERC Online service, please email
<EMAIL_ADDRESS>or call<PHONE_NUMBER> (toll free). For
TTY, call<PHONE_NUMBER>.

    Dated: June 20, 2019.
Nathaniel J. Davis, Sr.,
Deputy Secretary.
[FR Doc. 2019-13580 Filed 6-25-19; 8:45 am]
 BILLING CODE 6717-01-P


[Federal Register Volume 76, Number 96 (Wednesday, May 18, 2011)]
[Rules and Regulations]
[Pages 28664-28675]
[FR Doc No: 2011-12058]

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 63

[OAR-2004-0080, FRL-9306-8]
RIN 2060-AF00

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

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: This action amends EPA's Method 301, Field Validation of
Pollutant Measurement Methods from Various Waste Media. We revised the
procedures in Method 301 based on our experience in applying the method
and to correct errors that were brought to our attention. The revised
Method 301 is more flexible, less expensive, and easier to use. This
action finalizes amendments to Method 301 after considering comments
received on the proposed rule published in the Federal Register on
December 22, 2004.

DATES: This final rule is effective on May 18, 2011.

ADDRESSES: EPA has established a docket for this action under Docket ID
No. EPA-HQ-OAR-2004-0080. 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., confidential business
information (CBI) or other information whose disclosure is restricted
by statute. Certain other material, such as copyrighted material, is
not placed on the Internet and will be publicly available only in hard
copy form. Publicly available docket materials are available either
electronically at http://www.regulations.gov or in hard copy at the Air
Docket, EPA/DC, EPA West, Room 3334, 1301 Constitution Avenue, NW.,
Washington, DC. The Docket Facility and the Public Reading Room are
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
(202) 566-1744, and the telephone number for the Air Docket is (202)
566-1742.

FOR FURTHER INFORMATION CONTACT: Ms. Lula H. Melton, Office of Air
Quality Planning and Standards, Air Quality Assessment Division,
Measurement Technology Group (E143-02), U.S. Environmental Protection
Agency, Research Triangle Park, North Carolina 27711; telephone number:
(919) 541-2910; fax number:<PHONE_NUMBER>; e-mail address:
<EMAIL_ADDRESS>
SUPPLEMENTARY INFORMATION:

Table of Contents

I. General Information
    A. Does this action apply to me?
    B. Where can I obtain a copy of this action?
    C. Judicial Review
II. Background
III. Summary of the Final Method
IV. Significant Comments Received on the Proposed Amendments to
Method 301
    A. Applicability
    B. Reference Material
    C. Validation Testing Over a Broad Range of Concentrations and
Extended Period of Time
    D. Performance Audit
    E. Sample Stability Procedures
    F. Bias and Precision
    G. Limit of Detection
    H. Critical Values of t for the Two-Tailed 95 Percent Confidence
Limit
    I. Paired Sampling Procedure
    J. Standard Deviation
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
    C. Regulatory Flexibility Act
    D. Unfunded Mandates Reform Act
    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 Concerning Regulations That
Significantly Affect Energy Supply, Distribution or Use
    I. National Technology Transfer and Advancement Act
    J. Executive Order 12898--Federal Actions To Address
Environmental Justice in Minority Populations and Low-Income
Populations
    K. Congressional Review Act

I. General Information

A. Does this action apply to me?

    Method 301 affects/applies to you if you want to propose a new or
alternative test method to meet an EPA compliance requirement.

B. Where can I obtain a copy of this action?

    In addition to being available in the docket, an electronic copy of
this rule will also be available on the Worldwide Web (www) through the
Technology Transfer Network (TTN). Following the Administrator's
signature, a copy of the final rule will be placed on the TTN's policy
and guidance page for newly proposed or promulgated rules at http://www.epa.gov/ttn/oarpg. The TTN provides information and technology
exchange in various areas of air pollution control. A redline strikeout

document that compares this final rule to the proposed rule has also
been added to the docket.

C. Judicial Review

    Under section 307(b)(1) of the Clean Air Act (CAA), judicial review
of this final rule is available by filing a petition for review in the
United States Court of Appeals for the District of Columbia Circuit by
July 18, 2011. Under section 307(d)(7)(B) of the CAA, only an objection
to this final rule that was raised with reasonable specificity during
the period for public comment can be raised during judicial review.
Moreover, under section 307(b)(2) of the CAA, the requirements
established by this action may not be challenged separately in civil or
criminal proceedings brought by EPA to enforce these requirements.

II. Background

    This action amends EPA's Method 301, Field Validation of Pollutant
Measurement Methods from Various Waste Media. Method 301 was originally
promulgated in Appendix A of 40 CFR part 63 on June 3, 1991. We
proposed amendments to Method 301 on December 22, 2004 (69 FR 76642).
This action responds to comments received on that proposal and corrects
errors found in the method.

III. Summary of the Final Method

    You would use Method 301 whenever you propose to use a test method
to meet an EPA compliance requirement other than a method required
under a 40 CFR part 63 rule. The method specifies procedures for
determining and documenting the precision and bias of measured
concentrations from various media (e.g., sludge, exhaust gas,
wastewater) at the level of an applicable standard for a source. Bias
(or systemic error) is established by comparing your proposed method
against a reference value.
    A correction factor is employed to eliminate/minimize bias. This
correction factor is established from data obtained during your
validation test. Methods that have bias correction factors outside a
specified range are considered unacceptable. Method precision (or
random error) at the level of the standard must be demonstrated to be
as precise as the validated method for acceptance.

IV. Significant Comments Received on the Proposed Amendments to Method
301

    We proposed five major technical changes to Method 301. These
technical changes include the following:
    (1) Replacing the Practical Limit of Quantitation (PLQ) with a
procedure to determine the Limit of Detection (LOD),
    (2) Revising the bias acceptance criteria and eliminating
correction factors,
    (3) Revising precision acceptance criteria when using analyte
spiking,
    (4) Allowing analyte spiking even when there is an existing test
method, and
    (5) Establishing new procedures for ensuring sample stability.
    The following section provides our response to significant comments
received on the proposed technical changes and some inadvertant errors
that occurred with the restructuring of and addition of components to
the method.

A. Applicability

    Two commenters requested clarification that the final rule changes
made to Method 301 only apply to methods submitted to EPA after
promulgation of the changes and that Method 301 can be used whether or
not a validated method exists. We are clarifying in this final rule
that amendments to Method 301 do not apply to methods submitted for
approval prior to promulgation. Also, Method 301 can be used whether or
not a validated method exists. This action clarifies the effective date
of the amended Method 301, and Section 1.0 of the final method
clarifies that Method 301 can be used whether or not a validated method
exists.

B. Reference Material

    One commenter provided that, as written, reference material is
analogous to analyte. Inadvertantly, in Section 5 of Method 301,
``reference materials'' was followed by ``(analytes).'' This
paranthetical was modified for clarification purposes as noted below.
    A few commenters expressed concern that the standard against which
precision and bias are compared is not required to be compared against
a true value, usually a traceable standard. We agree that the reference
material should be compared to a traceable standard.
    We have amended Section 5 of the final method to state the
following:

    You must use reference materials (a material or substance whose
one or more properties 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 63 requires.

C. Validation Testing Over a Broad Range of Concentrations and Extended
Period of Time

    One commenter requested that validation testing over a broad range
of concentrations and/or over an extended period of time be allowed and
mentioned that they had developed technology that could test over a
broad range of concentrations for an extended time-period. The
commenter argued that if the accuracy and precision requirements can be
demonstrated with sequential sampling procedures, EPA should allow it.
We agree with the commenter. We have approved methods demonstrated with
sequential sampling to determine the precision of a proposed
alternative method in the past. The final method explicitly states that
sequential sampling procedures are allowed.

D. Performance Audit

    One commenter stated that they do not agree that the performance
audit requirements in Section 6 of the proposed rule should be included
in Method 301. The commenter supported their position by stating that
the audit material may not correspond to the matrix for which the
alternate test method was designed, and it is similar to having to ask
EPA permission to use a method that has passed Method 301 validation
criteria. In addition, the commenter stated that the 30-day lead time
for requesting the performance audit material reduces an affected
party's flexibility in meeting performance testing timing requirements.
    The function of an audit sample is to allow a tester to demonstrate
that their measurement system, using a well-established measurement
method, is operating within established quality assurance limits. If
the alternative method is being compared to a validated test method as
part of the Method 301 validation and an audit sample for the validated
method exists, then an audit should be used for the validated method.
Since the amendments to Method 301 were proposed on December 22, 2004,
EPA promulgated a rule on September 13, 2010 (75 FR 55636), that moves
all discussion of audits from the individual rules to the General
Provisions of Part 63. Therefore, we have removed the proposed Section
6 which discussed performance audits.

E. Sample Stability Procedures

    We proposed procedures for sample stability. Method 301 previously
lacked specific procedures for ensuring that samples collected under
proposed alternative methods were analyzed

within an appropriate time. We revised Section 7.4 to include a
requirement to calculate the difference in the sampling results at the
minimum and maximum storage times, determine the standard deviation of
the differences, and test the difference in the results for statistical
significance by calculating the t-statistic and determining if the mean
of the differences between the initial results and the results after
storage is significant at the 95 percent confidence level. We also
added Table 1 to compare the calculated t-statistic with the critical
value of the t-statistic. These procedures are necessary to ensure
sample stability and should have been included in Method 301.
    Several commenters provided comments on the minimum and maximum
storage holding time limits specified in Section 7.0 of Method 301.
Commenters recommended that either the minimum and maximum holding
times be removed and that holding times should be defined by the data
or that they be liberalized (e.g., increase the minimum hold time from
24 hours to 48 to 72 hours). We agree with the commenters and are
revising the minimum hold time to be seven days. The method will also
require that the samples be analyzed again at the proposed maximum
storage time or two weeks after the initial analysis.

F. Bias and Precision

    We proposed to change the acceptance criteria for the bias in a
proposed alternative method from  30 percent to  10 percent and concurrently to eliminate the requirement for
correcting all data collected with the method. We provided that we
believe that 12 pairs of results from a single source are not
sufficient to allow us to establish a correction factor that can or
should be applied to all future uses of the method.
    One commenter stated that they did not believe that bias acceptance
criteria should be changed unless uncertainties in the reference value
are included in determining the significance of differences.
    One commenter provided that the proposed reduction of bias from
 30 percent to  10 percent is too stringent.
One commenter suggested allowing a bias of  15 percent with
no correction factors while continuing to allow a bias of
30 percent with the use of correction factors for bias values between
15 percent and 30 percent. The commenter provided a summary of EPA
Method 301 validations of several methods to support their position.
    We agree that reducing the acceptable bias to  10
percent may be too stringent because there may be testing situations
that are so difficult that there are no methods readily available that
could meet this requirement. We believe that a reasonable solution is
to allow methods that have a bias greater than 10 percent if the
results from these methods are corrected to account for that bias.
However, we believe that we should not approve the use of methods with
greater than 30 percent bias even if the user was willing to correct
the results. We have changed the final method to allow a bias of  10 percent with no correction factors and allow a bias of  30 percent with the use of correction factors for bias values
between 10 percent and 30 percent.
    We proposed to change the acceptance criteria for method precision
when using analyte spiking from  50 percent to
20 percent. In addition, we proposed to eliminate the requirement for
different numbers of replicate samples depending on the method's
relative precision. We also proposed to tighten the acceptance criteria
for the precision of candidate alternative test methods.
    One commenter stated that the proposed reduction of precision
criteria from  50 percent to  20 percent is too
stringent. The commenter suggested allowing a precision of
30 percent with no use of replicate runs and the continued allowance of
a precision of  50 percent with the use of additional
sample runs for precision values between 30 percent and 50 percent. The
commenter provided a summary of EPA Method 301 validations of several
methods to support their position.
    Based on our evaluation of the summary provided by the commenter
and their suggestion, we have changed the final method. The method will
continue to require a precision of  20 percent when only
the required three runs per test are performed. However, we have added
an option to allow test methods with a precision greater than  20 percent, but less than  50 percent, provided that
the user collect nine sample runs per test during any compliance
testing where the method is used.

G. Limit of Detection

    We proposed to replace the determination of the PLQ with a
procedure to determine the LOD. The purpose of establishing a
measurement limit is to ensure that a test method is appropriate for
its intended use. The LOD is a better parameter for this purpose. We
provided that for most environmental measurements, it appears that
precision is a function of the concentration of the analyte being
measured. Thus, the relative imprecision will not decrease as the
quantity measured increases.
    In this case, we stated that the PLQ has no meaning. Several
commenters disagreed that the PLQ is a meaningless concept and that
there are instances that substituting the LOD for the PLQ is not always
appropriate. Some of these commenters stated that the Office of Water
formed a Federal Advisory Committee Act (FACA) Committee to consider
alternative approaches to similar procedures they proposed (40 CFR part
136 Appendix B) and that Method 301 should be deferred until after
those discussions have concluded and that consistent application be
applied across the Agency based on those discussions.
    The PLQ is a limit determined by the standard deviation of an
estimate of a concentration; if the standard deviation of the estimate
exceeds a threshold, then that estimate is unacceptable. The LOD is a
limit determined by the estimate of the concentration itself. If this
estimate possesses a value that cannot be distinguished from an
estimate resulting from a blank sample with a stated level of
confidence, then this estimate is unacceptable. The LOD is clearly a
threshold that should be used in Method 301 since an estimate that
cannot be distinguished from one resulting from a blank sample is
unlikely to provide meaningful results.
    The PLQ does not appear to have any relevance for Method 301. There
does not appear to be a good reason for a method that produces a
standard deviation that exceeds an established threshold to not go
through the full rigor of the bias and precision tests prescribed in
Method 301. For these reasons, Method 301 retains the use of the LOD in
lieu of the PLQ.
    One commenter provided that the proposed LOD determination does not
appear appropriate for radiochemical methods and suggested that the
content of the Multi-Agency Radiological Laboratory Analytical
Protocols Manual (MARLAP) be used. We agree with the commenter and have
amended Method 301 to allow for the use of the MARLAP for radiochemical
methods.
    A few commenters requested that the calculation of the LOD be
better defined and clarified in Table 4 of the method. One commenter
expressed that the description of the procedures used for estimating
the standard deviation at zero concentration (S0) in Table 4
needs to be clarified.
    The LOD is defined as the lowest quantity of a substance that can
be distinguished from the absence of that substance (i.e., blank value)
with a

stated level of confidence. For example, suppose blank samples are
normally distributed, and S0 represents the standard
deviation of the blank samples (i.e., the standard deviation of pure
``noise''). Then a sample value larger than 3S0 will have a
probability of not being a blank of at least 99 percent if
S0 is estimated with at least 14 degrees of freedom (or at
least 7 degrees of freedom if a 1-sided alternative hypothesis is
assumed). If S0 is ``known'', then the probability will be
99.74 percent, but this is often truncated to 99 percent.
    The method for obtaining S0 has been clarified to
proceed as follows:
    (1) Pick a concentration level that you think should approximate
the LOD and call this level LOD1. Prepare seven samples of a
standard set at a concentration of LOD1. Estimate the
standard deviation of these seven samples, and call it S1.
    (2) Define LOD0 = 3S1.
    (3) If LOD1 <= 2LOD0, then define
S0 = S1.
    (4) If LOD1 > 2LOD0, then proceed as follows:
    a. Prepare two additional standards at concentrations lower than
LOD1, and call these LOD2 and LOD3.
Prepare seven samples of each of these two standards and estimate their
standard deviations and call them S2 and S3,
respectively.
    b. Plot S1, S2, and S3 as a
function of concentration, draw a best-fit straight line through them,
and extrapolate to zero concentration.
    c. Define S0 as the extrapolation of the standard
deviation at zero concentration.

H. Critical Values of t for the Two-Tailed 95 Percent Confidence Limit

    Two commenters provided that the values of t for the two-tailed 95
percent confidence limit are wrong since they reflected an 80 percent
confidence limit and there are some apparent typesetting errors. We
corrected these values to reflect the 95 percent confidence limit and
eliminated the typesetting errors in the final method.

I. Paired Sampling Procedure

    Two commenters pointed out several errors and expressed concerns
with the methods to ascertain and test precision in Section 12.
    Upon evaluation, we have decided to revise Section 12.2 in Method
301. We are deleting the comparison of the precision of the alternative
method to that of the validated method. This decision was made because
the paired sampling method described in it does not allow for the
estimation of the within-sample standard deviation for either the
alternative or validated methods.

J. Standard Deviation

    One commenter expressed that the precision is a function of
concentration; in other words, as the concentration level increases, so
does the standard deviation of the estimate of that concentration. This
could render the relative standard deviation (Eq. 301-8 in Section
10.4) meaningless.
    A second commenter also expressed that the standard deviation is a
function of concentration. This commenter noted that pollutant
concentrations from an emission source are variable, resulting in a
range of possible concentration values being measured. The commenter
suggested that the appropriate procedure to compare two methods under
these circumstances is to compare the regression lines of the two
methods across a range of concentrations.
    We agree that this could be a potentially serious concern if there
is little control over the concentrations being measured. However, if
there is an appropriate level of control, then the procedures given in
Method 301 are sufficient. In most situations, we believe that an
appropriate level of control exists. For example, consider the case
where an alternative method is compared against a validated method
using quadruple samples. We believe that an appropriate level of
control exists if the following four conditions are met: (1) There is
positive correlation between the estimates within both alternative and
validated pairs in the quadruple samples, and the respective
correlation coefficients are reasonably constant as a function of
concentration; (2) there is positive correlation between the
alternative and validated estimates in the quadruple samples, and the
correlation coefficient is reasonably constant as a function of
concentration; (3) the within-quadruple sample concentrations are
reasonably similar; and (4) if the between-quadruple sample
concentrations vary greatly, then the functional relationship between
the standard deviation and concentration is reasonably similar for both
the alternative and validated methods. We believe that these four
conditions hold, for most cases, and an appropriate level of control
exists. If one or more of these conditions is violated, then the user
may request that they be allowed to compare the regression lines
resulting from the alternative and validated estimates as a function of
concentration as an alternative to the requirements in Method 301.

V. Statutory and Executive Order Reviews

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

    This action is not a ``significant regulatory action'' under the
terms of Executive Order 12866 (58 FR 51735, October 4, 1993) and is
therefore not subject to review under Executive Orders 12866 and 13563
(76 FR 3821, January 21, 2011).

B. Paperwork Reduction Act

    This action does not impose an information collection burden under
the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq.
Burden is defined at 5 CFR 1320.3(b). We are not promulgating any new
paperwork requirements (e.g., monitoring, reporting, recordkeeping) as
part of this final action. This final rule amends Method 301 which may
be used to validate test data or a new test method.

C. Regulatory Flexibility Analysis

    The Regulatory Flexibility Act (RFA) generally requires an agency
to prepare a regulatory flexibility analysis of any rule subject to
notice and comment rulemaking requirements under the Administrative
Procedure Act or any other statute unless the agency certifies that the
rule will not have a significant economic impact on a substantial
number of small entities. Small entities include small businesses,
small organizations, and small governmental jurisdictions.
    For purposes of assessing the impacts of this action on small
entities, a small entity is defined as: (1) A small business as defined
by the Small Business Administration's (SBA) regulations at 13 CFR
121.201; (2) a small governmental jurisdiction that is a government of
a city, county, town, school district or special district with a
population of less than 50,000; and (3) a small organization that is
any not-for-profit enterprise that is independently owned and operated
and is not dominant in its field.
    After considering the economic impacts of this final rule on small
entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. This final
rule will not impose any requirements on small entities. Small entities
may chose to use this regulatory option of validating their own new or
alternative compliance test method, but they are not required to choose
this option. Any small entity choosing to use Method 301 to validate a
new or

alternative test method would likely do so because this option is less
burdensome than the original method in the regulations.

D. Unfunded Mandates Reform Act

    This action contains no Federal mandates under the provisions of
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), 2 U.S.C.
1531-1538 for State, local, or Tribal governments or the private
sector. This action imposes no enforceable duty on any State, local or
Tribal governments or the private sector. Therefore, this action is not
subject to the requirements of sections 202 or 205 of the UMRA. This
action is also not subject to the requirements of section 203 of UMRA
because it contains no regulatory requirements that might significantly
or uniquely affect small governments. Any small entity that chooses to
use Method 301 would likely do so because this option is less
burdensome.

E. Executive Order 13132--Federalism

    This 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, as
specified in Executive Order 13132. This final rule simply amends
Method 301 which may be used to validate test data or a new test
method.

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

    This action does not have Tribal implications, as specified in
Executive Order 13175 (65 FR 67429, November 9, 2000). This final rule
amends Method 301 which can be used to validate a new or alternative
compliance test method. It does not add any new requirements and does
not affect pollutant emissions or air quality. Thus, Executive Order
13175 does not apply to this action.
    Although EO 13175 does not apply to this final rule, EPA
specifically solicited comment on the proposed rule from Tribal
officials. No comments were received.

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

    EPA interprets EO 13045 (62 FR 19885, April 23, 1997) as applying
only to those regulatory actions that concern health or safety risks,
such that the analysis required under section 5-501 of the EO has the
potential to influence the regulation. This action is not subject to EO
13045 because it does not establish an environmental standard intended
to mitigate health or safety risks.

H. Executive Order 13211--Actions Concerning Regulations That
Significantly Affect Energy Supply, Distribution, or Use

    This action is not subject to Executive Order 13211, (66 FR 28355
(May 22, 2001)) because it is not a significant regulatory action under
Executive Order 12866.

I. National Technology Transfer and Advancement Act

    Section 12(d) of the National Technology Transfer and Advancement
Act of 1995 (NTTAA), Public Law 104-113, 12(d) (15 U.S.C. 272 note)
directs EPA to use voluntary consensus standards in its regulatory
activities unless to do so would be inconsistent with applicable law or
otherwise impractical. Voluntary consensus standards are technical
standards (for example, materials specifications, test methods,
sampling procedures, and business practices) that are developed or
adopted by voluntary consensus standards bodies. The NTTAA directs EPA
to provide Congress, through OMB, explanations when the Agency decides
not to use available and applicable voluntary consensus standards.
    This action involves technical standards. While EPA has identified
ASTM D4855-97 as being potentially applicable, we have decided not to
use it in this rulemaking. The use of this voluntary consensus standard
would have been impractical as the ASTM standard is less prescriptive
than Method 301 for many procedures. For example, the ASTM standard
does not require the use of a t-test explicitly to test the precision
of an alternative method, but instead states that a t-test or F-test
should be used as appropriate. The primary difference between the ASTM
standard and EPA Method 301 is that the ASTM standard addresses the
testing of ``materials'' rather than environmental samples. Therefore,
we believe the ASTM is impractical as an alternative to Method 301.

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

    Executive Order (EO) 12898 (59 FR 7629 (Feb. 16, 1994)) establishes
Federal executive policy on environmental justice. Its main provision
directs Federal agencies, to the greatest extent practicable and
permitted by law, to make environmental justice part of their mission
by identifying and addressing, as appropriate, disproportionately high
and adverse human health or environmental effects of their programs,
policies, and activities on minority populations and low-income
populations in the United States.
    EPA has determined that this final rule will not have
disproportionately high and adverse human health or environmental
effects on minority or low-income populations because it does not
affect the level of protection provided to human health or the
environment. This action amends a method for validating new or
alternative compliance test methods. It does not change any existing
rules that limit air pollution emission limits.

K. Congressional Review Act

    The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the
Small Business Regulatory Enforcement Fairness Act of 1996, generally
provides that before a rule may take effect, the agency promulgating
the rule must submit a rule report, which includes a copy of the rule,
to each House of the Congress and to the Comptroller General of the
United States. EPA will submit a report containing this rule and other
required information to the U.S. Senate, the U.S. House of
Representatives, and the Comptroller General of the United States prior
to publication of the rule in the Federal Register. A major rule cannot
take effect until 60 days after it is published in the Federal
Register. This action is not a ``major rule'' as defined by 5 U.S.C.
804(2). This rule will be effective May 18, 2011.

List of Subjects in 40 CFR Part 63

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

    Dated: May 10, 2011.
Lisa P. Jackson,
Administrator.
    For the reasons stated in the preamble, title 40, chapter I of the
Code of the Federal Regulations is amended 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 is amended by revising Method 301 to read as follows:

Appendix A to Part 63--Test Methods

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 quadruplet 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 (LOD) for the
alternative method?

Other Requirements and Information

16.0 How do I apply for approval to use an alternative 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?

    The purpose of Method 301 is to provide a set of procedures that
you, the owner or operator of an affected source subject to
requirements under 40 CFR part 63 can use to validate an alternative
test method to a test method required in 40 CFR part 63 or to
validate a stand-alone alternative test method based on established
precision and bias criteria. If you use Method 301 to validate your
proposed alternative method, you must use the procedures described
in this method. This method describes the minimum procedures that
you must use to validate an alternative test method to meet 40 CFR
part 63 compliance requirements. If you choose to propose a
validation method other than Method 301, you must submit and obtain
the Administrator's approval for the alternative validation method.

2.0 When must I use Method 301?

    If you want to use an alternative test method to meet
requirements in a subpart of 40 CFR part 63, you can use Method 301
to validate the alternative test method. You must request approval
to use this alternative test method according to the procedures in
Sections 16 and 63.7(f). You must receive the Administrator's
written approval to use the alternative test method before you use
the alternative test method to meet requirements under 40 CFR part
63. In some cases, the Administrator may decide to waive the
requirement to use Method 301 for alternative test methods. Section
17 describes the requirements for obtaining a waiver.

3.0 What does Method 301 include?

    3.1 Procedures. This method 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. It contains procedures for
ensuring sample stability if such procedures are not included in the
test method. This method also includes optional procedures for
ruggedness and detection limits.
    3.2 Definitions.
    Affected source means affected source as defined in 40 CFR 63.2
and in the relevant subpart under 40 CFR part 63.
    Alternative test method means the sampling and analytical
methodology selected for field validation using the method described
in this appendix.
    Paired sampling system means a sampling system capable of
obtaining two replicate samples that were collected as closely as
possible in sampling time and sampling location.
    Quadruplet sampling system means a sampling system capable of
obtaining four replicate samples that were collected as closely as
possible in sampling time and sampling location.
    Surrogate compound means a compound that serves as a model for
the types of compounds being analyzed (i.e., similar chemical
structure, properties, behavior). The model can be distinguished by
the method from the compounds being analyzed.

4.0 How do I perform Method 301?

    First, you introduce a known concentration of an analyte or
compare the alternative test method against a validated test method
to determine the alternative test method's bias. Then, you collect
multiple, collocated simultaneous samples to determine the
alternative test method's precision. Alternatively, though it is not
required, we allow validation testing over a broad range of
concentrations over an extended time period to determine precision
of a proposed alternative method. Sections 5.0 through 17.0 describe
the procedures in detail.

Reference Materials

5.0 What reference materials must I use?

    You must use reference materials (a material or substance whose
one or more properties 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 63 requires. If you want to expand the applicable range of
the method, you must conduct additional runs with higher and lower
analyte concentrations. You must obtain information about your
analyte according to the procedures in Sections 5.1 through 5.4.
    5.1 Exhaust Gas Tests Concentration. You must get a known
concentration of each analyte from an independent source such as a
speciality gas manufacturer, specialty chemical company, or chemical
laboratory. You must also get the manufacturer's certification for
the analyte concentration and stability.
    5.2 Tests for Other Waste Media. You must get the pure liquid
components of each analyte from an independent manufacturer. The
manufacturer must certify the purity and shelf life of the pure
liquid components. You must dilute the pure liquid components in the
same type medium 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 one
that contains a unique element (for example, 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 isotope labeled analyte
concentration must be more than five times the natural concentration
of the analyte.

Sampling Procedures

6.0 What sampling procedures must I use?

    You may determine bias and precision by comparing against a
validated test method, using isotopic sampling, or using analyte
spiking (or the equivalent). Isotopic sampling can only be used for
procedures requiring mass spectrometry or radiological procedures.
You must collect samples according to the requirements in Table 1.
You must perform the sampling according to the procedures in
Sections 6.1 through 6.4.
    6.1 Isotopic Spiking. Spike all 12 samples with the analyte at
the concentration in the applicable emission limitation or standard
in the subpart of 40 CFR part 63. If there is no applicable emission
limitation or standard, spike at the expected level of the samples.
Follow the appropriate spiking procedures in Sections 6.3.1 through
6.3.2 for the applicable waste medium.
    6.2 Analyte Spiking. In each quadruplet set, spike half of the
samples (two out of the four) with the analyte according to the
applicable procedure in Section 6.3.
    6.3 Spiking Procedure.
    6.3.1 Gaseous Analyte with Sorbent or Impinger Sampling Trains.
Sample the analyte (in the laboratory or in the field) at a
concentration that is close to the concentration in the applicable
emission limitation or standard in the subpart of 40 CFR Part 63 (or
the expected sample concentration where there is no standard) for
the time required by the method, and then sample the gas stream for
an equal amount of time. The time for sampling both the analyte and
gas stream should be equal; however, the time should be adjusted to
avoid sorbent breakthrough. The stack gas and the gaseous analyte
may be sampled at the same time. The analyte must be

introduced as close to the tip of the sampling train 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 amount equal to the concentration in the applicable emission
limitation or standard in the subpart of 40 CFR part 63 (or the
expected sample concentration where there is no standard). The final
concentration of the analyte would be approximately equal to the
analyte concentration in the stack plus the applicable emission
standard (corrected for spike volume). The volume amount of analyte
must be less than 10 percent of the sample volume.
    6.3.3 Liquid and Solid Analyte with Sorbent or Impinger Trains.
Spike the trains with an amount equal to the concentration in the
applicable emission limitation or standard in the subpart of 40 CFR
part 63 (or the expected sample concentration 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 can do it 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 amount equal to the concentration in the applicable emission
limitation or standard in the subpart of 40 CFR part 63 (or the
expected sample concentration where there is no standard).
    6.4 Probe Placement and Arrangement for Stationary Source Stack
or Duct Sampling. To sample a stationary source as defined in 40 CFR
63.2, you must place the probe according to the procedures in this
subsection. You must place the probes in the same horizontal plane.
    6.4.1 Paired Sampling Probes. For paired sampling probes, the
probe tip should be 2.5 cm from the outside edge of the other sample
probe, with a pitot tube on the outside of each probe. The
Administrator may approve a validation request where other paired
arrangements for the pitot tube (where required) are used.
    6.4.2 Quadruplet Sampling Probes. For quadruplet 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 or two pitot tubes (where
required) with their location on either side of the probe tip
configuration. 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 Storage and Analysis Procedures. If the
alternative 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 alternative test
method. You are not required to conduct the procedures in Section
7.2 or 7.3. If the alternative test method does not include such
procedures, you must propose 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. The
minimum storage time should be as soon as possible, but no longer
than 72 hours after collection of the sample. The maximum storage
time should be no longer than two weeks.
    7.2 Storage and Sampling Procedures for Stack Test Emissions.
You must store and analyze samples of stack test emissions according
to Table 3. If you are using analyte spiking procedures, you must
include equal numbers of spiked and unspiked samples.
    7.3 Storage and Sampling Procedures for Testing Other Waste
Media (e.g., Soil/Sediment, Solid Waste, Water/Liquid). You must
analyze half of the replicate samples at the proposed minimum
storage time and the other half at the proposed maximum storage time
or within two weeks of the initial analysis to identify the effect
of storage times on analyte samples. The minimum storage time should
be as soon as possible, but no longer than seven days after
collection of the sample.
    7.4 Sample Stability. After you have conducted sampling and
analysis according to Section 7.2 or 7.3, compare the results at the
minimum and maximum storage times. Calculate the difference in the
results using Equation 301-1.
[GRAPHIC] [TIFF OMITTED] TR18MY11.002

Where:

di = difference between the results of the ith sample.
Rmini = results from the ith sample at the minimum
storage time.
Rmaxi = results from the ith sample at the maximum
storage time.

    7.4.1 Standard Deviation. Determine the standard deviation
(SDd) of the differences (di's) of the paired
samples using Equation 301-2.
[GRAPHIC] [TIFF OMITTED] TR18MY11.003

Where:

di = The difference between the results of the ith
sample, Rmini - Rmaxi.
dm = The 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 initial results and the results after
storage 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.
[GRAPHIC] [TIFF OMITTED] TR18MY11.004

Where:

n = The total number of paired samples.

    Compare the calculated t-statistic with the critical value of the
t-statistic from Table 2. If the calculated t-value is less than the
critical value, the difference is not statistically significant; thus,
the sampling and analysis procedure ensures stability, and you may
submit a request for validation of the proposed alternative 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 with new samples using shorter
proposed maximum storage times.

Bias and Precision

8.0 What are the requirements for bias?

    You must establish bias by comparing the results of the sampling
using the alternative test method against a reference value. The bias
must be no more than  10 percent without the use of
correction factors, and no more than  30 percent with the
use of correction factors for bias values between 10 and 30 percent for
the alternative test method to be acceptable.

9.0 What are the requirements for precision?

    At a minimum, you must use paired sampling systems to establish
precision. If you are using analyte spiking, including isotopic
samples, the precision expressed as the relative standard deviation
(RSD) of the alternative test method at the level of the applicable
emission limitation or standard in the subpart of 40 CFR part 63 must
be less than or equal to 20 percent. For samples with a precision
greater than 20 percent but less than 50

percent, a minimum of nine sample runs will be required. If you are
comparing to a validated test method, the alternative test method must
be at least as precise as the validated method at the level of the
applicable emission limitation or standard in the subpart of 40 CFR
part 63 as determined by an F test (Section 11.2.2).

10.0 What calculations must I perform for isotopic spiking?

    You must analyze the bias, precision, relative standard deviation,
and data acceptance for isotopic spiking tests according to the
provisions in Sections 10.1 through 10.3.
    10.1 Numerical Bias. Calculate the numerical value of the bias
using the results from the analysis of the isotopically spiked field
samples and the calculated value of the isotopically labeled spike
according to Equation 301-4.
[GRAPHIC] [TIFF OMITTED] TR18MY11.005

Where:

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

    10.2 Standard Deviation. Calculate the standard deviation of the
Si values according to Equation 301-5.
[GRAPHIC] [TIFF OMITTED] TR18MY11.006

Where:

Si = Measured value of the isotopically labeled analyte
in the i-th field sample,
n = Number of isotopically spiked samples, 12.

    10.3 t Test. Test the bias for statistical significance by
calculating the t-statistic using Equation 301-6. Use the standard
deviation determined in Section 10.2 and the numerical bias determined
in Section 10.1.
[GRAPHIC] [TIFF OMITTED] TR18MY11.007

    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. When spiking is conducted according to the procedures
specified in Sections 6.2 and 6.4 as required, this critical value is
2.201 for the 11 degrees of freedom. If the calculated t-value is less
than 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.
[GRAPHIC] [TIFF OMITTED] TR18MY11.008

Where:

BR = Relative bias.

    If the relative bias is less than or equal to ten percent, the bias
of the candidate test method is acceptable and no correction factors
are required. If the relative bias is greater than 10 percent but less
than 30 percent, and if you correct all future data collected with the
method for the magnitude of the bias, the bias of the candidate test
method is acceptable. If either of the preceding two cases applies, you
may continue to evaluate the method by calculating its precision. If
not, the candidate method will not meet the requirements of Method 301.
    10.4 Relative Standard Deviation. Calculate the RSD according to
Equation 301-8.
[GRAPHIC] [TIFF OMITTED] TR18MY11.009

Where:

Sm = The measured mean of the isotopically labeled spiked
samples.

    The data and alternative 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 quadruplet replicate sampling systems?

    If you are using quadruplet replicate sampling systems to compare
an alternative test method to a validated method, then you must analyze
the data according to the provisions in this section. If the data from
the alternative test method fail either the bias or precision test, the
data and the alternative 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 alternative test method and the validated
method (dm). Calculate di according to Equation
301-9.
[GRAPHIC] [TIFF OMITTED] TR18MY11.010

Where:

V1i = First measured value with the validated method in
the i-th sample.
V2i = Second measured value with the validated method in
the i-th sample.
P1i = First measured value with the alternative test
method in the i-th sample.
2i = Second measured value with the alternative test
method in the i-th sample.

    11.1.2 Standard Deviation of the Differences. Calculate the
standard deviation of the differences, SDd, using Equation
301-2.
    11.1.3 t Test. Calculate the t-statistic using Equation 301-3,
where n is the total number of test sample differences (di).
For the quadruplet sampling system procedure in Section 6.1 and Table
1, n equals four. 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 four runs are conducted, as specified in Section
6.2 and Table 1, the critical value of the t-statistic is 3.182 for
three 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
relative magnitude of the bias using Equation 301-10.
[GRAPHIC] [TIFF OMITTED] TR18MY11.011

Where:

B = Bias - mean of the di's.
VS = Mean measured by the validated method.

    If the relative bias is less than or equal to 10 percent, the bias
of the candidate test method is acceptable and no correction factors
are required. If the relative bias is greater than 10 percent but less
than 30 percent, and if you correct all future data collected with the
method for the magnitude of the bias, the bias of the candidate test
method is acceptable. If either of the preceding two cases applies, you
may continue to evaluate the method by calculating its precision. If
not, the candidate method will not meet the requirements of Method 301.
    11.2 Precision. Compare the estimated variance (or standard
deviation) of the alternative test method to that of the validated
method. If a significant difference is determined using the F test, the
alternative test method and the results are rejected. If the F test
does not show a significant difference, then the alternative test
method has acceptable precision. Use the value furnished with the
method. Calculate the estimated variance of the validated method using
Equation 301-11.
    11.2.1 Alternative Test Method Variance. Calculate the estimated
variance of the alternative test method, Sp\2\, according to
Equation 301-11.
[GRAPHIC] [TIFF OMITTED] TR18MY11.012

Where:

di = The difference between the i-th pair of samples
collected with the alternative test method.
n = Number of samples and the degrees of freedom.

    11.2.2 F Test. Determine if the estimated variance of the
alternative test method is greater than that of the validated method by
calculating the F-value using Equation 301-12.
[GRAPHIC] [TIFF OMITTED] TR18MY11.013

Where:

Sp\2\ = The estimated variance of the alternative method.
Sv\2\ = The estimated variance of the validated method.

    Compare the experimental F value with the one-sided confidence
level for F. The one-sided confidence level of 95 percent for F is
6.388 when the procedure specified in Section 6.1 and Table 1 for
quadruplet trains is followed. If the calculated F is outside the
critical range, 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 using the results from the analysis
of the spiked field samples, the unspiked field samples, and the
calculated value of the spike using Equation 301-13.
[GRAPHIC] [TIFF OMITTED] TR18MY11.014

Where:

S1i = First measured value of the ith spiked sample.
S2i = Second measured value of the ith spiked sample.
M1i = First measured value of the ith unspiked sample.
M2i = Second measured value of the ith unspiked sample.
CS = Calculted value of the spiked level.

    12.1.2 Standard Deviation of the Differences. Calculate the
standard deviation of the differences, SDd, using Equation
301-2.
    12.1.3 t Test. Calculate the t-statistic using Equation 301-3,
where n is the total number of test sample differences (di).
For the quadruplet sampling system procedure in Table 1, 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. When six runs are conducted, as specified in Table 1,
the two-sided confidence level critical value is 2.571 for the five
degrees of freedom. If the relative bias is less than or equal to 10
percent with no correction factors, or the bias is greater than 10
percent but less than 30 percent with the use of correction factors,
then the data are acceptable. Proceed to evaluate precision of the
candidate test method.
[GRAPHIC] [TIFF OMITTED] TR18MY11.015

Where:

B = Bias - mean of the di's.
VS = Mean measured by the validated method.

    12.2 Precision. Calculate the standard deviation and the
relative standard deviation of the candidate test method. The
relative standard deviation of the candidate test method can be
calculated using Equation 301-8.

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 63 for an affected
source, and the Administrator has approved the use of the
alternative test method at your similar source according to the
procedures in Section 17.1.1, you must meet the requirements in this
section. You must have at least three replicate samples for each
test that you conduct at the similar source. You must average the
results of the samples to determine the pollutant concentration.

Optional Requirements

14.0 How do I use and conduct ruggedness testing?

    If you want to use a validated test method at a concentration
that is different from the concentration in the applicable emission
limitation in the subpart of 40 CFR part 63 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 Citation 18.16 of Section 18.0 and submit a request
for a waiver according to Section 17.1.1.
    Ruggedness testing is a laboratory study to determine the
sensitivity of a method to parameters such as sample collection
rate, interferant concentration, collecting 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 eight experiments instead of one. (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 alternative
method?

    15.1 Limit of Detection. The Limit of Detection (LOD) is the
lowest level above which you may obtain quantitative results with an
acceptable degree of confidence. For this protocol, the LOD is
defined as three times the standard deviation, So, at the
blank level.
    15.2 Purpose. The LOD will be used to establish the lower limit
of the test method. If the estimated LOD is no more than twice the
calculated LOD, use Procedure I in Table 4 to determine
So. If the LOD is greater than twice the calculated LOD,
use Procedure II in Table 4 to determine So. 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://www.epa.gov/radiation/docs/marlap/402-b-04-001c-20_final.pdf.

Other Requirements and Information

16.0 How do I apply for approval to use an alternative test method?

    16.1 Submitting Requests. You must request to use an alternative
test method according to the procedures in Section 63.7(f). You may
not use an alternative test method to meet any requirement under 40
CFR part 63 until the Administrator has approved your request. The
request must include a field validation report containing the
information in Section 16.2. The request must be submitted to the
Director, Air Quality Assessment Division, U.S. Environmental
Protection Agency, C304-02, 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.
    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, as applicable.
    16.2.3 Analyte certification and value(s).
    16.2.4 Discussion of laboratory evaluations.
    16.2.5 Discussion of field sampling.
    16.2.6 Discussion of sample preparations 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
Sections 17.1.1 through 17.1.2, the Administrator may waive the
requirement to use the procedures in this method to validate an
alternative test method. In addition, if EPA currently recognizes an
appropriate test method or considers the analyst's 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 test method that you
want to use has been validated at another source and you can
demonstrate to the Administrator's satisfaction that your affected
source is similar to that source, then the Administrator may waive
the requirement for you to validate the alternative test method. One
procedure you may use to demonstrate the applicability of the method
to your affected source is by conducting a ruggedness test as
described in Section 14.0.
    17.1.2 Documented Methods. If the bias and precision of the
alternative 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 Director,
Air Quality Assessment Division, U.S. Environmental Protection
Agency, C304-02, Research Triangle Park, NC 27711.
    17.3 Information Application for Waiver. The request for a
waiver must contain a thorough description of the 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. 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 method should be
written preferably in the format of 40 CFR part 60, Appendix A Test
Methods. It must include an applicability statement, concentration
range, precision, bias (accuracy), and minimum and maximum storage
time in which samples must be analyzed.
    17.3.2 Summaries of previous validation tests or other
supporting documents. If a different procedure from that described
in this method was used, 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, sample
stability conducted according to Section 7.0, and detection limits
conducted according to Section 15.0, as applicable. For example, you
would not need to submit ruggedness testing results if you will be
using the method at the same concentration level as the
concentration level at which it was validated.
    17.3.4 Applicability Statement and Basis for Waiver Approval.
Your discussion of the applicability statement and basis for
approval of the waiver should address the following as applicable:
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 18.16.
    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. Statistical Manual of the Association of Official Analytical
Chemists, Association of Official Analytical Chemists, Washington,
DC, 1975, pp. 33-36.

               Table 1 of Appendix A--Sampling Procedures
------------------------------------------------------------------------
       If you are . . .                  You must collect . . .
------------------------------------------------------------------------
comparing against a validated  9 sets of replicate samples using a
 method.                        paired sampling system (a total of 18
                                samples) or 4 sets of replicate samples
                                using a quadruplet sampling system (a
                                total of 16 samples). In each sample
                                set, you must use the validated test
                                method to collect and analyze half of
                                the samples.
using isotopic spiking (can    a total of 12 replicate samples. You may
 only be used for procedures    collect the samples either by obtaining
 requiring mass spectrometry).  6 sets of paired samples or 3 sets of
                                quadruplet samples.
using analyte spiking........  a total of 24 samples using the
                                quadruplet sampling system (a total of 6
                                sets of replicate samples).
------------------------------------------------------------------------

    Table 2 of Appendix A--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.......................................................           2.776
5.......................................................           2.571
6.......................................................           2.447
7.......................................................           2.365
8.......................................................           2.306
9.......................................................           2.262
10......................................................           2.228
------------------------------------------------------------------------

  Table 3 of Appendix A--Storage and Sampling Procedures for Stack Test
                                Emissions
------------------------------------------------------------------------
      If you are . . .             With . . .        Then you must . . .
------------------------------------------------------------------------
using isotopic or analyte     sample container      analyze 6 of the
 spiking procedures.           (bag or canister)     samples within 7
                               and impinger          days and then
                               sampling systems.     analyze the same 6
                                                     samples at the
                                                     proposed maximum
                                                     storage time or 2
                                                     weeks after the
                                                     initial analysis.
                              sorbent and impinger  extract or digest 6
                               sampling systems      of the samples
                               that require          within 7 days and
                               extraction or         extract or digest 6
                               digestion.            other samples at
                                                     the proposed
                                                     maximum storage
                                                     time or 2 weeks
                                                     after the first
                                                     extraction or
                                                     digestion. Analyze
                                                     an aliquot of the
                                                     first 6 extracts
                                                     (digestates) within
                                                     7 days and proposed
                                                     maximum storage
                                                     times or 2 weeks
                                                     after the initial
                                                     analysis. This will
                                                     allow analysis of
                                                     extract storage
                                                     impacts.
                              sorbent sampling      analyze 6 samples
                               systems that          within 7 days.
                               require thermal       Analyze another set
                               desorption.           of 6 samples at the
                                                     proposed maximum
                                                     storage time or
                                                     within 2 weeks of
                                                     the initial
                                                     analysis.
comparing an alternative      sampling method that  analyze half of the
 test method against a         does not include      samples (8 or 9)
 validated test method.        sorbent and           within 7 days and
                               impinger sampling     half of the samples
                               systems that          (8 or 9) at the
                               require extraction    proposed maximum
                               or digestion.         storage time or
                                                     within 2 weeks of
                                                     the initial
                                                     analysis.
                              sorbent and impinger  extract or digest 6
                               sampling systems      of the samples
                               that require          within 7 days and
                               extraction or         extract or digest 6
                               digestion.            other samples at
                                                     the proposed
                                                     maximum storage
                                                     time or within 2
                                                     weeks of the first
                                                     extraction or
                                                     digestion. Analyze
                                                     an aliquot of the
                                                     first 6 extracts
                                                     (digestates) within
                                                     7 days and at the
                                                     proposed maximum
                                                     storage times or
                                                     within 2 weeks of
                                                     the initial
                                                     analysis. This will
                                                     allow analysis of
                                                     extract storage
                                                     impacts.
------------------------------------------------------------------------

                               Table 4 of Appendix A--Procedures for Estimating So
----------------------------------------------------------------------------------------------------------------

----------------------------------------------------------------------------------------------------------------
If the estimated LOD (LOD1, expected approximate LOD     If the estimated LOD (LOD1, expected approximate LOD
 concentration level) is no more than twice the           concentration level) is greater than twice the
 calculated LOD, use Procedure I as follows. Estimate     calculated LOD, use Procedure II as follows. Prepare
 the LOD (LOD1) and prepare a test standard at this       two additional standards (LOD2 and LOD3) at
 level. The test standard could consist of a dilution     concentration levels lower than the standard used in
 of the analyte described in Section 5.0.                 Procedure I (LOD1).
Using the normal sampling and analytical procedures for  Sample and analyze each of these standards (LOD2 and
 the method, sample and analyze this standard at least    LOD3) at least 7 times.
 7 times in the laboratory.
Calculate the standard deviation, S1, of the measured    Calculate the standard deviation (S2 and S3) for each
 values.                                                  concentration level.
Calculate the LOD0 (referred to as the calculated LOD)   Plot the standard deviations of the three test
 as 3 times S1, where S0 = S1.                            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.
----------------------------------------------------------------------------------------------------------------

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[FR Doc. 2011-12058 Filed 5-17-11; 8:45 am]
BILLING CODE 6560-50-P