[Federal Register Volume 75, Number 184 (Thursday, September 23, 2010)]
[Proposed Rules]
[Pages 58024-58076]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2010-20018]
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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
Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 /
Proposed Rules
[[Page 58024]]
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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 protected], 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 202-566-2426.
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 202-566-1744, and the
telephone number for the Water Docket is 202-566-2426.
FOR FURTHER INFORMATION CONTACT: Lemuel Walker, Engineering and
Analysis Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave., NW., Washington, DC 20460, 202-566-1077, (e-mail:
[email protected]), or Meghan Hessenauer, Engineering and Analysis
Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave., NW., Washington, DC 20460, 202-566-1040 (e-mail:
[email protected]).
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
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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
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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
[[Page 58028]]
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
[[Page 58029]]
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
[[Page 58030]]
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
[[Page 58031]]
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
[[Page 58032]]
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
[[Page 58033]]
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
[[Page 58034]]
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
[[Page 58035]]
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
[[Page 58036]]
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.
[[Page 58037]]
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 11.5.4.2.
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
[[Page 58038]]
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.
[[Page 58039]]
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: 202-566-2426); or at the National Archives and Records
Administration (NARA). For information on the availability of this
material at NARA, call 202-741-6030, 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\......
[[Page 58040]]
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.
[[Page 58041]]
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.
[[Page 58042]]
\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
Edition, U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/013.
\26\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms.
Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/014.
Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter Methodology \58\ EPA \52\ Standard methods ASTM USGS/AOAC/other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L......... Electrometric endpoint ...................... 2310 B-1997.......... D1067-06............. I-1020-85.\2\
or phenolphthalein
endpoint.
2. Alkalinity, as CaCO3, mg/L...... Electrometric or ...................... 2320 B-1997.......... D1067-06............. 973.43,\3\ I-1030-
Colorimetric 85.\2\
titration to pH 4.5,
Manual.
Automatic............. 310.2 (Rev. 1974) \1\. ..................... ..................... I-2030-85.\2\
3. Aluminum--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999 or E-1999 ..................... I-3051-85.\2\
aspiration \36\.
AA furnace......... ...................... 3113-2004............
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
Direct Current ...................... ..................... D4190-08............. See footnote.\34\
Plasma (DCP) \36\.
Colorimetric ...................... 3500-Al B-2001.......
(Eriochrome
cyanine R).
4. Ammonia (as N), mg/L............ Manual distillation 350.1, Rev. 2.0 (1993) 4500-NH3 B-1997...... ..................... 973.49.\3\
\6\ or gas diffusion
(pH > 11) followed by
any of the following:
Nesslerization..... ...................... ..................... D1426-08 (A)......... 973.49,\3\ I-3520-
85.\2\
Titration.......... ...................... 4500-NH3 C-1997......
Electrode.......... ...................... 4500-NH3 D-1997 or E- D1426-08 (B).........
1997.
Manual phenate, ...................... 4500-NH3 F-1997...... ..................... See Footnote.\60\
salicylate, or
other substituted
phenols in
Berthelot reaction
based methods.
Automated phenate, 350.1,\30\ Rev. 2.0 4500-NH3 G-1997 4500- ..................... I-4523-85.\2\
salicylate, or (1993). NH3 H-1997.
other substituted
phenols in
Berthelot reaction
based methods.
Automated electrode ...................... ..................... ..................... See footnote 7.
Ion Chromatography. ...................... ..................... D6919-09.............
5. Antimony--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration \36\.
AA furnace......... ...................... 3113-2004............
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
[[Page 58043]]
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
6. Arsenic--Total,\4\ mg/L......... Digestion \4\ followed 206.5 (Issued
by any of the 1978).\1\
following:
AA gaseous hydride. ...................... 3114 B-2009 or C-2009 D2972-08 (B)......... I-3062-85.\2\
AA furnace......... ...................... 3113-2004............ D2972-08 (C)......... I-4063-98.\49\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07.............
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
Colorimetric (SDDC) ...................... 3500-As B-1997....... D2972-08 (A)......... I-3060-85.\2\
7. Barium--Total,\4\ mg/L.......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999.......... ..................... I-3084-85.\2\
aspiration \36\.
AA furnace......... ...................... 3113-2004............ D4382-02(07). .....................
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ ..................... I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP \36\........... ...................... ..................... ..................... See footnote.\34\
8. Beryllium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999 or E-1999 D3645-08 (A)......... I-3095-85.\2\
aspiration.
AA furnace......... ...................... 3113-2004............ D3645-08 (B).........
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP................ ...................... ..................... D4190-08............. See footnote.\34\
Colorimetric ...................... ..................... ..................... See footnote.\61\
(aluminon).
9. Biochemical oxygen demand Dissolved Oxygen ...................... 5210 B-2001.......... D888-09.............. 973.44,\3\ p. 17,\9\
(BOD5), mg/L. Depletion. I-1578-78,\8\ See
footnote.\10\ \63\
10. Boron--Total,\37\ mg/L......... Colorimetric ...................... 4500-B B-2000........ ..................... I-3112-85.\2\
(curcumin).
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP................ ...................... ..................... D4190-08............. See footnote.\34\
11. Bromide, mg/L.................. Electrode............. ...................... ..................... D1246-05............. I-1125-85.\2\
Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000, C-2000, D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0 D-2000.
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
12. Cadmium--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D3557-02(07) (A or B) 974.27,\3\ p. 37.\9\,
aspiration \36\. I-3135-85 \2\ or
I-3136-85.\2\
AA furnace......... ...................... 3113-1999............ D3557-02(07) (D)..... I-4138-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-1472-85 \2\ or
(2003); 200.7, Rev. I-4471-97.\50\
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
Voltametry \11\.... ...................... ..................... D3557-02(07)(C)......
[[Page 58044]]
Colorimetric ...................... 3500 Cd-D 1990.......
(Dithizone).
13. Calcium--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... D511-08(B)........... I-3152-85.\2\
aspiration.
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ ..................... I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
DCP................ ...................... ..................... ..................... See footnote.\34\
Titrimetric (EDTA). ...................... 3500-Ca-1997......... D511-08(A)...........
Ion Chromatography. ...................... ..................... D6919-09.............
14. Carbonaceous biochemical oxygen Dissolved Oxygen ...................... 5210 B-2001.......... D888-09.............. See footnote.\35\
demand (CBOD5), mg/L.\12\ Depletion with \63\
nitrification
inhibitor.
15. Chemical oxygen demand (COD), Titrimetric........... 410.3 (Rev. 1978) \1\. 5220 B-1997 or C-1997 D1252-06 (A)......... 973.46,\3\ p. 17 \9\
mg/L. I-3560-85.\2\
Spectrophotometric, 410.4, Rev. 2.0 (1993) 5220 D-1997.......... D1252-06 (B)......... See footnotes.\13\
manual or automatic. \14\
I-3561-85.\2\
16. Chloride, mg/L................. Titrimetric: (silver ...................... 4500-Cl- B-1997...... D512-04 (B).......... I-1183-85.\2\
nitrate).
(Mercuric nitrate).... ...................... 4500-Cl- C-1997...... D512-04 (A).......... 973.51,\3\ I-1184-
85.\2\
Colorimetric: manual.. ...................... ..................... ..................... I-1187-85.\2\
Automated ...................... 4500-Cl- E-1997...... ..................... I-2187-85.\2\
(Ferricyanide).
Potentiometric ...................... 4500-Cl- D-1997......
Titration.
Ion Selective ...................... ..................... D512-04 (C)..........
Electrode.
Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30,\3\ I-2057-
and 300.1, Rev. 1.0 90.\51\
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
17. Chlorine--Total residual, mg/L. Amperometric direct... ...................... 4500-Cl D-2000....... D1253-08.............
Amperometric direct ...................... 4500-Cl E-2000.......
(low level).
Iodometric direct..... ...................... 4500-Cl B-2000.......
Back titration ether ...................... 4500-Cl C-2000.......
end-point \15\.
DPD-FAS............... ...................... 4500-Cl F-2000.......
Spectrophotometric, ...................... 4500-Cl G-2000.......
DPD.
Electrode............. ...................... ..................... ..................... See footnote.\16\
17A. Chlorine--Free Available, mg/L Amperometric direct... ...................... 4500-Cl D-2000....... D1253-08.............
Amperometric direct ...................... 4500-Cl E-2000.......
(low level).
DPD-FAS............... ...................... 4500-Cl F-2000.......
Spectrophotometric, ...................... 4500-Cl G-2000.......
DPD.
18. Chromium VI dissolved, mg/L.... 0.45-micron Filtration
followed by any of
the following:
AA chelation- ...................... 3111 C-1999.......... ..................... I-1232-85.\2\
extraction.
Ion Chromatography. 218.6, Rev. 3.3 (1994) 3500-Cr C-2009....... D5257-03............. 993.23.
Colorimetric ...................... 3500-Cr B-2009....... D1687-02(07)(A)...... I-1230-85.\2\
(Diphenyl-
carbazide).
19. Chromium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... D1687-02(07) (B)..... 974.27,\3\ I-3236-
aspiration \36\. 85.\2\
AA chelation- ...................... 3111 C-1999..........
extraction.
AA furnace......... ...................... 3113-1999............ D1687-02(07)(C)...... I-3233-93.\46\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
[[Page 58045]]
Colorimetric ...................... 3500-Cr B-2009.......
(Diphenyl-
carbazide).
20. Cobalt--Total,\4\ mg/L......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D3558-08 (A or B).... p. 37,\9\ I-3239-
aspiration. 85.\2\
AA furnace......... ...................... 3113-2004............ D3558-08 (C)......... I-4243-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07............. I-4471-97.\50\
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
DCP................ ...................... ..................... D4190-08............. See footnote.\34\
21. Color, platinum cobalt units or Colorimetric (ADMI)... ...................... ..................... ..................... See footnote.\18\
dominant wavelength, hue,
luminance purity.
(Platinum cobalt)..... ...................... 2120 B-2001.......... ..................... I-1250-85.\2\
Spectrophotometric....
22. Copper--Total,\4\ mg/L......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D1688-07 (A or B).... 974.27 \3\ p. 37 \9\
aspiration.\36\ I-3270-85 \2\ or
I-3271-85.\2\
AA furnace......... ...................... 3113-2004............ D1688-07 (C)......... I-4274-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
Colorimetric ...................... 3500-Cu B-1999.......
(Neocuproine).
(Bathocuproine).... ...................... 3500-Cu C-1999....... ..................... See footnote.\19\
23. Cyanide--Total, mg/L........... Automated UV digestion/ ...................... ..................... ..................... Kelada-01.\55\
distillation and
Colorimetry.
Segmented Flow ...................... ..................... D7511-09e2...........
Injection, In-Line
Ultraviolet Digestion
followed by gas
diffusion amperometry.
Manual distillation 335.4, Rev. 1.0 (1993) 4500-CN- B-1999 or C- D2036-09(A), D7284-08 10-204-00-1-X.\56\
with MgCl2 followed \57\. 1999.
by any of the
following:
Flow Injection, gas ...................... ..................... D2036-09(A) D7284-08.
diffusion
amperometry.
Titrimetric........ ...................... 4500-CN- D-1999...... D2036-09(A).......... p. 22.\9\
Spectrophotometric, ...................... 4500-CN- E-1999...... D2036-09(A).......... I-3300-85.\2\
manual.
Semi-Automated \20\ 335.4, Rev. 1.0 (1993) ..................... ..................... 10-204-00-1-X,\56\ I-
\57\. 4302-85.\2\
Ion Chromatography. ...................... ..................... D2036-09(A)..........
Ion Selective ...................... 4500-CN- F-1999...... D2036-09(A)..........
Electrode.
24. Cyanide-Available, mg/L........ Cyanide Amenable to ...................... 4500-CN- G-1999...... D2036-09(B)..........
Chlorination (CATC);
Manual distillation
with MgCl2 followed
by Titrimetric or
Spectrophotometric.
Flow injection and ...................... ..................... D6888-09............. OIA-1677-09.\44\
ligand exchange,
followed by gas
diffusion amperometry
\59\.
[[Page 58046]]
Automated Distillation ...................... ..................... ..................... Kelada-01.\55\
and Colorimetry (no
UV digestion).
24.A Cyanide-Free, mg/L............ Flow Injection, ...................... ..................... D7237-10............. OIA-1677-09.\44\
followed by gas
diffusion amperometry.
Manual micro-diffusion ...................... ..................... D4282-02.............
and colorimetry.
25. Fluoride--Total, mg/L.......... Manual distillation ...................... 4500-F- B-1997.......
\6\ followed by any
of the following:
Electrode, manual.. ...................... 4500-F- C-1997....... D1179-04(B)..........
Electrode, ...................... ..................... ..................... I-4327-85.\2\
automated.
Colorimetric, ...................... 4500-F- D-1997....... D1179-04(A)..........
(SPADNS).
Automated ...................... 4500-F- E-1997.......
complexone.
Ion Chromatography. 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0
(1997).
CIE/UV............. ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
26. Gold--Total,\4\ mg/L........... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration,.
AA furnace,........ 231.2 (Rev. 1978) \1\. 3113-2004............
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
DCP................ ...................... ..................... ..................... See footnote.\34\
27. Hardness--Total, as CaCO3, mg/L Automated 130.1 (Issued 1971)
colorimetric,. \1\.
Titrimetric (EDTA).... ...................... 2340 C-1997.......... D1126-02(07)......... 973.5 2B,\3\ I-1338-
85.\2\
Ca plus Mg as their ...................... 2340 B-1997..........
carbonates, by
inductively coupled
plasma or AA direct
aspiration. (See
Parameters 13 and 33).
28. Hydrogen ion (pH), pH units.... Electrometric ...................... 4500-H\+\-2000....... D1293-99 (A or B).... 973.41,\3\ I-1586-
measurement. 85.\2\
Automated electrode... 150.2 (Dec. 1982) \1\. ..................... ..................... See footnote,\21\
I-2587-85.\2\
29. Iridium--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration.
AA furnace......... 235.2 (Issued
1978).\1\
ICP/MS............. ...................... 3125-2009............
30. Iron--Total,\4\ mg/L........... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D1068-05 (A or B).... 974.27,\3\ I-3381-
aspiration \36\. 85.\2\
AA furnace......... ...................... 3113-1999............ D1068-05(C)..........
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
Colorimetric ...................... 3500-Fe-1997......... D1068-05 (D)......... See footnote.\22\
(Phenanthroline).
31. Kjeldahl Nitrogen \5\--Total, Manual digestion \20\ ...................... 4500-Norg B-1997 or C- D3590-02(06)(A)...... I-4515-91.\45\
(as N), mg/L. and distillation or 1997 and 4500-NH3 B-
gas diffusion 1997.
followed by any of
the following:
Titration.......... ...................... 4500-NH3 C-1997...... ..................... 973.48.\3\
Nesslerization..... ...................... ..................... D1426-08(A)..........
Electrode.......... ...................... 4500-NH3 D-1997 or E- D1426-08(B)..........
1997.
[[Page 58047]]
Semi-automated 350.1 Rev. 2.0 1993... 4500-NH3 G-1997 4500-
phenate. NH3 H-1997.
Manual phenate, ...................... 4500-NH3 F-1997...... ..................... See Footnote.\60\
salicylate, or
other substituted
phenols in
Berthelot reaction
based methods.
--------------------------------------------------------------------------------------------------------------------
Automated Methods for TKN that do not require manual distillation
--------------------------------------------------------------------------------------------------------------------
Automated phenate, 351.1, (Rev. 1978) \1\ ..................... ..................... I-4551-78.\8\
salicylate, or other
substituted phenols
in Berthelot reaction
based methods
colorimetric (auto
digestion and
distillation).
Semi-automated block 351.2, Rev. 2.0 (1993) 4500-Norg D-1997..... D3590-02(06) (B)..... I-4515-91.\45\
digestor colorimetric
(distillation not
required).
Block digester, ...................... ..................... ..................... See footnote.\39\
followed by Auto
distillation and
Titration.
Block digester, ...................... ..................... ..................... See footnote.\40\
followed by Auto
distillation and
Nesslerization.
Block Digester, ...................... ..................... ..................... See footnote.\41\
followed by Flow
injection gas
diffusion
(distillation not
required).
32. Lead--Total,\4\ mg/L........... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D3559-08(A or B)..... 974.27,\3\ I-3399-
aspiration.\36\ 85.\2\
AA furnace......... ...................... 3113-1999............ D3559-08(D).......... I-4403-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
Voltametry \11\.... ...................... ..................... D3559-08(C)..........
Colorimetric ...................... 3500-Pb B-1997.......
(Dithizone).
33. Magnesium--Total,\4\ mg/L...... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... D511-08(B)........... 974.27,\3\ I-3447-
aspiration. 85.\2\
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
DCP................ ...................... ..................... ..................... See footnote.\34\
Gravimetric........
Ion Chromatography. ...................... ..................... D6919-09.............
34. Manganese--Total,\4\ mg/L...... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... D858-07(A or B)...... 974.27,\3\ I-3454-
aspiration \36\. 85.\2\
AA furnace......... ...................... 3113-2004............ D858-07(C)...........
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
[[Page 58048]]
Colorimetric ...................... 3500-Mn B-1999....... ..................... 920.203.\3\
(Persulfate).
(Periodate)........ ...................... ..................... ..................... See footnote.\23\
35. Mercury--Total,\4\ mg/L........ Cold vapor, Manual.... 245.1, Rev. 3.0 (1994) 3112-2009............ D3223-07............. 977.22,\3\ I-3462-
85.\2\
Cold vapor, Automated. 245.2 (Issued 1974)...
Cold vapor atomic 245.7, Rev. 2.0 (2005) ..................... ..................... I-4464-01.
fluorescence \17\.
spectrometry (CVAFS).
Purge and Trap CVAFS.. 1631E.\43\
ICP/AES \36\.......... 200.7, Rev. 4.4 (1994) 3120-1999............ ..................... I-4471-97.\50\
ICP/MS................ ...................... 3125-2009............
36. Molybdenum--Total,\4\ mg/L..... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999.......... ..................... I-3490-85.\2\
aspiration.
AA furnace......... ...................... 3113-2004............ ..................... I-3492-96.\47\
ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07............. I-4471-97.\50\
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP................ ...................... ..................... ..................... See footnote.\34\
37. Nickel--Total,\4\ mg/L......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D1886-08(A or B)..... I-3499-85.\2\
aspiration \36\.
AA furnace......... ...................... 3113-2004............ D1886-08(C).......... I-4503-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
38. Nitrate (as N), mg/L........... Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
Ion Selective ...................... 4500-NO3- D-2000.....
Electrode.
Colorimetric (Brucine 352.1 \1\............. ..................... ..................... 973.50,\3\ 419D,\1\
sulfate). \7\ p. 28.\9\
Nitrate-nitrite N ...................... ..................... ..................... See footnote.\62\
minus Nitrite N (See
parameters 39 and 40).
39. Nitrate-nitrite (as N), mg/L... Cadmium reduction, ...................... 4500-NO3- E-2000..... D3867-04(B)..........
Manual.
Cadmium reduction, 353.2, Rev. 2.0 (1993) 4500-NO3- F-2000..... D3867-04(A).......... I-2545-90.\2\
Automated.
Automated hydrazine... ...................... 4500-NO3- H-2000.....
Reduction/Colorimetric ...................... ..................... ..................... See footnote.\62\
Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
40. Nitrite (as N), mg/L........... Spectrophotometric: ...................... 4500-NO2- B-2000..... ..................... See footnote.\25\
Manual.
Automated ...................... ..................... ..................... I-4540-85,\2\ See
(Diazotization). footnote.\62\
Automated (*bypass 353.2, Rev. 2.0 (1993) 4500-NO3- F-2000..... D3867-04 (A)......... I-4545-85.\2\
cadmium reduction).
Manual (*bypass ...................... 4500-NO3- E-2000..... D3867-04 (B).........
cadmium reduction).
Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev.2.\54\
41. Oil and grease--Total Hexane extractable 1664B \42\............ 5520 B-2001.\38\
recoverable, mg/L. material (HEM): n-
Hexane extraction and
gravimetry.
[[Page 58049]]
Silica gel treated HEM 1664B \42\............ 5520 B-2001 \38\ and
(SGT-HEM): Silica gel 5520 F-2001.\38\
treatment and
gravimetry.
42. Organic carbon--Total (TOC), mg/ Combustion............ ...................... 5310 B-2000.......... D7573-09............. 973.47,\3\ p. 14.\24\
L.
Heated persulfate or ...................... 5310 C 2000 5310 D D4839-03............. 973.47,\3\ p. 14.\24\
UV persulfate 2000.
oxidation.
43. Organic nitrogen (as N), mg/L.. Total Kjeldahl N
(Parameter 31) minus
ammonia N (Parameter
4).
44. Orthophosphate (as P), mg/L.... Ascorbic acid method:
Automated.......... 365.1, Rev. 2.0 (1993) 4500-P F-1999 or G- ..................... 973.56,\3\ I-4601-
1999. 85.\2\
Manual single ...................... 4500-P E-1999........ D515-88(A)........... 973.55.\3\
reagent.
Manual two reagent. 365.3 (Issued
1978).\1\
Ion Chromatography. 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30.\3\
and 300.1, Rev. 1.0
(1997).
CIE/UV............. ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
45. Osmium--Total,\4\ mg/L......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999..........
aspiration.
AA furnace......... 252.2 (Issued 1978)
\1\
46. Oxygen, dissolved, mg/L........ Winkler (Azide ...................... 4500-O B-2001, C- D888-09(A)........... 973.45B,\3\ I-1575-
modification). 2001, D-2001, E- 78.\8\
2001, F-2001.
Electrode............. ...................... 4500-O G-2001........ D888-09(B)........... I-1576-78.\8\
Luminescence Based ...................... ..................... D888-09 \68\ (C)..... See footnote \63\
Sensor. \68\ See
footnote.\64\
47. Palladium--Total,\4\ mg/L...... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration.
AA furnace......... 253.2 \1\ (Issued
1978).
ICP/MS............. ...................... 3125-2009............
DCP................ ...................... ..................... ..................... See footnote.\34\
48. Phenols, mg/L.................. Manual distillation 420.1 \1\ (Rev. 1978). 5530B-2005........... D1783-01.............
\26\ followed by any
of the following:
Colorimetric (4AAP) 420.1 \1\ (Rev. 1978). 5530D-2005 \27\...... D1783-01(A or B).....
manual.
Automated 420.4, Rev. 1.0 (1993)
colorimetric
(4AAP).
49. Phosphorus (elemental), mg/L... Gas-liquid ...................... ..................... ..................... See footnote.\28\
chromatography.
50. Phosphorus--Total, mg/L........ Persulfate digestion ...................... 4500-P B(5)-1999..... ..................... 973.55.\3\
\20\ followed by any
of the following:
Manual............. 365.3 \1\ (Issued 4500-P E-1999........ D515-88(A)...........
1978).
Automated ascorbic 365.1, Rev. 2.0 (1993) 4500-P F-1999, G- ..................... 973.56,\3\ I-4600-
acid reduction. 1999, H-1999. 85.\2\
ICP/AES \4\ \36\... 200.7, Rev. 4.4 (1994) 3120-1999............ ..................... I-4471-97.\50\
Semi-automated 365.4 \1\ (Issued ..................... D515-88(B)........... I-4610-91.\48\
block digestor 1974).
(TKP digestion).
51. Platinum--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration.
AA furnace......... 255.2.\1\
ICP/MS............. ...................... 3125-2009............
DCP................ ...................... ..................... ..................... See footnote.\34\
52. Potassium--Total,\4\ mg/L...... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... ..................... 973.53,\3\ I-3630-
aspiration. 85.\2\
[[Page 58050]]
ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
Flame photometric.. ...................... 3500-K B-1997........
Electrode.......... ...................... 3500-K C-1997........
Ion Chromatography. ...................... ..................... D6919-09.............
53. Residue--Total, mg/L........... Gravimetric, 103- ...................... 2540 B-1997.......... ..................... I-3750-85.\2\
105[deg].
54. Residue--filterable, mg/L...... Gravimetric, 180[deg]. ...................... 2540 C-1997.......... D5907-03............. I-1750-85.\2\
55. Residue--non-filterable (TSS), Gravimetric, 103- ...................... 2540 D-1997.......... D5907-03............. I-3765-85.\2\
mg/L. 105[deg] post washing
of residue.
56. Residue--settleable, mg/L...... Volumetric, (Imhoff ...................... 2540 F-1997..........
cone), or gravimetric.
57. Residue--Volatile, mg/L........ Gravimetric, 550[deg]. 160.4 \1\............. 2540-E-1997.......... ..................... I-3753-85.\2\
58. Rhodium--Total,\4\ mg/L........ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration, or.
AA furnace......... 265.2.\1\
ICP/MS............. ...................... 3125-2009............
59. Ruthenium--Total,\4\ mg/L...... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration, or.
AA furnace......... 267.2.\1\
ICP/MS............. ...................... 3125-2009............
60. Selenium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA furnace......... ...................... 3113-2004............ D3859-08 (B)......... I-4668-98.\49\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07.............
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05
AA gaseous hydride. ...................... 3114 B-2009, or C- D3859-08 (A)......... I-3667-85.\2\
2009.
61. Silica--Dissolved,\37\ mg/L.... 0.45 micron filtration
followed by any of
the following:
Colorimetric, ...................... 4500-SiO2 C-1997..... D859-05.............. I-1700-85.\2\
Manual.
Automated ...................... 4500-SiO2 E-1997 or F- ..................... I-2700-85.\2\
(Molybdosilicate). 1997.
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ ..................... I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
62. Silver--Total,4 31 mg/L........ Digestion 4 29
followed by any of
the following:
AA direct ...................... 3111 B-1999 or C-1999 ..................... 974.27,\3\ p. 37,\9\
aspiration. I-3720-85.\2\
AA furnace......... ...................... 3113 -1999........... ..................... I-4724-89.\51\
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
DCP................ ...................... ..................... ..................... See footnote.\34\
63. Sodium--Total,\4\ mg/L......... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... ..................... 973.54,\3\ I-3735-
aspiration. 85.\2\
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ ..................... I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
[[Page 58051]]
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
DCP................ ...................... ..................... ..................... See footnote.\34\
Flame photometric.. ...................... 3500-Na B-1997.......
Ion Chromatography. ...................... ..................... D6919-09.............
64. Specific conductance, micromhos/ Wheatstone bridge..... 120.1 \1\ (Rev. 1982). 2510 -1997........... D1125-99 (A)......... 973.40,\3\ I-2781-
cm at 25 [deg]C. 85.\2\
65. Sulfate (as SO4), mg/L......... Automated colorimetric 375.2, Rev. 2.0 (1993) 4500-SO42- F-1997 or
G-1997.
Gravimetric........... ...................... 4500-SO42- C-1997 or ..................... 925.54.\3\
D-1997.
Turbidimetric......... ...................... 4500-SO42- E-1997.... D516-07..............
Ion Chromatography.... 300.0, Rev. 2.1 (1993) 4110 B-2000 or C-2000 D4327-03............. 993.30,\3\ I-4020-05.
and 300.1, Rev. 1.0
(1997).
CIE/UV................ ...................... 4140-1997............ D6508-00(05)......... D6508, Rev. 2.\54\
66. Sulfide (as S), mg/L........... Sample Pretreatment... ...................... 4500-S 2- B, C-2000..
Titrimetric (iodine).. ...................... 4500-S 2- F-2000..... ..................... I-3840-85.\2\
Colorimetric ...................... 4500-S 2- D-2000.....
(methylene blue).
Ion Selective ...................... 4500-S 2- G-2000..... D4658-08.............
Electrode.
67. Sulfite (as SO3), mg/L......... Titrimetric (iodine- ...................... 4500-SO32- B-2000....
iodate).
68. Surfactants, mg/L.............. Colorimetric ...................... 5540 C-2000.......... D2330-02.............
(methylene blue).
69. Temperature, [deg]C............ Thermometric.......... ...................... 2550 B-2000.......... ..................... See footnote.\32\
70. Thallium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999..........
aspiration.
AA furnace......... 279.2 \1\ (Issued 3113-2004............
1978).
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES............ 200.7, Rev. 4.4 (1994) 3120-1999............ D1976-07.............
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4471-
97.\50\
71. Tin--Total,\4\ mg/L............ Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999.......... ..................... I-3850-78.\8\
aspiration.
AA furnace......... ...................... 3113-2004............
STGFAA............. 200.9, Rev. 2.2 (1994)
ICP/AES............ 200.5, Rev. 4.2
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
72. Titanium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999..........
aspiration.
AA furnace......... 283.2 \1\(Issued 1978)
DCP................ ...................... ..................... ..................... See footnote.\34\
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14.\3\
73. Turbidity, NTU \53\............ Nephelometric......... 180.1, Rev. 2.0 (1993) 2130-2001............ D1889-00............. I-3860-85.\2\ See
footnote.\65\ See
footnote.\66\ See
footnote.\67\
74. Vanadium--Total,\4\ mg/L....... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 D-1999..........
aspiration.
AA furnace......... ...................... 3113-2004............ D3373-03(07).........
ICP/AES............ 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
DCP................ ...................... ..................... D4190-08............. See footnote.\34\
[[Page 58052]]
Colorimetric ...................... 3500-V B-1997........
(Gallic Acid).
75. Zinc--Total,\4\ mg/L........... Digestion \4\ followed
by any of the
following:
AA direct ...................... 3111 B-1999 or C-1999 D1691-02(07) (A or B) 974.27,\3\ p. 37,\9\
aspiration \36\. I-3900-85.\2\
AA furnace......... 289.2\1\ (Issued 1978)
ICP/AES \36\....... 200.5, Rev. 4.2 3120-1999............ D1976-07............. I-4471-97.\50\
(2003); 200.7, Rev.
4.4 (1994).
ICP/MS............. 200.8, Rev. 5.4 (1994) 3125-2009............ D5673-05............. 993.14,\3\ I-4020-05.
DCP \36\........... ...................... ..................... D4190-08............. See footnote.\34\
Colorimetric
(Dithizone).
(Zincon)........... ...................... 3500-Zn-1997......... ..................... See footnote.\33\
76. Acid Mine Drainage............. ...................... 1627..................
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory--Cincinnati
(EMSL-CI), EPA-600/4-79-020 (NTIS PB 84-128677), Revised March 1983 and 1979 where applicable.
\2\ Fishman, M. J., et al. ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques
of Water-Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' Methods Manual, Sixteenth Edition, 4th Revision, 1998.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion
procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable
form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in
Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to
gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a
combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as
Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in
EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain
elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic
absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced
method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission
spectrometry (ICP-AES), the direct current plasma (DCP) technique or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use
EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB);
the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the
digestion procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation
step is not necessary: however, manual distillation will be required to resolve any controversies. In general, the analytical method should be
consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to
evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation
step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future
analysis. Comparable is defined as <20% RPD for all tested matrices). Alternatively the two populations of spike recovery percentages may be compared
using a recognized statistical test.
\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran &
Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.
\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5,
Chapter A1 (1979).
\9\ American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd St., New York, NY 10036.
\10\ In-Situ Method 1003-8-2009, ``Biochemical Oxygen Demand (BOD) Measurement by Optical Probe''. Available from In-Situ, Incorporated, 221 E. Lincoln
Avenue, Ft. Collins, CO 80524, Telephone: 970-498-1500.
\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\ Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ``total BOD.'' The
addition of the nitrification inhibitor is not a procedural option, but must be included to report the CBOD5 parameter. A discharger whose permit
requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's
permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 151 Graham Road, P.O. Box 9010, College Station, TX 77842.
\14\ Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\15\ The back titration method will be used to resolve controversy.
\16\ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA
02138. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing
0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
\17\ Method 245.7, Rev. 2.0, ``Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,'' February 2005, EPA-821-R-05-001, available from the
U.S. EPA Sample Control Center (operated by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100, Fax: 703-461-8056.
\18\ National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971.
\19\ Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\20\ When using a method with block digestion, this treatment is not required.
\21\ Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran &
Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.
[[Page 58053]]
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\23\ Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company,
Loveland, CO 80537.
\24\ Wershaw, R. L., et al., ``Methods for Analysis of Organic Substances in Water,'' Techniques of Water-Resources Investigation of the U.S. Geological
Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14.
\25\ Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The colorimetric reaction must be conducted at a pH of 10.0 0.2.
\28\ R.F. Addison and R. G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,'' Journal of Chromatography, Vol. 47,
No. 3, pp. 421-426, 1970.
\29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as
an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble
in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be
diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
approved method is satisfactory.
\30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method
specified quality control acceptance criteria are met.
\31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in
solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2
to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent
the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with
reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as
well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH >7 with NH4OH. Add 1 mL of the
cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ Stevens, H. H., Ficke, J. F., and Smoot, G. F., ``Water Temperature--Influential Factors, Field Measurement and Data Presentation,'' Techniques of
Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1, 1975.
\33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\ ``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--
Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin, MA 02038.
\35\ In-Situ Method 1004-8-2009, ``Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe''. Available from In-Situ, Incorporated,
221 E. Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970-498-1500.
\36\ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. ``Closed Vessel Microwave Digestion of Wastewater
Samples for Determination of Metals'', CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use n-hexane (n-Hexane -- 85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining
Oil and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664B). Use of other extraction
solvents is prohibited.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM,
P.O. Box 9010, College Station, TX 77842.
\40\ Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM,
P.O. Box 9010, College Station, TX 77842.
\41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/96, OI Analytical/ALPKEM, P.O. Box 9010,
College Station, TX 77842.
\42\ Method 1664, Revision B is the revised version of EPA Method 1664A.
\43\ USEPA. 2001. Method 1631, Revision E, ``Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry'' September
2002, Office of Water, U.S. Environmental Protection Agency (EPA-821-R-02-024). The application of clean techniques described in EPA's draft Method
1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels (EPA-821-R-96-011) are recommended to preclude contamination at low-
level, trace metal determinations.
\44\ Available Cyanide, Method OIA-1677-09, ``Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,'' ALPKEM, A Division of OI
Analytical, P.O. Box 9010, College Station, TX 77842-9010.
\45\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl
Digestion Method,'' Open File Report (OFR) 00-170.
\46\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by Graphite Furnace
Atomic Absorption Spectrophotometry,'' Open File Report (OFR) 93-449.
\47\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by Graphite Furnace Atomic
Absorption Spectrophotometry,'' Open File Report (OFR) 97-198.
\48\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by Kjeldahl Digestion
Method and an Automated Colorimetric Finish That Includes Dialysis'' Open File Report (OFR) 92-146.
\49\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium in Water and Sediment
by Graphite Furnace-Atomic Absorption Spectrometry'' Open File Report (OFR) 98-639.
\50\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-water Digests Using
Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry,'' Open File Report (OFR) 98-165.
\51\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water
and Fluvial Sediment,'' Open File Report (OFR) 93-125.
\52\ Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in ``Methods for the Determination of Metals in
Environmental Samples,'' Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/R-94/111, May 1994; and ``Methods for the
Determination of Inorganic Substances in Environmental Samples,'' NERL-CI, EPA/600/R-93/100, August, 1993. EPA Method 300.1 is available from http://www.epa.gov/safewater/methods/pdfs/met300.pdf.
\53\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable
substitutes for formazin.
\54\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and
Chromate Electrolyte,'' available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
\55\ Kelada-01, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,'' EPA 821-B-01-009, Revision 1.2, August
2001, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. Note: A 450-W UV lamp
may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the
method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC
acceptance criteria are met.
\56\ QuikChem Method 10-204-00-1-X, ``Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of
Cyanide by Flow Injection Analysis'' is available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414-358-4200.
[[Page 58054]]
\57\ When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to
distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method,
approved digestion and/or distillation are required prior to analysis.
\59\ Samples analyzed for available cyanide using Methods OIA-1677-09 or D6888-09 that contain particulate matter may be filtered only after the ligand
exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide,
which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample
filtration to no more than 30 minutes to preclude settling of materials in samples.
\60\ Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color
reagent in Berthelot Reaction (``phenol-hypochlorite reaction'') colorimetric ammonium determination methods. For example when phenol is used as the
color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively--see, C.J. Patton and S.R. Crouch, Anal. Chem.
(1977) 49, 464-469. These reaction parameters increase to pH >12.6 and 665 nm when salicylate is used as the color reagent--see, M.D. Krom, Analyst
(1980) 105, 305-316.
\61\ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may
be used. This method has poorer precision and bias than the methods of choice.
\62\ Systea Easy (1-Reagent) Nitrate Method, February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific, LLC., 900 Jorie Blvd., Suite
35, Oak Brook, IL 60523.
\63\ Hach Method 10360, ``Luminescence Measurement of Dissolved Oxygen (LDO[supreg]) in Water and Wastewater, Revision 1.1 dated January 4, 2006''.
Available from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539, Telephone: 970-669-3050.
\64\ In-Situ Method 1002-8-2009, ``Dissolved Oxygen (DO) Measurement by Optical Probe'', 1003-8-2009. Available from In-Situ, Incorporated, 221 E.
Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970-498-1500.
\65\ Mitchell Method M5331, ``Determination of Turbidity by Nephlometry'', Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 656
Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630-645-0600.
\66\ Mitchell Method M5271, ``Determination of Turbidity by Nephlometry'', Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 656
Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630-645-0600.
\67\ Thermo Scientific's Orion Method AQ4500, Revision 5, March 12, 2009, ``Determination of Turbidity by Nephlometry''. Available from Thermo
Scientific, 166 Cummings Center, Beverly, MA 01915, Phone: 1-800-225-1480, http://www.thermo.com.
\68\ This method may be used to measure dissolved oxygen when performing methods approved in Table 1B for measurement of biochemical oxygen demand for
compliance monitoring under the Clean Water Act.
Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter \1\ Method EPA \2\ \7\ Standard methods ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
2. Acenaphthylene.................. GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
3. Acrolein........................ GC.................... 603...................
GC/MS................. 624,\4\ 1624B.........
4. Acrylonitrile................... GC.................... 603...................
GC/MS................. 624,\4\ 1624B.........
5. Anthracene...................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440B-00............. D4657-92 (99)........
6. Benzene......................... GC.................... 602................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
7. Benzidine....................... Spectrophotometric.... ...................... ..................... ..................... See footnote,\3\ p.1.
GC/MS................. 625,\5\ 1625B......... 6410 B-00............
HPLC.................. 605...................
8. Benzo(a)anthracene.............. GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
9. Benzo(a)pyrene.................. GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
10. Benzo(b)fluoranthene........... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
11. Benzo(g,h,i)perylene........... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
12. Benzo(k)fluoranthene........... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
13. Benzylchloride................. GC.................... ...................... ..................... ..................... See footnote,\3\ p.
130.
[[Page 58055]]
GC/MS................. ...................... ..................... ..................... See footnote,\6\ p.
S102.
14. Butyl benzyl phthalate......... GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
15. Bis(2-chloroethoxy) methane.... GC.................... 611...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
16. Bis(2-chloroethyl) ether....... GC.................... 611...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
17. Bis(2-ethylhexyl) phthalate.... GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
18. Bromodichloromethane........... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
19. Bromoform...................... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
20. Bromomethane................... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
21. 4-Bromophenyl phenyl ether..... GC.................... 611...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
22. Carbon tetrachloride........... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
23. 4-Chloro-3-methylphenol........ GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
24. Chlorobenzene.................. GC.................... 601, 602.............. 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
25. Chloroethane................... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
26. 2-Chloroethylvinyl ether....... GC.................... 601...................
GC/MS................. 624, 1624B............
27. Chloroform..................... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
28. Chloromethane.................. GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
29. 2-Chloronaphthalene............ GC.................... 612................... 6410 B-00............
GC/MS................. 625, 1625B............ ..................... ..................... See footnote,\9\ p.
27.
30. 2-Chlorophenol................. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
31. 4-Chlorophenyl phenyl ether.... GC.................... 611...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
32. Chrysene....................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
33. Dibenzo(a,h)anthracene......... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
34. Dibromochloromethane........... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
35. 1,2-Dichlorobenzene............ GC.................... 601,602............... 6200 C-97............
GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p.
27.
36. 1,3-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-97............
GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p.
27.
37. 1,4-Dichlorobenzene............ GC.................... 601, 602.............. 6200 C-97............
GC/MS................. 624, 1625B............ 6200 B-97............ ..................... See footnote,\9\ p.
27.
38. 3,3-Dichlorobenzidine.......... GC/MS................. 625, 1625B........... 6410 B-00............
HPLC.................. 605...................
[[Page 58056]]
39. Dichlorodifluoromethane........ GC.................... 601...................
GC/MS................. ...................... 6200 C-97............
40. 1,1-Dichloroethane............. GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
41. 1,2-Dichloroethane............. GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
42. 1,1-Dichloroethene............. GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
43. trans-1,2-Dichloroethene....... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
44. 2,4-Dichlorophenol............. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
45. 1,2-Dichloropropane............ GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
46. cis-1,3-Dichloropropene........ GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
47. trans-1,3-Dichloropropene...... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
48. Diethyl phthalate.............. GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
49. 2,4-Dimethylphenol............. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
50. Dimethyl phthalate............. GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
51. Di-n-butyl phthalate........... GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
52. Di-n-octyl phthalate........... GC.................... 606...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
53. 2,3-Dinitrophenol.............. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............
54. 2,4-Dinitrotoluene............. GC.................... 609...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
55. 2,6-Dinitrotoluene............. GC.................... 609...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
56. Epichlorohydrin................ GC.................... ...................... ..................... ..................... See footnote,\3\ p.
130.
GC/MS................. ...................... ..................... ..................... See footnote,\6\ p.
S102.
57. Ethylbenzene................... GC.................... 602................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
58. Fluoranthene................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
59. Fluorene....................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
60. 1,2,3,4,6,7,8-Heptachloro- GC/MS................. 1613B.................
dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro- GC/MS................. 1613B.................
dibenzofuran.
62. 1,2,3,4,6,7,8- GC/MS................. 1613B.................
Heptachlorodibenzo-p-dioxin.
63. Hexachlorobenzene.............. GC.................... 612...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
64. Hexachlorobutadiene............ GC.................... 612...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
65. Hexachlorocyclopentadiene...... GC.................... 612...................
GC/MS................. 625,\5\ 1625B......... 6410 B-00............ ..................... See footnote,\9\ p.
27.
66. 1,2,3,4,7,8- GC/MS................. 1613B.................
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8- GC/MS................. 1613B.................
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9- GC/MS................. 1613B.................
Hexachlorodibenzofuran.
[[Page 58057]]
69. 2,3,4,6,7,8- GC/MS................. 1613B.................
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-Hexachlorodibenzo-p- GC/MS................. 1613B.................
dioxin.
71. 1,2,3,6,7,8-Hexachlorodibenzo-p- GC/MS................. 1613B.................
dioxin.
72. 1,2,3,7,8,9-Hexachlorodibenzo-p- GC/MS................. 1613B.................
dioxin.
73. Hexachloroethane............... GC.................... 612...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
74. Ideno(1,2,3-cd) pyrene......... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
75. Isophorone..................... GC.................... 609...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
76. Methylene chloride............. GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
77. 2-Methyl-4,6-dinitrophenol..... GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
78. Naphthalene.................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............
79. Nitrobenzene................... GC.................... 609...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. ...................... ..................... D4657-92 (99)........
80. 2-Nitrophenol.................. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
81. 4-Nitrophenol.................. GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
82. N-Nitrosodimethylamine......... GC.................... 607...................
GC/MS................. 625 \5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p.
27.
83. N-Nitrosodi-n-propylamine...... GC.................... 607...................
GC/MS................. 625\5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p.
27.
84. N-Nitrosodiphenylamine......... GC.................... 607...................
GC/MS................. 625 \5\, 1625B........ 6410 B-00............ ..................... See footnote,\9\ p.
27.
85. Octachlorodibenzofuran......... GC/MS................. 1613B \10\............
86. Octachlorodibenzo-p-dioxin..... GC/MS................. 1613B \10\............
87. 2,2'-Oxybis(2-chloropropane) GC.................... 611...................
[also known as bis(2-
chloroisopropyl) ether].
GC/MS................. 625, 1625B............ 6410 B-00............
88. PCB-1016....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See footnote.\8\
GC/MS................. 625................... 6410 B-00............
89. PCB-1221....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See footnote.\8\
GC/MS................. 625................... 6410 B-00............
90. PCB-1232....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See footnote.\8\
GC/MS................. 625................... 6410 B-00............
91. PCB-1242....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See footnote.\8\
GC/MS................. 625................... 6410 B-00............
92. PCB-1248....................... GC.................... 608...................
GC/MS................. 625................... 6410 B-00............
93. PCB-1254....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See footnote.\8\
GC/MS................. 625................... 6410 B-00............
[[Page 58058]]
94. PCB-1260....................... GC.................... 608................... ..................... ..................... See footnote,\3\ p.
43; See
footnote.\8\.
GC/MS................. 625................... 6410 B-00............
95. 1,2,3,7,8-Pentachloro- GC/MS................. 1613B.................
dibenzofuran.
96. 2,3,4,7,8-Pentachloro- GC/MS................. 1613B.................
dibenzofuran.
97. 1,2,3,7,8,-Pentachlorodibenzo-p- GC/MS................. 1613B.................
dioxin.
98. Pentachlorophenol.............. GC.................... 604................... 6420 B-00............ ..................... See footnote,\3\ p.
140.
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
99. Phenanthrene................... GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
100. Phenol........................ GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
101. Pyrene........................ GC.................... 610...................
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
HPLC.................. 610................... 6440 B-00............ D4657-92 (99)........
102. 2,3,7,8-Tetra- GC/MS................. 1613B.................
chlorodibenzofuran.
103. 2,3,7,8-Tetra-chlorodibenzo-p- GC/MS................. 613, 625,\5a\ 1613B...
dioxin.
104. 1,1,2,2-Tetra-chloro ethane... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
105. Tetrachloroethene............. GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
106. Toluene....................... GC.................... 602................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
107. 1,2,4-Trichlorobenzene........ GC.................... 612................... ..................... ..................... See footnote,\3\ p.
130.
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
108. 1,1,1-Trichloroethane......... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
109. 1,1,2-Trichloroethane......... GC.................... 601................... 6200 C-97............ ..................... See footnote,\3\ p.
130.
GC/MS................. 624, 1624B............ 6200 B-97............
110. Trichloroethene............... GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
111. Trichlorofluoromethane........ GC.................... 601................... 6200 C-97............
GC/MS................. 624................... 6200 B-97............
112. 2,4,6-Trichlorophenol......... GC.................... 604................... 6420 B-00............
GC/MS................. 625, 1625B............ 6410 B-00............ ..................... See footnote,\9\ p.
27.
113. Vinyl chloride................ GC.................... 601................... 6200 C-97............
GC/MS................. 624, 1624B............ 6200 B-97............
114. Nonylphenol................... GC/MS................. ...................... ..................... D7065-06.............
LC/MS/MS.............. ...................... ..................... D7485-09.............
115. Bisphenol A (BPA)............. GC/MS................. ...................... ..................... D7065-06.............
LC/MS/MS.............. ...................... ..................... D7574-09.............
116. p-tert-Octylphenol (OP)....... GC/MS................. ...................... ..................... D7065-06.............
LC/MS/MS.............. ...................... ..................... D7485-09.............
117. Nonylphenol Monoethoxylate GC/MS................. ...................... ..................... D7065-06.............
(NP1EO).
LC/MS/MS.............. ...................... ..................... D7485-09.............
118. Nonylphenol Diethoxylate GC/MS................. ...................... ..................... D7065-06.............
(NP2EO).
LC/MS/MS.............. ...................... ..................... D7485-09.............
119. Polybrominated diphenyl ethers HRGC/HRMS............. 1614A.................
(PBDEs) 49 congeners.
120. Polychlorinated biphenyls HRGC/HRMS............. 1668C.................
(PCBs) 209 Congeners.
121. Adsorbable Organic Halides Adsorption and 1650..................
(AOX). Coulometric Titration.
[[Page 58059]]
122. Chlorinated Phenolics......... In Situ Acetylation 1653..................
and GC/MS.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([mu]g/L) except for Method 1613B in which the parameters are expressed in picograms per liter
(pg/L).
\2\ The full text of Methods 601-613, 624, 625, 1624B, and 1625B, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of
this Part 136. The full text of Method 1613B is incorporated by reference into this Part 136 and is available from the National Technical Information
Services as stock number PB95-104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test
procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection Limit,'' of this Part 136. The full text
of Methods 1613B, 1614A, 1650, 1653, and 1668C are available from EPA Office of Water (4303T) 1200 Pennsylvannia Ave, NW, Washington, DC 20460.
\3\ ``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September, 1978.
\4\ Method 624 may be used for definitive determination of Acrolein and Acrylonitrile.
\5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they
are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.
\5a\ 625, screening only.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,'' Supplement to the Fifteenth Edition of
Standard Methods for the Examination of Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624,
625, 1624B, and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each
laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to
monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls
outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot
be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods
cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore \TM\ Disk'' 3M Corporation Revised 10/28/94.
\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic
Constituents in Water and Fluvial Sediments,'' U.S. Geological Survey, Open File Report 93-125.
\10\ Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method
1613B (as specified in Section 9 of the method) and permitting authorities.
Table ID--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter Method EPA 2 7 10 Standard methods ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin......................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812-96 See footnote,\3\ p.
(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
2. Ametryn........................ GC........................ 507, 619............. ..................... .................... See footnote,\3\ p.
83; See
footnote,\9\ O-3106-
93; See
footnote,\6\ p.
S68.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\14\ O-
1121-91.
3. Aminocarb...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
94; See
footnote,\6\ p.
S60.
HPLC...................... 632..................
4. Atraton........................ GC........................ 619.................. ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68.
5. Atrazine....................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68; See
footnote,\9\ O-3106-
93.
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
6. Azinphos methyl................ GC........................ 614, 622, 1657....... ..................... .................... See footnote,\3\ p.
25; See
footnote,\6\ p.
S51.
GC MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
7. Barban......................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
8. [alpha]-BHC.................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\8\
3M0222.
GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\11\ O-
1126-95.
9. [beta]-BHC..................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\8\
96(02). 3M0222.
GC/MS..................... 625.................. 6410 B-00............
10. [delta]-BHC................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\8\
96(02). 3M0222.
[[Page 58060]]
GC/MS..................... 625.................. 6410 B-00............
11. [gamma]-BHC (Lindane)......... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\11\ O-
1126-95.
12. Captan........................ GC........................ 617.................. 6630 B-00............ D3086-90, D5812- See footnote,\3\ p.
96(02). 7.
13. Carbaryl...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
94, See
footnote,\6\ p.
S60.
HPLC...................... 531.1, 632...........
HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O-
2060-01.
GC/MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
14. Carbophenothion............... GC........................ 617.................. 6630 B-00............ .................... See footnote,\6\ p.
S73.
15. Chlordane..................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
16. Chloropropham................. TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
17. 2,4-D......................... GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p.
115; See
footnote,\4\ O-3105-
83.
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
18. 4,4'-DDD...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3105-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
19. 4,4'-DDE...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............ .................... See footnote,\11\ O-
1126-95.
20. 4,4'-DDT...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
21. Demeton-O..................... GC........................ 614, 622............. ..................... .................... See footnote,\3\ p.
25; See
footnote,\6\ p.
S51.
22. Demeton-S..................... GC........................ 614, 622............. ..................... .................... See footnote,\3\ p.
25; See
footnote,\6\ p.
S51.
23. Diazinon...................... GC........................ 507, 614, 622, 1657.. ..................... .................... See footnote,\3\ p.
25; See
footnote,\4\ O-3104-
83; See
footnote,\6\ p.
S51.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
24. Dicamba....................... GC........................ 615.................. ..................... .................... See footnote,\3\ p.
115.
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
25. Dichlofenthion................ GC........................ 622.1................ ..................... .................... See footnote,\6\ p.
S73.
26. Dichloran..................... GC........................ 608.2, 617........... 6630 B-00............ .................... See footnote,\3\ p.
7.
27. Dicofol....................... GC........................ 617.................. 6630 B-00............ .................... See footnote,\4\ O-
3104-83.
28. Dieldrin...................... GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............ .................... See footnote,\11\ O-
1126-95.
29. Dioxathion.................... GC........................ 614.1, 1657.......... ..................... .................... See footnote,\6\ p.
S73.
30. Disulfoton.................... GC........................ 507, 614, 622, 1657.. ..................... .................... See footnote,\3\ p.
25; See
footnote,\6\ p.
S51.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
31. Diuron........................ TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O-
2060-01.
32. Endosulfan I.................. GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\ 3M022.
GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\13\ O-
2002-01.
33. Endosulfan II................. GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\8\
3M0222.
GC/MS..................... 625 \5\.............. 6410 B-00............ .................... See footnote,\13\ O-
2002-01.
34. Endosulfan Sulfate............ GC........................ 608, 617............. 6630 C-00............ .................... See footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
[[Page 58061]]
35. Endrin........................ GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
1656. 96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 525.1, 525.2, 625 \5\ 6410 B-00............
36. Endrin aldehyde............... GC........................ 608, 617............. 6630 C-00............ .................... See footnote,\8\
3M0222.
GC/MS..................... 625..................
37. Ethion........................ GC........................ 614, 614.1,1657...... ..................... .................... See footnote,\6\ p.
S73.
GC/MS..................... ..................... ..................... .................... See footnote,\13\ O-
2002-01.
38. Fenuron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
39. Fenuron-TCA................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
40. Heptachlor.................... GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
1656. 96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 525.1, 525.2, 625.... 6410 B-00............
41. Heptachlor epoxide............ GC........................ 608, 617............. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\6\ p.
S73; See
footnote,\8\
3M0222.
GC/MS..................... 625.................. 6410 B-00............
42. Isodrin....................... GC........................ 617.................. 6630 B-00 & C-00..... .................... See footnote,\4\ O-
3104-83; See
footnote,\6\ p.
S73.
43. Linuron....................... GC........................ ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... 553.................. ..................... .................... See footnote,\12\ O-
2060-01.
GC/MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
44. Malathion..................... GC........................ 614, 1657............ 6630 B-00............ .................... See footnote,\3\ p.
25; See
footnote,\6\ p.
S51.
GC/MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
45. Methiocarb.................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
94; See
footnote,\6\ p.
S60.
HPLC...................... 632..................
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
46. Methoxychlor.................. GC........................ 505, 508, 608.2, 617, 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
1656. 96(02). 7; See footnote,\4\
O-3104-83; See
footnote,\8\
3M0222.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
47. Mexacarbate................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
94; See
footnote,\6\ p.
S60.
HPLC...................... 632..................
48. Mirex......................... GC........................ 617.................. 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
96(02). 7; See footnote,\4\
O-3104-83.
49. Monuron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
50. Monuron-TCA................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
51. Neburon....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
52. Parathion methyl.............. GC........................ 614, 622, 1657....... 6630 B-00............ .................... See footnote,\3\ p.
25.
GC/MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
53. Parathion ethyl............... GC........................ 614.................. 6630 B-00............ .................... See footnote,\3\ p.
25.
GC/MS..................... ..................... ..................... .................... See footnote,\11\ O-
1126-95.
54. PCNB.......................... GC........................ 608.1, 617........... 6630 B-00............ D3086-90, D5812- See footnote,\3\ p.
96(02). 7.
55. Perthane...................... GC........................ 617.................. 6630 B-00............ D3086-90, D5812- See footnote,\4\ O-
96(02). 3104-83.
56. Prometon...................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68; See
footnote,\9\ O-3106-
93.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
[[Page 58062]]
57. Prometryn..................... GC........................ 507, 619............. ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68; See
footnote,\9\ O-3106-
93.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\13\ O-
2002-01.
58. Propazine..................... GC........................ 507, 619, 1656....... ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68; See
footnote,\9\ O-3106-
93.
GC/MS..................... 525.1, 525.2.........
59. Propham....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
60. Propoxur...................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
94; See
footnote,\6\ p.
S60.
HPLC...................... 632..................
61. Secbumeton.................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68.
GC........................ 619..................
62. Siduron....................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
HPLC/MS................... ..................... ..................... .................... See footnote,\12\ O-
2060-01.
63. Simazine...................... GC........................ 505, 507, 619, 1656.. ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68; See
footnote,\9\ O-3106-
93.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
64. Strobane...................... GC........................ 617.................. 6630 B-00 & C-00..... .................... See footnote,\3\ p.
7.
65. Swep.......................... TLC....................... ..................... ..................... .................... See footnote,\3\ p.
104; See
footnote,\6\ p.
S64.
HPLC...................... 632..................
66. 2,4,5-T....................... GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p.
115; See
footnote,\4\ O-3105-
83.
67. 2,4,5-TP (Silvex)............. GC........................ 615.................. 6640 B-01............ .................... See footnote,\3\ p.
115; See
footnote,\4\ O-3105-
83.
68. Terbuthylazine................ GC........................ 619, 1656............ ..................... .................... See footnote,\3\ p.
83; See
footnote,\6\ p.
S68.
GC/MS..................... ..................... ..................... .................... See footnote,\13\ O-
2002-01.
69. Toxaphene..................... GC........................ 505, 508, 608, 617, 6630 B-00 & C-00..... D3086-90, D5812- See footnote,\3\ p.
1656. 96(02). 115; See
footnote,\4\ O-3105-
83.
GC/MS..................... 525.1, 525.2, 625.... 6410 B-00............
70. Trifluralin................... GC........................ 508, 617, 627, 1656.. 6630 B-00............ .................... See footnote,\3\ p.
7; See footnote,\9\
O-3106-93.
GC/MS..................... 525.1, 525.2......... ..................... .................... See footnote,\11\ O-
1126-95.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where
entries are listed by chemical name.
\2\ The full text of Methods 608 and 625 are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The
standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition
and Procedure for the Determination of the Method Detection Limit,'' of this Part 136.
\3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September 1978. This EPA publication includes thin-layer chromatography (TLC) methods.
\4\ ``Methods for Analysis of Organic Substances in Water and Fluvial Sediments,'' Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5, Chapter A3 (1987).
\5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
Method 608 is the preferred method.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of
Standard Methods for the Examination of Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625
(See Appendix A of this Part 136) in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-
going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate
laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits,
the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate
regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'', 3M Corporation, Revised 10/28/94.
\9\ USGS Method 0-3106-93 from ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Triazine and
Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors'' U.S. Geological Survey Open File Report 94-37.
\10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in ``Methods for the Determination of Nonconventional
Pesticides in Municipal and Industrial Wastewater,'' EPA 821-R-92-002, April 1992.
[[Page 58063]]
\11\ O-1126-95 GC/MS: Zaugg, S.D., Sandstrom, M.W., Smith, S.G., and Fehlberg, K.M., 1995, Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory--Determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass
spectrometry with selected-ion monitoring: U.S. Geological Survey Open-File Report 95-181, Method O-1126-95, 49 p.
\12\ O-2060-01 LC/MS: Furlong, E.T., Anderson, B.D., Werner, S.L., Soliven, P.P., Coffey, L.J., and Burkhardt, M.R., 2001, Methods of Analysis by the
U.S. Geological Survey National Water Quality Laboratory-Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and
High-Performance Liquid Chromatography/Mass Spectrometry: U.S. Geological Survey Water-Resources Investigations Report 01-4134 Method O-2060-01, 73 p.
\13\ O-2002-01 Sandstrom, M.W., Stroppel, M.E., Foreman, W.T., and Schroeder, M.P., 2001, Methods of Analysis by the U.S. Geological Survey National
Water Quality Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/
mass spectrometry: U.S. Geological Survey Water-Resources Investigations Report 01-4098, Method O-2002-01, 70 p.
\14\ O-1121-91: Sandstrom, M.W., Wydoski, D.S., Schroeder, M.P., Zamboni, J.L., and Foreman, W.T., 1992, Methods of Analysis by the U.S. Geological
Survey National Water Quality Laboratory--Determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas
chromatography/mass spectrometry with selected-ion monitoring,: U.S. Geological Survey Open-File Report 91-519; O-1121-91, 34 p.
* * * * *
Table IG--Test Methods for Pesticide Active Ingredients
[40 CFR 455]
----------------------------------------------------------------------------------------------------------------
EPA survey code Pesticide name CAS No. EPA analytical method No.(s)
----------------------------------------------------------------------------------------------------------------
8........................... Triadimefon..................... 43121-43-3 507/633/525.1/525.2/1656
12.......................... Dichlorvos...................... 62-73-7 1657/507/622/525.1/525.2
16.......................... 2,4-D; 2,4-D Salts and Esters 94-75-7 1658/515.1/615/515.2/555
[2,4-Dichloro-phenoxyacetic
acid].
17.......................... 2,4-DB; 2,4-DB Salts and Esters 94-82-6 1658/515.1/615/515.2/555
[2,4-Dichlorophenoxybutyric
acid].
22.......................... Mevinphos....................... 7786-34-7 1657/507/622/525.1/525.2
25.......................... Cyanazine....................... 21725-46-2 629/507
26.......................... Propachlor...................... 1918-16-7 1656/508/608.1/525.1/525.2
27.......................... MCPA; MCPA Salts and Esters [2- 94-74-6 1658/615/555
Methyl-4-chlorophenoxyacetic
acid].
30.......................... Dichlorprop; Dichlorprop Salts 120-36-5 1658/515.1/615/515.2/555
and Esters [2-(2,4-
Dichlorophenoxy) propionic
acid].
31.......................... MCPP; MCPP Salts and Esters [2- 93-65-2 1658/615/555
(2-Methyl-4-chlorophenoxy)
propionic acid].
35.......................... TCMTB [2-(Thiocyanomethylthio) 21564-17-0 637
benzo-thiazole].
39.......................... Pronamide....................... 23950-58-5 525.1/525.2/507/633.1
41.......................... Propanil........................ 709-98-8 632.1/1656
45.......................... Metribuzin...................... 21087-64-9 507/633/525.1/525.2/1656
52.......................... Acephate........................ 30560-19-1 1656/1657
53.......................... Acifluorfen..................... 50594-66-6 515.1/515.2/555
54.......................... Alachlor........................ 15972-60-8 505/507/645/525.1/525.2/1656
55.......................... Aldicarb........................ 116-06-3 531.1
58.......................... Ametryn......................... 834-12-8 507/619/525.1/525.2
60.......................... Atrazine........................ 1912-24-9 505/507/619/525.1/525.2/1656
62.......................... Benomyl......................... 17804-35-2 631
68.......................... Bromacil; Bromacil Salts and 314-40-9 507/633/525.1/525.2/1656
Esters.
69.......................... Bromoxynil...................... 1689-84-5 1625/1661
69.......................... Bromoxynil octanoate............ 1689-99-2 1656
70.......................... Butachlor....................... 23184-66-9 507/645/525.1/525.2/1656
73.......................... Captafol........................ 2425-06-1 1656
75.......................... Carbaryl [Sevin]................ 63-25-2 531.1/632/553
76.......................... Carbofuran...................... 1563-66-2 531.1/632
80.......................... Chloroneb....................... 2675-77-6 1656/508/608.1/525.1/525.2
82.......................... Chlorothalonil.................. 1897-45-6 508/608.2/525.1/525.2/1656
84.......................... Stirofos........................ 961-11-5 1657/507/622/525.1/525.2
86.......................... Chlorpyrifos.................... 2921-88-2 1657/508/622
90.......................... Fenvalerate..................... 51630-58-1 1660
103......................... Diazinon........................ 333-41-5 1657/507/614/622/525.1/525.2
107......................... Parathion methyl................ 298-00-0 1657/614/622
110......................... DCPA [Dimethyl 2,3,5,- 1861-32-1 508/608.2/525.1/525.2/515.1/
tetrachloro-terephthalate]. 515.2/1656
112......................... Dinoseb......................... 88-85-7 1658/515.1/615/515.2/555
113......................... Dioxathion...................... 78-34-2 1657/614.1
118......................... Nabonate [Disodium cyanodithio- 138-93-2 630.1
imidocarbonate].
119......................... Diuron.......................... 330-54-1 632/553
123......................... Endothall....................... 145-73-3 548/548.1
124......................... Endrin.......................... 72-20-8 1656/505/508/608/617/525.1/525.2
125......................... Ethalfluralin................... 55283-68-6 1656/627 Note 1
126......................... Ethion.......................... 563-12-2 1657/614/614.1
127......................... Ethoprop........................ 13194-48-4 1657/507/622/525.1/525.2
132......................... Fenarimol....................... 60168-88-9 507/633.1/525.1/525.2/1656
133......................... Fenthion........................ 55-38-9 1657/622
138......................... Glyphosate [N-(Phosphonomethyl) 1071-83-6 547
glycine].
[[Page 58064]]
140......................... Heptachlor...................... 76-44-8 1656/505/508/608/617/525.1/525.2
144......................... Isopropalin..................... 33820-53-0 1656/627
148......................... Linuron......................... 330-55-2 553/632
150......................... Malathion....................... 121-75-5 1657/614
154......................... Methamidophos................... 10265-92-6 1657
156......................... Methomyl........................ 16752-77-5 531.1/632
158......................... Methoxychlor.................... 72-43-5 1656/505/508/608.2/617/525.1/
525.2
172......................... Nabam........................... 142-59-6 630/630.1
173......................... Naled........................... 300-76-5 1657/622
175......................... Norflurazon..................... 27314-13-2 507/645/525.1/525.2/1656
178......................... Benfluralin..................... 1861-40-1 \1\1656/\1\627
182......................... Fensulfothion................... 115-90-2 1657/622
183......................... Disulfoton...................... 298-04-4 1657/507/614/622/525.1/525.2
185......................... Phosmet......................... 732-11-6 1657/622.1
186......................... Azinphos Methyl................. 86-50-0 1657/614/622
192......................... Organo-tin pesticides........... 12379-54-3 Ind-01/200.7/200.9
197......................... Bolstar......................... 35400-43-2 1657/622
203......................... Parathion....................... 56-38-2 1657/614
204......................... Pendimethalin................... 40487-42-1 1656
205......................... Pentachloronitrobenzene......... 82-68-8 1656/608.1/617
206......................... Pentachlorophenol............... 87-86-5 625/1625/515.2/555/515.1/525.1/
525.2
208......................... Permethrin...................... 52645-53-1 608.2/508/525.1/525.2/1656/1660
212......................... Phorate......................... 298-02-2 1657/622
218......................... Busan 85 [Potassium 128-03-0 630/630.1
dimethyldithiocarbamate].
219......................... Busan 40 [Potassium N- 51026-28-9 630/630.1
hydroxymethyl-N-
methyldithiocarbamate].
220......................... KN Methyl [Potassium N-methyl- 137-41-7 630/630.1
dithiocarbamate].
223......................... Prometon........................ 1610-18-0 507/619/525.1/525.2
224......................... Prometryn....................... 7287-19-6 507/619/525.1/525.2
226......................... Propazine....................... 139-40-2 507/619/525.1/525.2/1656
230......................... Pyrethrin I..................... 121-21-1 1660
232......................... Pyrethrin II.................... 121-29-9 1660
236......................... DEF [S,S,S-Tributyl 78-48-8 1657
phosphorotrithioate].
239......................... Simazine........................ 122-34-9 505/507/619/525.1/525.2/1656
241......................... Carbam-S [Sodium 128-04-1 630/630.1
dimethyldithiocarbanate].
243......................... Vapam [Sodium 137-42-8 630/630.1
methyldithiocarbamate].
252......................... Tebuthiuron..................... 34014-18-1 507/525.1/525.2
254......................... Terbacil........................ 5902-51-2 507/633/525.1/525.2/1656
255......................... Terbufos........................ 13071-79-9 1657/507/614.1/525.1/525.2
256......................... Terbuthylazine.................. 5915-41-3 619/1656
257......................... Terbutryn....................... 886-50-0 507/619/525.1/525.2
259......................... Dazomet......................... 533-74-4 630/630.1/1659
262......................... Toxaphene....................... 8001-35-2 1656/505/508/608/617/525.1/525.2
263......................... Merphos [Tributyl 150-50-5 1657/507/525.1/525.2/622
phosphorotrithioate].
264......................... Trifluralin..................... 1582-09-8 1656/508/617/627/525.1/525.2
268......................... Ziram [Zinc 137-30-4 630/630.1
dimethyldithiocarbamate].
----------------------------------------------------------------------------------------------------------------
\1\ Monitor and report as total Trifluralin.
Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
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 (MPN), 5 tube, 3
gram dry weight. dilution, or.
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.
[[Page 58065]]
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 per 100 mL MPN 6 8 14, multiple ................... 9221 B.1-2006/9221
tube. F-2006.11 13
Multiple tube/ ................... 9223 B-2004 \12\... 991.15 \10\........ Colilert[supreg].12 16
multiple well. Colilert-18[supreg].12 15 16
MF 2 5 6 7 8, two 1103.1 \19\........ 9222 B-1997/9222 G- D5392-93.\9\
step, or. 1997,\18\ 9213 D-
1997.
Single step......... 1603 \20\, 1604 9213 D-2007....... ................... mColiBlue-24[supreg].\17\
\21\.
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 MPN 6 8, multiple ................... 9230 B-2007........
100 mL. tube.
Multiple tube/ ................... ................... D6503-99 \9\....... Enterolert[supreg].12 22
multiple well.
MF 2 5 6 7 8 two 1106.1 \23\........ 9230 C-2007....... D5259-92.\9\
step.
Single step, or..... 1600.\24\
Plate count......... p. 143.\3\
Protozoa:
8. Cryptosporidium........... Filtration/IMS/FA... 1622,\25\ 1623.\26\
9. Giardia................... Filtration/IMS/FA... 1623.\26\
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [micro]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 not 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\ The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate
and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent
of all total coliform-positive tubes on a seasonal basis.
\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\ After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth
or acidity within 48 h 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supplemented in the
laboratory with 50 [mu]g/mL of MUG may be used.
\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] or 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 may be obtained from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\18\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
\19\ USEPA. March 2010. Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar
(mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-10-002.
\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\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. September 2002.: Method
1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA 821-R-02-024.
[[Page 58066]]
\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 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-09-015.
\24\ 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.
\25\ Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
USEPA. December 2005. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington,
DC EPA-821-R-05-001.
\26\ Method 1623 uses a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
of Cryptosporidium and Giardia oocysts and cysts. USEPA. December 2005. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-05-002.
* * * * *
(b) * * *
(1) The full texts of the CWA U.S. EPA methods are available at
http://epa.gov/waterscience/methods/method. The full text for
determining the method detection limit when using the test procedures
is given in appendix B of this part 136.
* * * * *
(54) USEPA. March 2010. Method 1103.1: Escherichia coli (E. coli)
in Water by Membrane Filtration Using membrane-Thermotolerant
Escherichia coli Agar (mTEC). U.S. Environmental Protection Agency,
Office of Water, Washington, DC EPA-621-R-10-002. Available at http://www.epa.gov/waterscience/methods/method. Table IH, Note 19.
(55) USEPA. December 2009. Method 1106.1: Enterococci in Water by
Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-
EIA). U.S. Environmental Protection Agency, Office of Water,
Washington, DC EPA-621-R-09-015. Available at http://www.epa.gov/waterscience/methods/method. Table IH, Note 23.
(56) 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. Available at
http://www.epa.gov/waterscience/methods/method. Table IA, Note 20;
Table IH, Note 20.
* * * * *
(59) 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. Available at http://www.epa.gov/waterscience/methods/method. Table IA, Note 23; Table IH,
Note 24.
(60) USEPA. December 2005. Method 1622: Cryptosporidium in Water by
Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of
Water, Washington, DC EPA-821-R-05-001. Available at http://www.epa.gov/waterscience/methods/method. Table IA, Note 25.
(61) USEPA. December 2005. Method 1623: Cryptosporidium and Giardia
in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency,
Office of Water, Washington, DC EPA-821-R-05-002. Available at http://www.epa.gov/waterscience/methods/method. Table IA, Note 26.
* * * * *
(70) 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. Available at http://www.epa.gov/waterscience/methods/method. Table IA, Note 13.
* * * * *
(73) EPA Method 200.5, Revision 4.2. ``Determination of Trace
Elements in Drinking Water by Axially Viewed Inductively Coupled
Plasma-Atomic Emission Spectrometry.'' 2003. EPA/600/R-06/115.
(Available at http://www.epa.gov/nerlcwww/ordmeth.htm.)
* * * * *
(e) Sample preservation procedures, container materials, and
maximum allowable holding times for parameters are cited in Tables IA,
IB, IC, ID, IE, IF, IG and IH are prescribed in Table II. Information
in this table takes precedence over information provided in specific
methods or elsewhere unless a party documents the acceptability of an
alternative to the Table II instructions. Such alternatives may include
a change from the prescribed preservation techniques, container
materials, and maximum holding times applicable to samples collected
from a specific discharge. The nature and extent of the documentation
of such changes (how to apply as well as supporting data) is 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 Sec. 136.6.
Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
Maximum
Parameter number/name Container \1\ Preservation 2 3 holding time
(in hours) \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacterial Tests:
1-5. Coliform, total, fecal, and E. PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ \23\ 8
coli. Na2S2O3 \5\.
6. Fecal streptococci............... PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ 8
Na2S2O3 \5\.
7. Enterococci...................... PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ 8
Na2S2O3 \5\.
8. Salmonella....................... PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ 8
Na2S2O3 \5\.
Table IA--Aquatic Toxicity Tests: 9-12. P, FP, G.................. Cool, 0-6 [deg]C \16\..... 36
Toxicity, acute and chronic.
* * * * * * *
Table IH--Bacterial Tests:
[[Page 58067]]
1. E. coli.......................... PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ 8
Na2S2O3 \5\.
2. Enterococci...................... PA, G..................... Cool, < 10 [deg]C, 0.008% \22\ 8
Na2S2O3 \5\.
Table IH--Protozoan Tests:
8. Cryptosporidium.................. LDPE; field filtration.... 1-10 [deg]C............... \21\ 96
9. Giardia.......................... LDPE; field filtration.... 1-10 [deg]C............... \21\ 96
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is for polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE); Teflon[supreg]), or
other fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is
made of a sterilizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density
polyethylene.
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour
composite sample; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at < = 6
[deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at < = 6[deg],
unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
is completed. Add the preservative to the sample container prior to sample collection when the preservative
will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a composite
sample within 15 minutes of collection. If a composite measurement is required but a composite sample would
compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4
samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the
concentrations averaged. Alternatively, grab samples may be collected in the field and composited in the
laboratory if the compositing procedure produces results equivalent to results produced by arithmetic
averaging of results of analysis of individual grab samples. For examples of laboratory compositing
procedures, see EPA Method 1664A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and (v)
(volatile organics).
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering such
material for transportation is responsible for ensuring such compliance. For the preservation requirement of
Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
(HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater; Nitric acid
(HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before the start of analysis and still be considered valid (e.g., samples analyzed for
fecal coliforms may be held up to 6 hours prior to commencing analysis). Samples may be held for longer
periods only if the permittee or monitoring laboratory has data on file to show that, for the specific types
of samples under study, the analytes are stable for the longer time, and has received a variance from the
Regional Administrator under Sec. 136.3(e). For a grab sample, the holding time begins at the time of
collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, Appendix E), the holding time begins at the time of
the end of collection of the composite sample. For a set of grab samples composited in the field or
laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
sample stability. See 136.3(e) for details. The date and time of collection of an individual grab sample is
the date and time at which the sample is collected. For a set of grab samples to be composited, and that are
all collected on the same calendar date, the date of collection is the date on which the samples are
collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
automatically on a given date, the date of collection is the date on which the sample is collected. For a
composite sample collected automatically, and that is collected across two calendar dates, the date of
collection is the dates of the two days; e.g., November 14-15. 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.
\5\ ASTM D7365-09a specifies treatment options for samples containing oxidants (e.g. chlorine).
\6\ Sampling, preservation and mitigating interferences in water samples for analysis of cyanide are described
in ASTM D7365-09a. There may be interferences that are not mitigated by the analytical test methods or D7365-
09a. Any technique for removal or suppression of interference may be employed, provided the laboratory
demonstrates that it more accurately measures cyanide through quality control measures described in the
analytical test method. Any removal or suppression technique not described in D7365-09a or the analytical test
method must be documented along with supporting data.
* * * * * * *
\16\ Place sufficient ice with the samples in the shipping container to ensure that ice is still present when
the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately
measure the temperature of the samples and confirm that the preservation temperature maximum has not been
exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the
permittee can be given the option of on-site testing or can request a variance. The request for a variance
should include supportive data which show that the toxicity of the effluent samples is not reduced because of
the increased holding temperature. 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.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
\22\ Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later
than 8 hours from time of collection.
\23\ For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for
the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B
aerobically digested, and Class B anaerobically digested.
* * * * *
4. Section 136.4 is revised to read as follows:
Sec. 136.4 Application for and approval of alternate test procedures
for nationwide use.
(a) A written application for review of an alternate test procedure
(alternate method) for nationwide use may be made by letter via email
or by hard copy in triplicate to the National Alternate Test Procedure
Program Coordinator (National Coordinator), Office of Science and
Technology (4303T), Office of Water, U.S. Environmental Protection
Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460. Any
application for an alternate test procedure (ATP) under this paragraph
shall:
(1) Provide the name and address of the responsible person or firm
making the application.
(2) Identify the pollutant(s) or parameter(s) for which nationwide
[[Page 58068]]
approval of an alternate test procedure is being requested.
(3) Provide a detailed description of the proposed alternate test
procedure, together with references to published or other studies
confirming the general applicability of the alternate test procedure
for the analysis of the pollutant(s) or parameter(s) in wastewater
discharges from representative and specified industrial or other
categories.
(4) Provide comparability data for the performance of the proposed
alternative test procedure compared to the performance of the reference
method.
(b) The National Coordinator may request additional information and
analyses from the applicant in order to determine whether the alternate
test procedure satisfies the applicable requirements of this
(c) Approval for nationwide use. (1) After a review of the
application and any additional analyses requested from the applicant,
the National Coordinator will notify the applicant, in writing, of
acceptance or rejection of the alternate test procedure for nationwide
use in CWA programs. If the application is not approved, the National
Coordinator will specify what additional information might lead to a
reconsideration of the application, and notify the Regional Alternate
Test Procedure Coordinators of such rejection. Based on the National
Coordinator's rejection of a proposed alternate test procedure and an
assessment of any approvals for limited uses for the unapproved method,
the Regional Coordinator may decide to withdraw approval of the method
for limited use in the Region.
(2) Where the National Coordinator approved an applicant's request
for nationwide use of an alternate test procedure, the National
Coordinator will notify the applicant that the National Coordinator
will recommend rulemaking to approve the alternate test procedure. The
National Coordinator will notify the Regional Coordinators that they
may consider approval of this alternate test procedure for limited use
in their Regions based on the information and data provided in the
applicant's application.
(3) EPA will propose to amend 40 CFR part 136 to include the
alternate test procedure in Sec. 136.3. EPA shall make available for
review all the factual bases for its proposal, including any
performance data submitted by the applicant and any available EPA
analysis of those data.
(4) Following public comment, EPA shall publish in the Federal
Register a final decision on whether to amend 40 CFR part 136 to
include the alternate test procedure as an approved analytical method.
(5) Whenever the National Coordinator has approved an applicant's
request for nationwide use of an alternate test procedure, any person
may request an approval of the method for limited use under Sec. 136.5
from the EPA Region.
5. Section 136.5 is revised to read as follows:
Sec. 136.5 Approval of alternate test procedures for limited use.
(a) Any person may request the Regional Alternate Test Procedure
Coordinator to approved the use of an alternate test procedure in the
Region.
(b) When the request for the use of an alternate test procedure
concerns use in a State with an NPDES permit program approved pursuant
to section 402 of the Act, the requestor, shall first submit an
application for limited use to the Director of the State agency having
responsibility for issuance of NPDES permits within such State. The
Director will forward the application to the Regional Coordinator with
a recommendation for or against approval.
(c) Any application for approval of an alternate test procedure for
limited use may be made by letter, email or by hard copy. The
application shall include the following:
(1) Provide the name and address of the applicant and the
applicable ID number of the existing or pending permit and issuing
agency for which use of the alternate test procedure is requested, and
the discharge serial number.
(2) Identify the pollutant or parameter for which approval of an
alternate test procedure is being requested.
(3) Provide justification for using testing procedures other than
those specified in Table I or in the NPDES permit.
(4) Provide a detailed description of the proposed alternate test
procedure, together with references to published studies of the
applicability of the alternate test procedure to the effluents in
question.
(d) Approval for limited use. (1) After a review of the application
and in the case of a State with an approved NPDES permit program,
review of the recommendation of the Director, the Regional Coordinator
will notify the applicant and the appropriate State agency of approval
or rejection of the use of the alternate procedure. The approval may be
restricted to use only with request to a specific discharge or facility
(and its laboratory) or, at the discretion of the Regional Coordinator,
to all discharger or facilities (and their associated laboratories)
specified in the approval for the Region. If the application for
approval is not approved, the Regional Coordinator shall specify what
additional information might lead to a reconsideration of the
application.
(2) The Regional Coordinator will forward a copy of every approval
and rejection notification to the National Alternate Test Procedure
Coordinator.
6. Section 136.6 is revised to read as follows:
Sec. 136.6 Method modifications and analytical requirements.
(a) Definitions of terms used in this section.
(1) Analyst means the person or laboratory using a test procedure
(analytical method) in this Part.
(2) Chemistry of the method means the reagents and reactions used
in a test procedure that allow determination of the analyte(s) of
interest in an environmental sample.
(3) Determinative technique means the way in which an analyte is
identified and quantified (e.g., colorimetry, mass spectrometry).
(4) Equivalent performance means that the modified method produces
results that meet or exceed the QC acceptance criteria of the approved
method.
(5) Method-defined analyte means an analyte defined solely by the
method used to determine the analyte. Such an analyte may be a physical
parameter, a parameter that is not a specific chemical, or a parameter
that may be comprised of a number of substances. Examples of such
analytes include temperature, oil and grease, total suspended solids,
total phenolics, turbidity, chemical oxygen demand, and biochemical
oxygen demand.
(6) QC means ``quality control.''
(b) Method modifications. (1) If the underlying chemistry and
determinative technique in a modified method are essentially the same
as an unmodified part 136 method, then the modified method is an
equivalent and acceptable alternative to the approved method. However,
those who develop or use a modification to an approved (part 136)
method must document that the performance of the modified method, in
the matrix to which the modified method will be applied, is equivalent
to the performance of the approved method. This documentation should
include the routine initial demonstration of capability and ongoing QC
including determination of precision and accuracy, detection limits,
and matrix spike recoveries. Initial demonstration of capability
typically
[[Page 58069]]
includes analysis of a four replicate mid-level standard and a method
detection limit study. Ongoing quality control typically includes
method blanks, mid-level laboratory control samples, and matrix spikes.
The method is considered equivalent if the quality control requirements
in the reference method are achieved. The method user's Standard
Operating Procedure (SOP) must clearly document the modifications made
to the reference method. Examples of allowed method modifications are
listed below. The user must notify their permitting authority and/or
their certification authority/accreditation body of the intent to use a
modified method when accreditation is requested. Such notification
should be of the form ``Method xxx has been modified within the
flexibility allowed in 40 CFR Part 136.6''. Specific details of the
modification need not be provided, but must be documented in the
Standard Operating Procedure (SOP). The certification authority/
accreditation body may request a copy of the SOP.
(2) Requirements. The modified method must have sufficient
sensitivity to meet the data quality objectives. The modified method
must also meet or exceed performance of the approved method(s) for the
analyte(s) of interest, as documented by meeting the initial and
ongoing quality control requirements in the method.
(i) Requirements for establishing equivalent performance. If the
approved method contains QC tests and QC acceptance criteria, the
modified method must use these QC tests and the modified method must
meet the QC acceptance criteria with the following conditions:
(A) The analyst may only rely on QC tests and QC acceptance
criteria in a method if it includes wastewater matrix QC tests and QC
acceptance criteria (e.g., matrix spikes) and both initial (start-up)
and ongoing QC tests and QC acceptance criteria.
(B) If the approved method does not contain QC tests and QC
acceptance criteria or if the QC tests and QC acceptance criteria in
the method do not meet the requirements of this section, then the
analyst must employ QC tests published in the ``equivalent'' or part
136 method that has such QC, or the essential QC requirements specified
at 136.7. If the QC requirements are sufficient, but published in other
parts of an organization's compendium rather than within the part 136
method then that part of the organization's compendium must be used.
(C) In addition, the analyst must perform ongoing QC tests,
including assessment of performance of the modified method on the
sample matrix (e.g., analysis of a matrix spike/matrix spike duplicate
pair for every twenty samples), and analysis of an ongoing precision
and recovery sample (e.g., laboratory fortified blank or blank spike)
and a blank with each batch of 20 or fewer samples.
(D) Calibration must be performed using the modified method. The
modified method must be tested with every wastewater matrix and be
applied to up to nine distinct matrices in addition to any and all
reagent water tests. If the performance in the wastewater matrix or
reagent water does not meet the QC acceptance criteria, the method
modification may not be used.
(ii) Requirements for documentation. The modified method must be
documented in a method write-up or an addendum that describes the
modification(s) to the approved method prior to the use of the method
for compliance purposes. The write-up or addendum must include a
reference number (e.g., method number), revision number, and revision
date so that it may be referenced accurately. In addition, the
organization that uses the modified method must document the results of
QC tests and keep these records, along with a copy of the method write-
up or addendum, for review by an auditor.
(3) Restrictions. An analyst may not modify an approved Clean Water
Act analytical method for a method-defined analyte. In addition, an
analyst may not modify an approved method if the modification would
result in measurement of a different form or species of an analyte.
Changes in method parameters are not allowed if such changes would
alter the defined methodology (i.e. method principle) of the unmodified
method. For example, phenol method 420.1 or 420.4 defines phenolics as
ferric iron oxidized compounds that react with 4-aminoantipyrine (4-
AAP) at pH 10 after being distilled from acid solution. Because total
phenolics represents a group of compounds that all react at different
efficiencies with 4-AAP, changing test conditions likely would change
the behavior of these different phenolic compounds. An analyst may not
modify any sample preservation and/or holding time requirements of an
approved method.
(4) Allowable changes. Except as noted under Restrictions of this
section, an analyst may modify an approved test procedure (analytical
method) provided the underlying reactions and principles used in the
approved method remain essentially the same and provided that the
requirements of this section are met. If equal or better performance
can be obtained with an alternative reagent, then it is allowed. These
changes refer to modifications of the analytical procedures used for
identification and measurement of the analyte and do not apply to
sample collection and preservation procedures. Some examples of these
types of changes are:
(A) Use of gas diffusion in place of manual or automated
distillation.
(B) Changes in equipment operating parameters such as the
monitoring wavelength of a colorimeter or the reaction time and
temperature as needed to achieve the chemical reactions defined in the
unmodified CWA method. For example, molybdenum blue phosphate methods
have two absorbance maxima, one at about 660 nm and another at about
880 nm. The former is about 2.5 times less sensitive than the latter.
Wavelength choice provides a cost effective, dilution free means to
increase sensitivity of molybdenum blue phosphate methods.
(C) Interchange of oxidants, such as the use of titanium oxide in
UV assisted automated digestion of TOC and total Phosphorus as long as
complete oxidation can be demonstrated.
(5) Previously Accepted Modifications. The following modifications
have been used successfully in the laboratory community for many years.
Data have demonstrated that these modifications provide equivalent
performance to the methods approved at part 136 across a wide variety
of matrix types. Therefore, these modifications are allowed without the
need to generate additional equivalency data, or the specific
notification of permitting and/or certification authority/accreditation
bodies required for novel method modifications. However, a laboratory
wishing to use these modifications must continue to demonstrate
acceptable method performance by performing and documenting all
applicable initial demonstration of capability and ongoing QC tests and
meeting all applicable QC acceptance criteria as described in Sec.
136.7.
(i) Changes between manual method, flow analyzer and discrete
instrumentation.
(ii) Changes in chromatographic columns or temperature programs.
(iii) Changes between automated and manual sample preparation, such
as digestions, distillations, and extractions; in-line sample
preparation is an acceptable form of automated sample preparation for
CWA methods.
(iv) In general, ICP-MS is a sensitive and selective detector for
metal analysis; however, isobaric interference can cause
[[Page 58070]]
problems for quantitative determination as well as identification based
on the isotope pattern. Interference reduction technologies, such as
collision or reaction cells, are designed to reduce the effect of
spectroscopic interferences that may bias results for the element of
interest. The use of interference reduction technologies is allowed
provided the method performance specifications relevant to ICP-MS
measurements are met.
(v) The use of EPA Method 200.2 or the sample preparation steps
from EPA Method 1638 including the use of closed vessel digestion is
allowed for EPA Method 200.8 provided the method performance
specifications relevant to the ICP-MS are met.
(vi) Changes in pH adjustment reagents. Changes in compounds used
to adjust pH are acceptable as long as they do not produce
interference. For example, using a different acid to adjust pH in
colorimetric methods.
(vi) Changes in buffer reagents are acceptable provided that the
changes do not produce interferences.
(viii) Changes in the order of reagent addition are acceptable
provided that the change does not produce interference. For example
using the same reagents, but adding them in different order or
preparing them in combined or separate solutions (so they can be added
separately), is allowed provided reagent stability or method
performance is improved.
(ix) Changes in calibration range (provided that the modified range
covers any relevant regulatory limit.)
(x) Changes in calibration model. Linear calibration models do not
adequately fit calibration data with one or two inflection points. For
example, vendor-supplied data acquisition and processing software
provides quadratic fitting functions to handle such situations. If
calibration data for a particular analytical method routinely display
quadratic character, using quadratic fitting functions is acceptable.
In such cases, the minimum number of calibrators for second order fits
should be six and in no case should concentrations be extrapolated for
instrument responses that exceed that of the most concentrated
calibrator. Examples of methods with nonlinear calibration functions
include chloride by SM4500-Cl-E-1997, hardness by EPA 130.1, cyanide by
ASTM D6888 or OIA1677, Kjeldahl nitrogen by PAI-DK03, and anions by EPA
300.0. When a regression curve is calculated as an alternative to using
the average response factor, the quality of the calibration may be
evaluated using the Relative Standard Error (RSE). The acceptance
criterion for the RSE is the same as the acceptance criterion for
Relative Standard Deviation (RSD), in the method. RSE is calculated as:
[GRAPHIC] [TIFF OMITTED] TP23SE10.001
Using the RSE as a metric has the added advantage of allowing the
same numerical standard to be applied to the calibration model,
regardless of the form of the model. Thus, if a method states that the
RSD should be <= 20% for the traditional linear model through the
origin, then the RSE acceptance limit can remain <= 20% as well.
Similarly, if a method provides an RSD acceptance limit of <= 15%, then
that same figure can be used as the acceptance limit for the RSE. RSE
may be used as an alternative to correlation coefficients and
coefficients of determination for evaluating calibration curves for any
of the methods at part 136. If the method includes a numerical
criterion for the RSD, then the same numerical value is used for the
RSE. Some older methods do not include any criterion for the
calibration curve--for these methods if RSE is used the value should be
<= 20%. Note that RSE is included as an alternative to correlation
coefficient as a measure of the suitability of a calibration curve. It
is not necessary to evaluate both RSE and correlation coefficients.
(xi) Changes in equipment such as using similar equipment from a
vendor different from that mentioned in the method.
(xii) The use of micro or midi distillation apparatus in place of
macro distillation apparatus.
(xiii) The use of prepackaged reagents.
(xiv) The use of digital titrators and methods where the underlying
chemistry used for the determination is similar to that used in the
approved method.
(xv) Use of Selected Ion Monitoring (SIM) mode for analytes that
cannot be effectively analyzed in full scan mode and reach the required
minimum detectible concentration. False positives are more of a concern
when using SIM analysis, so at a minimum, one quantitation and two
qualifying ions
[[Page 58071]]
must be monitored for each analyte (unless less than three ions with
intensity greater than 15% of the base peak are available). The ratio
of the two qualifying ions to the quantitation ion must be evaluated
and should agree with the ratio of an authentic standard within plus/
minus 20 percent. Analyst judgment must be applied to the evaluation of
ion ratios since the ratios can be affected by co-eluting matrix
compounds. The signal to noise ratio of the least sensitive ion should
be at least 3:1. Retention time should match within 0.05 minute of an
authentic standard analyzed under identical conditions. Matrix
compounds can cause minor shifts in retention time and can be evaluated
by observing any shifts in the retention times of the internal
standards. The total scan time should be such that a minimum of eight
scans are obtained per chromatographic peak.
(xvi) Changes are allowed in purge-and-trap sample volumes or
operating conditions. Some examples are:
(A) Changes in purge time and purge-gas flow rate. A change in
purge time and purge-gas flow rate is allowed provided sufficient total
purge volume is used to achieve the required minimum detectible
concentration and calibration range for all compounds. In general, a
purge rate in the range 20-200 mL/min and a total purge volume in the
range 240-880 mL are recommended.
(B) Use of nitrogen or helium as a purge gas provided that the
minimum detectible concentrations for all compounds are met. Using
nitrogen as a purge gas can provide a significant cost saving to the
laboratory, compared to helium.
(C) Sample temperature during the purge state. Gentle heating of
the sample during purge (e.g. 40 [deg]C) increases purge efficiency of
the hydrophilic compounds and improves sample-to-sample repeatability
(%RSD) because all samples are purged under precisely the same
conditions.
(D) Trap sorbent. Any trap design is acceptable provided the data
acquired meet all QC criteria.
(E) Changes to the desorb time. Shortening the desorb time (e.g.
from 4 minutes to 1 minute) has no discernable effect on compound
recoveries, and can shorten overall cycle time and significantly reduce
the amount of water introduced to the analytical system improving the
precision of analysis, especially for water soluble analytes. A desorb
time of four minutes is recommended, however a desorb time in the range
of 0.5-2 minutes may be used provided that all QC specifications in the
method are met.
(F) Use of water management techniques is allowed. Water is always
collected on the trap along with the analytes and is a significant
interference for analytical systems (GC and GC/MS). Modern water
management techniques (e.g., dry purge or condensation points) can
remove moisture from the sample stream and improve analytical
performance.
(xvii) The following modifications are allowable when performing
EPA Method 625: The base/neutral and acid fractions may be added
together and analyzed as one extract provided that the analytes can be
reliably identified and quantified in the combined extracts; the pH
extraction sequence may be reversed to better separate acid and neutral
components; neutral components may be extracted with either acid or
base components; a smaller sample volume may be used to minimize matrix
interferences provided matrix interferences are demonstrated and
documented; an alternate surrogate and internal standard concentrations
other than those specified in the method are acceptable provided that
method performance is not degraded; an alternate calibration curve and
a calibration check other than those specified in the method may be
used; a different solvent for the calibration standards may be used to
match the solvent of the final extract.
(xviii) If the characteristics of a wastewater matrix prevent
efficient recovery of organic pollutants and prevent the method from
meeting QC requirements, the analyst may attempt to resolve the issue
by using salts provided that such salts do not react with or introduce
the target pollutant into the sample (as evidenced by the analysis of
method blanks, laboratory control samples, and spiked samples that also
contain such salts) and that all requirements of paragraph (b)(2) of
this section are met. Chlorinated samples must be dechlorinated prior
to the addition of such salts.
(xix) If the characteristics of a wastewater matrix result in poor
sample dispersion or reagent deposition on equipment and prevent the
analyst from meeting QC requirements, the analyst may attempt to
resolve the issue by adding a inert surfactant that does not affect the
chemistry of the method such as Brij-35 or sodium dodecyl sulfate
(SDS), provided that such surfactant does not react with or introduce
the target pollutant into the sample (as evidenced by the analysis of
method blanks, laboratory control samples, and spiked samples that also
contain such surfactant) and that all requirements of paragraph (b)(1)
and (b)(2) of this section are met. Chlorinated samples must be
dechlorinated prior to the addition of such surfactant.
7. Add new Sec. 136.7 to part 136 to read as follows:
Sec. 136.7 Quality assurance and quality control.
(a) Twelve essential Quality Control checks and acceptable
abbreviations are:
(1) Demonstration of Capability (DOC);
(2) Method Detection Limit (MDL);
(3) Laboratory reagent blank (LRB), also referred to as method
blank;
(4) Laboratory fortified blank (LFB), also referred to as a spiked
blank, or laboratory control sample (LCS);
(5) Matrix spike, matrix spike duplicate, or laboratory fortified
blank duplicate (LFBD) for suspected difficult matrices;
(6) Internal standards, surrogate standards (for organic analysis)
or tracers (for radiochemistry);
(7) Calibration (initial and continuing), initial and continuing
performance (ICP) solution also referred to as initial calibration
verification (ICV) and continuing calibration verification (CCV);
(8) Control charts (or other trend analyses of quality control
results);
(9) Corrective action (root cause analyses);
(10) QC acceptance criteria;
(11) Definitions of a batch (preparation and analytical); and
(12) Specify a minimum frequency for conducting these QC checks.
(b) These twelve quality control checks must be clearly documented
in the written method along with a performance specification or
description for each of the twelve quality control checks.
Appendix A [Removed and Reserved]
8. Remove and reserve Appendix A to Part 136.
Appendix C [Removed and Reserved]
9. Remove and reserve Appendix C to Part 136.
10. Revise Appendix D to Part 136 to read as follows:
Appendix D to Part 136--Precision and Recovery Statement for Methods
for Measuring Metals
Two selected methods from ``Methods for Chemical Analysis of Water
and Wastes'', EPA-600/4-79-020 (1979) have been subjected to
interlaboratory method validation studies. The two selected methods are
Thallium and Zinc. The following precision and recovery statements are
presented in this appendix and incorporated into part 136:
[[Page 58072]]
Method 279.2
For Thallium, Method 279.2 (Atomic Absorption, Furnace Technique)
replace the Precision and Accuracy Section statement with the
following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was
conducted by the Quality Assurance Branch (QAB) of the Environmental
Monitoring Systems Laboratory--Cincinnati (EMSL-CI). Synthetic
concentrates containing various levels of this element were added to
reagent water, surface water, drinking water and three effluents. These
samples were digested by the total digestion procedure, 4.1.3 in this
manual. Results for the reagent water are given below. Results for
other water types and study details are found in ``EPA Method Study 31,
Trace Metals by Atomic Absorption (Furnace Techniques),'' National
Technical Information Service, 5285 Port Royal Road, Springfield, VA
22161 Order No. PB 86-121 704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 10.00-252 [micro]g/L
X = 0.8781(C)-0.715
S = 0.1112(X) + 0.669
SR = 0.1005(X) + 0.241
Where:
C = True Value for the Concentration, [micro]g/L
X = Mean Recovery, [micro]g/L
S = Multi-laboratory Standard Deviation, [micro]g/L
SR = Single-analyst Standard Deviation, [micro]g/L
Method 289.2
For Zinc, Method 289.2 (Atomic Absorption, Furnace Technique)
replace the Precision and Accuracy Section statement with the
following:
Precision and Accuracy
An interlaboratory study on metal analyses by this method was
conducted by the Quality Assurance Branch (QAB) of the Environmental
Monitoring Systems Laboratory--Cincinnati (EMSL-CI). Synthetic
concentrates containing various levels of this element were added to
reagent water, surface water, drinking water and three effluents. These
samples were digested by the total digestion procedure, 4.1.3 in this
manual. Results for the reagent water are given below. Results for
other water types and study details are found in ``EPA Method Study 31,
Trace Metals by Atomic Absorption (Furnace Techniques),'' National
Technical Information Service, 5285 Port Royal Road, Springfield, VA
22161 Order No. PB 86-121 704/AS, by Copeland, F.R. and Maney, J.P.,
January 1986.
For a concentration range of 0.51-189 [micro]g/L
X = 1.6710(C) + 1.485
S = 0.6740(X)-0.342
SR = 0.3895(X)-0.384
Where:
C = True Value for the Concentration, [micro]g/L
X = Mean Recovery, [micro]g/L
S = Multi-laboratory Standard Deviation, [micro]g/L
SR = Single-analyst Standard Deviation, [micro]g/L
PART 260--HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL
11. The authority citation for part 260 continues to read as
follows:
Authority: 42 U.S.C. 6905, 6912(a), 6921-6927, 6930, 6934,
6935, 6937, 6938, 6939, and 6974.
Subpart B--Definitions
12. Section 260.11 is amended by revising paragraph (c)(2) to read
as follows:
Sec. 260.11 References.
* * * * *
(c) * * *
(2) Method 1664, Revision A and Revision B, 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, PB99-121949 and EPA-821-R-10-001, February 2010. IBR
approved for part 261, appendix IX.
* * * * *
PART 423--STEAM ELECTRIC POWER GENERATING POINT SOURCE CATEGORY
13. The authority citation for part 423 continues to read as
follows:
Authority: Secs. 301; 304(b), (c), (e), and (g); 306(b) and
(c); 307(b) and (c); and 501, Clean Water Act (Federal Water
Pollution Control Act Amendments of 1972, as amended by Clean Water
Act of 1977) (the ``Act''; 33 U.S.C. 1311; 1314(b), (c), (e), and
(g); 1316(b) and (c); 1317(b) and (c); and 1361; 86 Stat. 816, Pub.
L. 92-500; 91 Stat. 1567, Pub. L. 95-217), unless otherwise noted.
14. Section 423.11 is amended by revising paragraphs (a) and (l) to
read as follows:
Sec. 423.11 Specialized definitions.
* * * * *
(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.
* * * * *
(l) 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.
* * * * *
PART 430--PULP, PAPER, AND PAPERBOARD POINT SOURCE CATEGORY
15. The authority citation for part 430 continues to read as
follows:
Authority: Secs. 301, 304, 306, 307, 308, 402, and 501, Clean
Water Act as amended, (33 U.S.C. 1311, 1314, 1316, 1317, 1318, 1342,
and 1361) and Section 112 of the Clean Air Act, as amended (42
U.S.C. 7412).
General Provisions
16. Section 430.01 is amended by revising paragraph (a) and by
adding paragraphs (s) through (v) to read as follows:
Sec. 430.01 General definitions.
* * * * *
(a) Adsorbable organic halides (AOX). A bulk parameter that
measures the total mass of chlorinated organic matter in water and
wastewater. The approved method of analysis for AOX is Method 1650,
listed in Table 1C at 40 CFR 136.3.
* * * * *
(s) TCDD. 2,3,7,8-tetrachlorodibenzop-dioxin. The approved method
of analysis for TCDD is Method 1613B, listed in Table 1C at 40 CFR
136.3.
(t) TCDF. 2,3,7,8-tetrachlorodibenzop-furan. The approved method of
analysis for TCDF is Method 1613B, listed in Table 1C at 40 CFR 136.3.
(u) Chloroform is listed with approved methods of analysis in Table
1C at 40 CFR 136.3.
(v) The approved method of analysis for the following chlorinated
phenolic compounds is Method 1653, listed in Table 1C at 40 CFR 136.3:
(1) Trichlorosyringol.
(2) 3,4,5-trichlorocatechol.
(3) 3,4,6-trichlorocatechol.
(4) 3,4,5-trichloroguaiacol.
(5) 3,4,6-trichloroguaiacol.
(6) 4,5,6-trichloroguaiacol.
(7) 2,4,5-trichlorophenol.
(8) 2,4,6-trichlorophenol.
(9) Tetrachlorocatechol.
(10) Tetrachloroguaiacol.
(11) 2,3,4,6-tetrachlorophenol.
(12) Pentachlorophenol.
[[Page 58073]]
PART 435--OIL AND GAS EXTRACTION POINT SOURCE CATEGORY
17. The authority citation for part 435 continues to read as
follows:
Authority: 33 U.S.C. 1311, 1314, 1316, 1317, 1318, 1342, and
1361.
18. Section 435.11 is amended as follows:
a. By revising paragraph (d).
b. By revising paragraph (e).
c. By revising paragraph (k)(2).
d. By revising paragraph (o).
e. By revising paragraph (t).
f. By revising paragraph (u).
g. By revising paragraph (x).
h. By revising paragraph (ee).
i. By revising paragraph (gg).
j. By revising paragraph (hh).
k. By revising paragraph (ss).
l. By adding paragraph (uu).
Sec. 435.11 Specialized definitions.
* * * * *
(d) Base fluid retained on cuttings as applied to BAT effluent
limitations and NSPS refers to the ``Determination of the Amount of
Non-Aqueous Drilling Fluid (NAF) Base Fluid from Drill Cuttings by a
Retort Chamber (Derived from API Recommended Practice 13B-2)'', EPA
Method 1674, which is published in ``Analytic Methods for the Oil and
Gas Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph
(uu) of this section.
(e) Biodegradation rate as applied to BAT effluent limitations and
NSPS for drilling fluids and drill cuttings refers to the ``Protocol
for the Determination of Degradation of Non Aqueous Base Fluids in a
Marine Closed Bottle Biodegradation Test System: Modified ISO
11734:1995,'' EPA Method 1647, supplemented with ``Procedure for Mixing
Base Fluids With Sediments,'' EPA Method 1646. Both EPA Method 1646 and
1647 are published in ``Analytic Methods for the Oil and Gas Extraction
Point Source Category,'' EPA-821-R-09-013. See paragraph (uu) of this
section.
* * * * *
(k) * * *
(2) Dry drill cuttings means the residue remaining in the retort
vessel after completing the retort procedure specified in EPA Method
1674, which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph
(uu) of this section.
* * * * *
(o) Formation oil means the oil from a producing formation which is
detected in the drilling fluid, as determined by the GC/MS compliance
assurance method when the drilling fluid is analyzed before being
shipped offshore, and as determined by the RPE method, EPA Method 1670,
when the drilling fluid is analyzed at the offshore point of discharge.
The GC/MS compliance assurance method and the RPE method approved for
use with this part are published in the ``Analytic Methods for the Oil
and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See
paragraph (uu) of this section. Detection of formation oil by the RPE
method may be confirmed by the GC/MS compliance assurance method, and
the results of the GC/MS compliance assurance method shall apply
instead of those of the RPE method.
* * * * *
(t) Maximum weighted mass ratio averaged over all NAF well sections
for BAT effluent limitations and NSPS for base fluid retained on
cuttings means the weighted average base fluid retention for all NAF
well sections as determined by EPA Method 1674, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See paragraph (uu) of this section.
(u) Method 1654A refers to EPA Method 1654, Revision A, entitled
``PAH Content of Oil by HPLC/UV,'' December 1992, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See paragraph (uu) of this section.
* * * * *
(x) No discharge of free oil means that waste streams may not be
discharged that contain free oil as evidenced by the monitoring method
specified for that particular stream, e.g., deck drainage or
miscellaneous discharges cannot be discharged when they would cause a
film or sheen upon or discoloration of the surface of the receiving
water; drilling fluids or cuttings may not be discharged when they fail
EPA Method 1617 (Static Sheen Test), which is published in ``Analytic
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-09-013. See paragraph (uu) of this section.
* * * * *
(ee) Sediment toxicity as applied to BAT effluent limitations and
NSPS for drilling fluids and drill cuttings refers to the ASTM E 1367-
92 method: ``Standard Guide for Conducting 10-day Static Sediment
Toxicity Tests with Marine and Estuarine Amphipods,'' 1992, with
Leptocheirus plumulosus as the test organism and sediment preparation
procedures specified in EPA Method 1646, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See paragraph (uu) of this section. This
incorporation by reference was approved by the Director of the Federal
Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies
may be obtained from the American Society for Testing and Materials,
100 Barr Harbor Drive, West Conshohocken, PA, 19428. Copies may be
inspected at the National Archives and Records Administration (NARA).
For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be
inspected at EPA's Water Docket, 1200 Pennsylvania Ave., NW.,
Washington, DC 20460.
* * * * *
(gg) SPP toxicity as applied to BAT effluent limitations and NSPS
for drilling fluids and drill cuttings refers to the bioassay test
procedure, ``Suspended Particulate Phase (SPP) Toxicity Test,''
presented in EPA Method 1619, which is published in ``Analytic Methods
for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-
013. See paragraph (uu) of this section.
(hh) Static sheen test means the standard test procedure that has
been developed for this industrial subcategory for the purpose of
demonstrating compliance with the requirement of no discharge of free
oil. The methodology for performing the static sheen test is presented
in EPA Method 1617, which is published in ``Analytic Methods for the
Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See
paragraph (uu) of this section.
* * * * *
(ss) C16-C18 internal olefin drilling fluid
means a C16-C18 internal olefin drilling fluid
formulated as specified in Appendix 1 of Subpart A of this part.
* * * * *
(uu) Analytic Methods for the Oil and Gas Extraction Point Source
Category is the EPA document, EPA-821-R-09-013, that compiles analytic
methods for this category. This incorporation by reference was approved
by the Director of the Federal Register in accordance with 5 U.S.C.
552(a) and 1 CFR part 51. Copies may be inspected at the National
Archives and Records Administration (NARA). For information on the
availability of this material at NARA, call 202-741-6030, or go to:
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be inspected at EPA's
[[Page 58074]]
Water Docket, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
19. In Sec. 435.12, the first footnote to the table is revised to
read as follows:
Sec. 435.12 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
practicable control technology currently available (BPT).
* * * * *
BPT Effluent Limitations--Oil and Grease
* * * * *
* * * * *
\1\ No discharge of free oil. See Sec. 435.11(x).
* * * * *
20. In Sec. 435.13, footnotes 2, 3, and 5 through 11 to the table
are revised to read as follows:
Sec. 435.13 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
available technology economically achievable (BAT).
* * * * *
BAT Effluent Limitations
* * * *
\2\ As determined by the suspended particulate phase (SPP) toxicity
test. See Sec. 435.11(gg).
\3\ As determined by the static sheen test. See Sec. 435.11(hh).
* * * * *
\5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) of stock
base fluid as determined by EPA Method 1654, Revision A, [specified at
Sec. 435.11(u)] entitled ``PAH Content of Oil by HPLC/UV,'' December
1992, which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(uu).
\6\ Base fluid sediment toxicity ratio = 10-day LC50 of C16-C18 internal
olefin/10-day LC50 of stock base fluid as determined by ASTM E 1367-92
[specified at Sec. 435.11(ee)] method: ``Standard Guide for
Conducting 10-day Static Sediment Toxicity Tests with Marine and
Estuarine Amphipods,'' 1992, after preparing the sediment according to
the procedure specified in EPA Method 1646, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).
\7\ Biodegradation rate ratio = Cumulative headspace gas production (ml)
of C16-C18 internal olefin/Cumulative headspace gas production (ml) of
stock base fluid, both at 275 days as determined by EPA Method 1647,
which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(e) and (uu).
\8\ Drilling fluid sediment toxicity ratio = 4-day LC50 of C16-C18
internal olefin drilling fluid/4-day LC50 of drilling fluid removed
from drill cuttings at the solids control equipment as determined by
ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static
Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992,
with Leptocheirus plumulosus as the test organism and sediment
preparation procedures specified in EPA Method 1646, which is
published in ``Analytic Methods for the Oil and Gas Extraction Point
Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu).
\9\ As determined before drilling fluids are shipped offshore by the GC/
MS compliance assurance method (EPA Method 1655), and as determined
prior to discharge by the RPE method (EPA Method 1670) applied to
drilling fluid removed from drill cuttings. If the operator wishes to
confirm the results of the RPE method (EPA Method 1670), the operator
may use the GC/MS compliance assurance method (EPA Method 1655).
Results from the GC/MS compliance assurance method (EPA Method 1655)
shall supersede the results of the RPE method (EPA Method 1670). EPA
Method 1655 and 1670 are published in ``Analytic Methods for the Oil
and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(uu).
\10\ Maximum permissible retention of non-aqueous drilling fluid (NAF)
base fluid on wet drill cuttings averaged over drilling intervals
using NAFs as determined by EPA Method 1674, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation
is applicable for NAF base fluids that meet the base fluid sediment
toxicity ratio (Footnote 6), biodegradation rate ratio (Footnote 7),
PAH, mercury, and cadmium stock limitations (C16-C18 internal olefin)
defined above in this table.
\11\ Maximum permissible retention of non-aqueous drilling fluid (NAF)
base fluid on wet drill cuttings averaged over drilling intervals
using NAFs as determined by EPA Method 1674, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation
is applicable for NAF base fluids that meet the ester base fluid
sediment toxicity ratio and ester biodegradation rate ratio stock
limitations defined as:
(a) Ester base fluid sediment toxicity ratio = 10-day LC50 of C12-C14
ester or C8 ester/10-day LC50 of stock base fluid as determined by
ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static
Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992,
with Leptocheirus plumulosus as the test organism and sediment
preparation procedures specified in EPA Method 1646, which is
published in ``Analytic Methods for the Oil and Gas Extraction Point
Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu);
(b) Ester biodegradation rate ratio = Cumulative headspace gas
production (ml) of C12-C14 ester or C8 ester/Cumulative headspace gas
production (ml) of stock base fluid, both at 275 days as determined by
EPA Method 1647, which is published in ``Analytic Methods for the Oil
and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(e) and (uu); and (c) PAH mass ratio (Footnote 5), mercury,
and cadmium stock limitations (C16-C18 internal olefin) defined above
in this table.
21. In Sec. 435.14, footnote 2 to the table is revised to read as
follows:
Sec. 435.14 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
conventional pollutant control technology (BCT).
* * * * *
BAT Effluent Limitations
* * * *
\2\ As determined by the static sheen test. See Sec. 435.11(hh).
* * * * *
22. In Sec. 435.15, footnotes 2, 3, and 5 through 11 to the table
are revised to read as follows:
Sec. 435.15 Standards of performance for new sources (NSPS).
* * * * *
New Source Performance Standards
* * * * *
\2\ As determined by the suspended particulate phase (SPP) toxicity
test. See Sec. 435.11(gg).
\3\ As determined by the static sheen test. See Sec. 435.11(hh).
* * * * *
\5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) of stock
base fluid as determined by EPA Method 1654, Revision A, [specified at
Sec. 435.11(u)] entitled ``PAH Content of Oil by HPLC/UV,'' December
1992, which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(uu).
\6\ Base fluid sediment toxicity ratio = 10-day LC50 of C16-C18 internal
olefin/10-day LC50 of stock base fluid as determined by ASTM E 1367-92
[specified at Sec. 435.11(ee)] method: ``Standard Guide for
Conducting 10-day Static Sediment Toxicity Tests with Marine and
Estuarine Amphipods,'' 1992, after preparing the sediment according to
the procedure specified in EPA Method 1646, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu).
\7\ Biodegradation rate ratio = Cumulative headspace gas production (ml)
of C16-C18 internal olefin/Cumulative headspace gas production (ml) of
stock base fluid, both at 275 days as determined by EPA Method 1647,
which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(e) and (uu).
\8\ Drilling fluid sediment toxicity ratio = 4-day LC50 of C16-C18
internal olefin drilling fluid/4-day LC50 of drilling fluid removed
from drill cuttings at the solids control equipment as determined by
ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static
Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992,
with Leptocheirus plumulosus as the test organism and sediment
preparation procedures specified in EPA Method 1646, which is
published in ``Analytic Methods for the Oil and Gas Extraction Point
Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu).
[[Page 58075]]
\9\ As determined before drilling fluids are shipped offshore by the GC/
MS compliance assurance method (EPA Method 1655), and as determined
prior to discharge by the RPE method (EPA Method 1670) applied to
drilling fluid removed from drill cuttings. If the operator wishes to
confirm the results of the RPE method (EPA Method 1670), the operator
may use the GC/MS compliance assurance method (EPA Method 1655).
Results from the GC/MS compliance assurance method (EPA Method 1655)
shall supersede the results of the RPE method (EPA Method 1670). EPA
Method 1655 and 1670 are published in ``Analytic Methods for the Oil
and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(uu).
\10\ Maximum permissible retention of non-aqueous drilling fluid (NAF)
base fluid on wet drill cuttings averaged over drilling intervals
using NAFs as determined by EPA Method 1674, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation
is applicable for NAF base fluids that meet the base fluid sediment
toxicity ratio (Footnote 6), biodegradation rate ratio (Footnote 7),
PAH, mercury, and cadmium stock limitations (C16-C18 internal olefin)
defined above in this table.
\11\ Maximum permissible retention of non-aqueous drilling fluid (NAF)
base fluid on wet drill cuttings average over drilling intervals using
NAFs as determined by EPA Method 1674, which is published in
``Analytic Methods for the Oil and Gas Extraction Point Source
Category,'' EPA-821-R-09-013. See Sec. 435.11(uu). This limitation
is applicable for NAF base fluids that meet the ester base fluid
sediment toxicity ratio and ester biodegradation rate ratio stock
limitations defined as:
(a) Ester base fluid sediment toxicity ratio = 10-day LC50 of C12-C14
ester or C8 ester/10-day LC50 of stock base fluid as determined by
ASTM E 1367-92 method: ``Standard Guide for Conducting 10-day Static
Sediment Toxicity Tests with Marine and Estuarine Amphipods,'' 1992,
with Leptocheirus plumulosus as the test organism and sediment
preparation procedures specified in EPA Method 1646, which is
published in ``Analytic Methods for the Oil and Gas Extraction Point
Source Category,'' EPA-821-R-09-013. See Sec. 435.11(ee) and (uu);
(b) Ester biodegradation rate ratio = Cumulative headspace gas
production (ml) of C12-C14 ester or C8 ester/Cumulative headspace gas
production (ml) of stock base fluid, both at 275 days as determined by
EPA Method 1647, which is published in ``Analytic Methods for the Oil
and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See Sec.
435.11(e) and (uu); and (c) PAH mass ratio (Footnote 5), mercury,
and cadmium stock limitations (C16-C18 internal olefin) defined above
in this table.
23. Subpart A of part 435 is amended by removing Appendices 1
through 7.
24. Subpart A of part 435 is amended by redesignating Appendix 8 as
Appendix 1.
Subpart D--Coastal Subcategory
25. Section 435.41 is amended,
a. By revising paragraph (d).
b. By revising paragraph (e).
c. By revising paragraph (k).
d. By revising paragraph (m)(2).
e. By revising paragraph (q).
f. By revising paragraph (r).
g. By revising paragraph (y).
h. By revising paragraph (ee).
i. By revising paragraph (ff).
j. By adding paragraph (mm).
Sec. 435.41 Specialized definitions.
* * * * *
(d) Base fluid retained on cuttings as applied to BAT effluent
limitations and NSPS refers to the ``Determination of the Amount of
Non-Aqueous Drilling Fluid (NAF) Base Fluid from Drill Cuttings by a
Retort Chamber (Derived from API Recommended Practice 13B-2)'', EPA
Method 1674, which is published in ``Analytic Methods for the Oil and
Gas Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph
(mm) of this section.
(e) Biodegradation rate as applied to BAT effluent limitations and
NSPS for drilling fluids and drill cuttings refers to the ``Protocol
for the Determination of Degradation of Non Aqueous Base Fluids in a
Marine Closed Bottle Biodegradation Test System: Modified ISO
11734:1995,'' EPA Method 1647, supplemented with ``Procedure for Mixing
Base Fluids With Sediments,'' EPA Method 1646. Both EPA Method 1646 and
1647 are published in ``Analytic Methods for the Oil and Gas Extraction
Point Source Category,'' EPA-821-R-09-013. See paragraph (mm) of this
section.
* * * * *
(k) Diesel oil refers to the grade of distillate fuel oil, as
specified in the American Society for Testing and Materials Standard
Specification for Diesel Fuel Oils D975-91, that is typically used as
the continuous phase in conventional oil-based drilling fluids. This
incorporation by reference was approved by the Director of the Federal
Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies
may be obtained from the American Society for Testing and Materials,
100 Barr Harbor Drive, West Conshohocken, PA 19428. Copies may be
inspected at the National Archives and Records Administration (NARA).
For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be
inspected at EPA's Water Docket, 1200 Pennsylvania Ave., NW.,
Washington, DC 20460.
* * * * *
(m) * * *
(2) Dry drill cuttings means the residue remaining in the retort
vessel after completing the retort procedure specified in EPA Method
1674, which is published in ``Analytic Methods for the Oil and Gas
Extraction Point Source Category,'' EPA-821-R-09-013. See paragraph
(mm) of this section.
* * * * *
(q) Formation oil means the oil from a producing formation which is
detected in the drilling fluid, as determined by the GC/MS compliance
assurance method, EPA Method 1655, when the drilling fluid is analyzed
before being shipped offshore, and as determined by the RPE method, EPA
Method 1670, when the drilling fluid is analyzed at the offshore point
of discharge. The GC/MS compliance assurance method and the RPE method
approved for use with this part are published in the ``Analytic Methods
for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-
013. See paragraph (mm) of this section. Detection of formation oil by
the RPE method may be confirmed by the GC/MS compliance assurance
method, and the results of the GC/MS compliance assurance method shall
supersede those of the RPE method.
(r) Garbage means all kinds of victual, domestic, and operational
waste, excluding fresh fish and parts thereof, generated during the
normal operation of coastal oil and gas facility and liable to be
disposed of continuously or periodically, except dishwater, graywater,
and those substances that are defined or listed in other Annexes to
MARPOL 73/78. A copy of MARPOL may be inspected at EPA's Water Docket,
1200 Pennsylvania Ave., NW., Washington, DC 20460.
* * * * *
(y) No discharge of free oil means that waste streams may not be
discharged that contain free oil as evidenced by the monitoring method
specified for that particular stream, e.g., deck drainage or
miscellaneous discharges cannot be discharged when they would cause a
film or sheen upon or discoloration of the surface of the receiving
water; drilling fluids or cuttings may not be discharged when they fail
EPA Method 1617 (Static Sheen Test), which is published in ``Analytic
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-09-013. See paragraph (mm) of this section.
* * * * *
(ee) SPP toxicity as applied to BAT effluent limitations and NSPS
for drilling fluids and drill cuttings refers to the bioassay test
procedure, ``Suspended Particulate Phase (SPP) Toxicity Test,''
presented in EPA Method 1619, which is published in ``Analytic Methods
for the Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-
013. See paragraph (mm) of this section.
(ff) Static sheen test means the standard test procedure that has
been
[[Page 58076]]
developed for this industrial subcategory for the purpose of
demonstrating compliance with the requirement of no discharge of free
oil. The methodology for performing the static sheen test is presented
in EPA Method 1617, which is published in ``Analytic Methods for the
Oil and Gas Extraction Point Source Category,'' EPA-821-R-09-013. See
paragraph (mm) of this section.
* * * * *
(mm) Analytic Methods for the Oil and Gas Extraction Point Source
Category is the EPA document, EPA-821-R-09-013, that compiles analytic
methods for this category. This incorporation by reference was approved
by the Director of the Federal Register in accordance with 5 U.S.C.
552(a) and 1 CFR part 51. Copies may be inspected at the National
Archives and Records Administration (NARA). For information on the
availability of this material at NARA, call 202-741-6030, or go to:
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be inspected at EPA's
Water Docket, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
26. In Sec. 435.42, footnote 1 to the table is revised to read as
follows:
Sec. 435.42 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
practicable control technology currently available (BPT).
* * * * *
\1\ No discharge of free oil. See Sec. 435.41(y).
* * * * *
27. In Sec. 435.43, footnotes 2 and 4 are revised to read as
follows:
Sec. 435.43 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
available technology economically achievable (BAT).
* * * * *
Bat Effluent Limitations
* * * * *
\2\ As determined by the static sheen test. See Sec. 435.41(ff).
* * * * *
\4\ As determined by the suspended particulate phase (SPP) toxicity
test. See Sec. 435.41(ee).
* * * * *
28. In Sec. 435.44 footnote 2 to the table is revised to read as
follows:
Sec. 435.44 Effluent limitations guidelines representing the degree
of effluent reduction attainable by the application of the best
conventional pollutant control technology (BCT).
* * * * *
Bat Effluent Limitations
* * * * *
\2\ As determined by the static sheen test. See Sec. 435.41(ff).
* * * * *
29. In Sec. 435.45, footnotes 2 and 4 to the table are revised to
read as follows:
Sec. 435.45 Standards of performance for new sources (NSPS).
* * * * *
NSPS Effluent Limitations
* * * * *
\2\ As determined by the static sheen test. See Sec. 435.41(ff).
* * * * *
\4\ As determined by the suspended particulate phase (SPP) toxicity
test. See Sec. 435.41(ee).
* * * * *
[FR Doc. 2010-20018 Filed 9-22-10; 8:45 am]
BILLING CODE 6560-50-P