[Federal Register: September 23, 2010 (Volume 75, Number 184)]
[Proposed Rules]
[Page 58023-58076]
[DOCID:fr23se10-18]

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Part II

Environmental Protection Agency

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40 CFR Parts 136, 260, 423, et al.

Guidelines Establishing Test Procedures for the Analysis of Pollutants
Under the Clean Water Act; Analysis and Sampling Procedures; Proposed
Rule

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 136, 260, 423, 430, and 435

[EPA-HQ-OW-2010-0192; FRL-9189-4]
RIN 2040-AF09

Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the Clean Water Act; Analysis and Sampling Procedures

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: EPA is proposing changes to analysis and sampling test
procedures in wastewater regulations. These changes 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. The changes include proposal of EPA methods
and methods published by voluntary consensus standard bodies, such as
ASTM International and the Standard Methods Committee and updated
versions of currently approved methods. EPA is also proposing to add
certain methods reviewed under the alternate test procedures program.
Further, EPA is proposing changes to the current regulations to clarify
the process for EPA approval for use of alternate procedures for
nationwide and Regional use. In addition, EPA is proposing minimum
quality control requirements to improve consistency across method
versions; corrections to previously approved methods; and changes to
sample collection, preservation, and holding time requirements.
Finally, EPA is proposing changes to how EPA cites methods in three
effluent guideline regulations.

DATES: EPA must receive your comments on this proposal on or before
November 22, 2010.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-OW-
2010-0192, by one of the following methods:
     http://www.regulations.gov: Follow the on-line
instructions for submitting comments.
     E-mail<EMAIL_ADDRESS>Attention Docket ID No. EPA-HQ-
OW-2010-0192.
     Mail: Water Docket, U.S. Environmental Protection Agency,
Mailcode: 2822T, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
Attention Docket ID No. EPA-HQ-OW-2010-0192. Please include a total of
3 copies.
     Hand Delivery: Water Docket, EPA Docket Center, EPA West
Building Room 3334, 1301 Constitution Ave., NW., Washington, DC,
Attention Docket ID No. EPA-HQ-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 by
calling<PHONE_NUMBER>.
    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
http://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. Do not submit information that you
consider to be CBI or otherwise protected through http://
www.regulations.gov or e-mail. The http://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 e-mail comment directly to EPA without
going through http://www.regulations.gov your e-mail 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.
    Docket: All documents in the docket are listed in the http://
www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, will be publicly available only in hard copy.
Publicly available docket materials are available either electronically
in http://www.regulations.gov or in hard copy at the Water Docket in
the EPA Docket Center, EPA/DC, EPA West, Room 3334, 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<PHONE_NUMBER>, and the
telephone number for the Water Docket is<PHONE_NUMBER>.

FOR FURTHER INFORMATION CONTACT: Lemuel Walker, Engineering and
Analysis Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave., NW., Washington, DC 20460,<PHONE_NUMBER>, (e-mail:
walker.lemuel@epa.gov), or Meghan Hessenauer, Engineering and Analysis
Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave., NW., Washington, DC 20460,<PHONE_NUMBER> (e-mail:
hessenauer.meghan@epa.gov).

SUPPLEMENTARY INFORMATION:

A. General Information

1. Does this action apply to me?

    This proposed rule could affect a number of different entities.
Potential regulators may include EPA Regions, as well as States,
Territories and Tribes authorized to implement the National Pollutant
Discharge Elimination System (NPDES) program, and 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 permitee 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 regulated by the actions in this
rulemaking. Categories and entities that may potentially be subject to
the requirements of today's rule include:

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                                   Examples of potentially regulated
           Category                             entities
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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.
Industry.....................  Facilities that must conduct monitoring
                                to comply with NPDES permits.
Municipalities...............  POTWs that must conduct monitoring to
                                comply with NPDES permits.
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    This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be regulated by this
action. This table lists types of entities that EPA is now aware that
could potentially be regulated by this action. Other types of entities
not listed in the table could also be regulated. To determine whether
your facility is regulated by this action, you should carefully examine
the applicability language at 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 Confidential Business Information (CBI). Do not
submit this information to EPA through http://www.regulations.gov or e-
mail. 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.
     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.

C. Abbreviations and Acronyms Used in the Preamble and Proposed Rule
Text

ASTM: ASTM International
ATP: Alternate Test Procedure
CFR: Code of Federal Regulations
CWA: Clean Water Act
EPA: Environmental Protection Agency
FLAA: Flame Atomic Absorption Spectroscopy
HRGC: High Resolution Gas Chromatography
HRMS: High Resolution Mass Spectrometry
ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy
ICP/MS: Inductively Coupled Plasma-Mass Spectrometry
MS: Mass Spectrometry
NPDES: National Pollutant Discharge Elimination System
QA: Quality Assurance
QC: Quality Control
SDWA: Safe Drinking Water Act
SM: Standard Methods
STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption
Spectroscopy
USGS: United States Geological Survey
VCSB: Voluntary Consensus Standards Body
WET: Whole Effluent Toxicity

Table of Contents

I. Statutory Authority
II. Summary of Proposed Rule
    A. Changes to 40 CFR 136.3 To Include New EPA Methods and New
Versions of Previously Approved EPA Methods
    B. Changes to 40 CFR 136.3 To Include New Standard Methods and
New Versions of Approved Standard Methods
    C. Changes to 40 CFR 136.3 To Include New ASTM Methods or New
Versions of Previously Approved ASTM Methods
    D. Changes to 40 CFR 136.3 To Include Alternate Test Procedures
    E. Clarifications and Corrections to Previously Approved Methods
in 40 CFR 136.3
    F. Proposed Revisions in Table II at 40 CFR 136.3(e) to Required
Containers, Preservation Techniques, and Holding Times
    G. Proposed Revisions to 40 CFR 136.4 and 136.5
    H. Proposed Revisions to Method Modification Provisions at 40
CFR 136.6
    I. Proposed New Quality Assurance and Quality Control Language
at 40 CFR 136.7
    J. Proposed Withdrawal of Appendices at 40 CFR 136
    K. Proposed Revisions to 40 CFR 423
    L. Proposed Revisions to 40 CFR 430
    M. Proposed Revisions to 40 CFR 435
III. Statutory and Executive Order Reviews
    A. Executive Order 12866: Regulatory Planning and 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 That Significantly Affect
Energy Supply, Distribution, or Use
    I. National Technology Transfer and Advancement Act of 1995
    J. Executive Order 12898: Federal Actions To Address
Environmental Justice in Minority Populations and Low-Income
Populations
IV. References

I. Statutory Authority

    EPA is proposing today's rule pursuant to the authority of sections
301(a), 304(h), and 501(a) of the Clean Water Act (``CWA'' or the
``Act''), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of the
Act prohibits the discharge of any pollutant into navigable waters
unless the discharge complies with a National Pollutant Discharge
Elimination System (NPDES) permit issued under section 402 of the Act.
Section 304(h) of the Act requires the Administrator of the EPA to ``*
* * promulgate guidelines establishing test procedures for the analysis
of pollutants that shall include the factors which must be provided in
any certification pursuant to [section 401 of this Act] or permit
application pursuant to [section 402 of this Act].'' Section 501(a) of
the Act authorizes the Administrator to ``* * * prescribe such
regulations as are necessary to carry out this function under [the
Act].'' EPA generally has codified its test procedure regulations
(including analysis and sampling

requirements) for CWA programs at 40 CFR part 136, though some
requirements are codified in other Parts (e.g., 40 CFR chapter I,
subchapters N and O).

II. Summary of Proposed Rule

    EPA's regulations at 40 CFR part 136 identify test procedures that
must be used for the analysis of pollutants in all applications and
report under the CWA NPDES program as well as State certifications
pursuant to section 401 of the CWA. Included among the approved test
procedures are analytical methods developed by EPA as well as methods
developed by voluntary standards development organizations such as ASTM
International and by the joint efforts of the Standard Methods
Committee which is comprised of three technical societies (American
Public Health Association, American Water Works Association and the
Water Environment Federation) and produce Standard Methods for the
Examination of Water and Wastewater. EPA approves analytical methods
(test procedures) for measuring regulated pollutants in wastewater.
Regulated and regulatory entities use these approved methods for
determining compliance with NPDES permits or other monitoring
requirements. Often, these entities have a choice in deciding which
approved method they will use because EPA has approved the use of more
than one method. This rule proposes to add to this list of approved
methods. Associated with the proposed approved methods are their
regulated analytes (parameters) within the method. Some of these
proposed methods introduce new technologies to the NPDES program, while
others are updated versions of previously approved methods. These
additions will improve data quality and provide the regulated community
with greater flexibility. Further, EPA is aware that organizations
sometimes republish methods to correct errors or revise the
description. These changes do not affect the performance of the method.
Therefore, if there are changes for methods in this proposed rule
before publication of a final rule, EPA will include the updated
versions. In the tables at Section 136.3, EPA lists the parameters in
alphabetical order. To better identify new parameters proposed in this
rule EPA added some of these parameters, such as bisphenol A and
nonylphenol, at the end of these lists. In the final rule, EPA may
choose to reorder the listings to arrange all parameters
alphabetically.

A. Changes to 40 CFR 136.3 To Include New EPA Methods and New Versions
of Previously Approved EPA Methods

    EPA is proposing to add new EPA methods that require new
technologies to its Part 136 test procedures. EPA also is proposing new
versions of already approved EPA methods with technologies that have
been in use for many years. The new EPA methods and new versions of EPA
approved methods are described in the following paragraphs.
    1. EPA is proposing a new version of EPA Method 1664, 1664B: N-
Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel
Treated N-Hexane Extractable Material (SGT-HEM; Non-polar Material) by
Extraction and Gravimetry for use in CWA programs. In addition, EPA is
proposing to amend the RCRA regulations at 40 CFR 260.11, which
currently specify use of method 1664A, to additionally specify the
revised version, 1664B.
    Currently, Method 1664A is used as a required testing method to
determine eligibility of materials for certain conditional exclusions
from RCRA regulations under 40 CFR 260.20 and 260.22. These exclusions
are known as ``delistings.'' These delistings provide that certain
wastes generated at particular facilities are no longer classified as
hazardous wastes under RCRA. When delistings are granted by EPA, the
Agency describes them, along with applicable conditions, in appendix IX
to 40 CFR part 261.
    A number of delistings specify, among other things, the following
test method: ``Method 9070A (uses EPA Method 1664, Rev. A).'' This
testing method must be used by waste generators to determine if their
wastes are an oily waste for delisting purposes. The language used in
Appendix IX reads this way because Method 9070A in SW-846 (including on
the SW-846 Web site, http://www.epa.gov/epawaste/hazard/testmethods/
sw846/pdfs/9070a.pdf ) simply reads that Method 1664A is to be used.
Thus, although Method 9070A is cited, it is actually Method 1664A.
Method 9070A does not exist independently of Method 1664A.
    Once this rule becomes final, we would encourage future delistings,
if applicable, to cite the test method as ``Method 9070A (uses Method
EPA 1664, Rev. B).'' EPA is not proposing to amend delistings granted
in previous years that reference Method 1664A at this time, since it
would require additional review to assess the need for such a change
and an analysis of each delisting.
    Oil and Grease is a method-defined parameter that measures hexane
extractable material (HEM) using n-hexane (85% minimum purity, 99.0%
minimum saturated C6 isomer, residue < 1mg/L.) Before the use of
Freon[supreg] was banned, EPA defined oil and grease as Freon[supreg]-
extractable material. To replace Freon[supreg] for oil and grease
determinations (64 FR 26315, May 14, 1999) EPA conducted extensive
side-by-side studies of several extracting solvents on a variety of
samples to determine how the values compared to Freon[supreg]-
extractable material values.
    In today's proposed rule, EPA describes six oil and grease methods,
and proposes only the three methods in Table IB that use n-hexane to
extract the sample because the solvent-defined definition of oil and
grease measurements precludes use of any other extraction solvent or
extraction technique. Without extensive side-by-side testing, permit
writers, permitees, and data reviewers lack a basis for comparing HEM
permit limits or measurements to values obtained with other extraction
solvents or techniques. EPA lacks information about whether permit
writers or permitees would value having more ways to extract oil and
grease samples, or about how much effort they or others would be
willing to exert to determine if the alternate values were equal to HEM
values or convertible to HEM values by a conversion factor.
    Although solvents may not be changed, EPA has described some
allowable changes to the proposed EPA Method 1664B. This method
describes (1) modifications allowable for nationwide use without prior
EPA reviews (cf. documentation procedures described at 40 CFR 136.6),
and (2) describes modifications not allowable including the use of any
extraction solvent other than n-hexane or determination technique other
than gravimetry. Although Method 1664B allows use of alternate
extraction techniques, such as solid phase extraction (SPE) some
discharges or waste streams may not be amenable to SPE. For these
samples, 1664B should be applied as written. Conditioning of the solid-
phase disk or device with solvents other than n-hexane (e.g., alcohol,
acetone, etc) is allowed, only if this solvent(s) is completely removed
from the SPE disk or device prior to passing the sample through the SPE
disk or device.
    2. EPA is proposing to include in Table IB new EPA Method 200.5 and
clarifying that the axial orientation of the torch is allowed for use
with EPA Method 200.7. EPA Method 200.5 ``Determination of Trace
Elements in

Drinking Water by Axially Viewed Inductively Coupled Plasma--Atomic
Emission Spectrometry'' employs a plasma torch viewed in the axial
orientation to measure chemical elements (metals). It also includes
performance data for the axial configuration that is not in Method
200.7 because the axial technology torch results were not available
when Method 200.7 was developed. For some elements the axial
orientation results in greater sensitivity and lower detection limits
than the radial orientation. EPA now authorizes the use of Method 200.5
in testing under its Safe Drinking Water Act Program (73 FR 31616, June
6, 2008). Approval of Method 200.5 and the flexibility within Method
200.7 will allow laboratories to use either axial instruments or radial
instruments to measure metals in water samples.
    3. EPA is proposing to add EPA Method 525.2, an updated version of
EPA Method 525.1, in Table IG (Test Methods for Pesticide Active
Ingredients) as an additional approved method for all parameters for
which EPA has previously approved Method 525.1. Further, EPA is
soliciting comment on whether EPA should substitute Method 525.2 for
Method 525.1.
    EPA is proposing to include Pesticide Methods from Table IG in
Table ID (Test Procedures for Pesticides). Specifically, EPA is
proposing to add EPA Method 525.2 for the same pesticides for which EPA
has approved Method 525.1 in Table IG. Both methods use GC/MS
methodology.
    EPA is proposing to add some of the Pesticide Active Ingredients
methods in Table IG that have been in use for more than 10 years to
Table ID for general use. These methods are:
    a. EPA Method 608.1, ``The Determination of Organochloride
Pesticides in Municipal and Industrial Wastewater.'' This is a gas
chromatographic (GC) method used to determine certain organochlorine
pesticide compounds listed in industrial and municipal discharges. This
method measures chlorobenzilate, chloroneb, chloropropylate,
dibromochloropropane, etridiazole, PCNB, and propachlor.
    b. EPA Method 608.2, ``The Determination of Certain Organochlorine
Pesticides in Municipal and Industrial Wastewater.'' This is a GC
method used to determine certain organochlorine pesticides compounds in
industrial and municipal discharges. This method measures
chlorothalonil, DCPA, dichloran, methoxychlor, and permethrin.
    c. EPA Method 614, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' This is a GC
method used to determine organophosphorus compounds in industrial and
municipal discharges. This method measures azinphos methyl, demeton,
diazinon, disulfoton, ethion, malathion, parthion methyl, and parathion
ethyl.
    d. EPA Method 614.1, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' This is a GC
method used to determine organophosphorus compounds in industrial and
municipal discharges. This method measures dioxathion, EPN, ethion, and
terbufos.
    e. EPA Method 615, ``The Determination of Chlorinated Herbicides in
Municipal and Industrial Wastewater.'' This is a GC method used to
determine chlorinated herbicides compounds in industrial and municipal
discharges. This method measures 2,4-D, dalapon, 2,4-DB, dicamba,
dichlorprop, dinoseb, MCPA, MCPP, 2,4,5-T, and 2,4,5-TP.
    f. EPA Method 617, ``The Determination of Organohalide Pesticides
and PCBs in Municipal and Industrial Wastewater.'' This is a GC method
used to determine organohalide compounds in industrial and municipal
discharges. This method measures aldrin, [alpha]-BHC, [beta]-BHC,
[gamma]-BHC (lindane), captan, carbophenothion, chlordane, 4,4'-DDD,
4,4'-DDE, 4,4'-DDT, dichloran, dicofol, dieldrin, endosulfan I,
endosulfan II, endosulfan sulfate, endrin, endrin aldehyde, heptachlor,
heptachlor epoxide, isodrin, methoxychlor, mirex, PCNB, perthane,
strobane, toxaphene, trifluralin, PCB-1016, PCB-1221, PCB-1232, PCB-
1242, PCB-1248, PCB-1254, and PCB-1260.
    g. EPA Method 619, ``The Determination of Triazine Pesticides in
Municipal and Industrial Wastewater.'' This is a GC method used to
determine triazine pesticides compounds in industrial and municipal
discharges. This method measures ametryn, atraton, atrazine, prometon,
prometryn, propazine, sec-bumeton, simetryn, simazine, terbuthylazine,
terbutryn.
    h. EPA Method 622, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' This is a GC
method used to determine organophosphorus pesticides compounds in
industrial and municipal discharges. This method measures azinphos
methyl, bolstar, chlorpyrifos, chlorpyrifos methyl, coumaphos, demeton,
diazinon, dichlorvos, disulfoton, ethoprop, fensulfothion, fenthion,
merphos, mevinphos, naled, parathion methyl, phorate, ronnel, stirofos,
tokuthion, and trichloronate.
    i. EPA Method 622.1, ``The Determination of Thiophosphate
Pesticides in Municipal and Industrial Wastewater.'' This is a GC
method used to determine thiophosphate pesticides compounds in
municipal and industrial discharges. This method measures aspon,
dichlofenthion, famphur, fenitrothion, fonophos, phosmet, and
thionazin.
    j. EPA Method 632, ``The Determination of Carbamate and Urea
Pesticides in Municipal and Industrial Wastewater.'' This is a high-
performance liquid chromatographic (HPLC) method used to determine
carbamate and urea pesticide compounds in industrial and municipal
discharges. This method measures aminocarb, barban, carbaryl,
carbofuran, chlorpropham, diuron, fenuron, fenuron-TCA, fluometuron,
linuron, methiocarb, methomyl, mexacarbate, monuron, neburon, oxamyl,
propham, propoxur, siduron, swep.
    4. EPA is proposing to add in Table IC EPA Method 1614A,
``Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by
HRGC/HRMS.'' EPA developed this method to determine 49 polybrominated
diphenyl ether (PBDE) congeners in aqueous, solid, tissue, and multi-
phase matrices. These ethers are used in brominated flame retardants.
This method uses isotope dilution and internal standard high resolution
gas chromatography/high resolution mass spectrometry (HRGC/HRMS). This
method allows use of a temperature-programmed injector/vaporizer and a
short column to improve recoveries of the octa-, nona-, and
decabrominated diphenyl ethers.
    5. EPA is proposing to add in Table IC EPA Method 1668C,
``Chlorinated Biphenyl Congeners in Water, Soil, Sediment, Biosolids,
and Tissue by HRGC/HRMS.'' This method determines individual
chlorinated biphenyl congeners in environmental samples by isotope
dilution and internal standard high resolution gas chromatography/high
resolution mass spectrometry (HRGC/HRMS). Current Part 136 methods only
measure a mixture of congeners in seven Aroclors--PCB-1016, PCB-1221,
PCB-1232, PCB-1242, PCB-1248, PCB-1254, and PCB-1260. EPA Method 1668C
can measure the 209 individual PCB congeners in these mixtures. EPA
developed Method 1668 for use in wastewater, surface water, soil,
sediment, biosolids, and tissue matrices.
    EPA first published Method 1668 in 1999 and it is being used in
several environmental applications, including

NPDES permits. EPA based today's proposed version, 1668C, on the
results of an interlaboratory validation study (EPA 2010a, b), peer
reviews (EPA 2010c), and user experiences. In the development and
subsequent multi-laboratory validation of this method, EPA has
evaluated method performance characteristics, such as selectivity,
calibration, bias, precision, quantitation and detection limits. For
example, EPA has observed that detection limits and quantitation levels
are usually dependent on the level of interferences and laboratory
background levels rather than instrumental limitations. Thus, the
published minimum levels of quantitation are conservative estimates of
the concentrations at which a congener can be measured with laboratory
contamination present (EPA 2010d).
    EPA recognizes that the performance of this Method may vary among
the 209 congeners, and in different matrices. This is typical of multi-
analyte methods because not all chemicals respond identically to
extraction and clean up techniques, or have identical instrument
responses. In a study of data comparability between two laboratories on
samples collected from the Passaic River in New Jersey, in which 151
PCB congeners were identified and measured, accuracy as measured by
analysis of a NIST SRM was 15% or better. Recoveries of the PCB
congeners ranged from 90% to 124% and averaged 105%; precision ranged
from 4.2% to 23% (Passaic River 2010).
    This PCB method and the polybrominated diphenyl ether (PBDE) Method
1614A are performance-based methods. This means that users have the
flexibility to modify the method to adapt to the sometimes unique
characteristics of the user's sample. There is flexibility to modify
the sample preparation steps to remove substances that interfere with
measurement of the PCB congeners. A consequence of this flexibility is
that, after customizing a performance-based method for a specific
sample or application, the user should continue to use the same
customized procedures on these samples or applications to maintain data
comparability.
    EPA Method 1668C, the interlaboratory study report, and peer
reviews are in the docket for today's rule and on EPA's CWA methods Web
site at http://www.epa.gov/waterscience/methods. EPA lists Method 1668C
in Table IC as the parameter, ``PCBs 209 Congeners.''
    6. EPA is proposing to update in Table IH EPA Method 1622,
``Cryptosporidium in Water by Filtration/IMS/FA'' and EPA Method 1623,
``Cryptosporidium and Giardia in Water by Filtration/IMS/FA'' to
reflect changes made in the December 2005 versions of these methods.
EPA's drinking water program uses the 2005 versions of the methods. The
methods allow the flexibility to choose among several types of filters,
quality controls, and stains, as well as clarification on measuring
sample temperatures, quality control sample requirements and use of
quality control sample results, minimizing carry-over debris, analyst
verification procedures and sample condition criteria upon receipt.
This method substitution necessitates a change in the holding
temperature (Table II) for Cryptosporidium and Giardia from 0-8 [deg]C
to refrigerate between 1-10 [deg]C.
    7. EPA is proposing in Table IH revised versions of EPA Methods
1103.1, 1106.1, 1600 (also in Table IA), 1603, and 1680 to correct
technical errors. Specifically, for Methods 1103.1 and 1603, tryptone
broth should be tryptone water (section 12.4.3). In addition, in Tables
2 and 3, respectively, of these two methods, the positive control
organism for the cytochrome oxidase reagent has been changed to P.
aeruginosa from E. faecalis, and the negative control organism for
Simmons citrate agar has been changed to S. flexneri from E. coli for
more definitive results. In section 7.5.2 of Method 1603, the formula
for magnesium chloride hexahydrate should have a dot before the waters
rather than an alpha sign (MgCl2[middot]6H2O). In
Methods 1106.1 and 1600, in Tables 6 and 7, respectively, the true
spiked Enterococci ``T (CFU/100 mL)'' in the spiked sample based on the
lot mean valued provided by the manufacturer should be 32 instead of
11.2. In Method 1680, the lactose for Lauryl Tryptose Broth (LTB)
should be 5.0 g, not 25.0 g (section 7.6.1), and the dipotassium
hydrogen phosphate for EC medium should be 4.0 g, not 44.0 g (section
7.7.1).
    8. EPA is proposing to add Method 1627, ``Kinetic Test Method for
the Prediction of Mine Drainage Quality.'' The method is a standardized
simulated weathering test that provides information to predict the
quality of mine drainage from coal mining operations or weathering. The
method also can be a tool with which to generate data in the design and
implementation of best management practices and treatment processes
needed by mining operations to meet U.S. EPA discharge requirements at
40 CFR part 434. Other publications have referred to this method
generically as the ADTI Weathering Procedure 2 (ADTI-WP2). EPA lists
Method 1627 in Table IB as ``Acid Mine Drainage.'' The method is
suitable for determinations of probable hydrologic consequences and to
develop cumulative hydrologic impact assessment data to support Surface
Mining Control and Reclamation Act (SMCRA) permit application
requirements. Although this method is directed toward the coal mining
industry and regulatory agencies, the method may be applicable to
highway and other construction involving cut and fill of potentially
acid-producing rock. This method may be used to predict the water
quality characteristics (e.g., pH, acidity, metals) of mine site
discharges using observations from sample behavior under simulated and
controlled weathering conditions. The method was developed and
evaluated in single, multiple and interlaboratory method validation
studies in laboratories representing the mining industry, private
sector, federal agencies, and academia.
    9. EPA proposes to approve EPA Method 624, ``Purgeables,'' for
definitive measurements of acrolein and acrylonitrile in wastewater.
Currently this method is approved only to screen samples for the
presence of acrolein and acrylonitrile. Footnote 4 to Table IC requires
that the analyst confirm occurrences with either EPA Method 603 or 1624
because, when EPA promulgated this method, EPA believed the
confirmatory step was necessary. Commenters on a previous proposed rule
to amend part 136 (69 FR 18166, April 6, 2004) requested that EPA allow
use of Method 624 for definitive determination of acrolein and
acrylonitrile in wastewater without a confirmatory step and provided
EPA with data. EPA has considered this comment and after reviewing
additional data (Test America 1, 2) is proposing to revise the listing
of Method 624 in Table IC to remove footnote 4 that requires a
confirmatory analysis.

B. Changes to 40 CFR 136.3 To Include New Standard Methods and New
Versions of Approved Standard Methods

    EPA is proposing to revise how we identify approved methods that
are published by the Standard Methods Committee. Currently in the
tables at 136.3(a), EPA lists these methods in one or more columns as
being in the 18th, 19th, 20th printed compendiums, or in the On-line
editions published by the Standard Methods Committee. EPA identifies
which versions are approved by the printed edition in which the

method is published or, in the case of the electronic version of the
method, by the last two digits of the year in which the method was
published by the Standard Methods Committee (e.g., Standard Method 2320
B-97). In some cases, EPA has approved more than one version of a
Standard Method. Approval of several versions of the same Standard
Method has led to inconsistencies in how laboratories conduct these
analyses especially in quality assurance/quality control (QA/QC)
practices. For this reason, EPA is proposing to approve only the most
recent version of a method published by the Standard Methods Committee
with as few exceptions as possible by listing only one version of the
method with the year of publication designated by the last four digits
in the method number (e.g., Standard Method 2320 B-1997). This change
allows use of a specific method in any edition that includes a method
with the same method number and year of publication. Previously, a
laboratory only could use the method that was published in the edition
of Standard Methods listed in the tables at 136.3(a). In some cases,
EPA used footnotes to designate approved Standard Methods that are no
longer published in Standard Methods.
    In addition, EPA is proposing to approve new Standard Methods, SM,
new versions of currently approved SM, and the use of an already
approved SM for a chemical that is not currently listed in Table IB.
The new versions of currently approved SM have been revised to clarify
or improve the instructions in the method, improve the quality control
(QC) instructions, or make editorial corrections. The proposed new SM
and new versions of SM are described in the following paragraphs.
    1. EPA is proposing to add SM 5520 B-2001 and SM 5520 F-2001 for
Oil and Grease determinations. These methods measure hexane extractable
material (HEM). EPA is proposing these methods because they use n-
hexane as the extraction solvent. EPA is not proposing SM 5520 G-2001
because it allows use of a co-solvent, such as acetone. In the
preceding description of EPA's proposed Method 1664B, EPA explained
that oil and grease is a measurement defined by the solvent, in this
case n-hexane, used to extract oil and grease from the sample. Thus,
use of any other solvent system, such as a co-solvent is precluded.
    2. EPA is proposing to add SM 4500-NH3 G-1997, Ammonia
(as N) and TKN, Phenate Method, which is an automated version of the
previous version of a previously approved SM 4500-NH3 F-
1997.
    3. EPA is proposing to add SM 4500-B B-2000, Boron, Curcumin
Method, which uses the same chemistry and instruments as Method I-3112-
85.
    4. EPA is proposing to add SM 4140-1997, Inorganic Ions (Bromide,
Chloride, Fluoride, Orthophosphate, and Sulfate), Capillary Ion
Electrophoresis with Indirect UV Detection, which uses the same
technology as the EPA approved ASTM Method D6508-00.
    5. EPA is proposing to add SM 3114 C-2009, Arsenic and Selenium by
Continuous Hydride Generation/Atomic Absorption Spectrometry, which is
an automated version of the approved manual method, and uses the same
technology as Method I-2062-85.
    6. EPA is proposing to add SM 3111 E-1999 for determinations of
aluminum and beryllium. The method uses the same instrumental
techniques as SM 3111D with an additional chelation concentration step
for increased sensitivity.
    7. EPA is proposing to add SM 5220 B-1997 for Chemical Oxygen
Demand which is similar to EPA Method 410.3.
    8. EPA is proposing to add SM 4500 NORG D-1997 for
determinations of Kjeldahl Nitrogen--Total, which has a similar
chemical and instrument setup as in EPA Method 351.2 in Table IB. The
same chemical reaction is measured in both of these methods.
    9. EPA is proposing to add SM 4500 P G-1999 and SM 4500 P H-1999,
Phosphorus. Both of these methods use separate flow injection
instrumentation that is the same as EPA Method 365.1.
    10. EPA is proposing to add SM 4500 P E-1999 and SM 4500 P F-1999,
Phosphorus. These methods, 4500 P E-1999 Manual Single Reagent and F-
1999 Automated Ascorbic Acid, have been approved for drinking water
analyses (73 FR 31616, June 3, 2008).
    11. EPA is proposing to add SM 4500 O B, D, E and F-2001, Oxygen,
Iodometric Methods. EPA is proposing these methods because Standard
Methods has broken down the Winkler titration method into several
sections. Sections 4500 O B, D, E and F have been added to provide a
more detailed Winkler titration. Section B contains information on how
to collect the sample and what pretreatment may be needed for just the
Winkler titrations. Sections D, E, and F contain specific sample
pretreatment for interferences. Section D (see Item 12) is for ferrous
iron interferences. Section E (see Item 13) is for samples with a high
concentration of Total Suspended Solids. Section F is for samples with
large concentrations of biological solids. These sections are similar
to the instructions in ASTM D888, AOAC 973.45, and USGS I-1575-78.
    12. EPA is proposing to add SM 4500 O D-2001, Oxygen, Permanganate
Modification. This method for determinations of dissolved oxygen
contains the same permanganate pretreatment step that is specified in
ASTM D 888 and AOAC 973.45.
    13. EPA is proposing to add SM 4500 O E-2001, Oxygen, Alum
Flocculation Modification. This method for dissolved oxygen describes a
pretreatment step that removes high concentrations of suspended solids.
    14. EPA is proposing to add SM 3500 K C-1997, Potassium, Selective
Electrode Method. This method uses the same electrochemical procedure
to measure Potassium that is used in the Standard Methods for ammonia,
chloride, cyanide, and nitrate. Only the electrode construction is
different.
    15. EPA is proposing to add SM 2540 E-1997 for determinations of
Residues--Volatile. This fixed and volatile solids method uses the same
equipment and procedures to measure this method defined parameter as
approved EPA Method 160.4.
    16. EPA is proposing to add SM 4500 SiO2 E-1997 and SM
4500 SiO2 F-1997, Silica. These methods have the same
instrument setup and molybdate color reagent as USGS Method I-2700, but
utilize different reducing agents to produce molybdenum blue color.
There are slight modifications in the chemical reaction, but the
molybdenum blue final analyte is the same.
    17. EPA is proposing to add SM 4500 SO4 C-1997, D-1997,
E-1997, F-1997 and G-1997, Sulfate. EPA is proposing to approve the
online version of these methods because they are identical to the
approved versions published in the 18th, 19th and 20th edition of
Standard Methods. EPA approved the online versions for drinking water
use (73 FR 31616, June 3, 2008).
    18. EPA is proposing to add SM 4500 S\2\-B-2000 and C-2000,
Sulfide. These approved methods have been revised to describe more
completely the sample collection, transportation and analysis steps.

C. Changes to 40 CFR 136.3 To Include New ASTM Methods and New Versions
of Previously Approved ASTM Methods

    EPA is proposing to add to the list of approved testing procedures
new ASTM methods for existing pollutants in Table IB, such as cyanide,
and methods for new pollutants, such as the nonylphenols in Table IC.
EPA also is

proposing new versions of previously approved ASTM methods.
    1. EPA is proposing to add ASTM D2036-09 Standard Test Methods for
Cyanides in Water, Test Method A Total Cyanide after Distillation. In
2009, ASTM revised the version of this method currently listed in part
136. The method measures cyanides that are free, and strong-metal-
cyanide complexes (e.g. iron cyanides) that dissociate and release free
cyanide when refluxed under strongly acidic conditions. The cyanide in
some cyano complexes of transition metals, for example, cobalt, gold,
platinum, etc., is not determined. Samples are digested with sulfuric
acid in the presence of magnesium chloride in a distillation reaction
vessel that consists of a 1-L round bottom flask, with provision for an
inlet tube and a condenser connected to a vacuum-type absorber. The
flask is heated with an electric heater. Smaller distillation tubes
such as 50-mL midi tubes or 6-mL MicroDist\TM\ tubes described in
D7284-08 can be used if the quality control requirements in D2036-09
are satisfied. After distillation, the cyanide concentration can be
determined with titration, ion chromatography, colorimetric procedure
(spectrophotometric), selective ion electrode, or flow injection
analysis with gas diffusion separation and amperometric detection. The
inclusion of ion chromatography and gas diffusion separation with
amperometric detection as determinative steps (D2036-09, sections 16.5
and 16.6) will give users additional options to measure cyanide after
distillation. Furthermore, these determinative steps can be used to
mitigate interferences that have been associated with conventional
colorimetric test methods.
    2. EPA is proposing to add ASTM D6888-09 Standard Test Method for
Available Cyanide with Ligand Displacement and Flow Injection Analysis
(FIA) Utilizing Gas Diffusion Separation and Amperometric Detection.
This method is used to determine the concentration of available
inorganic cyanide in an aqueous wastewater or effluent. The method
detects the cyanides that are free and metal-cyanide complexes that are
easily dissociated into free cyanide ions. The method does not detect
the less toxic strong metal-cyanide complexes, cyanides that are not
``amenable to chlorination.'' Total cyanide can be determined for
samples that have been distilled as described in Test Methods D2036-09,
Test Method A, Total Cyanides after Distillation. Complex cyanides
bound with nickel or mercury are released by ligand displacement with
the addition of a ligand displacement agent prior to analysis. Other
available cyanide species do not require ligand displacement under the
test conditions. If samples are distilled for total cyanide, ligand
exchange reagents are not required since the cyanide complexes are
dissociated and absorbed into the sodium hydroxide capture solution
during distillation. The treated or distilled sample is introduced into
a flow injection analysis (FIA) system where it is acidified to form
hydrogen cyanide. The hydrogen cyanide gas diffuses through a
hydrophobic gas diffusion membrane, from the acidic donor stream into
an alkaline acceptor stream. Up to 50-mg/L sulfide is removed during
flow injection to mitigate sulfide interference. The captured cyanide
is sent to an amperometric flow cell detector with a silver-working
electrode. In the presence of cyanide, silver in the working electrode
is oxidized at the applied potential. The anodic current measured is
proportional to the concentration of cyanide in the standard or sample
injected.
    3. EPA is proposing to add ASTM D7284-08 Standard Test Method for
Total Cyanide in Water by Micro Distillation followed by Flow Injection
Analysis with Gas Diffusion Separation and Amperometric Detection. This
method determines the concentration of total cyanide in wastewater, and
detects the cyanides that are free and strong-metal-cyanide complexes
(e.g., iron cyanides) that dissociate and release free cyanide when
refluxed under strongly acidic conditions. This method has a range of
approximately 2 to 400 [mu]g/L (parts per billion) total cyanide.
Higher concentrations can be measured with sample dilution or lower
injection volume. The determinative step of this method utilizes flow
injection with amperometric detection based on ASTM D6888-09. Sample
distillation is based on Lachat QuikChem Method 10-204-00-1-X. Prior to
analysis, samples must be distilled with a micro-distillation apparatus
described in the test method or with a suitable cyanide distillation
apparatus specified in Test Methods D 2036-09. The samples are
distilled with a strong acid in the presence of magnesium chloride
catalyst and captured in sodium hydroxide absorber solution. The
absorber solution from the distillation is introduced into a flow
injection analysis (FIA) system where it is acidified to form hydrogen
cyanide. The hydrogen cyanide gas diffuses through a hydrophobic gas
diffusion membrane, from the acidic donor stream into an alkaline
acceptor stream. The captured cyanide is sent to an amperometric flow
cell detector with a silver-working electrode. In the presence of
cyanide, silver in the working electrode is oxidized at the applied
potential. The anodic current measured is proportional to the
concentration of cyanide. This method has been shown to be less
susceptible to interferences compared to conventional
spectrophotometric determinations for total cyanide.
    4. EPA is proposing to add ASTM D7511-09e2 Standard Test Method for
Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet
Digestion and Amperometric Detection. This method determines the
concentration of total cyanide in drinking and surface waters, as well
as domestic and industrial wastes. Cyanide ion (CN-), hydrogen cyanide
in water (HCN(aq)), and the cyano-complexes of zinc, copper, cadmium,
mercury, nickel, silver, and iron may be determined by this method.
Cyanide ions from Au(I), Co(III), Pd(II), and Ru(II) complexes are only
partially determined. The applicable range of the method is 3 to 500
[mu]g/L cyanide using a 200-[mu]L sample loop. The range can be
extended to analyze higher concentrations by sample dilution or by
changing the sample loop volume. ASTM D7511-09e2 decomposes complex
cyanides by narrow band, low watt UV irradiation in a continuously
flowing acidic stream at room temperature. Reducing and complexing
reagents, combined with the room temperature narrow band low watt UV,
minimize interferences. The hydrogen cyanide generated passes through a
hydrophobic membrane into a basic carrier stream. The cyanide
concentration is determined by amperometry. This method operates
similarly to available cyanide methods OIA1677 and ASTM D6888-09. The
available cyanide methods employ a preliminary ligand addition to
liberate cyanide ion from weak to moderate metal cyanide complexes.
These available cyanide methods were developed because they overcome
significant interferences caused by the preliminary chlorination and/or
distillation processes. Instead of ligands, ASTM D7511-09e2 irradiates
the sample causing strong metal cyanide complexes plus all complexes
measured by the available cyanide methods to liberate cyanide and
generate hydrogen cyanide. Once the sample solution passes from the UV
irradiation, the measurement principle is equivalent to OIA1677 and/or
ASTM D6888-09.
    5. Because there were no EPA-approved methods for free cyanide when
water quality criteria were

established for free cyanide EPA recommended measurement of cyanide
after a ``total'' distillation. Analytical methods for free cyanide
have been developed, and in today's rule EPA is proposing to add free
cyanide as a parameter (24A in Table IB.) For determinations of this
parameter, EPA is proposing to allow use of the approved available
cyanide method, OIA 1677-09, and two ASTM methods (D4282-02 and D7237-
10.) ASTM D4282-02 Standard Test Method for Determination of Free
Cyanide in Water and Wastewater by Microdiffusion determines free
cyanide as the cyanide that diffuses into a sodium hydroxide solution
from a solution at pH 6. It is not applicable to cyanide complexes that
resist dissociation, such as hexacyanoferrates and gold cyanide, and it
does not include thiocyanate and cyanohydrin. ASTM D7237-10 Standard
Test Method for Free Cyanide with Flow Injection Analysis (FIA)
Utilizing Gas Diffusion Separation and Amperometric Detection
determines free cyanide with the same instrumentation and technology as
approved methods, ASTM D6888-09 and OIA 1677-09, but under milder (less
acidic) conditions and without use of ligand replacement reagents.
    6. EPA is proposing to add ASTM D888-09 Standard Test Method for
Dissolved Oxygen in Water. This method determines dissolved oxygen
concentrations in water using the titrimetric (Part A), polarographic
(Part B) and luminescence-based (Part C) detection methods. This
standard test method is applicable to the determination of dissolved
oxygen between 0.05-20 ppm in influent, effluent or ambient water
testing. ASTM recently updated Part C of this method to include a
detailed description of the technology and to update calibration
procedures to include a two-point calibration and an air saturated
water calibration in addition to a water saturated air calibration.
This method may be used for Biological Oxygen Demand (BOD) and
Carbonaceous Oxygen Demand (CBOD.)
    7. EPA is proposing to add ASTM D7573-09 Standard Test Method for
Total Carbon and Organic Carbon in Water by High Temperature Catalytic
Combustion and Infrared Detection. This Method has the same chemical
and instrument setup as approved SM 5310 B-2000.
    8. EPA is proposing to add in Table IC ASTM D7065-06: Standard Test
Method for Determination of five chemicals: Nonylphenol (NP), Bisphenol
A (BPA), p-tert-Octylphenol (OP), Nonylphenol Monoethoxylate (NP1EO),
and Nonylphenol Diethoxylate (NP2EO) in Environmental Waters by Gas
Chromatography Mass Spectrometry. These five chemicals are partitioned
into an organic solvent, separated using gas chromatography and
detected with mass selective detection. These chemicals or isomer
mixtures are qualitatively and quantitatively determined. Although this
method adheres to selected ion monitoring mass spectrometry, full scan
mass spectrometry has also been shown to work well under these
conditions. This method has been multi-laboratory validated for use
with surface water and waste treatment effluent samples and is
applicable to these matrices. It has not been investigated for use with
salt water or solid sample matrices. The reporting limit for
nonylphenol is 5 [mu]g/L (ppb); the chronic Freshwater Aquatic Life
Ambient Water Quality Criterion is 6.6 ppb.
    9. EPA is proposing to add in Table IC ASTM D7574-09: Standard Test
Method for Determination of BPA in Environmental Waters by Liquid
Chromatography/Tandem Mass Spectrometry. BPA is an organic chemical
produced in large quantities. BPA is soluble in water and undergoes
degradation in the environment. The reporting limit for BPA is 20 ng/L
which is fifty times less than the limit in D7065-06 (see preceding
Item 8). The method is based on a solid phase extraction (SPE) followed
by separation with liquid chromatography and tandem mass spectrometry
(LC/MS/MS), which reduces the amount of sample required, solvents, the
analysis time, and the reporting limits. The method has been tested in
effluents from secondary and tertiary publicly owned treatment works
(POTW), and fresh surface and ground water.
    10. EPA is proposing to add in Table IC ASTM D7485-09: Standard
Test Method for Determination of NP, OP, NP1EO, and NP2EO in
Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry.
The method extracts these four chemicals from water with SPE followed
by LC/MS/MS separation and detection. These chemicals are qualitatively
and quantitatively determined by this method. This method uses single
reaction monitoring (SRM) mass spectrometry. Environmental waters
tested using this method were sewage treatment plant effluent, river
water, seawater, and a modified ASTM D5905 artificial wastewater. The
reporting limit for nonylphenol is 100 ng/L, ppt. The Freshwater and
Saltwater Aquatic Life Ambient acute criterion is 7.0 ppb, and the
chronic criterion is 1.7 ppb.
    11. EPA is not proposing to include in Table IB two ASTM oil and
grease methods, D7066-04 and D7575-10 because neither method uses n-
hexane to determine oil and grease as hexane extractable material
(HEM). As previously explained in the discussion of Method 1664B, HEM
is a measurement defined by the solvent (n-hexane) used to extract oil
and grease from the sample. D7066-04 employs a proprietary solvent, S-
316, a dimer/trimer of chlorotrifluoroethylene to measure S-316-
extractable substances from an acidified sample. Method D7066 may be
useful for determinations of total petroleum hydrocarbons (TPH).
Although TPH has been measured in some applications, EPA has never
included it as a Part 136 pollutant nor received any convincing
evidence that it should do so. Although S-316 is not the same solvent
as the fluorocarbon, Freon[supreg], it is a fluorochlorohydrocarbon.
    Instead of n-hexane, ASTM D7575-10 uses a different extracting
process, an extracting membrane, followed by infrared measurement of
the materials in the sample that can pass through the membrane. Several
other steps in D7575-10 significantly differ from 1664 including: Use
of 10-mL sample aliquot from sample bottle vs. entire contents of 1-L
sample; homogenization of samples; and the challenge of pushing solid
oil and grease samples through a membrane. The results of a multi-
laboratory study (OSS 2009) that the developer conducted as part of
ASTM's evaluation of D7575 are in the docket.

D. Changes to 40 CFR 136.3 To Include Alternate Test Procedures

    To promote method innovation, EPA maintains a program whereby
method developers may apply for an EPA review and potentially for
approval of alternate test procedures. This Alternate Test Procedure
(ATP) program is described for Clean Water Act applications at Parts
136.4 and 136.5. EPA has reviewed and is proposing for nationwide use
eight alternate test procedures. These proposed new methods include:
Hach Company's Method 10360 Luminescence Measurement of Dissolved
Oxygen (LDO[supreg]) in Water, In-Situ Incorporated's Method 1002-8-
2009 Dissolved Oxygen (DO) Measurement by Optical Probe, Method 1003-8-
2009 Biochemical Oxygen Demand (BOD) Measurement by Optical Probe, and
Method 1004-8-2009 Carbonaceous Biochemical Oxygen Demand (CBOD)
Measurement by Optical Probe August 2009, Mitchell Method M5271 and
M5331 for measuring turbidity in wastewater; Thermo Scientific's Orion
Method

AQ4500 for measuring turbidity in wastewater; and Systea Scientific,
LLC's Systea Easy (1-Reagent) Nitrate Method. Descriptions of these new
methods included for approval are as follows:
    1. EPA is proposing to approve Hach Company's Method 10360
Luminescence Measurement of Dissolved Oxygen (LDO[supreg]) in
wastewater, Revision 1.1 dated January 4, 2006. EPA has reviewed this
method and the data generated in a multi-laboratory validation study
performed by Hach Company and is proposing to approve it for use in
measuring dissolved oxygen. EPA is also proposing to approve the Hach
method 10360 to be used for Dissolved Oxygen (DO) when determining BOD
and CBOD.
    This method uses an optical probe to measure the light emission
characteristics from a luminescence-based reaction that takes place at
the sensor-water interface. A light emitting diode (LED) provides
incident light required to excite the luminophore substrate. In the
presence of dissolved oxygen, the reaction is suppressed. The resulting
dynamic lifetime of the excited luminophore is evaluated and equated to
DO concentration.
    The method involves the following steps:
     Calibration of the probe using water-saturated air, and
     Measurement of the dissolved oxygen in the sample using
the probe.
    Approved methods for measuring dissolved oxygen are listed at 40
CFR 136.3, Table IB. The performance characteristics of the Hach
Company Method 10360 were compared to the characteristics of the
methods listed at 40 CFR 136.3, Table IB for measurement of dissolved
oxygen. Because the Hach Company Method 10360 is equally effective
relative to the methods already promulgated in the regulations, EPA is
proposing to include this method in the list of methods approved for
measuring dissolved oxygen concentrations in wastewater when
determining BOD and CBOD.
    2. EPA is proposing to approve In-Situ Incorporated's Method 1002-
8-2009 Dissolved Oxygen Measurement by Optical Probe. EPA has reviewed
this method and the data generated in a multi-laboratory validation
study performed by In-Situ Incorporated and is proposing to approve it
for use in measuring dissolved oxygen. In-Situ Method 1002-8-2009 uses
a new form of electrode based on the luminescence emission of a
photoactive chemical compound and the quenching of that emission by
oxygen to measure dissolved oxygen concentration.
    The method involves the following steps:
     Calibration of the probe using water-saturated air, and
     Measurement of the dissolved oxygen in the sample using
the probe.
    Approved methods for measuring dissolved oxygen are listed at 40
CFR 136.3, Table IB. The performance characteristics of the In Situ
Method 1002-8-2009 were compared to the characteristics of the methods
listed at 40 CFR 136.3, Table IB for measurement of dissolved oxygen.
Because the In-Situ Method 1002-8-2009 is equally effective relative to
the methods already promulgated in the regulations, EPA is proposing
In-Situ Method 1002-8-2009 for inclusion in the list of methods
approved for measuring dissolved oxygen concentrations in wastewater.
    3. EPA is proposing to approve In-Situ Incorporated's Method 1003-
8-2009 Biochemical Demand (BOD) Measurement by Optical Probe. EPA has
reviewed this method and the data generated in a multi-laboratory
validation study performed by In-Situ Incorporated and is proposing to
approve it for measuring BOD.
    In-Situ Method 1003-8-2009 uses a new form of electrode based on
the luminescence emission of a photoactive chemical compound and the
quenching of that emission by oxygen to measure dissolved oxygen
concentration when performing the 5-day BOD test.
    The method involves the following steps:
     Filling a BOD bottle with diluted seeded sample,
     Measuring the dissolved oxygen in the sample using an
optical DO probe,
     Sealing and incubating the bottle for five days,
     Measuring the dissolved oxygen with an optical probe after
the five day incubation period, and
     Calculating the BOD from the difference between the
initial and final dissolved oxygen measurements.
    Approved methods for measuring BOD are listed at 40 CFR 136.3,
Table IB. The performance characteristics of In-Situ Method 1003-8-2009
were compared to the characteristics of the methods listed at 40 CFR
136.3, Table IB for measurement of BOD. Because In-Situ Method 1003-8-
2009 is equally effective relative to the methods already promulgated
in the regulations, EPA is proposing In-Situ Method 1003-8-2009 for
inclusion in the list of methods approved for measuring BOD.
    4. EPA is proposing to approve In-Situ Incorporated's Method 1004-
8-2009 Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by
Optical Probe. EPA has reviewed this method and the data generated in a
multi-laboratory validation study performed by In-Situ Incorporated and
is proposing to approve it for use in measuring carbonaceous
biochemical oxygen demand (CBOD). In-Situ Method 1004-8-2009 uses a new
form of electrode based on the luminescence emission of a photoactive
chemical compound and the quenching of that emission by oxygen to
measure dissolved oxygen concentration when performing the CBOD test.
    The method involves the following steps:
     Filling a BOD bottle with diluted seeded sample,
     Adding a chemical nitrification inhibitor,
     Measuring the dissolved oxygen in the sample using an
optical dissolved oxygen probe,
     Sealing and incubating the bottle for five days,
     Measuring the dissolved oxygen with an optical probe after
the five day incubation period, and
     Calculating the CBOD from the difference between the
initial and final dissolved oxygen measurements.
    Approved methods for measuring CBOD are listed at 40 CFR 136.3,
Table IB. The performance characteristics of In Situ-Method 1004-8-2009
were compared to the characteristics of the methods listed for
measurement of CBOD. Because In-Situ Method 1004-8-2009 is equally
effective relative to the methods already promulgated in the
regulations, EPA is proposing In-Situ Method 1004-8-2009 for inclusion
in the list of methods approved for measuring CBOD.
    5. EPA is proposing to approve the Mitchell Method M5271 dated July
31, 2008. This method uses laser based nephelometry to measure
turbidity in drinking water and wastewater. The method involves the
following steps for instruments other than on-line continuous models:
     Mixing the sample to thoroughly disperse the solids,
     Waiting until air bubbles disappear,
     Pouring a sample into a turbidimeter tube, and
     Reading turbidity directly from the instrument scale or
from the appropriate calibration curve.
    Approved methods for turbidity are listed at 40 CFR 136.3 Table 1B.
The performance characteristics of Mitchell Method M5271 were compared
to the performance characteristics of EPA Method 180.1 listed at 40 CFR
136.3 for measurement of turbidity. Comparisons were based on results
obtained from turbidimeters placed in series which took measurements at
one minute

intervals over a 20 to 30 hour time period at three different public
water supply systems (in one case measurements were taken at 15 minute
intervals). Testing included source water from one ground water source
and two surface water sources and included at least one natural filter
event (back-flush) in lieu of artificially calibrated spikes using a
primary standard spiking solution. Additionally, a demonstration of
performance at higher turbidities was conducted by making replicate
measurements of primary standards at four levels (5 NTU, 10 NTU, 20 NTU
and 40 NTU). Results showed excellent correlation between measurements
made using a tungsten filament incandescent bulb as specified in EPA
Method 180.1 and those made using the laser light source specified in
Mitchell Method M5271. Based on the results of these studies, EPA has
determined that Mitchell Method M5271 is as effective as the methods
already promulgated in the regulations. EPA is proposing to add this
method to the list of methods approved for measurement of turbidity in
wastewater.
    6. EPA is proposing Mitchell Method M5331 dated July 31, 2008. This
method uses LED based nephelometry to measure turbidity. The method
involves the following steps for instruments other than on-line
continuous models:
     Mixing the sample to thoroughly disperse the solids,
     Waiting until air bubbles disappear,
     Pouring the sample into turbidimeter tube, and
     Reading turbidity directly from the instrument scale or
from the appropriate calibration curve.
    Approved methods for turbidity are listed at 40 CFR 136.1 Table 1B.
The performance characteristics of Mitchell Method 5331 were compared
to the performance characteristics of EPA Method 180.1 listed at 40 CFR
136.3 for measurement of turbidity. Comparisons were based on results
obtained from turbidimeters placed in series, which took measurements
at one minute intervals over a 20 to 30 hour time period at three
different public water supply systems (in one case measurements were
taken at 15 minute intervals). Testing included source water from one
ground water source and two surface water sources and included at least
one natural filter event (back-flush) in lieu of artificially
calibrated spikes using a primary standard spiking solution.
Additionally, a demonstration of performance at higher turbidities was
conducted by making replicate measurements of primary standards at four
levels (5 NTU, 10 NTU, 20 NTU and 40 NTU). Results showed excellent
correlation between measurements made using a tungsten filament
incandescent bulb as specified in EPA Method 180.1 and the LED light
source specified in Mitchell Method M5331. Based on the results of
these studies, EPA has determined that Mitchell Method M5331 is equally
effective relative to the methods already promulgated in the
regulations. EPA is proposing to add this method to the list of methods
approved for measurement of turbidity in wastewater.
    7. EPA is proposing to approve Thermo Scientific's Orion Method
AQ4500 dated March 12, 2009. This method uses LED-based nephelometry to
measure turbidity. The method involves the following steps:
     Calibration of the instrument using a primary calibration
standard,
     Placing the sample into the sample chamber, and
     Reading the turbidity result displayed on the instrument.
    Approved methods for turbidity are listed at 40 CFR 136.3 Table IB.
The performance characteristics of Thermo Scientific's Orion Method
AQ4500 were compared to the performance characteristics of EPA Method
180.1 listed at 40 CFR 136.3 for measurement of turbidity. Comparisons
were based on an ASTM round robin study comparing results from analyses
of 28 different samples of various types including formazin standards,
styrene divinyl benzene (SDVB) co-polymer bead standards and real world
samples ranging from approximately 2 NTU to over 1,000 NTU. These
analyses were conducted using turbidimeters with various light sources
including tungsten filament incandescent bulbs as specified in EPA
Method 180.1 and white LEDs as specified in Thermo Scientific's Orion
Method AQ4500. Additionally, a demonstration of performance at lower
turbidities was conducted by making 20 replicate measurements of dilute
formazin standards at four levels (0.2 NTU, 0.5 NTU, 1 NTU, and 2 NTU)
using turbidimeters with tungsten filament incandescent bulbs as
specified in EPA Method 180.1 and turbidimeters using white LEDs as
specified in Thermo Scientific Orion Method AQ4500. Results showed
significant correlation between measurements made using a tungsten
filament incandescent bulb as specified in EPA Method 180.1 and those
made using the LED light source specified in Thermo Scientific's Orion
Method AQ4500. Based on the results of these studies, EPA has
determined that Thermo Scientific's Orion Method AQ4500 is as effective
as the methods already promulgated in the regulations. EPA is proposing
to add this method to the list of methods approved for measurement of
turbidity in wastewater.
    8. EPA is proposing to approve Systea Scientific, LLC's Systea Easy
(1-Reagent) Nitrate Method dated February 4, 2009. This is a method
that uses automated discrete analysis, and spectrophotometry to
determine concentrations of nitrate and nitrite combined or singly. The
method involves the following steps:
     Reduction of nitrate in a sample to nitrite using a non-
hazardous proprietary reagent,
     Diazotizing the nitrite originally in the sample plus the
reduced nitrate with sulfanilamide followed by coupling with N-(1-
napthyl) ethylenediamine dihydrochloride under acidic conditions to
form a highly colored azo dye,
     Colorimetric determination in which the absorbance of
color at 546 nm is directly proportional to the concentration of the
nitrite plus the reduced nitrate in the sample,
     Measurement of nitrite singly, if needed, by analysis of
the sample while eliminating the reduction step, and
     Subtraction of the nitrite value from that of the combined
nitrate plus nitrite value to measure nitrate singly if needed.
    Approved methods for nitrate, nitrite and combined nitrate/nitrite
are listed at 40 CFR 136.3, Table 1B. The performance characteristics
of the Systea Easy (1-Reagent) Nitrate Method were compared to the
characteristics of the methods listed at 40 CFR 136.3 for nitrate and
nitrite. Based on the results of the comparative studies, EPA has
determined that the Systea Easy (1-Reagent) Nitrate Method is as
effective as the methods already promulgated in the regulations for use
in determining concentrations of nitrate and nitrite and combined
nitrate/nitrite. The method is a ``green'' alternative to other
approved methods that use cadmium, a known carcinogen, for the
reduction of nitrate to nitrite. The performance of Systea Easy (1-
Reagent) Nitrate Method is equivalent to other methods already approved
for measurement of nitrate, nitrite and combined nitrate/nitrite in
wastewater.

E. Clarifications and Corrections to Previously Approved Methods in 40
CFR 136.3

    EPA is proposing a clarification to procedures for measuring
orthophosphate, and is proposing to correct typographical or other
citation errors in part 136.
    1. EPA is clarifying the purpose of the immediate filtration
requirement in

orthophosphate measurements, which is to assess the dissolved or bio-
available form of orthophosphorus (i.e., that which passes through a
0.45 micron filter), hence the requirement to filter the sample
immediately upon collection. This filtration excludes any particulate
forms of phosphorus that might hydrolyze into orthophosphorus in a
slightly acidic sample during the allowed 48 hour holding time. Each
grab sample must be filtered within 15 minutes of collection to prevent
orthophosphate formation. Specifically, filtration may not be delayed
until the final grab sample is collected; each grab sample must be
filtered upon collection. However, the filtered grab samples may be
held for compositing up to the 48-hour holding time.
    2. EPA is proposing to correct missing citations to the table of
microbiological methods for ambient water monitoring which are
specified in Table IH at 40 CFR 136.3. Stakeholders asked EPA to
separately specify the microbiological methods that EPA has approved
for wastewater (Table IA) from those for ambient water. On August 15,
2005 (70 FR 48256), EPA proposed to move microbial (bacterial and
protozoan) methods which were applicable to ambient water to a new
table, Table IH. However, in the final rule of March 26, 2007 (72 FR
14220), EPA inadvertently omitted fecal coliform, total coliform, and
fecal streptococcus methods from the table. EPA is proposing to add
these methods to Table IH.
    3. EPA is proposing to correct several other typographical or minor
citation errors, such as incomplete or incorrect method citations.

F. Proposed Revisions in Table II at 40 CFR 136.3(e) to Required
Containers, Preservation Techniques, and Holding Times

    EPA is proposing revisions to Table II at 136.3(e) to clarify how
to resolve conflicts between instructions in this table and
instructions in an approved method or other source, and to amend some
of the current requirements in Table II.
    1. The introductory text to Table II at 136.3(e) specifies that the
instructions in the table take precedence over other sources of this
information. EPA publishes holding time and related instructions in
Table II to provide a consistent set of instructions, and for other
reasons. Not all methods contain complete instructions, and some
otherwise equivalent methods (or methods for the same parameter) have
conflicting instructions. For example, Table II instructions specify
the 48 hour BOD holding time while some Part 136 methods recommend 24
hours. In this instance Table II instructions take precedence. EPA
recognizes that there may be cases where new technologies or
advancements in current technologies may produce approved methods with
instructions for a specific parameter that differ from Table II
instructions, and provide better results. Cyanide determinations and
some automated methods may fall into this category. Therefore, EPA is
proposing to revise the text at 136.3(e) to allow a party to submit
documentation to their permitting or other authority that supports use
of an alternative approach. EPA is proposing to revise the introductory
text to the table to read as follows: ``Information in this table takes
precedence over instructions provided in specific methods or elsewhere
unless a party documents the acceptability of an alternative to the
Table II instructions. The nature, timing and extent of the required
documentation (i.e. how to apply and review as well as the amount of
supporting data) are left to the discretion of the permitting authority
(State Agency or EPA Region) or other authority and may rely on
instructions, such as those provided for method modifications at
136.6.'' Thus, an alternate sample container, preservation and/or
holding time may be considered at the discretion of the permitting
authority or other authority.
    2. Some stakeholders have asked EPA to extend the holding time for
Escherichia coli and Enterococcus. In 2006, EPA conducted a nationwide
holding time study (EPA 2006) for fresh and marine ambient waters and
concluded that, on a nationwide basis, the Agency was unable to justify
extending the holding time for Escherichia coli or Enterococcus in
these water matrices. However, EPA is proposing to provide some relief
by revising footnote 22 to Table II, which applies to bacterial tests.
This footnote currently reads as follows: ``Sample analysis should
begin immediately, preferably within 2 hours of collection. The maximum
transport time to the laboratory is 6 hours, and samples should be
processed (in incubator) within 2 hours of receipt at the laboratory.''
    Stakeholders have commented that laboratories must meet the two-
hour analysis start time, even if they receive the samples early enough
that they could start after two hours and still meet the overall six-
hour time limit. EPA is proposing to revise the footnote to read
``Sample analysis should begin as soon as possible after receipt;
sample incubation must be started no later than 8 hours from time of
collection.''
    3. EPA is proposing to revise the cyanide sample handling
instructions in Footnote 5 of Table II to recommend the treatment
options for samples containing oxidants described in ASTM's sample
handling practice for cyanide samples, D7365-09a. This practice advises
analysts to add a reducing agent only if an oxidant is present, and use
of the reducing agents sodium thiosulfate
(Na2S2O3), ascorbic acid, sodium
arsenite (NaAsO2), or sodium borohydride (NaBH4).
    4. EPA is proposing to revise the cyanide sample handling
instructions in Footnote 6 of Table II to describe options available
when the interference mitigation instructions in D7365-09a are not
effective. EPA proposes to allow use of any technique for removal or
suppression of interference, provided the laboratory demonstrates and
documents that the alternate technique more accurately measures cyanide
through quality control measures described in the analytical test
method.
    5. EPA is proposing to revise footnote 16 of Table II instructions
for handling Whole Effluent Toxicity (WET) samples to be consistent
with the November 19, 2002 (67 FR 69951) ``Guidelines for Establishing
Test Procedures for the Analysis of Pollutants; Whole Effluent Toxicity
Test Methods; Final Rule,'' as well as the three toxicity methods
(Methods for Measuring the Acute Toxicity of Effluents and Receiving
Waters to Freshwater and Marine Organisms (5th Edition, October 2002),
Short-term Methods for Estimating the Chronic Toxicity of Effluents and
Receiving Waters to Freshwater Organisms (4th Edition, October 2002),
and Short-term Methods for Estimating the Chronic Toxicity of Effluents
and Receiving Waters to Marine and Estuarine Organisms (3rd Edition,
October 2002). In the 2002 final rule, EPA established the acceptable
range for the current sampling holding temperature for aquatic toxicity
tests as 0 to 6 [deg]C based on current National Environmental
Laboratory Accreditation Conference (NELAC) standards. EPA also
clarified in the final rule that hand-delivered samples used on the day
of collection do not need to be cooled to 0 to 6 [deg]C prior to test
initiation. Section 8.5.1 of all three WET methods listed previously
states, ``Unless the samples are used in an on-site toxicity test the
day of collection (or hand delivered to the testing laboratory for use
on the day of collection) it is recommended that they be held at 0 to 6
[deg]C until used to inhibit microbial degradation, chemical
transformation, and loss of highly volatile toxic substances.'' EPA is
proposing to add two sentences to the

end of Footnote 16 of Table II based on this information. The two
sentences are ``Aqueous samples must not be frozen. Hand-delivered
samples used on the day of collection do not need to be cooled to 0 to
6 [deg]C prior to test initiation.'' In addition, EPA will post, on the
WET Web site, corrections to errata in the ``Short-term Methods for
Estimating the Chronic Toxicity of Effluents and Receiving Waters to
Freshwater Organisms'' manual (EPA 2010e.)
    6. EPA is proposing to add a sentence to footnote 4 of Table II to
clarify the sample holding time for the Whole Effluent Toxicity (WET)
samples for the three toxicity methods (Methods for Measuring the Acute
Toxicity of Effluents and Receiving Waters to Freshwater and Marine
Organisms (5th Edition, October 2002), Short-term Methods for
Estimating the Chronic Toxicity of Effluents and Receiving Waters to
Freshwater Organisms (4th Edition, October 2002), and Short-term
Methods for Estimating the Chronic Toxicity of Effluents and Receiving
Waters to Marine and Estuarine Organisms (3rd Edition, October 2002) to
indicate that one sample of the minimum of three required samples may
be used for the renewal of the test solutions and that the sample
holding time refers to first use of each sample collected for the
toxicity test. The sentence to be added is, ``For static-renewal
toxicity tests, each grab or composite sample may also be used to
prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after
first use, if stored at 0-6 [deg]C, with minimum head space.''

G. Proposed Revisions to 40 CFR 136.4 and 136.5

    EPA is proposing to revise Sec. Sec.  136.4 and 136.5 to describe
the procedures for obtaining review and EPA approval for the use of
alternate test procedures (alternate methods or ATPs). The proposed
changes would revise 40 CFR 136.4 to establish the procedures for
obtaining approval for nationwide use of an ATP. The proposed changes
would modify 40 CFR 136.5 to establish the procedures for obtaining
approval for use of an ATP in a State within a particular EPA Region.
It should be noted that in its ATP program, EPA considers for review
only those methods for which EPA has published an ATP protocol.
Presently, EPA has published protocols for chemistry, radiochemical,
and culture microbiological methods. EPA does not have ATP protocols
for Whole Effluent Toxicity (WET) methods or genetic methods.
    In today's rule, EPA proposes to clarify that the intent of the
limited use authority is to allow limited use of an alternate method
for a specific application at a facility or type of discharge without
requiring the same level of supporting test data that would be required
for approval for nationwide use. Thus, limited use authority is not
intended to be used as a means of avoiding the full examination of
comparability that is required when EPA considers a method for
nationwide use and decides to amend its list of approved CWA methods at
40 CFR part 136 to include alternative test procedures. In the event
that EPA decides not to approve an application for approval of an
alternate method for nationwide use, the Regional Alternate Test
Procedures Coordinator may choose to reconsider any previous limited
use approvals of the alternate method. Based on this reconsideration,
the Regional Coordinator will notify the user, if the limited use
approval is withdrawn.

H. Proposed Revisions to Method Modification Provisions at 40 CFR 136.6

    EPA encourages regulatory authorities to allow analysts the
flexibility to modify CWA methods without prior approval provided the
user has documented equivalent or better performance of the method in
the matrix type to which the user will apply the modified method. EPA
recognizes that addressing specific matrix interferences may require
modifications to approved methods that do not require the extensive
review and approval process specified for an alternate test procedure
at 136.4 and 136.5. Based on users' experiences with 136.6, since it
was promulgated on March 12, 2007 (72 FR 11199), EPA proposes to revise
this section to provide more examples of allowed and prohibited method
modifications. Acceptable reasons for an analyst to modify a method
include analytical practices that lower detection limits, improve
precision, reduce interferences, lower laboratory costs, and promote
environmental stewardship by reducing generation of laboratory wastes.
Acceptable modifications may use existing or emerging analytical
technologies that achieve these ends provided that they do not depart
substantially from the underlying chemical principles employed in
methods currently approved in 40 CFR part 136. Analysts may use the
examples in this section to assess and document that their modification
is acceptable and does not depart substantially from the chemical
principles in the method being modified. EPA specifically invites
comment on the examples of flexibility specified at 136.6 and the
documentation that a method modifier must have to demonstrate the
equivalency of the modified method. In particular, EPA is interested in
public comment on what additional controls, if any, should be applied
when changing pH, purge times, buffers, or applying the relative
standard error calibration alternative.

I. Proposed New Quality Assurance and Quality Control Language at 40
CFR 136.7

    EPA is proposing to specify ``essential'' quality control at Sec.
136.7 for use in conducting an analysis with an approved method and
when insufficient instructions are contained in an approved method.
Auditors, co-regulators, laboratory personnel, and the regulated
community have noted the different amounts and types of quality
assurance (QA) and quality control (QC) procedures practiced by
laboratories that use 40 CFR part 136 methods. Some of these methods
are published by voluntary consensus standards bodies, such as the
Standard Methods Committee, and ASTM International. ASTM and Standard
Methods are contained in printed compendium volumes, electronic
compendium volumes, or as individual online files. Each organization
has its unique compendium structure. QA and QC method guidance or
requirements may be listed directly in the approved consensus method,
or, as is more often the case, these requirements are listed in other
parts of the compendium. For example, the publisher of Standard Methods
for the Examination of Water and Wastewater consolidates the general
quality assurance and quality control requirements for all methods.
Each specific Part and section can contain additional QA and QC
requirements (for example, see part 2020, 3020, 6020, and 9020). ASTM
specifies QA and QC requirements in the analyte method's Referenced
Documents section and in the analyte method. Both organizations require
the analyst to reference this additional information within the
respective compendiums to achieve the QA and QC expected for valid
results.
    Regardless of the publisher, edition or source of an analytical
method approved for CWA compliance monitoring, analysts must use
suitable QA/QC procedures whether EPA or other method publishers have
specified these procedures in a specific part 136 method, or referenced
these procedures by other means. Consequently, EPA

expects that an analyst using these consensus body methods for
reporting under the CWA will also comply with the quality assurance and
quality control requirements listed in the appropriate sections in the
consensus body compendium. EPA's approval of use of these voluntary
consensus standard body methods contemplated that any analysis using
such methods would also meet the quality assurance and quality control
requirements prescribed for the particular method. Thus, not following
the applicable and appropriate quality assurance and quality control
requirements of the respective method means that the analysis would not
comply with the requirements in EPA's NPDES regulations to monitor in
accordance with the procedures of 40 CFR part 136 for analysis of
pollutants.
    For methods that have insufficient QA/QC requirements, analysts
could refer to and follow the QC published in several public sources.
Examples of these sources include the instructions in an equivalent
approved EPA method or standards published by the National
Environmental Laboratory Accreditation Conference (cf. Chapter 5 of the
compendium published in 2003.)
    In addition to and regardless of the source of the laboratory's QA
and QC instructions, EPA is proposing at 136.7 to specify twelve
essential quality control checks that must be in the laboratory's
documented quality system unless a written rationale is provided to
explain why these controls are inappropriate for a specific analytical
method or application. This written rationale will be included in the
laboratory's Standard Operating Procedure (SOP) for each method to
which specific controls do not apply (e.g., internal standards,
surrogate standards or tracers do not apply to analyses of inorganic
parameters) as well as being included with the monitoring data produced
using each method. These twelve essential quality control checks must
be clearly documented in the written SOP (or method) along with a
performance specification or description for each of the twelve checks.

J. Proposed Withdrawal of Appendices at 40 CFR 136

    EPA is proposing to incorporate by reference all of the methods
printed in 40 CFR part 136 appendices A and C, and to remove most of
the information in Appendix D. EPA is proposing to remove EPA Method
numbers 601 through 613, 624, 625, 1613B, 1624B and 1625B from Appendix
A. All of these methods are readily accessible from a variety of
sources including EPA's CWA methods Web site http://www.epa.gov/
waterscience/methods/. Removing this appendix would decrease the
resources associated with the annual publication of 40 CFR part 136
regulations. EPA would incorporate these methods by reference in Tables
IC and ID at 136.3(a).
    EPA is proposing to remove Appendix C--Method 200.7 Inductively
Couple Plasma--Atomic Emission Spectrometric Method for Trace Element
Analysis of Water and Waste Method because this method has been
superseded by Rev. 5.4 of Method 200.7, which is incorporated by
reference in Table IB.
    Finally, EPA is proposing to remove from Appendix D the data for
all EPA methods that are no longer approved. This would result in
Appendix D containing Precision and Recovery Statements only for EPA
Method 279.2 for thallium and EPA Method 289.2 for zinc. EPA will
correct any typographical errors in the Appendix, such as the
misspelling of thallium. EPA requests comment on whether to publish and
make available, at least temporarily, the current version of Appendix D
online at the CWA methods Web site for historical purposes.

K. Proposed Revisions at 40 CFR 423

    EPA is proposing two changes to part 423, Steam Electric Power
Generating Point Source Category. First, EPA proposes to revise the
definitions for total residual chlorine and free available chlorine at
Sec. Sec.  423.11(a) and 423.11(l), respectively. The current
definitions restrict the permittee to the use of the specific
amperometric titration method cited in the definitions. The revised
definitions will allow the permittee flexibility to use additional
approved methods. EPA proposes to revise the definitions as follows:
    a. The term total residual chlorine (or total residual oxidants for
intake water with bromides) means the value obtained using any of the
``chlorine--total residual'' methods in Table IB 136.3(a), or other
methods approved by the permitting authority.
    b. The term free available chlorine means the value obtained using
any of the ``chlorine--free available'' methods in Table IB 136.3(a)
where the method has the capability of measuring free available
chlorine, or other methods approved by the permitting authority.
    Second, EPA is proposing to move the current citations of methods
from Part 423 and reference a new parameter, ``chlorine-free
available'', in Table IB at 136.3(a). Under this parameter, EPA will
list any Part 136 methods for total residual chlorine that also provide
instructions for determining free chlorine. The tables at 136.3 are
well known as the source of most methods that are approved for CWA
programs. For this reason EPA is proposing to move the citations of
specific methods from part 423 to Table IB, and as described in the
following sections, also for Parts 430 and 435.

L. Proposed Revisions at 40 CFR 430

    EPA is proposing several editorial changes to 40 CFR part 430, The
Pulp, Paper, and Paperboard Point Source Category. Currently the
complete text of EPA Methods 1650 and 1653 are published in Appendix A
of part 430. EPA is proposing to cite these two methods in Table IC, at
Sec.  136.3, and to incorporate by reference the full text of these
methods. EPA will list these two methods in Table IC--List of Approved
Test Procedures for Non-Pesticide Organic Compounds, under adsorbable
organic halides (AOX) by Method 1650 and chlorinated phenolics by
Method 1653. This action would remove Appendix A at 40 CFR part 430,
and organize the analytical methods for the Pulp, Paper, and Paperboard
category into one part, the Part 136 CWA methods tables, of the CFR.
    To help users more readily identify approved compliance monitoring
methods, EPA is proposing to cite at part 430 the Part 136 methods that
are approved for these pollutants: Chloroform, 2,3,7,8-
tetrachlorodibenzo-p-dioxin (TCDD), and 2,3,7,8- tetrachlorodibenzo-p-
furan (TCDF).

M. Proposed Revisions at 40 CFR 435

    EPA is proposing several changes to Part 435, Oil and Gas
Extraction Point Source Category. EPA is proposing to move, and in two
cases revise, the methods from 40 CFR part 435, subpart A (Offshore
Subcategory) to an EPA document (``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013), which is
included in the record for this rulemaking. This proposed approach
organizes the analytical methods for the Offshore Subcategory into one
document and allows for easier access to the methods for this category.
The following table lists the methods EPA proposes to move from Part
435 to the cited document, EPA-821-R-09-013.

 EPA Method Numbers for Oil and Gas Extraction Point Source Category Analytical Methods and Prior CFR References
----------------------------------------------------------------------------------------------------------------
                                          EPA method      Date first
        Analytical/test method              number        promulgated           Previous CFR  references
----------------------------------------------------------------------------------------------------------------
Static Sheen Test.....................            1617            1993  Subpart A, Appendix 1.
Drilling Fluids Toxicity Test.........            1619            1993  Subpart A, Appendix 2.
Procedure for Mixing Base Fluids With             1646            2001  Subpart A, Appendix 3.
 Sediments.
Protocol for the Determination of                 1647            2001  Subpart A, Appendix 4.
 Degradation of Non Aqueous Base
 Fluids in a Marine Closed Bottle
 Biodegradation Test System: Modified
 ISO 11734:1995.
Determination of Crude Oil                        1655            2001  Subpart A, Appendix 5.
 Contamination in Non-Aqueous Drilling
 Fluids by Gas Chromatography/Mass
 Spectrometry (GC/MS).
Reverse Phase Extraction (RPE) Method             1670            2001  Subpart A, Appendix 6.
 for Detection of Oil Contamination in
 Non-Aqueous Drilling Fluids (NAF).
Determination of the Amount of Non-               1674            2001  Subpart A, Appendix 7.
 Aqueous Drilling Fluid (NAF) Base
 Fluid from Drill Cuttings by a Retort
 Chamber (Derived from API Recommended
 Practice 13B-2).
----------------------------------------------------------------------------------------------------------------

    EPA is also proposing to incorporate additional quality assurance
procedures in the marine anaerobic biodegradation analytic method
(Appendix 4 of Subpart A of Part 435) and to correct some erroneous
references and omissions in the method for identification of crude oil
contamination (Appendix 5 of Subpart A of Part 435). EPA is proposing
to include these revisions in the EPA document (EPA-821-R-09-013).
    EPA promulgated the use of the marine anaerobic biodegradation
analytic method (closed bottle test, ISO 11734:1995 as clarified by
Appendix 4 to Subpart A of Part 435) in 2001 because it most closely
modeled the ability of a drilling fluid to biodegrade anaerobically in
marine environments (January 22, 2001; 66 FR 6864). Subsequent to this
promulgation, EPA incorporated additional quality assurance procedures
for the marine anaerobic biodegradation analytic method in the NPDES
permit for the Western Gulf of Mexico (``Final NPDES General Permit for
New and Existing Sources and New Dischargers in the Offshore
Subcategory of the Oil and Gas Extraction Category for the Western
Portion of the Outer Continental Shelf of the Gulf of Mexico,''
GMG290000, Appendix B). The additional quality assurance instructions
in the GMG290000 more clearly describe the sample preparation and
compliance determination steps. Specifically, these additional quality
assurance procedures clarify that users must only use headspace gas to
determine compliance with the Part 435 effluent guidelines.
    Additionally, EPA is proposing to correct some erroneous references
and omissions in the method for identification of crude oil
contamination (Appendix 5 of Subpart A of Part 435). Specifically, EPA
is proposing to:
    a. Add a schematic flow for qualitative identification of crude
oil, which was erroneously omitted in Appendix 5 to Subpart A of Part
435,
    b. Correct erroneous citations in sections 9.5, 9.6, 11.3, and
11.3.1 of Appendix 5, and
    c. Add a missing ``<'' sign for identification of crude oil
contamination in the asphaltene crude discussion at Section <IP_ADDRESS>.
The asphaltene discussion now reads as follows: ``Asphaltene crude oils
with API gravity < 20 may not produce chromatographic peaks strong
enough to show contamination at levels of the calibration. Extracted
ion peaks should be easier to see than increased intensities for the C8
to C13 peaks. If a sample of asphaltene crude from the formation is
available, a calibration standard shall be prepared.''
    As previously noted, EPA is proposing to include these revisions to
these two methods in the EPA document (EPA-821-R-09-013), which is
included in the record for this rulemaking.

III. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review

    This rule is not a ``significant regulatory action'' under the
terms of Executive Order (EO) 12866 (58 FR 51735, October 4, 1993) and
is therefore not subject to review under the EO.

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). This rule does not impose any
information collection, reporting, or recordkeeping requirements. This
rule merely adds new and updated versions of testing procedures, and
sample preservation requirements.

C. Regulatory Flexibility Act

    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 rule on small
entities for methods under the Clean Water Act, small entity is defined
as: (1) A small business that meets RFA default definitions (based on
SBA size standards) found in 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 less than 50,000; and
(3) a small organization that is any not-for-profit enterprise which is
independently owned and operated and is not dominant in its field.
    After considering the economic impacts of today's proposed rule on
small entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. This action
approves new and updated versions of testing procedures. Generally,
these changes will have a positive impact on small entities by
increasing method flexibility, thereby allowing entities to reduce
costs by choosing more cost-effective methods. In some cases,
analytical costs may increase slightly due to the additional QC
requirements included in the methods that are being approved to replace
older EPA methods. However, most laboratories that analyze samples

for EPA compliance monitoring have already instituted QC requirements
as part of their laboratory practices.
    We continue to be interested in the potential impacts of the
proposed rule on small entities and welcome comments on issues related
to such impacts.

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.
    EPA has determined that this rule contains no regulatory
requirements that might significantly or uniquely affect small
governments. Generally, this action will have a positive impact by
increasing method flexibility, thereby allowing method users to reduce
costs by choosing more cost effective methods. In some cases,
analytical costs may increase slightly due to changes in methods, but
these increases are neither significant nor unique to small
governments. This rule merely approves new and updated versions of
testing procedures. Thus, the proposed rule is not subject to the
requirements of Section 203 of UMRA.

E. Executive Order 13132: Federalism

    This proposed rule does not have federalism implications. It will
not have substantial direct effects on the States, on the relationship
between the national government and the States, or on the distribution
of power and responsibilities among the various levels of government,
as specified in Executive Order 13132 (64 FR 43255, Aug. 10, 1999).
This proposed rule merely approves new and updated versions of testing
procedures. The costs to State and local governments will be minimal
(in fact, governments may see a cost savings), and the rule does not
preempt State law. Thus, Executive Order 13132 does not apply to this
rule.
    In the spirit of Executive Order 13132, and consistent with EPA
policy to promote communications between EPA and State and local
governments, EPA specifically solicits comment on this proposed action
from State and local officials.

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

    This proposed rule does not have tribal implications, as specified
in Executive Order 13175, (65 FR 67249, Nov. 9, 2000). It will not have
substantial direct effects on Tribal governments, on the relationship
between the Federal government and Indian tribes, or on the
distribution of power and responsibilities between the Federal
government and Indian tribes. This rule merely approves new and updated
versions of testing procedures. The costs to Tribal governments will be
minimal (in fact, governments may see a cost savings), and the rule
does not preempt State law. Thus, Executive Order 13175 does not apply
to this rule.
    In the spirit of Executive Order 13175, and consistent with EPA
policy to promote communications between EPA and Indian tribes, EPA
specifically solicits comment on this proposed action from tribal
officials.

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. This action proposes to approve new
and updated versions of testing procedures.

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

    This action is not subject to Executive Order 13211, ``Actions
Concerning Regulations That Significantly Affect Energy Supply,
Distribution, or Use'' (66 FR 28355 (May 22, 2001)) because it is not a
significant regulatory action under Executive Order 12866.

I. National Technology Transfer and Advancement Act of 1995

    Section 12(d) of the National Technology Transfer and Advancement
Act of 1995, (NTTAA), Public Law 104-113, section 12(d) (15 U.S.C. 272
note), directs EPA to use voluntary consensus standards in its
regulatory activities unless to do so would be inconsistent with
applicable law or otherwise impractical. Voluntary consensus standards
are technical standards (e.g., material specifications, test methods,
sampling procedures, and business practices) that are developed or
adopted by voluntary consensus standard bodies. The NTTAA directs EPA
to provide Congress, through the OMB, explanations when the Agency
decides not to use available and applicable voluntary consensus
standards.
    This proposed rulemaking involves technical standards. As described
throughout this document, EPA is proposing many standards developed by
the Standard Methods Committee, and ASTM International. In Sections
IIB, IIC of this preamble, and the tables at Sec.  136.3, EPA specifies
these proposed methods, provides information on how to obtain copies of
these methods, and describes the rationale for employing these methods.
EPA welcomes comments on this aspect of the proposed rulemaking and,
specifically, invites the public to identify potentially applicable
voluntary consensus standards and to explain why EPA should include
such standards in future revisions to Part 136.

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.
    This proposed rule provides additional compliance methods for use
by any facility or laboratory with no disproportionate impact on
minority or low-income populations because it merely proposes to
approve new and updated versions of testing procedures to measure
pollutants in water.

IV. References

EPA 2006, ``Assessment of the Effects of Holding Time on Enterococci
Concentrations in Fresh and Marine Recreational Waters and
Escherichia coli Concentrations in Fresh Recreational Waters'' (EPA-
821-R-06-019, December 2006)
EPA 2010a, ``Method 1668A Interlaboratory Validation Study Report''
(EPA-820-R-10-004, March 2010)
EPA 2010b, ``Addendum to the Method 1668A Interlaboratory Validation
Study Report'' (EPA-820-R-10-003, March 2010)
EPA 2010c, ``Peer Review of the Method 1668A Interlaboratory
Validation Study'' (EPA 820-R-10-007, April 2010)
EPA 2010d, ``Development of Pooled Method Detection Limits (MDLs)
and Minimum Levels of Quantitation (MLs) for EPA Method 1668C (May
2010)
EPA 2010e, Errata for ``Short-term Methods for Estimating the
Chronic Toxicity of Effluents and Receiving Waters to Freshwater
Organisms'' (4th edition, October 2002) manual.

OSS 2009, ASTM D7575 ``Inter-Laboratory Study to Establish Precision
Statements for ASTM WK23240--Standard Test Method for Solvent-Free
Membrane Recoverable Oil and Grease by Infrared Determination''
Passaic River 2010 ``Summary of Passaic River Split Sample
Results'', EPA, April 2010
Test America 1 ``Acrolein Acrylonitrile Stability Study''
Test America 2 ``Acrolein Acrylonitrile Control Charts''

List of Subjects

40 CFR Part 136

    Environmental protection, Test procedures, Incorporation by
reference, Reporting and recordkeeping requirements, Water pollution
control.

40 CFR Part 260

    Environmental protection, Administrative practice and procedure,
Confidential business information, Hazardous waste, Incorporation by
reference, Reporting and recordkeeping requirements.

40 CFR Part 423

    Environmental protection, Steam Electric Power Generating Point
Source Category, Incorporation by reference, Reporting and
recordkeeping requirements, Water pollution control.

40 CFR Part 430

    Environmental protection, Pulp, Paper, and Paperboard Point Source
Category, Incorporation by reference, Reporting and recordkeeping
requirements, Water pollution control.

40 CFR Part 435

    Environmental protection, Oil and Gas Extraction Point Source
Category, Incorporation by reference, Reporting and recordkeeping
requirements, Water pollution control.

    Dated: August 6, 2010.
Lisa P. Jackson,
Administrator.
    For the reasons set out in the preamble, title 40, chapter I of the
Code of Federal Regulations, is proposed to be amended as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS

    1. The authority citation for part 136 continues to read as
follows:

    Authority:  Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217,
91 Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977.)

    2. Section 136.1 is amended by revising paragraph (a) to read as
follows:

Sec.  136.1  Applicability.

    (a) The procedures prescribed herein shall, except as noted in
Sec. Sec.  136.4, 136.5, and 136.6, be used to perform the measurements
indicated whenever the waste constituent specified is required to be
measured for:
    (1) An application submitted to the Administrator, or to a State
having an approved NPDES program for a permit under section 402 of the
Clean Water Act of 1977, as amended (CWA), and/or to reports required
to be submitted under NPDES permits or other requests for quantitative
or qualitative effluent data under parts 122 to 125 of title 40; and
    (2) Reports required to be submitted by dischargers under the NPDES
established by parts 124 and 125 of this chapter; and
    (3) Certifications issued by States pursuant to section 401 of the
CWA, as amended.
* * * * *
    3. Section 136.3 is amended:
    a. By revising paragraph (a) introductory text;
    b. In paragraph (a), revise Table IA, IB, IC, ID, IG, and IH;
    c. By revising paragraphs (b)(1), (b)(54), (b)(55), (b)(56),
(b)(59), (b)(60), (b)(61), (b)(70), and adding paragraph (b)(73);
    d. By revising paragraph (e) introductory text;
    e. In Table II to paragraph (e), by revising entries ``Table IA--
Bacterial Tests'', ``Table IA--Aquatic Toxicity Tests'', ``Table IH--
Bacterial Tests'', and ``Table IH--Protozoan Tests, and footnote 6''.
    These revisions and additions read as follows:

Sec.  136.3  Identification of test procedures.

    (a) Parameters or pollutants, for which methods are approved, are
listed together with test procedure descriptions and references in
Tables IA, IB, IC, ID, IE, IF, IG, and IH. In the event of a conflict
between the reporting requirements of 40 CFR parts 122 and 125 and any
reporting requirements associated with the methods listed in these
tables, the provisions of 40 CFR Parts 122 and 125 are controlling and
will determine a permittee's reporting requirements. The full text of
the referenced test procedures are incorporated by reference into
Tables IA, IB, IC, ID, IE, IF, IG, and IH. The incorporation by
reference of these documents, as specified in paragraph (b) of this
section, was approved by the Director of the Federal Register in
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of the
documents may be obtained from the sources listed in paragraph (b) of
this section. Documents may be inspected at EPA's Water Docket, EPA
West, 1301 Constitution Avenue, NW., Room 3334, Washington, DC
(Telephone:<PHONE_NUMBER>); or at the National Archives and Records
Administration (NARA). For information on the availability of this
material at NARA, call<PHONE_NUMBER>, or go to: http://www.archives.gov/
federal_register/code_of_federal_regulations/ibr_locations.html.
These test procedures are incorporated as they exist on the day of
approval and a notice of any change in these test procedures will be
published in the Federal Register. The discharge parameter values for
which reports are required must be determined by one of the standard
analytical test procedures incorporated by reference and described in
Tables IA, IB, IC, ID, IE, IF, IG, and IH or by any alternate test
procedure which has been approved by the Administrator under the
provisions of paragraph (d) of this section and Sec.  136.4. Under
certain circumstances paragraph (c) of this section, Sec.  136.5 or 40
CFR 401.13, other additional or alternate test procedures may be used.

                                     Table IA--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units               Method \1\                EPA              Standard methods         AOAC, ASTM, USGS              Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
    1. Coliform (fecal), number     Most Probable Number   p. 132 \3\...........  9221 C E-2006........
     per 100 mL or number per gram   (MPN), 5 tube, 3      1680 \11\, \13\......
     dry weight.                     dilution, or          1681 \11\, \18\......

                                    Membrane filter (MF)   p. 124 \3\...........  9222 D-1997..........  B-0050-85.\4\
                                     \2\, single step.
    2. Coliform (fecal) in          MPN, 5 tube, 3         p. 132 \3\...........  9221 C E-2006........
     presence of chlorine, number    dilution, or
     per 100 mL.
                                    MF \2\, single step..  p. 124 \3\...........  9222 D-1997..........
    3. Coliform (total), number     MPN, 5 tube, 3         p. 114 \3\...........  9221 B-2006..........
     per 100 mL.                     dilution, or
                                    MF \2\, single step    p. 108 \3\...........  9222 B-1997..........  B-0025-85.\4\
                                     or two step.
    4. Coliform (total), in         MPN, 5 tube, 3         p. 114 \3\...........  9221 B-2006..........
     presence of chlorine, number    dilution, or
     per 100 mL.
                                    MF \2\ with            p. 111 \3\...........  9222 (B+B.5c)-1997...
                                     enrichment.
    5. E. coli, number............  MPN \6\, \8\, \14\     .....................  9223 B-2004 \12\.....  991.15 \10\..............  Colilert[supreg]\12\
     per 100 mL.\19\..............   multiple tube/                                                                                , \16\
                                     multiple well.                                                                                Colilert-
                                                                                18[supreg].\12\
                                                                                ,\15\, \16\
                                    MF \2\, \5\, \6\,      1603 \20\............  .....................  .........................  mColiBlue-
                                     \7\, \8\ single step.                                                                           24[supreg].\17\
    6. Fecal streptococci, number   MPN, 5 tube, 3         p. 139 \3\...........  9230 B-2007..........
     per 100 mL.                     dilution,
                                    MF \2\, or...........  p. 136 \3\...........  9230 C-2007..........  B-0055-85.\4\
                                    Plate count..........  p. 143.\3\
    7. Enterococci, number per 100  MPN \6\ \8\, multiple  .....................  .....................  D6503-99 \9\.............  Enterolert[supreg].\
     mL.\19\......................   tube/multiple well.                                                                             12\ \22\
                                    MF \2\ \5\ \6\ \7\     1600.\23\
                                     \8\ single step.
    8. Salmonella, number per gram  MPN multiple tube....  1682.\21\
     dry.
     weight.\11\..................
Aquatic Toxicity:
    9. Toxicity, acute, fresh       Ceriodaphnia dubia     2002.0.\24\
     water organisms, LC50,          acute.
     percent effluent.
                                    Daphnia puplex and     2021.0.\24\
                                     Daphnia magna acute.
                                    Fathead minnow,        2000.0.\24\
                                     Pimephales promelas,
                                     and Bannerfin
                                     shiner, Cyprinella
                                     leedsi, acute.
                                    Rainbow Trout,         2019.0.\24\
                                     Oncorhynchus mykiss,
                                     and brook trout,
                                     Salvelinus
                                     fontinalis, acute.
    10. Toxicity, acute, estuarine  Mysid, Mysidopsis      2007.0.\24\
     and marine organisms of the     bahia, acute.
     Atlantic Ocean and Gulf of
     Mexico, LC50, percent
     effluent.
                                    Sheepshead Minnow,     2004.0.\24\
                                     Cyprinodon
                                     variegatus, acute.
                                    Silverside, Menidia    2006.0.\24\
                                     beryllina, Menidia
                                     menidia, and Menidia
                                     peninsulae, acute.

    11. Toxicity, chronic, fresh    Fathead minnow,        1000.0.\25\
     water organisms, NOEC or        Pimephales promelas,
     IC25, percent effluent.         larval survival and
                                     growth.
                                    Fathead minnow,        1001.0.\25\
                                     Pimephales promelas,
                                     embryo-larval
                                     survival and
                                     teratogenicity.
                                    Daphnia, Ceriodaphnia  1002.0.\25\
                                     dubia, survival and
                                     reproduction.
                                    Green alga,            1003.0.\25\
                                     Selenastrum
                                     capricornutum,
                                     growth.
    12. Toxicity, chronic,          Sheepshead minnow,     1004.0.\26\
     estuarine and marine            Cyprinodon
     organisms of the Atlantic       variegatus, larval
     Ocean and Gulf of Mexico,       survival and growth.
     NOEC or IC25, percent
     effluent.
                                    Sheepshead minnow,     1005.0.\26\
                                     Cyprinodon
                                     variegatus, embryo-
                                     larval survival and
                                     teratogenicity.
                                    Inland silverside,     1006.0.\26\
                                     Menidia beryllina,
                                     larval survival and
                                     growth.
                                    Mysid, Mysidopsis      1007.0.\26\
                                     bahia, survival,
                                     growth, and
                                     fecundity.
                                    Sea urchin, Arbacia    1008.0.\26\
                                     punctulata,
                                     fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
  Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.
\4\ USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and
  Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of the Interior, Reston, VA.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
  organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
  results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. ASTM International. 100 Barr Harbor Drive,
  West Conshohocken, PA 19428.
\10\ AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists
  International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.
\11\ Recommended for enumeration of target organism in sewage sludge.
\12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
  glucuronidase produced by E. coli.
\13\ USEPA. April 2010. Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC
  Medium. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-10-003.
\14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg], Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories, Inc. 1 IDEXX Drive, Westbrook, ME 04092.

\17\ A description of the mColiBlue24[supreg] test, is available from Hach Company. 100 Dayton Ave., Ames, IA 50010.
\18\ USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. U.S. Environmental
  Protection Agency, Office of Water, Washington, DC, EPA-821-R-06-013.
\19\ Recommended for enumeration of target organism in wastewater effluent.
\20\ USEPA. December 2009. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia
  coli Agar (modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-09-007.
\21\ USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. U.S.
  Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-06-014.
\22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\23\ USEPA. December 2009. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI).
  U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-09-016.
\24\ USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition.
  U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/012.
\25\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth