[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]



[[Page 58023]]

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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

[[Page 58026]]

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