Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures; Notice of Data Availability, 77742-77747 [2011-32063]
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Federal Register / Vol. 76, No. 240 / Wednesday, December 14, 2011 / Proposed Rules
• Does not have Federalism
implications as specified in Executive
Order 13132 (64 FR 43255, August 10,
1999);
• Is not an economically significant
regulatory action based on health or
safety risks subject to Executive Order
13045 (62 FR 19885, April 23, 1997);
• Is not a significant regulatory action
subject to Executive Order 13211 (66 FR
28355, May 22, 2001);
• Is not subject to requirements of
Section 12(d) of the National
Technology Transfer and Advancement
Act of 1995 (15 U.S.C. 272 note) because
application of those requirements would
be inconsistent with the Clean Air Act;
and
• Does not provide EPA with the
discretionary authority to address, as
appropriate, disproportionate human
health or environmental effects, using
practicable and legally permissible
methods, under Executive Order 12898
(59 FR 7629, February 16, 1994).
In addition, this action does not have
tribal implications as specified by
Executive Order 13175 (65 FR 67249,
November 9, 2000), because the SIP is
not approved to apply in Indian country
located in the state, and EPA notes that
it will not impose substantial direct
costs on tribal governments or preempt
tribal law.
List of Subjects in 40 CFR Part 52
Environmental protection, Air
pollution control, Incorporation by
reference, Intergovernmental relations,
Nitrogen dioxide, Ozone, Reporting and
recordkeeping requirements, Volatile
organic compounds.
Authority: 42 U.S.C. 7401 et seq.
Dated: December 6, 2011.
H. Curtis Spalding,
Regional Administrator, EPA New England.
[FR Doc. 2011–32059 Filed 12–13–11; 8:45 am]
BILLING CODE 6560–50–P
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Parts 52 and 70
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[EPA–R07–OAR–2011–0822; FRL–9505–7]
Approval and Promulgation of
Implementation Plans; State of
Missouri
Environmental Protection
Agency (EPA).
ACTION: Proposed rule.
AGENCY:
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Comments on this proposed
action must be received in writing by
January 13, 2012.
DATES:
Submit your comments,
identified by Docket ID No. EPA–R07–
OAR–2011–0822, by mail to Amy
Bhesania, Environmental Protection
Agency, Air Planning and Development
Branch, 901 North 5th Street, Kansas
City, Kansas 66101. Comments may also
be submitted electronically or through
hand delivery/courier by following the
detailed instructions in the ADDRESSES
section of the direct final rule located in
the rules section of this Federal
Register.
ADDRESSES:
FOR FURTHER INFORMATION CONTACT:
Amy Bhesania at (913) 551–7147, or by
email at bhesania.amy@epa.gov.
In the
final rules section of the Federal
Register, EPA is approving the State’s
SIP revision as a direct final rule
without prior proposal because the
Agency views this as a noncontroversial
revision amendment and anticipates no
relevant adverse comments to this
action. A detailed rationale for the
approval is set forth in the direct final
rule. If no relevant adverse comments
are received in response to this action,
no further activity is contemplated in
relation to this action. If EPA receives
relevant adverse comments, the direct
final rule will be withdrawn and all
public comments received will be
addressed in a subsequent final rule
based on this proposed action. EPA will
not institute a second comment period
on this action. Any parties interested in
commenting on this action should do so
at this time. Please note that if EPA
receives adverse comment on part of
this rule and if that part can be severed
from the remainder of the rule, EPA may
adopt as final those parts of the rule that
are not the subject of an adverse
comment. For additional information,
see the direct final rule which is located
in the rules section of this Federal
Register.
SUPPLEMENTARY INFORMATION:
Dated: November 28, 2011.
Karl Brooks,
Regional Administrator, Region 7.
EPA proposes to approve the
State Implementation Plan (SIP) and
Operating Permits Program revisions
submitted by the state of Missouri
SUMMARY:
which align the state’s rule entitled
‘‘Submission of Emission Data,
Emission Fees and Process Information’’
with the Federal Air Emissions
Reporting Requirements Rule (AERR).
[FR Doc. 2011–31908 Filed 12–13–11; 8:45 am]
BILLING CODE 6560–50–P
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ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Part 136
[EPA–HQ–OW–2010–0192; FRL–9504–2]
Guidelines Establishing Test
Procedures for the Analysis of
Pollutants Under the Clean Water Act;
Analysis and Sampling Procedures;
Notice of Data Availability
Environmental Protection
Agency (EPA).
ACTION: Notice of data availability.
AGENCY:
On September 23, 2010, EPA
proposed to approve a number of new
and revised test procedures (i.e.,
analytical methods) for measuring
pollutants under the Clean Water Act.
Today’s notice announces the
availability of new data on an analytical
method for the measurement of oil and
grease that EPA described in the earlier
notice but did not propose to approve it
for use. This notice discusses how EPA
is considering revising its proposed
regulatory requirements for this method.
EPA is soliciting comment only on
EPA’s consideration of this method.
DATES: Comments must be received on
or before February 13, 2012.
ADDRESSES: Submit your comments,
identified by Docket ID No. EPA–HQ–
2010–0192, by one of the following
methods:
• https://www.regulations.gov: Follow
the on-line instructions for submitting
comments.
• Email: OW-docket@epamail.epa.gov
Attention Docket ID No. OW–2010–
0192.
• Mail: Water Docket, Environmental
Protection Agency, Mailcode: 28221T,
1200 Pennsylvania Ave. NW.,
Washington, DC 20460.
• Hand Delivery: EPA Water Center,
EPA West Building, Room B102, 1301
Constitution Avenue NW., Washington,
DC, Attention Docket ID No. OW–2010–
0192. Such deliveries are only accepted
during the Docket’s normal hours of
operation, and special arrangements
should be made for deliveries of boxed
information.
Instructions: Direct your comments to
Docket ID No. EPA–HQ–OW–2010–
0192. EPA’s policy is that all comments
received will be included in the public
docket without change and may be
made available online at https://
www.regulations.gov, including any
personal information provided, unless
the comment includes information
claimed to be Confidential Business
Information (CBI) or other information
whose disclosure is restricted by statute.
SUMMARY:
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Do not submit information that you
consider to be CBI or otherwise
protected through https://
www.regulations.gov or email. The
https://www.regulations.gov Web site is
an ‘‘anonymous access’’ system, which
means EPA will not know your identity
or contact information unless you
provide it in the body of your comment.
If you send an email comment directly
to EPA without going through https://
www.regulations.gov your email address
will be automatically captured and
included as part of the comment that is
placed in the public docket and made
available on the Internet. If you submit
an electronic comment, EPA
recommends that you include your
name and other contact information in
the body of your comment and with any
disk or CD–ROM you submit. If EPA
cannot read your comment due to
technical difficulties and cannot contact
you for clarification, EPA may not be
able to consider your comment.
Electronic files should avoid the use of
special characters, any form of
encryption, and be free of any defects or
viruses. For additional information
about EPA’s public docket visit the EPA
Docket Center homepage at https://
www.epa.gov/epahome/dockets.htm.
Docket: All documents in the docket
are listed in the https://
www.regulations.gov index. Although
listed in the index, some information is
not publicly available, e.g., CBI or other
information whose disclosure is
restricted by statute. Certain other
material, such as copyrighted material,
will be publicly available only in hard
copy. Publicly available docket
materials are available either
electronically in https://
www.regulations.gov or in hard copy at
the Water Docket, EPA/DC, EPA West,
Room B102, 1301 Constitution Ave.
NW., Washington, DC. The Public
Reading Room is open from 8:30 a.m. to
4:30 p.m., Monday through Friday,
excluding legal holidays. The telephone
number for the Public Reading Room is
(202) 566–1744, and the telephone
number for the Water Docket is (202)
566–2426.
FOR FURTHER INFORMATION CONTACT:
Maria Gomez-Taylor, Office of Science
and Technology, Office of Water (4303–
T), Environmental Protection Agency,
1200 Pennsylvania Avenue NW;
Washington, DC 20460; telephone
number: (202) 566–1005; fax number:
(202) 566–1053; email address: Gomeztaylor.maria@epa.gov.
SUPPLEMENTARY INFORMATION:
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I. General Information
A. Does this action apply to me?
EPA Regions, as well as States,
Territories and Tribes authorized to
implement the National Pollutant
Discharge Elimination System (NPDES)
program, issue permits with conditions
designed to ensure compliance with the
technology-based and water qualitybased requirements of the Clean Water
Act (CWA). These permits may include
restrictions on the quantity of pollutants
that may be discharged as well as
pollutant measurement and reporting
requirements. If EPA has approved a test
procedure for analysis of a specific
pollutant, the NPDES permittee must
use an approved test procedure (or an
approved alternate test procedure) for
the specific pollutant when measuring
the required waste constituent.
Similarly, if EPA has established
sampling requirements, measurements
taken under an NPDES permit must
comply with these requirements.
Therefore, entities with NPDES permits
will potentially be affected by the
actions in this rulemaking. Categories
and entities that may potentially be
affected by the requirements of today’s
rule include:
Category
Examples of potentially affected entities
State, Territorial, and Indian Tribal Governments.
States, Territories, and Tribes authorized to administer the NPDES permitting program; States,
Territories, and Tribes providing certification under Clean Water Act section 401;
State, Territorial, and Indian Tribal owned facilities that must conduct monitoring to comply
with NPDES permits.
Facilities that must conduct monitoring to comply with NPDES permits.
POTWs or other municipality owned facilities that must conduct monitoring to comply with
NPDES permits.
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Industry ...............................................................
Municipalities ......................................................
This table is not intended to be
exhaustive, but rather provides a guide
for readers regarding entities likely to be
affected by this action. This table lists
types of entities that EPA is now aware
of that could potentially be affected by
this action. Other types of entities not
listed in the table could also be affected.
To determine whether your facility is
affected by this action, you should
carefully examine the applicability
language at 40 CFR 122.1 (NPDES
purpose and scope), 40 CFR 136.1
(NPDES permits and CWA) and 40 CFR
403.1 (Pretreatment standards purpose
and applicability). If you have questions
regarding the applicability of this action
to a particular entity, consult the
appropriate person listed in the
preceding FOR FURTHER INFORMATION
CONTACT section.
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B. What should I consider as I prepare
my comments for EPA?
1. Submitting CBI. Do not submit this
information to EPA through https://
www.regulations.gov or email. Clearly
mark the part or all of the information
that you claim to be CBI. For CBI
information in a disk or CD ROM that
you mail to EPA, mark the outside of the
disk or CD ROM as CBI and then
identify electronically within the disk or
CD ROM the specific information that is
claimed as CBI. In addition to one
complete version of the comment that
includes information claimed as CBI, a
copy of the comment that does not
contain the information claimed as CBI
must be submitted for inclusion in the
public docket. Information so marked
will not be disclosed except in
accordance with procedures set forth in
40 CFR part 2.
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2. Tips for Preparing Your Comments.
When submitting comments, remember
to:
• Identify the rulemaking by docket
number and other identifying
information (subject heading, Federal
Register date and page number).
• Follow directions—The agency may
ask you to respond to specific questions
or organize comments by referencing a
Code of Federal Regulations (CFR) part
or section number.
• Explain why you agree or disagree;
suggest alternatives and substitute
language for your requested changes.
• Describe any assumptions and
provide any technical information and/
or data that you used.
• If you estimate potential costs or
burdens, explain how you arrived at
your estimate in sufficient detail to
allow for it to be reproduced.
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• Provide specific examples to
illustrate your concerns, and suggest
alternatives.
• Explain your views as clearly as
possible, avoiding the use of profanity
or personal threats.
• Make sure to submit your
comments by the comment period
deadline identified.
II. Summary of New Information and
Request for Comment
A. Background on Proposed Rule
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On September 23, 2010, EPA
proposed to add new and revised EPA
methods to its Part 136 test procedures
(75 FR 58024). The regulated
community and laboratories use these
approved methods for determining
compliance with National Pollutant
Discharge Elimination System (NPDES)
permits or other monitoring
requirements under the Clean Water Act
(CWA). EPA periodically updates the
list of approved methods to reflect
advances in technology and provide
entities more choices of approved
compliance monitoring methods.
Among other methods, in the September
2010 proposal, EPA proposed to add
two oil and grease methods published
by the Standard Methods Committee
that use the same solvent as the existing
Part 136 oil and grease methods. In the
Notice, EPA also described three oil and
grease methods published by ASTM
International or the Standard Methods
Committee that require a different
extractant and/or a different
measurement (i.e., determinative)
technique than the existing Part 136 oil
and grease methods. As explained in the
Notice, oil and grease is a methoddefined parameter. That is, the
measurements obtained by the method
are a specific artifact of the method and
defined solely by the elements (solvent,
determinative technique) used to
measure the analyte. Because these
three methods use a different extractant
and/or a different determinative
technique, how to translate
measurements using these methods to
those obtained under existing methods
for purposes of comparison was not
clear. Consequently, consistent with
past practices, EPA did not propose to
include these methods in Part 136.
B. Method-Defined Analytes
A method-defined analyte includes
certain parameters where the
measurement results obtained are solely
dependent on the method used. As a
consequence, the results obtained are
not directly comparable to results
obtained by another method (i.e., the
data derived from method-defined
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protocols cannot be reliably verified
outside the method itself). EPA has
defined a method-defined analyte in 40
CFR 136.6(a)(5) as ‘‘.* * * an analyte
defined solely by the method used to
determine the analyte. Such an analyte
may be a physical parameter, a
parameter that is not a specific
chemical, or a parameter that may be
comprised of a number of substances.
Examples of such analytes include
temperature, oil and grease, total
suspended solids, total phenolics,
turbidity, chemical oxygen demand, and
biochemical oxygen demand.’’
C. Oil and Grease
Unlike many parameters, oil and
grease is not a unique chemical entity,
but is a mixture of chemical species that
varies from source to source. Common
substances that may contribute to oil
and grease include petroleum based
compounds such as fuels, motor oil,
lubricating oil, soaps, waxes, and
hydraulic oil and vegetable based
compounds such as cooking oil and
other fats. Oil and grease is defined by
the method used to measure it (i.e., a
method-defined analyte). The CWA
defines oil and grease as a conventional
parameter and hundreds of thousands of
NPDES permits and indirect discharging
permits contain oil and grease
numerical limits. Currently, Part 136
lists three references to analytical
methods for the measurement of oil in
grease in such discharge permits.
Overwhelmingly, the vast majority of
discharges use EPA Method 1664A to
measure compliance with such
discharge limits. Method 1664A is a
liquid/liquid extraction (LLE),
gravimetric procedure that employs
normal hexane (n-hexane) as the
extraction solvent. This method also
allows the use of solid-phase extraction
(SPE) provided that the results obtained
by SPE are equivalent to the results
obtained by LLE.
D. Public Comments Related to Oil and
Grease
In response to the September 2010
proposal, EPA received several
comments recommending that EPA
approve recent methods that include
new technologies, including alternative
methods for oil and grease. One
commenter stated that EPA’s reasoning
for not approving alternative test
methods for oil and grease is
contradictory to the Agency’s
‘‘Summary’’ statement that these
regulations will ‘‘provide increased
flexibility to the regulated community
and laboratories in their selection of
analytical methods (test procedures) for
use in Clean Water Act programs.’’ This
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commenter added that approving the
new technologies would be more
consistent with EPA’s mission and
purpose to ‘‘ensure that all Americans
are protected from significant risks to
human health and the environment
where they live, learn and work.’’
Another commenter indicated that
EPA should approve new technologies
for oil and grease because n-hexane is a
dangerous solvent. This commenter
cited literature that describes n-hexane’s
toxicity to humans and to the
environment. Still another commenter
stated that fats, oils and greases are not
exclusively ‘‘hexane extractable’’
compounds and claimed that other
technologies and methods may be better
at measuring these compounds, and
may be used to better quantify how
much fat, oil or grease is toxic to aquatic
life or interferes with wastewater
treatment. This commenter also stated
that EPA should not specifically and
uniquely endorse a solvent-specific
method for ‘‘oil and grease’’ and
requested that EPA reverse its decision
that only n-hexane extractable oil and
grease methods are acceptable.
III. ASTM Method D7575–10 for Oil
and Grease
Some of the comments focused
exclusively on one particular oil and
grease method EPA discussed in its
proposal, ASTM D7575–10. Unlike EPA
Method 1664A which uses n-hexane as
the extractant and gravimetry for the
measurement of the extracted materials,
ASTM D7575–10 uses an extracting
membrane followed by infrared
measurement of the sample materials
that can be retained on the membrane.
This method was originally developed
by Orono Spectral Solutions (OSS), and
approved by ASTM on January 1, 2010
(Standard Test Method for Solvent-Free
Membrane Recoverable Oil and Grease
by Infrared Determination, ASTM
D7575–10). Certain commenters to
EPA’s September 2010 proposal,
including ASTM and OSS, requested
that EPA re-consider ASTM D7575–10
for the measurement of oil and grease
under Clean Water Act programs. In
particular, they cited that ASTM
D7575–10 is solvent free and provides
reliable and comparable results to EPA
Method 1664A. As part of this reconsideration, these commenters
submitted additional information on the
health hazards associated with hexane
as well as additional single laboratory
comparability data between Method
1664A and ASTM D7575–10 and on
additional matrices tested after the
initial comparability study and
associated statistical analysis. These
data, EPA’s analyses of these data, and
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communications related to the
alternative ASTM method between EPA,
OSS and ASTM are included as part of
the record for today’s notice.
EPA’s consideration of ASTM D7575–
10 is entirely novel. Because oil and
grease is a method-defined parameter,
with one exception, EPA has not
considered promulgating multiple
methods to measure oil and grease that
are based on different extractants.
Moreover, EPA has not considered
multiple oil and grease methods that are
based on different determinative
techniques. The only exception to this
was EPA’s promulgation of EPA Method
1664A in 1999 to replace Method 413.1,
a similar procedure that used Freon®
(1,1, 2-trichloro-1,2,2-trifluoroethane
(CFC–113; Freon-113)) as the extraction
solvent. EPA made this exception
because Freon® was banned by an
international treaty, and until the ban
went into effect, EPA allowed either of
these oil and grease methods for CWA
compliance. In both methods, the
determinative technique is gravimetry
and the only change was the extraction
solvent (n-hexane instead of Freon®).
EPA is persuaded by commenters to
its September 23, 2010 Notice that it
should re-consider its position on
ASTM D7575–10. Such a consideration
represents a new path for EPA. As is
always the case, EPA is proceeding
carefully, with a particular focus on the
underlying data. EPA’s consideration is
specific to ASTM D7575–10 and should
not be interpreted broadly to other oil
and grease methods that use different
extractants and/or determinative
techniques, or more generally to other
method-defined analytes. If EPA
receives similar requests for other
methods, it will evaluate each one
individually.
Although the September 2010
proposal discussed the current use of
EPA Method 1664A as a required testing
method to determine the eligibility of
materials for certain conditional
exclusions for RCRA regulations under
40 CFR260.20 and 260.22 (i.e.,
delistings), and additionally proposed to
allow the revised version of this testing
method (Method 1664, Rev. B) for future
delistings, EPA is not considering
ASTM D7575–10 for use under the
RCRA program. Until ASTM D7575–10
is validated for a full range of matrices
covered by the RCRA program, EPA
considers this new testing method to be
limited to the Clean Water Act program.
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A. Technical Considerations Related to
ASTM Method D7575–10
1. EPA Evaluation of This New Method
Based on the data and information
available in EPA’s record, EPA
concludes ASTM D7575–10 is a good
stand-alone method for the
measurement of oil and grease in
wastewater. The method was single- and
multi-lab tested following ASTM
Standard Practice D2777 (Standard
Practice for the Determination of
Precision and Bias of Applicable Test
methods of Committee D19 on Water)
and produces similar recoveries and
precision to EPA Method 1664A for
those matrices tested and in the range of
method applicability (5–200 mg/L).
In reviewing the method, EPA
requested that ASTM revise its new
standard to provide additional details
on the underlying procedural steps—
specifically in regard to sample
homogenization and calibration
verification—and to clarify the
applicability (or lack thereof) of the
method to non-wastewater matrices.
ASTM revised the method write-up
accordingly. See DCN xxx for additional
information.
2. Comparability of Results Between
ASTM D7575–10 and EPA Method
1664A
As explained above, with the
exception of EPA’s promulgation of
Method 1664A to replace Method 413.1,
EPA has not considered promulgating
multiple methods to measure oil and
grease that are based on different
extractants nor has EPA considered
promulgating oil and grease methods
with different determinative techniques.
As a result, EPA does not have a defined
‘‘process’’ for such considerations. For
non-method-defined parameters where
the analyte being measured is a single
compound (e.g., copper, benzene), EPA
often promulgates multiple methods
that may be based on different
determinative techniques for
nationwide use. In such cases, EPA has
a well-defined process for ensuring that
the performance of a proposed method
is acceptable (i.e., the proposed test
procedure must demonstrate an
improvement over current EPAapproved methods such as fewer matrix
interferences, and better sensitivity,
precision and recovery). For a new
candidate test method employing a
determinative technique that is different
from those techniques used in existing
approved methods, the applicant must
develop quality control (QC) acceptance
criteria based on the validation protocol
for nationwide use applications (9
laboratories, each analyzing a different
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matrix). The QC acceptance criteria for
the candidate method must then be
compared to the QC acceptance criteria
specifications for methods in Part 136
and the performance of the candidate
method must be as good or better than
that of an approved method. This
process is described in the ‘‘Protocol for
EPA Approval of New Methods for
Organic and Inorganic Analytes in
Wastewater and Drinking Water,’’
March 1999.
In contrast, there is no well-defined
process for the evaluation of a proposed
test method for method-defined
parameters. In addition to ensuring that
the performance of the proposed
method is acceptable as described above
for non-method-defined parameters,
EPA wants to ensure that results
produced by the proposed method are
comparable to results produced with the
approved method. When EPA
promulgated EPA Method 1664A to
replace EPA Method 413.1, a similar
procedure that used Freon® (1,1, 2trichloro-1,2,2-trifluoroethane (CFC–
113; Freon-113)) as the extraction
solvent, EPA evaluated a variety of
possible replacement extracting solvents
in addition to n-hexane. EPA selected nhexane and promulgated Method 1664A
after conducting extensive side-by-side
studies of several extracting solvents on
a variety of samples representing a wide
range of matrices (see ‘‘Preliminary
Report of EPA Efforts to Replace Freon
for the Determination of Oil and
Grease,’’ EPA–821–R–93–011,
September 1993, and Report of EPA
Efforts to Replace Freon for the
Determination of Oil and Grease and
Total Petroleum Hydrocarbons, EPA–
820–R–95003, April 1995). In
considering which solvent produced
results most comparable to results
obtained with Freon®, EPA conducted a
Root Mean Squared Deviation (RMSD)
evaluation of the data collected in the
side-by-side studies. None of the
alternative solvents produced results
statistically comparable to results
produced by Freon®. However, EPA
concluded at the time that n-hexane was
appropriate as an alternative solvent,
based on overall extraction results (96%
versus 100% for Freon) and analytical
practical considerations (e.g., boiling
point).
In considering ASTM D7575–10, EPA
reviewed the available single laboratory
comparability data between ASTM
D7575–10 and EPA Method 1664A.
Initially, these data included triplicate
analyses of samples from seven different
wastewater matrices (eight POTWs,
dairy, machine shop, gunsmith, auto
garage, auto salvage yard, and fish
processor). Later, OSS submitted
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additional data for three matrices (bilge
water, peanut processor, and lunchmeat
processor) that were collected after the
single laboratory study.1 EPA conducted
a Root Mean Squared Deviation (RMSD)
comparability assessment with these
data, following the methodology set
forth in ‘‘Analytical Method Guidance
for EPA Method 1664A Implementation
and Use (40 CFR part 136), EPA/821–R–
00–003, February 2000.’’ For this
assessment, EPA first used the original
data set and subsequently included the
additional data for three matrices and
determined the results were not
statistically comparable, with or without
the data for the additional matrices.
This outcome was not unexpected
because of the intrinsic differences in
the two methods and the nature of
method-defined parameters. Similarly,
when EPA performed an RMSD
comparability assessment before
promulgating EPA Method 1664A in
place of EPA Method 413.1, EPA did not
find the results to be statistically
comparable.2
As explained in Section II.B, the
comparability of results is a significant
issue with method-defined analytes
such as oil and grease because the
results depend on the method used. For
oil and grease, the amount of oil and
grease material extracted depends on
the solvent or membrane used for the
extraction of oil and grease. As such, it
may not be possible for results from
methods that use different extraction
techniques to be compared statistically.
For example, EPA Method 1664A
employs distillation at 85°C, and as
such, petroleum materials from gasoline
through #2 fuel oil and non-petroleum
materials including carboxylic and other
organic acids may be partially lost
during this solvent removal operation.
Similarly, some crude oils and heavy
fuel oils contain a significant percentage
of materials that are not soluble in the
n-hexane solvent of EPA Method 1664A
resulting in low recoveries for these
materials. ASTM D7575–10 has no such
solvent removal step which could
increase or decrease the amount of
petroleum and non-petroleum materials
1 OSS also submitted data for several other
matrices that EPA did not include in the analysis
because these data were based on only one sample
result per matrix and thus lacked the required
replicates for a statistical analysis. Additionally,
ASTM recently submitted triplicate data for three
other matrices. Because EPA received this data after
conducting its statistical analysis, this data is not
included in the RMSD assessment described in this
paragraph, but is included in the record for today’s
notice.
2 Note that in absence of statistical comparability,
EPA ultimately determined that EPA Method 1664A
could be used as a direct replacement for EPA
Method 413.1.
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measured by ASTM D7575–10 relative
to Method 1664A.
For the reason identified above, in the
case of ASTM D7575–10, EPA
concludes it is not appropriate to apply
the same statistical assessment as is
done for non-method-defined
parameters. As a result, EPA applied
similar comparison techniques as those
performed in replacing EPA Method
413.1 with EPA Method 1664A. As
mentioned above, during that
replacement analysis, n-hexane was
found to extract 96% of the oil and
grease that could be extracted by Freon.
This 4% difference was deemed
insignificant based on the variability of
oil and grease measurements (around
the order of 10% relative standard
deviation) and the confidence intervals
about the 96% extraction (plus or minus
20% extracted). When comparing the
results of ASTM D7575–10 to EPA
Method 1664A, the non-solvent method
removes an average of 99.6% of the oil
and grease that was removed by nhexane under the same conditions. The
variability of the situational
comparisons along with the 10%
relative standard deviation for oil and
grease measurements once again allow
us to conclude that the 0.4% difference
is not significant. Using this approach,
for the range of the ASTM D7575–10
applicability (5–200 mg/L), ASTM
D7575–10 could serve as a substitute for
Method 1664A in the same fashion as nhexane served as a replacement for
Freon.
B. Summary of EPA’s Reconsideration
of ASTM D7575–10
Based on the information presented in
today’s Notice, EPA is re-considering its
decision not to include ASTM D7575–
10 in 40 CFR Part 136 as an alternative
to EPA Method 1664A for measuring oil
and grease. EPA has three main reasons
for this reconsideration. First, EPA’s
analysis demonstrates ASTM D7575–10
is an acceptable stand-alone method for
the measurement of oil in grease in
wastewater for the applicable reporting
range (5–200 mg/L) and it produces
results that are generally very close to
those obtained using EPA Method
1664A for the matrices tested. Second,
this method has certain advantages over
the currently approved method. EPA
supports pollution prevention, and is
particularly persuaded by the
substantial advantages associated with
the green aspects of this membrane
technology (e.g., it uses a solventless
extraction, there is no solvent waste,
and no analyst exposure to solvent).
Finally, ASTM D7575–10 may offer
other advantages such as ease of
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analysis, reduced analysis time, and
lower analytical costs.
C. Implementation Considerations
Related to Multiple Oil and Grease
Methods
EPA recognizes that if it promulgates
ASTM D7575–10 in 40 CFR Part 136 as
an alternative to EPA method 1664A,
permittees and control authorities may
still have concerns related to the results
obtained from ASTM D7575–10 relative
to EPA Method 1664A, particularly for
matrices not evaluated to date. While
EPA has determined that the results of
the two methods are comparable over
the applicable range where the two
methods overlap (5–200 mg/L), because
of the wide variety and type of
individual compounds that may be
measured by oil and grease and because
oil and grease are extensively
incorporated in permits covering a wide
variety of wastewater matrices,
permittees or control authorities may
continue to have compliance concerns
(i.e., a permittee could be in or out of
compliance) simply due to a change in
the test method used to evaluate
samples.
When EPA promulgated EPA Method
1664A to replace EPA Method 413.1,
EPA and other stakeholders had similar
concerns. These concerns were
magnified because Method 1664A was a
replacement, rather than an alternative,
to the existing method at that time. To
accommodate concerns about
differences in results, EPA allowed
permitting authorities to establish a
conversion factor by having the
discharger perform a side-by-side
comparison of Method 1664 and the
Freon® extraction method and then
adjusting the discharge limits, if
necessary, to account for differences in
the permit. EPA further recommended a
specific process to follow for the sideby-side comparison in the guidance
document mentioned earlier [Analytical
Method Guidance for EPA Method
1664A Implementation and Use (40 CFR
part 136), EPA/821–R–00–003, February
2000].
In contrast to EPA’s replacement of
Freon with n-hexane, if EPA were to
promulgate ASTM D7575–10, it would
not lead to any requirement on permit
holders. In this case, unless ASTM
D7575–10 is specified in the permit,
promulgating ASTM D7575–10 would
simply provide additional flexibility to
permit holders in analyzing for oil and
grease. Because this would be optional
and because of the burden that would be
placed on the permitting authorities in
reviewing side-by-side data, EPA is not
currently persuaded that it should
include a provision providing the same
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Federal Register / Vol. 76, No. 240 / Wednesday, December 14, 2011 / Proposed Rules
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ability to adjust discharge limits based
on side-by side-comparison of EPA
Method 1664A to ASTM D7575–10 as it
did when it replaced Freon with nhexane. However, to the extent that
permittees would elect to use ASTM
D7575–10 and permitting authorities
would accept the use of ASTM D–7575–
10 rather than EPA Method 1664A,
nothing would prevent them from
conducting a side-by-side comparison of
the two methods. EPA would
recommend such a side-by-side
comparison if permittees and/or
permitting authorities have concerns
about a specific matrix, particularly
when the measured oil and grease
values when switching to ASTM
D7575–10 are more than 20% lower
from values routinely measured by EPA
Method 1664A (the 20% variability
around oil and grease measurements is
discussed in section III.A.2 of today’s
Notice).
IV. Request for Comments
Based on the new information and
EPA’s analysis of this information as
described in this Notice, EPA is
reconsidering whether to promulgate
ASTM D7575–10 in 40 CFR Part 136 as
an alternative method for oil and grease
where the applicable ranges overlap (5–
200 mg/L) and requests public
comments on this reconsideration, the
supporting data, and the resulting
analysis. While ASTM D7575–10 has
significant pollution prevention
advantages over the currently approved
method, EPA recognizes the potential
impact that this new method could have
on the hundreds of thousands of oil and
grease determinations in regulatory
Clean Water Act programs and desires
to obtain additional input from
stakeholders. Specifically, EPA requests
comments on the following:
1. Whether EPA should reconsider
promulgating this additional method for
oil and grease based on different
extractants and determinative
techniques than EPA Method 1664A.
2. EPA’s current view, based on the
data it has reviewed to date, that ASTM
D7575–10 is an acceptable choice for
the determination of oil and grease for
the range (5 to 200 mg/L) evaluated.
3. EPA’s current conclusion that
permit limit adjustment based on sideby-side comparisons of EPA Method
1664A and ASTM D7575–10 is not
appropriate. EPA is particularly
interested in obtaining comments from
permitting authorities on this issue and
estimates of the burden associated with
reviewing such requests.
4. If EPA were to allow a side-by-side
comparison with limit adjustment as
necessary, should EPA look to the
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approach used for n-hexane in place of
Freon (see section III.C above) or should
EPA consider a different approach?
V. Referenced New Docket Materials
1. January 16, 2009 Memorandum from
Richard Reding on Modifications to
Method 1664A.
2. May 14, 1999 Federal Register (64 FR
26315).
3. Preliminary Report of EPA Efforts to
Replace Freon for the Determination of
Oil and Grease, EPA–821–R–93–011,
September 1993.
4. Report of EPA Efforts to Replace Freon for
the Determination of Oil and Grease and
Total Petroleum Hydrocarbons: Phase II,
EPA–820–R–95–003, April 1995.
5. October 15, 2010 email from Tyler Martin
containing the following data files:
a. Multi-Lab Validation Raw Data
b. Expanded ASTM D7575 Validation
Report
c. Single-Lab Validation Raw Data
d. Comparability Analysis from Single-Lab
Validation Results
6. October 19, 2010 email from Tyler Martin
containing additional comparability data
between Method 1664 and ASTM D7575.
7. October 21, 2010 email from Tyler Martin
with clarification on data submitted.
8. June 28, 2011 letter from James A. Thomas,
ASTM President to Mary Smith, EPA,
with ASTM International D19 Water
Response to US EPA Questions
Concerning ASTM Standard D7575.
9. Analytical Method Guidance for EPA
Method 1664A Implementation and Use
(40 CFR part 136), EPA/821–R–00–003,
February 2000.
10. Protocol for EPA Approval of New
Methods for Organic and Inorganic
Analytes in Wastewater and Drinking
Water, March 1999.
11. Study Report from the Testing of
Additional Industrial Wastewater
Matrices in Support of ASTM D7575 for
USEPA’s Reconsideration of this Method
in the Forthcoming Method Update Rule,
November 2011.
Dated: December 2, 2011.
Nancy K. Stoner,
Acting Assistant Administrator for Water.
[FR Doc. 2011–32063 Filed 12–13–11; 8:45 am]
BILLING CODE 6560–50–P
FEDERAL COMMUNICATIONS
COMMISSION
47 CFR Part 20
[WT Docket No. 07–250; DA 11–1707]
Amendment of the Commission’s
Rules Governing Hearing AidCompatible Mobile Handsets
Federal Communications
Commission.
ACTION: Proposed rule.
AGENCY:
In this document the
Commission seeks comment on
SUMMARY:
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77747
revisions to the Commission’s wireless
hearing aid compatibility rules. The
Commission’s rules define hearing aid
compatibility by reference to a third
party technical standard. Recently, a
new version of that technical standard
was developed to test the hearing aid
compatibility of the newest generation
of digital wireless handsets. The
proposed rules would adopt the revised
version of the technical standard into
the Commission’s rules.
DATES: Interested parties may file
comments on or before January 13,
2012, and reply comments on or before
January 30, 2012.
ADDRESSES: You may submit comments,
identified by WT Docket No. 07–250, by
any of the following methods:
• Federal eRulemaking Portal:
https://www.regulations.gov. Follow the
instructions for submitting comments.
• Federal Communications
Commission’s Web site: https://
www.fcc.gov/cgb/ecfs/. Follow the
instructions for submitting comments.
• Mail: Filings can be sent by hand or
messenger delivery, by commercial
overnight courier, or by first-class or
overnight U.S. Postal Service mail
(although the Commission continues to
experience delays in receiving U.S.
Postal Service mail). All filings must be
addressed to the Commission’s
Secretary, Office of the Secretary,
Federal Communications Commission.
• People with Disabilities: Contact the
FCC to request reasonable
accommodations (accessible format
documents, sign language interpreters,
CART, etc.) by email: FCC504@fcc.gov
or phone: (202) 418–0530 or TTY: (202)
418–0432.
For detailed instructions for
submitting comments and additional
information on the rulemaking process,
see the SUPPLEMENTARY INFORMATION
section of the document.
FOR FURTHER INFORMATION CONTACT:
Michael Rowan, Wireless
Telecommunications Bureau, (202) 418–
1883, email Michael.Rowan@fcc.gov, or
Saurbh Chhabra, Wireless
Telecommunications Bureau, (202) 418–
2266, email Saurbh.Chhabra@fcc.gov.
SUPPLEMENTARY INFORMATION: This is a
summary of the Commission’s Second
Further Notice of Proposed Rulemaking
(SFNPRM) in WT Docket No. 07–250,
adopted November 1, 2010, and released
on November 1, 2010. The full text of
the SFNPRM is available for public
inspection and copying during business
hours in the FCC Reference Information
Center, Portals II, 445 12th Street SW.,
Room CY–A257, Washington, DC 20554.
It also may be purchased from the
Commission’s duplicating contractor at
E:\FR\FM\14DEP1.SGM
14DEP1
Agencies
[Federal Register Volume 76, Number 240 (Wednesday, December 14, 2011)]
[Proposed Rules]
[Pages 77742-77747]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 2011-32063]
-----------------------------------------------------------------------
ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 136
[EPA-HQ-OW-2010-0192; FRL-9504-2]
Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the Clean Water Act; Analysis and Sampling Procedures;
Notice of Data Availability
AGENCY: Environmental Protection Agency (EPA).
ACTION: Notice of data availability.
-----------------------------------------------------------------------
SUMMARY: On September 23, 2010, EPA proposed to approve a number of new
and revised test procedures (i.e., analytical methods) for measuring
pollutants under the Clean Water Act. Today's notice announces the
availability of new data on an analytical method for the measurement of
oil and grease that EPA described in the earlier notice but did not
propose to approve it for use. This notice discusses how EPA is
considering revising its proposed regulatory requirements for this
method. EPA is soliciting comment only on EPA's consideration of this
method.
DATES: Comments must be received on or before February 13, 2012.
ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
2010-0192, by one of the following methods:
https://www.regulations.gov: Follow the on-line
instructions for submitting comments.
Email: OW-docket@epamail.epa.gov Attention Docket ID No.
OW-2010-0192.
Mail: Water Docket, Environmental Protection Agency,
Mailcode: 28221T, 1200 Pennsylvania Ave. NW., Washington, DC 20460.
Hand Delivery: EPA Water Center, EPA West Building, Room
B102, 1301 Constitution Avenue NW., Washington, DC, Attention Docket ID
No. OW-2010-0192. Such deliveries are only accepted during the Docket's
normal hours of operation, and special arrangements should be made for
deliveries of boxed information.
Instructions: Direct your comments to Docket ID No. EPA-HQ-OW-2010-
0192. EPA's policy is that all comments received will be included in
the public docket without change and may be made available online at
https://www.regulations.gov, including any personal information
provided, unless the comment includes information claimed to be
Confidential Business Information (CBI) or other information whose
disclosure is restricted by statute.
[[Page 77743]]
Do not submit information that you consider to be CBI or otherwise
protected through https://www.regulations.gov or email. The https://www.regulations.gov Web site is an ``anonymous access'' system, which
means EPA will not know your identity or contact information unless you
provide it in the body of your comment. If you send an email comment
directly to EPA without going through https://www.regulations.gov your
email address will be automatically captured and included as part of
the comment that is placed in the public docket and made available on
the Internet. If you submit an electronic comment, EPA recommends that
you include your name and other contact information in the body of your
comment and with any disk or CD-ROM you submit. If EPA cannot read your
comment due to technical difficulties and cannot contact you for
clarification, EPA may not be able to consider your comment. Electronic
files should avoid the use of special characters, any form of
encryption, and be free of any defects or viruses. For additional
information about EPA's public docket visit the EPA Docket Center
homepage at https://www.epa.gov/epahome/dockets.htm.
Docket: All documents in the docket are listed in the https://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, will be publicly available only in hard copy.
Publicly available docket materials are available either electronically
in https://www.regulations.gov or in hard copy at the Water Docket, EPA/
DC, EPA West, Room B102, 1301 Constitution Ave. NW., Washington, DC.
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal holidays. The telephone number for the
Public Reading Room is (202) 566-1744, and the telephone number for the
Water Docket is (202) 566-2426.
FOR FURTHER INFORMATION CONTACT: Maria Gomez-Taylor, Office of Science
and Technology, Office of Water (4303-T), Environmental Protection
Agency, 1200 Pennsylvania Avenue NW; Washington, DC 20460; telephone
number: (202) 566-1005; fax number: (202) 566-1053; email address:
Gomez-taylor.maria@epa.gov.
SUPPLEMENTARY INFORMATION:
I. General Information
A. Does this action apply to me?
EPA Regions, as well as States, Territories and Tribes authorized
to implement the National Pollutant Discharge Elimination System
(NPDES) program, issue permits with conditions designed to ensure
compliance with the technology-based and water quality-based
requirements of the Clean Water Act (CWA). These permits may include
restrictions on the quantity of pollutants that may be discharged as
well as pollutant measurement and reporting requirements. If EPA has
approved a test procedure for analysis of a specific pollutant, the
NPDES permittee must use an approved test procedure (or an approved
alternate test procedure) for the specific pollutant when measuring the
required waste constituent. Similarly, if EPA has established sampling
requirements, measurements taken under an NPDES permit must comply with
these requirements. Therefore, entities with NPDES permits will
potentially be affected by the actions in this rulemaking. Categories
and entities that may potentially be affected by the requirements of
today's rule include:
------------------------------------------------------------------------
Category Examples of potentially affected entities
------------------------------------------------------------------------
State, Territorial, and States, Territories, and Tribes
Indian Tribal Governments. authorized to administer the NPDES
permitting program; States, Territories,
and Tribes providing certification under
Clean Water Act section 401;
State, Territorial, and Indian Tribal
owned facilities that must conduct
monitoring to comply with NPDES permits.
Industry..................... Facilities that must conduct monitoring
to comply with NPDES permits.
Municipalities............... POTWs or other municipality owned
facilities that must conduct monitoring
to comply with NPDES permits.
------------------------------------------------------------------------
This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be affected by this
action. This table lists types of entities that EPA is now aware of
that could potentially be affected by this action. Other types of
entities not listed in the table could also be affected. To determine
whether your facility is affected by this action, you should carefully
examine the applicability language at 40 CFR 122.1 (NPDES purpose and
scope), 40 CFR 136.1 (NPDES permits and CWA) and 40 CFR 403.1
(Pretreatment standards purpose and applicability). If you have
questions regarding the applicability of this action to a particular
entity, consult the appropriate person listed in the preceding FOR
FURTHER INFORMATION CONTACT section.
B. What should I consider as I prepare my comments for EPA?
1. Submitting CBI. Do not submit this information to EPA through
https://www.regulations.gov or email. Clearly mark the part or all of
the information that you claim to be CBI. For CBI information in a disk
or CD ROM that you mail to EPA, mark the outside of the disk or CD ROM
as CBI and then identify electronically within the disk or CD ROM the
specific information that is claimed as CBI. In addition to one
complete version of the comment that includes information claimed as
CBI, a copy of the comment that does not contain the information
claimed as CBI must be submitted for inclusion in the public docket.
Information so marked will not be disclosed except in accordance with
procedures set forth in 40 CFR part 2.
2. Tips for Preparing Your Comments. When submitting comments,
remember to:
Identify the rulemaking by docket number and other
identifying information (subject heading, Federal Register date and
page number).
Follow directions--The agency may ask you to respond to
specific questions or organize comments by referencing a Code of
Federal Regulations (CFR) part or section number.
Explain why you agree or disagree; suggest alternatives
and substitute language for your requested changes.
Describe any assumptions and provide any technical
information and/or data that you used.
If you estimate potential costs or burdens, explain how
you arrived at your estimate in sufficient detail to allow for it to be
reproduced.
[[Page 77744]]
Provide specific examples to illustrate your concerns, and
suggest alternatives.
Explain your views as clearly as possible, avoiding the
use of profanity or personal threats.
Make sure to submit your comments by the comment period
deadline identified.
II. Summary of New Information and Request for Comment
A. Background on Proposed Rule
On September 23, 2010, EPA proposed to add new and revised EPA
methods to its Part 136 test procedures (75 FR 58024). The regulated
community and laboratories use these approved methods for determining
compliance with National Pollutant Discharge Elimination System (NPDES)
permits or other monitoring requirements under the Clean Water Act
(CWA). EPA periodically updates the list of approved methods to reflect
advances in technology and provide entities more choices of approved
compliance monitoring methods. Among other methods, in the September
2010 proposal, EPA proposed to add two oil and grease methods published
by the Standard Methods Committee that use the same solvent as the
existing Part 136 oil and grease methods. In the Notice, EPA also
described three oil and grease methods published by ASTM International
or the Standard Methods Committee that require a different extractant
and/or a different measurement (i.e., determinative) technique than the
existing Part 136 oil and grease methods. As explained in the Notice,
oil and grease is a method-defined parameter. That is, the measurements
obtained by the method are a specific artifact of the method and
defined solely by the elements (solvent, determinative technique) used
to measure the analyte. Because these three methods use a different
extractant and/or a different determinative technique, how to translate
measurements using these methods to those obtained under existing
methods for purposes of comparison was not clear. Consequently,
consistent with past practices, EPA did not propose to include these
methods in Part 136.
B. Method-Defined Analytes
A method-defined analyte includes certain parameters where the
measurement results obtained are solely dependent on the method used.
As a consequence, the results obtained are not directly comparable to
results obtained by another method (i.e., the data derived from method-
defined protocols cannot be reliably verified outside the method
itself). EPA has defined a method-defined analyte in 40 CFR 136.6(a)(5)
as ``.* * * an analyte defined solely by the method used to determine
the analyte. Such an analyte may be a physical parameter, a parameter
that is not a specific chemical, or a parameter that may be comprised
of a number of substances. Examples of such analytes include
temperature, oil and grease, total suspended solids, total phenolics,
turbidity, chemical oxygen demand, and biochemical oxygen demand.''
C. Oil and Grease
Unlike many parameters, oil and grease is not a unique chemical
entity, but is a mixture of chemical species that varies from source to
source. Common substances that may contribute to oil and grease include
petroleum based compounds such as fuels, motor oil, lubricating oil,
soaps, waxes, and hydraulic oil and vegetable based compounds such as
cooking oil and other fats. Oil and grease is defined by the method
used to measure it (i.e., a method-defined analyte). The CWA defines
oil and grease as a conventional parameter and hundreds of thousands of
NPDES permits and indirect discharging permits contain oil and grease
numerical limits. Currently, Part 136 lists three references to
analytical methods for the measurement of oil in grease in such
discharge permits. Overwhelmingly, the vast majority of discharges use
EPA Method 1664A to measure compliance with such discharge limits.
Method 1664A is a liquid/liquid extraction (LLE), gravimetric procedure
that employs normal hexane (n-hexane) as the extraction solvent. This
method also allows the use of solid-phase extraction (SPE) provided
that the results obtained by SPE are equivalent to the results obtained
by LLE.
D. Public Comments Related to Oil and Grease
In response to the September 2010 proposal, EPA received several
comments recommending that EPA approve recent methods that include new
technologies, including alternative methods for oil and grease. One
commenter stated that EPA's reasoning for not approving alternative
test methods for oil and grease is contradictory to the Agency's
``Summary'' statement that these regulations will ``provide increased
flexibility to the regulated community and laboratories in their
selection of analytical methods (test procedures) for use in Clean
Water Act programs.'' This commenter added that approving the new
technologies would be more consistent with EPA's mission and purpose to
``ensure that all Americans are protected from significant risks to
human health and the environment where they live, learn and work.''
Another commenter indicated that EPA should approve new
technologies for oil and grease because n-hexane is a dangerous
solvent. This commenter cited literature that describes n-hexane's
toxicity to humans and to the environment. Still another commenter
stated that fats, oils and greases are not exclusively ``hexane
extractable'' compounds and claimed that other technologies and methods
may be better at measuring these compounds, and may be used to better
quantify how much fat, oil or grease is toxic to aquatic life or
interferes with wastewater treatment. This commenter also stated that
EPA should not specifically and uniquely endorse a solvent-specific
method for ``oil and grease'' and requested that EPA reverse its
decision that only n-hexane extractable oil and grease methods are
acceptable.
III. ASTM Method D7575-10 for Oil and Grease
Some of the comments focused exclusively on one particular oil and
grease method EPA discussed in its proposal, ASTM D7575-10. Unlike EPA
Method 1664A which uses n-hexane as the extractant and gravimetry for
the measurement of the extracted materials, ASTM D7575-10 uses an
extracting membrane followed by infrared measurement of the sample
materials that can be retained on the membrane. This method was
originally developed by Orono Spectral Solutions (OSS), and approved by
ASTM on January 1, 2010 (Standard Test Method for Solvent-Free Membrane
Recoverable Oil and Grease by Infrared Determination, ASTM D7575-10).
Certain commenters to EPA's September 2010 proposal, including ASTM and
OSS, requested that EPA re-consider ASTM D7575-10 for the measurement
of oil and grease under Clean Water Act programs. In particular, they
cited that ASTM D7575-10 is solvent free and provides reliable and
comparable results to EPA Method 1664A. As part of this re-
consideration, these commenters submitted additional information on the
health hazards associated with hexane as well as additional single
laboratory comparability data between Method 1664A and ASTM D7575-10
and on additional matrices tested after the initial comparability study
and associated statistical analysis. These data, EPA's analyses of
these data, and
[[Page 77745]]
communications related to the alternative ASTM method between EPA, OSS
and ASTM are included as part of the record for today's notice.
EPA's consideration of ASTM D7575-10 is entirely novel. Because oil
and grease is a method-defined parameter, with one exception, EPA has
not considered promulgating multiple methods to measure oil and grease
that are based on different extractants. Moreover, EPA has not
considered multiple oil and grease methods that are based on different
determinative techniques. The only exception to this was EPA's
promulgation of EPA Method 1664A in 1999 to replace Method 413.1, a
similar procedure that used Freon[supreg] (1,1, 2-trichloro-1,2,2-
trifluoroethane (CFC-113; Freon-113)) as the extraction solvent. EPA
made this exception because Freon[supreg] was banned by an
international treaty, and until the ban went into effect, EPA allowed
either of these oil and grease methods for CWA compliance. In both
methods, the determinative technique is gravimetry and the only change
was the extraction solvent (n-hexane instead of Freon[supreg]).
EPA is persuaded by commenters to its September 23, 2010 Notice
that it should re-consider its position on ASTM D7575-10. Such a
consideration represents a new path for EPA. As is always the case, EPA
is proceeding carefully, with a particular focus on the underlying
data. EPA's consideration is specific to ASTM D7575-10 and should not
be interpreted broadly to other oil and grease methods that use
different extractants and/or determinative techniques, or more
generally to other method-defined analytes. If EPA receives similar
requests for other methods, it will evaluate each one individually.
Although the September 2010 proposal discussed the current use of
EPA Method 1664A as a required testing method to determine the
eligibility of materials for certain conditional exclusions for RCRA
regulations under 40 CFR260.20 and 260.22 (i.e., delistings), and
additionally proposed to allow the revised version of this testing
method (Method 1664, Rev. B) for future delistings, EPA is not
considering ASTM D7575-10 for use under the RCRA program. Until ASTM
D7575-10 is validated for a full range of matrices covered by the RCRA
program, EPA considers this new testing method to be limited to the
Clean Water Act program.
A. Technical Considerations Related to ASTM Method D7575-10
1. EPA Evaluation of This New Method
Based on the data and information available in EPA's record, EPA
concludes ASTM D7575-10 is a good stand-alone method for the
measurement of oil and grease in wastewater. The method was single- and
multi-lab tested following ASTM Standard Practice D2777 (Standard
Practice for the Determination of Precision and Bias of Applicable Test
methods of Committee D19 on Water) and produces similar recoveries and
precision to EPA Method 1664A for those matrices tested and in the
range of method applicability (5-200 mg/L).
In reviewing the method, EPA requested that ASTM revise its new
standard to provide additional details on the underlying procedural
steps--specifically in regard to sample homogenization and calibration
verification--and to clarify the applicability (or lack thereof) of the
method to non-wastewater matrices. ASTM revised the method write-up
accordingly. See DCN xxx for additional information.
2. Comparability of Results Between ASTM D7575-10 and EPA Method 1664A
As explained above, with the exception of EPA's promulgation of
Method 1664A to replace Method 413.1, EPA has not considered
promulgating multiple methods to measure oil and grease that are based
on different extractants nor has EPA considered promulgating oil and
grease methods with different determinative techniques. As a result,
EPA does not have a defined ``process'' for such considerations. For
non-method-defined parameters where the analyte being measured is a
single compound (e.g., copper, benzene), EPA often promulgates multiple
methods that may be based on different determinative techniques for
nationwide use. In such cases, EPA has a well-defined process for
ensuring that the performance of a proposed method is acceptable (i.e.,
the proposed test procedure must demonstrate an improvement over
current EPA-approved methods such as fewer matrix interferences, and
better sensitivity, precision and recovery). For a new candidate test
method employing a determinative technique that is different from those
techniques used in existing approved methods, the applicant must
develop quality control (QC) acceptance criteria based on the
validation protocol for nationwide use applications (9 laboratories,
each analyzing a different matrix). The QC acceptance criteria for the
candidate method must then be compared to the QC acceptance criteria
specifications for methods in Part 136 and the performance of the
candidate method must be as good or better than that of an approved
method. This process is described in the ``Protocol for EPA Approval of
New Methods for Organic and Inorganic Analytes in Wastewater and
Drinking Water,'' March 1999.
In contrast, there is no well-defined process for the evaluation of
a proposed test method for method-defined parameters. In addition to
ensuring that the performance of the proposed method is acceptable as
described above for non-method-defined parameters, EPA wants to ensure
that results produced by the proposed method are comparable to results
produced with the approved method. When EPA promulgated EPA Method
1664A to replace EPA Method 413.1, a similar procedure that used
Freon[supreg] (1,1, 2-trichloro-1,2,2-trifluoroethane (CFC-113; Freon-
113)) as the extraction solvent, EPA evaluated a variety of possible
replacement extracting solvents in addition to n-hexane. EPA selected
n-hexane and promulgated Method 1664A after conducting extensive side-
by-side studies of several extracting solvents on a variety of samples
representing a wide range of matrices (see ``Preliminary Report of EPA
Efforts to Replace Freon for the Determination of Oil and Grease,''
EPA-821-R-93-011, September 1993, and Report of EPA Efforts to Replace
Freon for the Determination of Oil and Grease and Total Petroleum
Hydrocarbons, EPA-820-R-95003, April 1995). In considering which
solvent produced results most comparable to results obtained with
Freon[supreg], EPA conducted a Root Mean Squared Deviation (RMSD)
evaluation of the data collected in the side-by-side studies. None of
the alternative solvents produced results statistically comparable to
results produced by Freon[supreg]. However, EPA concluded at the time
that n-hexane was appropriate as an alternative solvent, based on
overall extraction results (96% versus 100% for Freon) and analytical
practical considerations (e.g., boiling point).
In considering ASTM D7575-10, EPA reviewed the available single
laboratory comparability data between ASTM D7575-10 and EPA Method
1664A. Initially, these data included triplicate analyses of samples
from seven different wastewater matrices (eight POTWs, dairy, machine
shop, gunsmith, auto garage, auto salvage yard, and fish processor).
Later, OSS submitted
[[Page 77746]]
additional data for three matrices (bilge water, peanut processor, and
lunchmeat processor) that were collected after the single laboratory
study.\1\ EPA conducted a Root Mean Squared Deviation (RMSD)
comparability assessment with these data, following the methodology set
forth in ``Analytical Method Guidance for EPA Method 1664A
Implementation and Use (40 CFR part 136), EPA/821-R-00-003, February
2000.'' For this assessment, EPA first used the original data set and
subsequently included the additional data for three matrices and
determined the results were not statistically comparable, with or
without the data for the additional matrices. This outcome was not
unexpected because of the intrinsic differences in the two methods and
the nature of method-defined parameters. Similarly, when EPA performed
an RMSD comparability assessment before promulgating EPA Method 1664A
in place of EPA Method 413.1, EPA did not find the results to be
statistically comparable.\2\
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\1\ OSS also submitted data for several other matrices that EPA
did not include in the analysis because these data were based on
only one sample result per matrix and thus lacked the required
replicates for a statistical analysis. Additionally, ASTM recently
submitted triplicate data for three other matrices. Because EPA
received this data after conducting its statistical analysis, this
data is not included in the RMSD assessment described in this
paragraph, but is included in the record for today's notice.
\2\ Note that in absence of statistical comparability, EPA
ultimately determined that EPA Method 1664A could be used as a
direct replacement for EPA Method 413.1.
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As explained in Section II.B, the comparability of results is a
significant issue with method-defined analytes such as oil and grease
because the results depend on the method used. For oil and grease, the
amount of oil and grease material extracted depends on the solvent or
membrane used for the extraction of oil and grease. As such, it may not
be possible for results from methods that use different extraction
techniques to be compared statistically. For example, EPA Method 1664A
employs distillation at 85[deg]C, and as such, petroleum materials from
gasoline through 2 fuel oil and non-petroleum materials
including carboxylic and other organic acids may be partially lost
during this solvent removal operation. Similarly, some crude oils and
heavy fuel oils contain a significant percentage of materials that are
not soluble in the n-hexane solvent of EPA Method 1664A resulting in
low recoveries for these materials. ASTM D7575-10 has no such solvent
removal step which could increase or decrease the amount of petroleum
and non-petroleum materials measured by ASTM D7575-10 relative to
Method 1664A.
For the reason identified above, in the case of ASTM D7575-10, EPA
concludes it is not appropriate to apply the same statistical
assessment as is done for non-method-defined parameters. As a result,
EPA applied similar comparison techniques as those performed in
replacing EPA Method 413.1 with EPA Method 1664A. As mentioned above,
during that replacement analysis, n-hexane was found to extract 96% of
the oil and grease that could be extracted by Freon. This 4% difference
was deemed insignificant based on the variability of oil and grease
measurements (around the order of 10% relative standard deviation) and
the confidence intervals about the 96% extraction (plus or minus 20%
extracted). When comparing the results of ASTM D7575-10 to EPA Method
1664A, the non-solvent method removes an average of 99.6% of the oil
and grease that was removed by n-hexane under the same conditions. The
variability of the situational comparisons along with the 10% relative
standard deviation for oil and grease measurements once again allow us
to conclude that the 0.4% difference is not significant. Using this
approach, for the range of the ASTM D7575-10 applicability (5-200 mg/
L), ASTM D7575-10 could serve as a substitute for Method 1664A in the
same fashion as n-hexane served as a replacement for Freon.
B. Summary of EPA's Reconsideration of ASTM D7575-10
Based on the information presented in today's Notice, EPA is re-
considering its decision not to include ASTM D7575-10 in 40 CFR Part
136 as an alternative to EPA Method 1664A for measuring oil and grease.
EPA has three main reasons for this reconsideration. First, EPA's
analysis demonstrates ASTM D7575-10 is an acceptable stand-alone method
for the measurement of oil in grease in wastewater for the applicable
reporting range (5-200 mg/L) and it produces results that are generally
very close to those obtained using EPA Method 1664A for the matrices
tested. Second, this method has certain advantages over the currently
approved method. EPA supports pollution prevention, and is particularly
persuaded by the substantial advantages associated with the green
aspects of this membrane technology (e.g., it uses a solventless
extraction, there is no solvent waste, and no analyst exposure to
solvent). Finally, ASTM D7575-10 may offer other advantages such as
ease of analysis, reduced analysis time, and lower analytical costs.
C. Implementation Considerations Related to Multiple Oil and Grease
Methods
EPA recognizes that if it promulgates ASTM D7575-10 in 40 CFR Part
136 as an alternative to EPA method 1664A, permittees and control
authorities may still have concerns related to the results obtained
from ASTM D7575-10 relative to EPA Method 1664A, particularly for
matrices not evaluated to date. While EPA has determined that the
results of the two methods are comparable over the applicable range
where the two methods overlap (5-200 mg/L), because of the wide variety
and type of individual compounds that may be measured by oil and grease
and because oil and grease are extensively incorporated in permits
covering a wide variety of wastewater matrices, permittees or control
authorities may continue to have compliance concerns (i.e., a permittee
could be in or out of compliance) simply due to a change in the test
method used to evaluate samples.
When EPA promulgated EPA Method 1664A to replace EPA Method 413.1,
EPA and other stakeholders had similar concerns. These concerns were
magnified because Method 1664A was a replacement, rather than an
alternative, to the existing method at that time. To accommodate
concerns about differences in results, EPA allowed permitting
authorities to establish a conversion factor by having the discharger
perform a side-by-side comparison of Method 1664 and the Freon[supreg]
extraction method and then adjusting the discharge limits, if
necessary, to account for differences in the permit. EPA further
recommended a specific process to follow for the side-by-side
comparison in the guidance document mentioned earlier [Analytical
Method Guidance for EPA Method 1664A Implementation and Use (40 CFR
part 136), EPA/821-R-00-003, February 2000].
In contrast to EPA's replacement of Freon with n-hexane, if EPA
were to promulgate ASTM D7575-10, it would not lead to any requirement
on permit holders. In this case, unless ASTM D7575-10 is specified in
the permit, promulgating ASTM D7575-10 would simply provide additional
flexibility to permit holders in analyzing for oil and grease. Because
this would be optional and because of the burden that would be placed
on the permitting authorities in reviewing side-by-side data, EPA is
not currently persuaded that it should include a provision providing
the same
[[Page 77747]]
ability to adjust discharge limits based on side-by side-comparison of
EPA Method 1664A to ASTM D7575-10 as it did when it replaced Freon with
n-hexane. However, to the extent that permittees would elect to use
ASTM D7575-10 and permitting authorities would accept the use of ASTM
D-7575-10 rather than EPA Method 1664A, nothing would prevent them from
conducting a side-by-side comparison of the two methods. EPA would
recommend such a side-by-side comparison if permittees and/or
permitting authorities have concerns about a specific matrix,
particularly when the measured oil and grease values when switching to
ASTM D7575-10 are more than 20% lower from values routinely measured by
EPA Method 1664A (the 20% variability around oil and grease
measurements is discussed in section III.A.2 of today's Notice).
IV. Request for Comments
Based on the new information and EPA's analysis of this information
as described in this Notice, EPA is reconsidering whether to promulgate
ASTM D7575-10 in 40 CFR Part 136 as an alternative method for oil and
grease where the applicable ranges overlap (5-200 mg/L) and requests
public comments on this reconsideration, the supporting data, and the
resulting analysis. While ASTM D7575-10 has significant pollution
prevention advantages over the currently approved method, EPA
recognizes the potential impact that this new method could have on the
hundreds of thousands of oil and grease determinations in regulatory
Clean Water Act programs and desires to obtain additional input from
stakeholders. Specifically, EPA requests comments on the following:
1. Whether EPA should reconsider promulgating this additional
method for oil and grease based on different extractants and
determinative techniques than EPA Method 1664A.
2. EPA's current view, based on the data it has reviewed to date,
that ASTM D7575-10 is an acceptable choice for the determination of oil
and grease for the range (5 to 200 mg/L) evaluated.
3. EPA's current conclusion that permit limit adjustment based on
side-by-side comparisons of EPA Method 1664A and ASTM D7575-10 is not
appropriate. EPA is particularly interested in obtaining comments from
permitting authorities on this issue and estimates of the burden
associated with reviewing such requests.
4. If EPA were to allow a side-by-side comparison with limit
adjustment as necessary, should EPA look to the approach used for n-
hexane in place of Freon (see section III.C above) or should EPA
consider a different approach?
V. Referenced New Docket Materials
1. January 16, 2009 Memorandum from Richard Reding on Modifications
to Method 1664A.
2. May 14, 1999 Federal Register (64 FR 26315).
3. Preliminary Report of EPA Efforts to Replace Freon for the
Determination of Oil and Grease, EPA-821-R-93-011, September 1993.
4. Report of EPA Efforts to Replace Freon for the Determination of
Oil and Grease and Total Petroleum Hydrocarbons: Phase II, EPA-820-
R-95-003, April 1995.
5. October 15, 2010 email from Tyler Martin containing the following
data files:
a. Multi-Lab Validation Raw Data
b. Expanded ASTM D7575 Validation Report
c. Single-Lab Validation Raw Data
d. Comparability Analysis from Single-Lab Validation Results
6. October 19, 2010 email from Tyler Martin containing additional
comparability data between Method 1664 and ASTM D7575.
7. October 21, 2010 email from Tyler Martin with clarification on
data submitted.
8. June 28, 2011 letter from James A. Thomas, ASTM President to Mary
Smith, EPA, with ASTM International D19 Water Response to US EPA
Questions Concerning ASTM Standard D7575.
9. Analytical Method Guidance for EPA Method 1664A Implementation
and Use (40 CFR part 136), EPA/821-R-00-003, February 2000.
10. Protocol for EPA Approval of New Methods for Organic and
Inorganic Analytes in Wastewater and Drinking Water, March 1999.
11. Study Report from the Testing of Additional Industrial
Wastewater Matrices in Support of ASTM D7575 for USEPA's
Reconsideration of this Method in the Forthcoming Method Update
Rule, November 2011.
Dated: December 2, 2011.
Nancy K. Stoner,
Acting Assistant Administrator for Water.
[FR Doc. 2011-32063 Filed 12-13-11; 8:45 am]
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