[Federal Register Volume 77, Number 97 (Friday, May 18, 2012)]
[Rules and Regulations]
[Pages 29758-29846]
[FR Doc No: 2012-10210]

Vol. 77

Friday,

No. 97

May 18, 2012

Part II

Environmental Protection Agency

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40 CFR Parts 136, 260, et al.

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

Federal Register / Vol. 77 , No. 97 / Friday, May 18, 2012 / Rules
and Regulations

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ENVIRONMENTAL PROTECTION AGENCY

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

[EPA-HQ-OW-2010-0192; FRL-9664-6]
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: Final rule.

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SUMMARY: This rule modifies the testing procedures approved for
analysis and sampling under the Clean Water Act. EPA proposed these
changes for public comment on September 23, 2010. The changes adopted
in this final rule fall into the following categories: New and revised
EPA methods and new and revised methods published by voluntary
consensus standard bodies (VCSB), such as ASTM International and the
Standard Methods Committee; updated versions of currently approved
methods; methods reviewed under the alternate test procedures (ATP)
program; clarifications to the process for EPA approval for use of
alternate procedures for nationwide and Regional use; minimum quality
control requirements to improve consistency across method versions;
corrections to previously approved methods; and revisions to sample
collection, preservation, and holding time requirements. Finally, EPA
makes changes to three effluent guideline regulations.

DATES: This regulation is effective on June 18, 2012. The incorporation
by reference of these methods is approved by the Director of the
Federal Register on June 18, 2012. For judicial review purposes, this
final rule is promulgated as of 1:00 p.m. (Eastern time) on June 1,
2012 as provided at 40 CFR 23.2 and 23.7.

ADDRESSES: EPA has established a docket for this action under Docket ID
No. EPA-HQ-OW-2010-0192. All documents in the docket are listed on the
http://www.regulations.gov Web site. Although listed in the index, some
information is not publically available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other materials,
such as copyrighted material, are not placed on the Internet and will
be publicly available only in hard copy form. Publicly available docket
materials are available either electronically through http://www.regulations.gov or in hard copy at the HQ Water Docket Center, EPA/
DC, EPA West, Room 3334, 1301 Constitution Ave. NW., Washington, DC.
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal holidays. The telephone number for the
Public Reading Room is<PHONE_NUMBER>, and the telephone number is 202-
566-2426 for the HQ Water Docket.

FOR FURTHER INFORMATION CONTACT: For information regarding the changes
to inorganic chemical methods, contact Lemuel Walker, Engineering and
Analysis Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave. NW., Washington, DC 20460,<PHONE_NUMBER> (email:
walker.lemuel@epa.gov). For information regarding the changes to
organic chemical methods, contact Maria Gomez-Taylor, Engineering and
Analysis Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave. NW., Washington, DC 20460,<PHONE_NUMBER> (email:
gomez-taylor.maria@epa.gov). For information regarding the changes to
microbiological and whole effluent toxicity methods, contact Robin
Oshiro, Engineering and Analysis Division (4303T), USEPA Office of
Science and Technology, 1200 Pennsylvania Ave. NW., Washington, DC
20460,<PHONE_NUMBER> (email: oshiro.robin@epa.gov).

SUPPLEMENTARY INFORMATION:

A. General Information

1. Does this action apply to me?

    EPA Regions, as well as States, Territories and Tribes authorized
to implement the National Pollutant Discharge Elimination System
(NPDES) program, issue permits with conditions designed to ensure
compliance with the technology-based and water quality-based
requirements of the Clean Water Act (CWA). These permits may include
restrictions on the quantity of pollutants that may be discharged as
well as pollutant measurement and reporting requirements. If EPA has
approved a test procedure for analysis of a specific pollutant, the
NPDES permittee must use an approved test procedure (or an approved
alternate test procedure if specified by the permitting authority) for
the specific pollutant when measuring the required waste constituent.
Similarly, if EPA has established sampling requirements, measurements
taken under an NPDES permit must comply with these requirements.
Therefore, entities with NPDES permits will potentially be affected by
the actions in this rulemaking. Categories and entities that may
potentially be affected by the requirements of today's rule include:

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                                      Examples of potentially affected
             Category                             entities
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State, Territorial, and Indian      States, Territories, and Tribes
 Tribal Governments.                 authorized to administer the NPDES
                                     permitting program; States,
                                     Territories, and Tribes providing
                                     certification under Clean Water Act
                                     section 401; State, Territorial,
                                     and Indian Tribal owned facilities
                                     that must conduct monitoring to
                                     comply with NPDES permits.
Industry..........................  Facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
Municipalities....................  POTWs or other municipality owned
                                     facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
------------------------------------------------------------------------

    This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be affected by this
action. This table lists types of entities that EPA is now aware of
that could potentially be affected by this action. Other types of
entities not listed in the table could also be affected. To determine
whether your facility is affected by this action, you should carefully
examine the applicability language at 40 CFR 122.1 (NPDES purpose and
scope), 40 CFR 136.1 (NPDES permits and CWA) and 40 CFR 403.1
(Pretreatment standards purpose and applicability). If you have
questions regarding the applicability of this action to a particular
entity, consult the appropriate person listed in the preceding FOR
FURTHER INFORMATION CONTACT section.

B. What process governs judicial review of this rule?

    Under Section 509(b)(1) of the Clean Water Act (CWA), judicial
review of today's CWA rule may be obtained by filing a petition for
review in a United States Circuit Court of Appeals within 120 days from
the date of promulgation of this rule. For judicial review purposes,
this final rule is promulgated as of 1 p.m. (Eastern time) on June 1,
2012 as provided at 40 CFR 23.2. The

requirements of this regulation may also not be challenged later in
civil or criminal proceedings brought by EPA.

C. Abbreviations and Acronyms Used in the Preamble and Final Rule

AOAC: AOAC International
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
ISO: International Organization for Standardization
MS: Mass Spectrometry
NIST: National Institute of Standards and Technology
NPDES: National Pollutant Discharge Elimination System
QA: Quality Assurance
QC: Quality Control
SDWA: Safe Drinking Water Act
SM: Standard Methods
SRM: Standard Reference Material
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 Final Rule
    A. New EPA Methods and New Versions of Previously Approved EPA
Methods
    B. New Standard Methods and New Versions of Approved Standard
Methods
    C. New ASTM Methods and New Versions of Previously Approved ASTM
Methods
    D. New Alternate Test Procedures at 40 CFR 136.3
    E. Clarifications and Corrections to Previously Approved Methods
in 40 CFR 136.3
    F. Revisions in Table II at 40 CFR 136.3(e) to Required
Containers, Preservation Techniques, and Holding Times
    G. Revisions to 40 CFR 136.4 and 136.5
    H. Revisions to Method Modification Provisions at 40 CFR 136.6
    I. New Quality Assurance and Quality Control Language at 40 CFR
136.7
    J. Revisions to 40 CFR part 423 (Steam Electric Power Generating
Point Source Category)
III. Changes Between the Proposed Rule and the Final Rule
    A. EPA Is Not Adding EPA Method 1614A
    B. Deferral of Action on EPA Method 1668C
    C. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09
    D. Revisions and Clarifications to EPA Method 200.7
    E. Revisions and Corrections to Certain Citations in Tables IB
and ID
    F. Continued Approval of Method 1664 Revision A
    G. Revision to Footnote 63 of Table IB at 40 CFR 136.3
    H. Revision to Footnote 4 of Table IC at 40 CFR 136.3
    I. Revisions to Table II Language
    J. Approval of Alternate Test Procedures for Limited Use at 40
CFR 136.5
    K. Revisions to Language at Sec.  136.6
    L. Revisions to New Quality Assurance and Quality Control
Language
    M. Withdrawal of Appendices at 40 CFR part 136
    N. Revisions to 40 CFR Part 430 (Pulp, Paper, and Paperboard
Point Source Category)
    O. Revisions to 40 CFR Part 435 (Oil and Gas Extraction Point
Source Category)
IV. Response to Comments
    A. How Standard Methods are Identified in Part 136 Tables
    B. Preservation and Holding Time Requirements for EPA Method 624
    C. Quality Assurance and Quality Control Requirements
V. Statutory and Executive Order Reviews
    A. Executive Order 12866: Regulatory Planning and Review and
Review and Executive Order 13563: Improving Regulation and
Regulatory Review
    B. Paperwork Reduction Act
    C. Regulatory Flexibility Act
    D. Unfunded Mandates Reform Act
    E. Executive Order 13132: Federalism
    F. Executive Order 13175: Consultation and Coordination With
Indian Tribal Governments
    G. Executive Order 13045: Protection of Children From
Environmental Health Risks and Safety Risks
    H. Executive Order 13211: Actions 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
    K. Congressional Review Act

I. Statutory Authority

    EPA is promulgating today's rule pursuant to the authority of
sections 301(a), 304(h), and 501(a) of the Clean Water Act (``CWA'' or
the ``Act''), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of
the Act prohibits the discharge of any pollutant into navigable waters
unless the discharge complies with a National Pollutant Discharge
Elimination System (NPDES) permit issued under section 402 of the Act.
Section 304(h) of the Act requires the Administrator of the EPA to ``*
* * promulgate guidelines establishing test procedures for the analysis
of pollutants that shall include the factors which must be provided in
any certification pursuant to [section 401 of this Act] or permit
application pursuant to [section 402 of this Act].'' Section 501(a) of
the Act authorizes the Administrator to ``* * * prescribe such
regulations as are necessary to carry out this function under [the
Act].'' EPA generally has codified its test procedure regulations
(including analysis and sampling requirements) for CWA programs at 40
CFR part 136, though some requirements are codified in other Parts
(e.g., 40 CFR Chapter I, Subchapters N and O).

II. Summary of Final Rule

    The following sections describe the changes EPA is making in
today's final rule.

A. New EPA Methods and New Versions of Previously Approved EPA Methods

    This rule approves new EPA methods and new versions of already
approved EPA methods. The following discussion briefly describes the
EPA methods added today to Part 136.
    1. Oil and grease. Today's rule adds a new version of EPA Method
1664, 1664 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 for use in CWA
programs. Today, EPA is also amending the RCRA regulations at 40 CFR
260.11, which currently specify the use of Method 1664 Rev. A, to
provide additionally for use of the revised version, 1664 Rev. B. As
stated in the preamble to the proposal (75 FR 58026, Sept. 23, 2010),
EPA encourages that future delistings cite ``Method 1664 Rev. B'' while
delistings already granted may continue to use Method 1664 Rev. A.
    On December 14, 2011, EPA published a notice of data availability
(NODA) on a new method for oil and grease for use in Clean Water Act
programs (see 76 FR 77742). This method, ASTM D-7575-10, uses a
different extractant (a membrane filter instead of n-hexane for the
extraction of oil and grease material) and a different measurement
technique (infrared absorption instead of gravimetry) from the
extractant and measurement technique of currently approved methods for
oil and grease. The new method was discussed in the September 23, 2010
notice but EPA did not propose it for use as an approved method to be
codified at 40 CFR 136.3 because oil and grease is a method-defined
parameter. By definition, the measurement results of method-defined
parameters are specific to the described method and are not directly
comparable to results obtained by another method. However, since
publication of the Methods Update Rule proposal, the Agency received
additional data and information about this method and is re-considering
whether it should add this

method to the list of approved methods for oil and grease at 40 CFR
136.3. In the NODA, EPA proposed to include ASTM D-7575 for the
measurement of oil and grease based on comments received in response to
its September 23, 2010 proposal and the additional data. EPA will make
a decision on the inclusion of the new method once it reviews the
public comments received in response to the NODA and will then publish
that decision in a separate Federal Register notice.
    2. Metals. Today's rule adds EPA Method 200.5 (Revision 4.2):
``Determination of Trace Elements in Drinking Water by Axially Viewed
Inductively Coupled Plasma--Atomic Emission Spectrometry'' to Table IB.
The rule also clarifies that the axial orientation of the torch is
allowed for use with EPA Method 200.7. Thus, EPA will allow the use of
axial instruments or radial instruments to measure metals in water
samples.
    3. Pesticides. Today's rule adds EPA Method 525.2 to Table IG (Test
Methods for Pesticide Active Ingredients) as an additional approved
method for all parameters for which EPA has previously approved EPA
Method 525.1, and also adds Methods 525.1 and 525.2 to Table ID for the
same parameters for which EPA had previously approved Method 525.1 in
Table IG. The rule also adds some of the methods for Pesticide Active
Ingredients (Table IG) to applicable parameters listed in Table ID for
general use. These methods are:
    a. EPA Method 608.1, ``The Determination of Organochlorine
Pesticides in Municipal and Industrial Wastewater.'' 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 method
measures chlorothalonil, DCPA, dichloran, methoxychlor, and permethrin.
    c. EPA Method 614, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' This method
measures azinphos methyl, demeton, diazinon, disulfoton, ethion,
malathion, parathion methyl, and parathion ethyl.
    d. EPA Method 614.1, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' This method
measures dioxathion, EPN, ethion, and terbufos.
    e. EPA Method 615, ``The Determination of Chlorinated Herbicides in
Municipal and Industrial Wastewater.'' 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 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 method measures ametryn,
atraton, atrazine, prometon, prometryn, propazine, sec-bumeton,
simetryn, simazine, terbuthylazine, and terbutryn.
    h. EPA Method 622, ``The Determination of Organophosphorus
Pesticides in Municipal and Industrial Wastewater.'' 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 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 method
measures aminocarb, barban, carbaryl, carbofuran, chlorpropham, diuron,
fenuron, fenuron-TCA, fluometuron, linuron, methiocarb, methomyl,
mexacarbate, monuron, monuron-TCA, neburon, oxamyl, propham, propoxur,
siduron, and swep.
    4. Microbiologicals. Today's rule approves the 2005 versions of EPA
Method 1622, ``Cryptosporidium in Water by Filtration/IMS/FA'' and EPA
Method 1623, ``Cryptosporidium and Giardia in Water by Filtration/IMS/
FA'' in Table IH for ambient water.
    The rule approves revised versions of EPA Methods 1103.1, 1106.1,
1600, 1603, and 1680 in Table IH. The rule also approves the revised
version of EPA Methods 1600, 1603 and 1680 in Table IA. We corrected
technical errors in these revisions.
    5. Non-Conventionals. Today's rule adds EPA Method 1627, ``Kinetic
Test Method for the Prediction of Mine Drainage Quality'' to Table IB
as a new parameter termed ``Acid Mine Drainage.''
    6. Organics. Today's rule approves EPA Method 624, ``Purgeables,''
for the determination of acrolein and acrylonitrile in wastewater and
revises footnote 4 to Table IC to specify that the laboratory must
provide documentation about its ability to measure these analytes at
the levels necessary to comply with associated regulations.

B. New Standard Methods and New Versions of Approved Standard Methods

    This rule approves the following Standard Methods (SM) for certain
pollutants currently listed in Table IB at Part 136. Laboratories
performing measurements using any of the approved Standard Methods must
follow the quality control (QC) procedures specified in the 20th or
21st edition of Standard Methods. Below is a list of the Standard
Methods added to Table IB in Part 136:

1. SM 5520 B-2001 and SM 5520 F-2001, Oil and Grease, gravimetric
2. SM 4500-NH3 G-1997, Ammonia (as N) and TKN, automated
phenate method
3. SM 4500-B B-2000, Boron, curcumin method
4. SM 4140 B-1997, Inorganic Ions (Bromide, Chloride, Fluoride,
Orthophosphate, and Sulfate), capillary ion electrophoresis with
indirect UV detection
5. SM 3114 B-2009, Arsenic and Selenium, AA gaseous hydride
6. SM 3114 C-2009, Arsenic and Selenium, AA gaseous hydride
7. SM 3111 E-1999, Aluminum and Beryllium, direct aspiration atomic
absorption spectrometry
8. SM 5220 B-1997, Chemical Oxygen Demand (COD), titrimetric
9. SM 3500-Cr B-2009, Chromium, colorimetric method
10. SM 4500-Norg D-1997, Kjeldahl Nitrogen, semi-automated
block digestor colorimetric
11. SM 3112 B-2009, Mercury, cold vapor, manual
12. SM 4500-P G-1999 and SM 4500-P H-1999, Phosphorus, Total, automated
ascorbic acid reduction
13. SM 4500-P E-1999 and SM 4500-P F-1999, Phosphorus, Total, manual,
and automated ascorbic acid reduction
14. SM 4500-O B, D, E and F-2001, Oxygen, Dissolved, Winkler
15. SM 4500-O D-2001, Oxygen, Dissolved, Winkler

16. SM 4500-O E-2001, Oxygen, Dissolved, alum flocculation modification
17. SM 5530 B-2005, Phenols, manual distillation
18. SM 5530 D-2005, Phenols, colorimetric
19. SM 3500-K C-1997, Potassium, Total, selective electrode method
20. SM 2540 E-1997, Residues--Volatile, gravimetric
21. SM 4500-SiO2 E-1997 and SM 4500-SiO2 F-1997,
Silica, Dissolved, automated molybdosilicate
22. SM 4500-SO42- C-1997, D-1997, E-1997, F-1997
and G-1997, Sulfate, gravimetric, and automated colorimetric
23. SM 4500-S2- B-2000 and C-2000, Sulfide, sample
pretreatment

 C. New ASTM Methods and New Versions of Previously Approved ASTM
Methods

    The rule approves the following ASTM methods for existing
pollutants and ASTM methods for new pollutants to 40 CFR part 136,
Table IB for inorganic compounds, and Table IC for organic compounds.
1. ASTM D2036-09 (B), Cyanide--Total, Cyanide amenable to cholorination
2. ASTM D6888-09, Cyanide--Available, flow injection and ligand
exchange
3. ASTM D7284-08, Cyanide--Total, flow injection
4. ASTM D7511-09, Cyanide--Total, segmented flow injection
5. Free cyanide is added as a new parameter (24A in Table IB); two ASTM
methods (D4282-02 and D7237-10) are approved, in addition to a new
version of OIA 1677(2009) for this parameter. D4282-02 is a Standard
Test Method for Determination of Free Cyanide in Water and Wastewater
by Microdiffusion, and Method D7237-10 is a Standard Test Method for
Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion
Separation and Amperometric Detection.
6. ASTM D888-09 (A), Oxygen Dissolved, Winkler
7. ASTM D7573-09, Organic Carbon--Total, combustion
8. ASTM D7065-06, Five new chemicals in water: Nonylphenol (NP),
Bisphenol A (BPA), p-tert-Octylphenol (OP), Nonylphenol Monoethoxylate
(NP1EO), and Nonylphenol Diethoxylate (NP2EO), Gas Chromatography/Mass
Spectrometry

D. New Alternate Test Procedures at 40 CFR 136.3

The rule approves eight methods submitted to EPA for review through the
alternate test procedures (ATP) program and deemed acceptable based on
the evaluation of documented method performance. The eight methods
approved are added to Table IB:

1. Hach Company's Method 10360 Luminescence Measurement of Dissolved
Oxygen in Water and Wastewater and for Use in the Determination of
BOD5 and cBOD5, Revision 1.2 dated October 2011
2. In-Situ Incorporated's Method 1002-8-2009 Dissolved Oxygen
Measurement by Optical Probe
3. In-Situ Incorporated's Method 1003-8-2009 Biochemical Demand (BOD)
Measurement by Optical Probe
4. In-Situ Incorporated's Method 1004-8-2009 Carbonaceous Biochemical
Oxygen Demand (CBOD) Measurement by Optical Probe
5. Mitchell Method M5271 dated July 31, 2008 for turbidity
6. Mitchell Method M5331 dated July 31, 2008 for turbidity
7. Thermo Scientific's Orion Method AQ4500 dated March 12, 2009 for
turbidity
8. Easy (1-Reagent) Nitrate Method dated November 12, 2011 for nitrate,
nitrite and combined nitrate/nitrite

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

    The rule also clarifies the procedures for measuring orthophosphate
and corrects typographical or other citation errors in Part 136.
Specifically, the rule clarifies the purpose of the immediate
filtration requirement in orthophosphate measurements (Table IB,
parameter 44), which is to assess the dissolved or bio-available form
of orthophosphorus (i.e., that portion which passes through a 0.45-
micron filter)--hence the requirement to filter the sample immediately
upon collection (i.e., within 15 minutes of collection). EPA has added
a footnote (24) to Table II providing this clarification. The rule also
corrects missing citations to the table of microbiological methods for
ambient water monitoring which are specified in Table IH at 40 CFR
136.3. When EPA approved the use of certain microbiological methods on
March 26, 2007 (72 FR 14220), EPA inadvertently omitted fecal coliform,
total coliform, and fecal streptococcus methods from the table. This
omission is corrected in today's rule.

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

    The rule revises some of the current requirements in Table II at
136.3(e).
    1. The rule revises footnote 4 of Table II to clarify the sample
holding time for the Whole Effluent Toxicity (WET) samples for the
three toxicity methods by adding the following sentence: ``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.'' 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).
    2. The rule revises 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.
    3. The rule revises 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,
and to allow the 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.
    4. The rule revises footnote 16 of Table II instructions for
handling Whole Effluent Toxicity (WET) samples by adding two sentences:
``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.''
    5. The rule revises footnote 22 to Table II 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.''
    6. The rule adds three entries at the end of Table II with the
containers, preservation, and holding times for the alkylated phenols,
adsorbable organic halides, and chlorinated phenolics. When EPA
proposed ASTM D7065-06 for the alkylated phenols, commenters noted that
EPA did not include preservation and holding time information in Table
II. When EPA moved EPA Methods 1650 and 1653

from 40 CFR part 430 to Table IC, EPA inadvertently omitted the
associated parameters to Table II, and is correcting this omission in
today's rule. The Table II information for containers, preservation,
and holding times for these three new entries are taken from the
approved methods.

G. Revisions to 40 CFR 136.4 and 136.5

    This rule changes Sec. Sec.  136.4 and 136.5 to clarify the
procedures for obtaining review and approval for the use of alternate
test procedures (alternate methods or ATPs) for those methods for which
EPA has published an ATP protocol (there are published protocols for
chemistry, radiochemical, and microbiological culture methods). In
particular, it establishes separate sections outlining the procedures
for obtaining EPA review and approval for nationwide use of an ATP
(Sec. Sec.  136.4), and the procedures for obtaining approval for
limited use of an ATP (Sec. Sec.  136.5).
    In addition, this rule adds language to Part 136.5 to clarify the
purpose and intent of limited use applications. This provision only
allows use of an alternate method for a specific application at a
facility or type of discharge. The Regional Alternate Test Procedure
(ATP) Coordinator or the permitting authority, at his/her discretion,
may grant approval to all discharges or facilities specified in the
approval letter. However, the appropriate permitting authority within a
state may request supporting test data from each discharger or facility
prior to allowing any such approvals.
    Today's rule further clarifies that the limited use provision
cannot be used to gain nationwide approval and is not a way to avoid
the full examination of comparability that is required for alternate
test procedures when EPA considers a method for nationwide use with the
ultimate goal of listing it as an approved CWA method at 40 CFR part
136. As further clarification, in the event that EPA decides not to
approve a method proposed for nationwide use, the Regional ATP
Coordinator or the permitting authority may choose to reconsider any
previous limited use approvals of the alternate method. Based on this
reconsideration, the Regional ATP Coordinator or the permitting
authority will notify the user(s) if the limited use approval is
withdrawn. Otherwise, the limited use approvals remain in effect.

H. Revisions to Method Modification Provisions at 40 CFR 136.6

    This section allows users to make certain modifications to an
approved method to address matrix interferences without the extensive
review and approval process specified for an alternate test procedure
at 136.4 and 136.5. Today's rule revises 136.6 to provide more examples
of allowed and prohibited method modifications. The intent of today's
revisions is to clarify those situations in which an ATP is required
and those where it is not. Analysts may use the examples to help assess
the need for a formal ATP, and in the event an ATP is not needed to
document that their modification is acceptable and does not depart
substantially from the chemical principles in the method being
modified.
    In response to comments, EPA has included additional examples of
allowed and prohibited method modifications and has made some revisions
to the text language as discussed in Section III below.

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

    EPA is specifying ``essential'' quality control elements at Sec.
136.7 for use in conducting an analysis for CWA compliance monitoring.
This new language is added because auditors, co-regulators, laboratory
personnel, and the regulated community have noted the variations in
quality assurance (QA) and quality control (QC) procedures practiced by
laboratories that use 40 CFR part 136 methods for compliance
monitoring. Some of these methods are published by voluntary consensus
standards bodies, such as the Standard Methods Committee, and ASTM
International. Standard Methods and ASTM are available in printed or
electronic compendia, or as individual online files. As mentioned in
the proposal, each organization has a 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.
    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 particular Part 136 method, or
referenced these procedures by other means. These records must be kept
in-house as part of the method testing documentation. Consequently,
today's rule clarifies that an analyst using these consensus standard
body methods for reporting under the CWA must also comply with the
quality assurance and quality control requirements listed in the
appropriate sections in that consensus standard 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 does 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 lack QA/QC requirements (as specified in this new
section at 40 CFR 136.7), whether developed by EPA, a vendor, or a
consensus standard body, analysts can refer to and follow the QA/QC
published in several public sources. Examples of these sources include
the relevant QA/QC sections of an equivalent approved EPA method, or
voluntary consensus standards published as Part 136 approved methods
(e.g., Standard Methods, ASTM International, and AOAC). In addition to
and regardless of the source of the laboratory's or method's QA and QC
instructions, for methods that lack QA/QC requirements, EPA is adding
requirements at 136.7 to specify twelve essential quality control
elements that must be in the laboratory's documented quality system
unless a written rationale is provided to explain why these quality
control elements are inappropriate for a specific analytical method or
application. 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,
as applicable to the specific method. EPA has clarified the language in
this section in response to public comments. The revised language is
discussed in section III below.

J. Revisions at 40 CFR Part 423 (Steam Electric Power Generating Point
Source Category)

    The rule revises the 40 CFR part 423 definitions for total residual
chlorine and free available chlorine at Sec. Sec.  423.11(a) and
423.11(l) to allow the use of ``chlorine--total residual'' and
``chlorine--free available'' methods in Sec.  136.3(a), Table IB, or
other methods approved by the permitting authority.

III. Changes Between the Proposed Rule and the Final Rule

    Except as noted below, the content of the final rule is the same as
that of the proposed rule.

A. EPA Is Not Adding EPA Method 1614A

    The Agency proposed to add 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.
This method uses isotope dilution and internal standard high resolution
gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The
commenters were divided on whether EPA should approve this method. Two
commenters stated that Method 1614A would be a valuable addition to the
list of approved methods, while two other commenters stated that the
method has not been sufficiently validated for use in Clean Water Act
programs. Upon further evaluation of the data supporting the use of
this test procedure and the peer review comments, EPA agrees with those
commenters who stated that additional validation data are needed to
fully characterize the performance of this method for various matrices
and has decided not to include Method 1614A in today's final rule.

B. Deferral of Action on EPA Method 1668C

    The Agency proposed to add EPA Method 1668C, ``Chlorinated Biphenyl
Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/
HRMS.'' This method measures individual chlorinated biphenyl congeners
in environmental samples by isotope dilution and internal standard high
resolution gas chromatography/high resolution mass spectrometry (HRGC/
HRMS). As discussed in the proposal, Part 136 methods for chlorinated
biphenyls (PCBs) only measure a mixture of congeners in seven
Aroclors--PCB-1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254,
and PCB-1260, while Method 1668C can measure the 209 PCB congeners in
these mixtures.
    EPA began development of this method in 1995, initially covering 13
congeners labeled ``toxic'' by the World Health Organization. In 1999,
EPA expanded the scope of the method to include all 209 PCB congeners.
The method has been used to support several studies, including the 2001
National Sewage Sludge Survey and the National Lake Fish Tissue Survey.
Since 1999, EPA has revised the method to incorporate additional
information and data collected such as the results of an inter-
laboratory validation study, peer reviews of the method and the
validation study data, additional QC performance criteria and MDL data,
and user experiences. In the development and subsequent multi-
laboratory validation of this method, EPA evaluated method performance
characteristics, such as selectivity, calibration, bias, precision,
quantitation and detection limits. The Agency is aware that this method
is being used in some states in their regulatory programs and by other
groups for some projects with good success. For example, 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 an 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 type of data shows that recoveries and precision for
this method are within the performance achievable with other approved
methods.
    EPA received comments from thirty-five individuals or organizations
on this method. Of these commenters, five (three states, one
laboratory, and one laboratory organization) supported the approval of
this method. Some states indicated that they are already requiring this
method for use in permits and for other purposes. On the other hand,
industry and industry groups/associations were critical of the method
for various reasons. Commenters opposing the method provided a detailed
critique of the method, the inter-laboratory study, the peer reviews
and the other supporting documentation. Among the criticisms of the
inter-laboratory study, commenters argued that: (1) EPA did not produce
documentation supporting changes to the method approved by EPA for the
interlaboratory study, (2) the raw data for wastewater and biosolids
was poor and is not fit for use in a comprehensive interlaboratory
study, (3) EPA cited certain guidelines such as ASTM but deviated from
those guidelines (e.g., used only one Youden pair per matrix), (4) the
peer reviewers' qualifications were questioned, (5) the addendum and
the pooled MDLs/MLs were not subjected to peer review, (6) MDL/ML are
flawed, the process to calculate MDLs/MLs for congeners that co-elute
was flawed, the MDL/ML ignored the ubiquitous problem of background
contamination, and (7) the validation study did not include all
matrices in the method (soil and sediment excluded). In addition, some
commenters also suggested that EPA should first promulgate new
detection and quantitation procedures. Further, commenters raised
questions about possible adverse effects of this new method on
compliance monitoring as well as concerns about data reporting and
costs.
    EPA is still evaluating the large number of public comments and
intends to make a determination on the approval of this method at a
later date. In the meantime, the Agency has decided to go forward with
the promulgation of the other proposed analytical methods to expedite
their implementation by the regulated community and laboratories. This
decision does not negate the merits of this method for the
determination of PCB congeners in regulatory programs or for other
purposes when analyses are performed by an experienced laboratory.

C. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09

    In today's rule, EPA is not adding two proposed ASTM methods, ASTM
D7574-09 ``Standard Test Method for Determination of Bisphenol A
(BPA),'' and ASTM D7485-09 ``Standard Test Method for Determination of
NP, OP, NP1EO, and NP2EO.'' These two methods involve liquid
chromatography and tandem mass spectrometry (LC/MS/MS). The methods
have been tested by a single laboratory in several environmental
waters, and may be useful for many applications. However, EPA has
decided to postpone approval of these two methods for general use until
completion of a full inter-laboratory validation study designed to
fully characterize the performance of these methods across multiple
laboratories and matrices.

D. Revisions and Clarifications to EPA Method 200.7

    EPA Method 200.5 ``Determination of Trace Elements in Drinking
Water by Axially Viewed Inductively Coupled Plasma--Atomic Emission
Spectrometry'' employs a plasma torch viewed in the axial orientation
to measure chemical elements (metals). As stated earlier in today's
rule, EPA is adding Method 200.5 for some metals in Table IB. Both
Methods 200.5 and 200.7 are acceptable methods under Part 136 and both
methods employ ICP/AES technology. However, Method 200.5 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
parameters listed in Table IB, the axial orientation using ICP/AES
technology results in greater sensitivity and lower detection limits
than the radial orientation. Thus, today's approval of Method 200.5 and
the additional flexibility to modify Method 200.7 to use the axial
orientation discussed in the proposal will allow laboratories to use
either axial instruments or radial instruments to measure metals in
water samples with Method 200.7. In response to EPA's proposal to allow
the use of the axial orientation of the torch with EPA Method 200.7,
commenters expressed support for this added flexibility. Thus, today's
rule clarifies that the use of the axial orientation of the torch to
measure metals is an acceptable modification to Method 200.7. EPA has
added new text at Part 136.6(b)(5) to allow the use of the axial
orientation of the torch for Method 200.7 as an acceptable method
modification that does not require an ATP application.
    EPA further notes that there was a typographical error in Section
II.J of the proposed rule which stated that the version of EPA Method
200.7 (which the Agency proposed to remove; with Appendix C, see
section IIIM below) has been superseded by Revision 5.4 of Method
200.7. Today's final rule reflects that the correct reference is
Revision 4.4 of EPA Method 200.7. In today's rule, EPA has added Method
200.7 Revision 4.4 as an additional approved method for the measurement
of titanium. As some commenters pointed out, EPA Method 200.7 covers
this parameter and exclusion of this method for the measurement of
titanium in Table IB was an oversight.
    In addition, EPA has removed EPA Method 200.7 from Table IB for the
measurement of mercury. The addition of EPA Method 200.7 to the list of
approved methods for mercury in Table IB was an error. Although this
pollutant is on the list of analytes in EPA Method 200.7, mercury may
be lost to the atmosphere through the use of the approved total
recoverable metals digestion procedures (e.g., EPA Method 200.2, or the
digestion procedures listed in EPA Method 200.7) that must be applied
to the wastewater samples of interest under the Clean Water Act
program. Such losses can lead to poor recovery in the samples compared
to the sample preparation procedures included in other mercury methods
approved at 40 CFR part 136. Therefore, EPA Method 200.7 has not been
included in Table IB for mercury.

E. Revisions and Corrections to Certain Citations in Tables IA, IB, IC,
ID, and IG

    EPA proposed some additions to Table IB which include some new
Standard Methods or new versions of approved Standard Methods. Today's
rule revises the applicability of some methods and makes some
corrections to the method citations. Specifically, EPA removed SM 3120
and SM 3125 for the measurement of mercury because mercury is not on
the list of analytes for these methods. In addition, EPA corrected the
citation of SM 3113 to SM 3113B-2004 in the final rule and has added SM
3113B-2004 for the measurement of cadmium, chromium, iron, lead, and
silver, because these analytes are covered by the method and they
exhibit acceptable analytical performance. These omissions were an
oversight.
    EPA also deleted from Table ID an EPA GC/MS method, Method 525.1,
for the measurement of ametryn, diazinon, disulfoton, prometon, and
trifluoralin. These analytes are not listed within the scope of this
method and their inclusion in the proposal was an error.
    EPA has corrected a number of typographical errors in the tables
and footnotes, correcting spelling and method availability information,
method title names, and document identification numbers. A complete
list of these changes has been included in a memo to the docket.

F. Continued Approval of Method 1664 Rev. A

    EPA proposed to replace Method 1664 Rev. A for the measurement of
oil and grease with a revised version (Method 1664 Rev. B). This new
version of the method describes modifications that are allowed and
modifications that are not allowed when using this method for
compliance with Clean Water Act regulations. Comments were generally
supportive of the revised method but some commenters recommended that
Method 1664 Rev. A not be withdrawn immediately because many permits
currently specify the use of this method. In response to these
comments, EPA will continue to allow the use of Method 1664 Rev. A for
current permits because this method is not significantly different from
the revised version of the method. However, EPA strongly encourages the
use of the revised method (Method 1664 Rev. B) in the future. EPA may
revisit this decision in a future rulemaking.

G. Revision to Footnote 63 of Table IB at 40 CFR 136.3

    EPA received comments that the Hach Method 10360, described in
footnote 63 of Table IB, is a dissolved oxygen procedure, and as such,
should only be listed as a procedure for dissolved oxygen, and not for
BOD and CBOD. EPA disagrees with these commenters because the method on
its face is clearly applicable to dissolved oxygen measurements in
conjunction with BOD and CBOD analyses, as described in the method. As
a result, in today's final rule, EPA added language to the end of this
footnote to clarify that Part 136 allows the use of Hach Method 10360
for measurement of dissolved oxygen in conjunction with the methods
approved for measurement of biochemical demand (BOD) and carbonaceous
biochemical oxygen demand (CBOD).

H. Revision to Footnote 4 of Table IC at 40 CFR 136.3

    EPA received comments on the proposed approval of Method 624 for
the definitive determination of acrolein and acrylonitrile. Commenters
agreed with the addition of these two analytes, but one of these
commenters expressed concern about a blanket approval without requiring
a demonstration of adequate performance and appropriate sample
introduction techniques. This commenter recommended that performance
criteria and information about appropriate sample introduction
techniques be added to footnote 4 of Table IC. EPA agrees with this
commenter's suggestions because this requirement would ensure that the
laboratory has the ability to measure these analytes at the levels
necessary to comply with any associated regulations. In response to
these concerns, in today's rule, the Agency revised the footnote to add
a statement requiring documentation of the ability to quantitatively
measure these analytes and advising analysts that other sample
introduction techniques may be required to achieve adequate
performance.

I. Revisions to Table II Language

    EPA proposed to revise the text at 136.3(e) to allow any party to
modify sample preservation and holding times after submitting
documentation to its permitting or other authority that supports use of
an alternative approach. Commenters expressed concern that this change
would present a burden both to permitting authorities to review and
approve changes, and for laboratories that work in different states
because each state could have different requirements. In response to
public comments, EPA has removed the proposed language at 136.3(e) that
would have allowed such modifications based on documentation and
procedures

determined by individual permitting authorities. Instead, such
modifications must continue to be requested via a limited use ATP
application to the Regional Alternate Test Procedure Coordinator or
permitting authority, as appropriate. Thus, approval of any changes in
sample preservation procedures, container materials, and maximum
allowable holding time will remain unchanged and continue to be the
responsibility of EPA through its Alternate Test Procedure program. EPA
clarified language regarding the limited use application process
procedure. Additionally, in today's rule, EPA added a clarifying
sentence at the end of the current language to emphasize that an
analyst cannot modify any sample preservation or holding time
requirements in an approved method unless the requirements in Section
136.3(e) are met.
    EPA also revised footnote 4 to Table II to delete the parenthetical
statement specifying that samples analyzed for fecal coliforms may be
held up to six hours prior to commencing analysis. That statement in
footnote 4 is inconsistent with the requirement for an eight-hour
holding time, as pointed out by a commenter.
    In response to comments, EPA included a new entry in Table II for
the alkylated phenols (parameters 114 to 118 in Table IC) that was
inadvertently omitted from the proposal. Similarly, when EPA moved EPA
Methods 1650 and 1653 to Table IC, EPA inadvertently omitted to add the
parameters adsorbable organic halides (AOX) and chlorinated phenolics
to Table II. The Table II information for containers, preservation, and
holding times for these three new entries are taken from the approved
methods.

J. Approval of Alternate Test Procedures for Limited Use at 40 CFR
136.5

    EPA proposed changes to 40 CFR 136.4 and 136.5 that establish the
procedures for obtaining approval for use of a nationwide or limited
use ATP. The proposed revisions established separate sections outlining
the procedures for obtaining EPA review and approval for nationwide use
of an ATP (Sec. Sec.  136.4), and the procedures for obtaining approval
for limited use of an ATP (Sec. Sec.  136.5). The proposal also
included language to clarify that limited use approvals do not require
the same level of supporting data that would be required for nationwide
approvals and that limited use approvals are not intended to be used as
a means to avoid the full examination of comparability that is required
for an application for approval of an alternative test procedure for
nationwide use.
    Today's rule finalizes these sections as proposed with one
exception. EPA received comments that the proposed language under Sec.
136.5 does not require that comparability data be submitted when
seeking a Regional limited use ATP approval. EPA agrees that
comparability data is an essential component of the ATP approval
process and had inadvertently omitted this language. As a result, the
Agency added language in today's final rule that requires an applicant
to provide comparability data specific to the limited use for the
performance of the proposed alternative test procedure relative to the
performance of the reference method.

K. Revisions to Language at Sec.  136.6

    EPA proposed to revise the section on method modification
provisions at 40 CFR 136.6 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 in methods currently approved in 40 CFR part 136. Analysts
may use the examples in this section to help assess whether the
modifications require an ATP and if not, to document that their
modification is acceptable. The additional examples provide further
guidance to laboratories and permittees on allowable method
modifications that do not require an application through the ATP
program. Proposal comments generally expressed support for allowing the
flexibility to make certain changes to methods and for the specific
examples of allowable changes included in the proposal. In addition,
some commenters suggested revisions to clarify EPA's intent in Sections
(b)(4) and (b)(5) of 40 CFR 136.6. EPA reviewed the suggestions and
agrees with commenters that the revisions will provide additional
clarity. In addition, as discussed in Section III.D of this preamble,
EPA added the use of axially viewed torch as an allowable modification
to Method 200.7. Today's rule includes the following revisions to the
regulatory text:
    (a) Adds language to Section (b)(3) to clarify that modifications
to sample collection, preservation, and holding time do not fall within
the scope of 136.6,
    (b) Revises the language at (b)(4)(T) be more specific with respect
to the use of gas diffusion across a hydrophobic semi-permeable
membrane to separate the analyte of interest from the sample matrix in
place of manual or automated distillation for the analysis of certain
analytes,
    (c) Revises the equation for Relative Standard Error (RSE) in
(b)(4)(J) to make it consistent with the description in other EPA
methods, and
    (d) Adds the use of an axially viewed torch with Method 200.7 as an
allowable modification.

L. Revisions to New Quality Assurance and Quality Control Language

    For today's rule, EPA added some introductory language to this
section to clarify the new requirements. EPA added this language to
provide some additional clarity as to when the new requirements are
applicable and, thus, must be incorporated into the laboratory's
documented standard operating procedures. Additional discussion of the
revisions is provided under section IV.C below.

M. Withdrawal of Appendices at 40 CFR Part 136

    EPA proposed to incorporate by reference in Table IB all of the
methods printed in 40 CFR part 136 Appendices A and C, and to remove
most of the information in Appendix D. The methods in Appendix A are
EPA Method Numbers 601 through 613, 624, 625, 1613B, 1624B, and 1625B.
Appendix C contains EPA Method 200.7, ``Determination of Metals and
Trace Elements in Water and Wastes by Inductively Coupled Plasma--
Atomic Emission Spectrometry''. However, Federal regulations at 1 CFR
part 51.7(c)(1) prohibit the incorporation by reference of material
previously published in the Federal Register. Thus, EPA is not
withdrawing Appendices A or C. Because EPA Method 200.7 has been
revised, EPA is replacing the current version of this method in
Appendix C with Rev. 4.4 of Method 200.7. All of these methods are
readily accessible from a variety of sources, including EPA's CWA
methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm.
    The rule also removes most of the data from Appendix D for all EPA
methods that are no longer approved, and retains only the Precision and
Recovery Statements for EPA Method 279.2 for thallium and EPA Method
289.2 for zinc, and corrects

typographical errors in the Appendix. The current version of Appendix D
will be available online at the CWA methods Web site for historical
purposes.

N. Revisions at 40 CFR Part 430 (Pulp, Paper, and Paperboard Point
Source Category)

    EPA also proposed to remove Appendix A at 40 CFR part 430 and to
incorporate by reference the methods in this Appendix. Appendix A
contains two methods, EPA Method 1650 for adsorbable organic halides or
AOX, and EPA Method 1653 for chlorinated phenolics. As explained above,
we cannot incorporate by reference this material, so Appendix A remains
unchanged in the Code of Federal Regulations. These methods are also
readily available from a variety of sources, including EPA's CWA
methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm.
EPA is also adding these two methods to Table IC for general use.

O. Revisions at 40 CFR Part 435 (Oil and Gas Extraction Point Source
Category)

    The rule makes several changes to Part 435, Oil and Gas Extraction
Point Source Category. First, EPA is moving the methods and associated
quality assurance requirements 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-11-004), and
incorporating by reference this document in the revised regulation at
40 CFR part 435. This 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 moved from part 435 to the cited document, EPA-821-R-11-004.

 EPA Method Numbers for Oil and Gas Extraction Point Source Category Analytical Methods and Prior CFR References
----------------------------------------------------------------------------------------------------------------
                                                                  Date first
            Analytical/Test method              EPA Method No.    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 Degradation             1647            2001  Subpart A, Appendix 4.
 of Non-Aqueous Base Fluids in a Marine Closed
 Bottle Biodegradation Test System: Modified
 ISO 11734:1995.
Determination of Crude Oil Contamination in               1655            2001  Subpart A, Appendix 5.
 Non-Aqueous Drilling Fluids by Gas
 Chromatography/Mass Spectrometry (GC/MS).
Reverse Phase Extraction (RPE) Method for                 1670            2001  Subpart A, Appendix 6.
 Detection of Oil Contamination in Non-Aqueous
 Drilling Fluids (NAF).
Determination of the Amount of Non-Aqueous                1674            2001  Subpart A, Appendix 7.
 Drilling Fluid (NAF) Base Fluid from Drill
 Cuttings by a Retort Chamber (Derived from
 API Recommended Practice 13B-2).
----------------------------------------------------------------------------------------------------------------

    As noticed in the proposed rule, EPA is also incorporating
additional quality assurance procedures in the marine anaerobic
biodegradation method (Appendix 4 of Subpart A of part 435) and is
correcting some erroneous references and omissions in the method for
identification of crude oil contamination (Appendix 5 of Subpart A of
part 435) into the new document (EPA-821-R-11-004).
    EPA promulgated the use of the marine anaerobic biodegradation
method (closed bottle test, ISO 11734:1995 as clarified by Appendix 4
to Subpart A of part 435) as an Appendix to the rule 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 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. EPA worked
with the same industry consortium that assisted EPA in the development
of the analytical methods used in the effluent guidelines for the Oil
and Gas Extraction point source category (40 CFR part 435) to develop
these additional quality assurance measures. Thus, the quality
assurance procedures are generally applicable to this industry.
    Additionally, as noticed in the proposed rule, EPA is correcting
some erroneous references and omissions in the method for
identification of crude oil contamination (Appendix 5 of Subpart A of
Part 435), as follows:
    a. Adding a schematic flow for qualitative identification of crude
oil, which was erroneously omitted in Appendix 5 to Subpart A of part
435,
    b. Correcting erroneous citations in sections 9.5, 9.6, 11.3, and
11.3.1 of Appendix 5, and
    c. Adding a missing ``<'' (less than) sign for identification of
crude oil contamination in the asphaltene crude discussion at Section
<IP_ADDRESS>. The asphaltene discussion now reads as follows: ``Asphaltene
crude oils with API gravity < 20 may not produce chromatographic peaks
strong enough to show contamination at levels of the calibration.
Extracted ion peaks should be easier to see than increased intensities
for the C8 to C13 peaks. If a sample of asphaltene crude from the
formation is available, a calibration standard shall be prepared.''
    EPA received three comments on the proposed changes. One commenter
was concerned that the EPA document (EPA-821-R-11-004) would not have
the same legal status as publishing the methods in the CFR. EPA
disagrees with this comment. The incorporation by reference of this
document has the same legal standing as publishing the text of the
methods in the CFR. EPA has a long standing practice of publishing test
methods using incorporation by reference and the cited test methods are

as legally enforceable as those published in full in the CFR. EPA is
consolidating these methods into one document to allow for easier
access to these methods. The incorporation by reference of this
document also allows for better formatting of the methods and
eliminates the redundant publication of these methods each year in the
Code of Federal Regulations. Two other commenters had some
recommendations for additional revisions to the EPA document (EPA-821-
R-09-013). EPA has not adopted these suggestions, given the absence of
an opportunity for the public generally to comment on them. EPA will,
however, consider these comments and may propose additional revisions
in a future rulemaking. As noticed in the proposed rulemaking, the
final rule consolidates the oil and gas test methods into a single
document and references this document in the effluent guidelines (40
CFR part 435). Like any other changes to an EPA-approved method, any
changes to the methods in the EPA document (EPA-821-R-11-004) will
require a rulemaking.

IV. Summary of EPA's Response to Comments

    The Agency received comments from 117 different individuals or
organizations on the September 23, 2010 proposal (75 FR 58024).
Commenters represented a variety of different interests, including
analytical laboratories, water utilities, instrument manufacturers,
State and local governments, trade associations, and industry. A
summary of major public comments on the proposed rule and the Agency's
responses is presented in this section. The public docket for this rule
includes all of the comments received and the Agency's responses.

A. Approval of Standard Methods

    EPA proposed to revise how to identify EPA-approved Part 136
methods that are published by the Standard Methods Committee (i.e.,
Standard Methods). EPA proposed two changes. First, EPA proposed to
change the way it identifies an EPA-approved version of a Standard
Method in Part 136. Second, EPA proposed to identify only the most
recently EPA-approved version of a Standard Method in Part 136. In the
past, EPA listed multiple versions of these methods from the 18th,
19th, 20th editions of the printed compendiums, or from the on-line
editions published by the Standard Methods Committee, in one or more
columns in the Part 136.3 tables. In some cases, EPA approved more than
one version of a Standard Method for a particular analyte in Part 136.
Approval of several versions of the same Standard Method for an analyte
has led to inconsistencies in how laboratories conduct these analyses,
especially in quality assurance/quality control (QA/QC) practices. For
this reason, EPA proposed to list only the most recently EPA-approved
version of a Standard Method (regardless of the printed or on-line
edition) in Part 136, with few exceptions, to identify the method with
the year of Standard Methods approval or adoption designated by the
last four digits in the method number (e.g., Standard Method 3113B-
2004). This approach clearly identifies the version of the standard
method approved under Part 136 and no longer ties it to a particular
compendium printing or edition of Standard Methods. For example, the
exact method, Standard Method 3113B-2004 appears in the 18th, 19th, and
20th edition of Standard Methods. Because this method is the same in
all of these editions, a laboratory may refer to any of these editions
when using Standard Method 3113B-2004 to measure the analytes listed in
Table IB that are approved for this method. Thus, EPA's proposed
approach to identify Part 136 approved standard methods does not rely
on the particular edition of a compendium but rather on the latest
Standard Methods approved version (by indicating the year of approval).
    EPA received numerous comments concerning the proposed changes to
specify the method with the year of publication, rather than specifying
the editions of Standard Methods in which the method is printed, and to
list in Part 136 only the most recent EPA-approved version of a
Standard Method if Standard Methods has multiple versions of a method
for a pollutant. Some commenters expressed concern about other economic
impacts related to laboratory start-up tests, and the need for training
and revised standard operating procedures (SOPs) associated with the
use of the most recently approved method. In response, EPA maintains
that the economic impacts of start-up tests or the need for revised
SOPs are part of the necessary expenses to maintain a laboratory
producing data of known and acceptable quality and these costs are not
unusual. Training new staff or training current staff on new procedures
is also a cost that any laboratory must consider as part of doing
business.
    EPA is aware that Standard Methods and other voluntary consensus
organizations such as ASTM and AOAC periodically revise existing
methods and publish them on-line and/or as a compendium. In addition to
EPA-developed methods, the Agency approves certain methods developed by
these and other organizations as required under the National Technology
Transfer and Advancement Act (NTTAA) and lists them in Part 136
periodically. Often, after EPA approves a Standard Method for use in
Part 136, Standard Methods releases or adopts a revised version of that
method. Generally, these revised Standard Methods involve the use of
new technologies or improvements to previously approved methods. By
referencing the year of adoption by Standard Methods, EPA's proposed
change in its method citations was intended to clarify which version of
a Standard Method is approved by EPA in Part 136. The on-line site for
Standard Methods allows electronic release of new methods and revisions
to existing methods prior to the publication of the compendium edition.
Currently, Standard Methods is on a 5-7 year cycle for publication of
the compendium and is set to release its 22nd edition soon. In some
cases, an older version of a method approved by the Standard Methods
Committee may appear on the on-line or compendium version of Standard
Methods. The date of adoption is on the first page of the compendium or
on-line method.
    Commenters are correct in pointing out that, in the event that they
elect to use an EPA-approved Standard Method for compliance purposes,
they would be required to use the most recently EPA-approved version of
a Standard Method. EPA is not requiring any EPA-approved Standard
Method in today's rule. Dischargers may use any approved Part 136
method for compliance monitoring unless the method is specified in its
discharge permit by the permitting authority, or the method is not
sufficiently sensitive to comply with the permit limit. Also, if the
discharger elects to use an EPA-approved Standard Method and does not
have the most recent EPA-approved version, EPA finds the costs would
not be significant. The discharger/laboratory would need to purchase
the on-line version for the individual method and would not need to
absorb the cost of a full subscription to the on-line service. On-line
versions of a single method generally cost $69. Relative to the costs
that laboratories charge to run such an analysis (generally many times
over), this cost is negligible. Therefore, EPA does not agree with
commenters that they will have to purchase an on-line subscription to
Standard Methods nor does it conclude that this change will

present a significant financial burden to laboratories.
    Another concern raised was that any changes in Standard Methods in
the future would be automatically approved without EPA review. This
assertion is incorrect. Any new or revised Standard Methods would be
proposed in the Federal Register for public comment before inclusion in
Part 136 as required under the Clean Water Act.
    Some commenters also expressed concern that this change may affect
the approval status of existing alternate test procedures that were
evaluated by EPA relative to older Standard Methods. With respect to
this concern, the Agency is not withdrawing any approved ATPs. EPA's
withdrawal of its earlier approved versions of Standard Methods is not
intended to affect the acceptance of any vendor-developed methods based
on older Standard Methods that EPA previously determined to be
acceptable versions, because the changes in Standard Methods are mostly
editorial (e.g., clarifications, increased flexibility) and not
procedural changes.
    In making this change in today's rule, EPA also considered that
beginning with the publication of the 20th edition of Standard Methods,
the Standard Methods Committee included the quality control (QC)
procedures which are similar to the QC procedures that have been
included by EPA in methods published in Part 136 over the last two
decades for use in compliance monitoring programs under the Clean Water
Act and the Safe Drinking Water Act. These procedures are specified in
Part 1000 of the Standard Methods compendium and include the
``essential'' quality control checks that EPA has added at 40 CFR 136.7
as part of this final rule.

B. Preservation and Holding Time Requirements for EPA Method 624

    In response to the proposed use of EPA Method 624 as a definitive
measurement method for acrolein and acrylonitrile, EPA received
comments on the preservation and holding time requirements for these
two pollutants. Commenters noted that the preservation and holding time
requirements in Part 136 Table II for these two analytes currently
differ from the requirements for other Method 624 analytes.
Historically, these two analytes have had different preservation and
requirements than the analytes currently listed in EPA Method 624. The
current requirements in Table II date to 1984 and specify that samples
for acrolein and acrylonitrile must be preserved at a pH in the range
of 4 to 5. This pH range is based on concerns about degradation of
these two analytes in strongly acidic samples (e.g., pH < 2). Footnote
10 to Table II currently states that pH adjustment is not required if
acrolein will not be measured, but that samples for acrolein receiving
no pH adjustment at all must be analyzed within 3 days of sampling. In
contrast, samples to be analyzed by EPA Method 624 for purgeable
halocarbons are not preserved by adjusting the pH, and samples to be
analyzed for the purgeable aromatic hydrocarbons (benzene, ethylbenzene
and toluene) are preserved at a pH of 2. Thus, in the case where a
permittee wants to use EPA Method 624 to measure acrolein or
acrylonitrile in addition to other analytes included in Method 624, the
sampler has to take an additional sample, preserve the sample for
acrolein and acrylonitrile to pH 4 to 5, and then perform separate
analyses. Commenters stated that EPA does not have a basis for
requiring a different preservation and holding times for these two
analytes and submitted data that support their assertion that sample
preservation be allowed at either a pH of 7 or a pH of 2. EPA has
reviewed the data, but the Agency has concluded that these data are not
sufficient or compelling to change the current preservation and holding
time requirements for these analytes because the data are anecdotal
rather than the result of a well-planned and properly documented
stability study. As a result, EPA's final rule retains the current
sample preservation and holding time requirements for acrolein and
acrylonitrile.

C. Quality Assurance and Quality Control Requirements

    EPA proposed to specify minimal essential quality control
requirements at Part 136.7 for use in conducting analyses to comply
with CWA monitoring requirements. The purpose of this requirement is to
ensure that laboratories conducting CWA compliance monitoring use
suitable QA/QC procedures. These QA/QC procedures were included in a
memorandum to EPA's Regional Quality Assurance Managers (May 7, 2009
memorandum from Richard Reding) and have been posted on EPA's Web page
since 2009. These requirements do not apply in the case of the use of
Part 136 approved methods that contain (or reference) their own QA/QC
procedures, or to any non-compliance analyses. Most analytical methods
currently listed in Part 136 contain QA/QC procedures, and permittees/
laboratories using those methods are not affected by the new
requirement. However, there are a few older methods approved for use in
Part 136 from the 1970s that contain no QA/QC requirements. Examples of
Part 136 methods that lack QA/QC are Method 283.2 for titanium and
Method 289.2 for zinc, both furnace atomic absorption methods issued in
1978. As explained previously, an additional issue identified in the
May 7, 2009 memorandum is that approved methods from consensus
organizations such as Standard Methods contain the QA/QC requirements
in a different section of their methods compendium (e.g., Standard
Methods consolidates general QA/QC requirements for all methods in Part
1000 of their methods compendium). Thus, EPA wants to clarify that it
expects permittees/laboratories using Part 136 approved methods
developed by consensus organizations for reporting compliance under the
CWA to also comply with the QA/QC requirements listed in the
appropriate sections in that consensus organization's compendium.
    In addition to following QA/QC requirements from consensus
organizations for Part 136 methods without QA/QC procedures, the
analyst has the option to follow the QA/QC published in another EPA-
approved method for that parameter that contains such QA/QC.
    As discussed in Section II.I of this preamble, EPA is reiterating
the requirement to include QA/QC in any chemical method used for CWA
compliance purposes. For those few Part 136 methods that lack QA/QC
requirements, EPA is adding quality control requirements at Sec.
136.7. EPA received numerous comments on this aspect of the proposed
rule. Although some commenters expressed support for EPA's intent to
ensure the quality of data by adding the new QC language, many
commenters noted problems with the specific language, including that
many of the QC elements do not apply to common parameters (e.g., MDLs
cannot be calculated for pH or BOD, and surrogates and internal
standards have no counterparts in microbiological methods). Other
commenters expressed concern that the new language was either
duplicative or contradicted language in existing EPA-approved methods,
or presented conflicts with various state or national accreditation
programs. Other commenters objected to the perceived costs associated
with this new requirement and suggested that the QC checks simply will
not occur, regardless of the new Part 136.7 requirement. A few
commenters suggested improvements to the proposed language, should EPA
decide to proceed with this new section. One commenter stated that the
section was

not needed, since EPA should not be approving methods at 40 CFR part
136 that do not already contain appropriate QA/QC. EPA addresses these
issues below.
    With respect to the issue of applicability of the QC elements, EPA
agrees with commenters who stated that some QC elements listed in Sec.
136.7 may not apply to common parameters (e.g., matrix spike and matrix
spike duplicates do not apply to pH measurements). For any of the Part
136 methods that include (or reference) appropriate QC elements for
these parameters, these new QA/QC requirements are not applicable. As a
result, in today's final rule, EPA has added introductory language in
Sec.  136.7 to clarify how laboratories should comply with this new
requirement when one or more of the twelve essential quality control
elements is not applicable to a method. This new introductory language
states that in cases where one or more of the twelve QC elements do not
apply to a given method, the laboratory may provide a written rationale
for not including those elements in their standard operating procedures
(SOP) for that analysis. This may be something as simple as stating
that the given QC element does not apply to that analysis or is not
possible to perform (as the example above for pH measurements). In
addition, the final rule states that the twelve QC elements, as
applicable, must be included in a laboratory's SOP for conducting an
analysis with an approved method only when there are no QA/QC
procedures in the Part 136 method. Again, as discussed above, this QA/
QC requirement at Part 136 does not apply to approved methods
containing (or referencing) QA/QC procedures.
    In response to the comment that the language is either duplicative
or contradicted in existing approved methods or accreditation programs,
EPA has added this new section to the regulations at Part 136.7 to
address concerns that certain approved methods do not contain QA/QC
procedures. In those cases where an approved method incorporates these
QC procedures (as applicable to that method), the laboratory can follow
the method as written without creating any duplication or conflict. As
mentioned in Section IV.A of this preamble, Standard Methods
incorporated new QC requirements starting with the 20th edition of
Standard Methods similar to the QC requirements included in EPA methods
for the last two decades. Thus, most Standard Methods that are also
approved methods in Part 136 already contain QA/QC requirements, as
applicable. Similarly, EPA does not anticipate conflicts with
laboratory accreditation programs because these programs generally
follow the QC requirements in the method or as otherwise specified in
regulatory programs. The purpose of this new section is to ensure that
analyses conducted for compliance monitoring with CWA regulatory
programs contain appropriate QA/QC and the Agency's view is that this
is already occurring in most laboratories (with a few exceptions as
discussed above). This new requirement is added to clarify that
laboratories must implement proper QA/QC, as needed, for all CWA
compliance related analyses to provide quality data that will withstand
regulatory and legal challenges.
    In response to the comment that this new requirement will be
costly, proper QA/QC is essential for obtaining results of known and
acceptable quality. In the long run, it could be much more costly to
use data which lacks proper QC in demonstrating or enforcing discharge
requirements. In the short run, laboratories would only incur costs
associated with this new requirement when the method lacks QA/QC and
when they have not included QA/QC as part of their SOPs. EPA estimates
that this would not have a significant impact on laboratories because
the vast majority of Part 136 methods already include or reference QA/
QC requirements. Further, most laboratories already implement the QC
checks prescribed by the newer methods and are already documenting
these QC checks in the laboratory SOPs. Some of the QC checks are a
one-time or infrequent expense (e.g., demonstration of capability and
determination of a method detection limit), while other checks are
routine (e.g., running a method blank). Typically, laboratories include
QC as part of the overall analysis costs, and these costs generally add
10-20% to the analysis cost initially for an analyst demonstration of
capability, and less (5-10%) after the initial cost for routine QC
(e.g., running a blank with every batch of samples). For a typical
analysis of a metal using furnace atomic absorption, at a cost of $35-
50 per sample, the QC costs would be typically 5-10% of the total
costs, and are generally included in the laboratory pricing schedule.
Thus, EPA expects that any costs associated with this aspect of today's
rule will be minimal and limited to a few older methods that some
laboratories may still elect to use rather than the many other methods
that contain QA/QC requirements. EPA considers these QC checks to be an
essential part of an overall approach to producing data of known
quality and defensibility when a particular method is used to measure
pollutants for compliance monitoring purposes. Ignoring these QC
checks, as a commenter suggested, is inconsistent with EPA's NPDES
permit requirements. Thus, 40 CFR 122.41(e) of EPA's NPDES permitting
regulations provides that the permittee ``shall at all times properly
operate and maintain all facilities and systems of treatment and
control * * * Proper operation and maintenance also includes adequate
laboratory controls and appropriate quality assurance procedures * *
*.'' In most cases, these procedures are already a part of the quality
control practices of most laboratories and will not create an
additional burden. However, in codifying QC requirements, EPA provides
clarification that these procedures are mandatory, as applicable, and
not merely optional.

V. Statutory and Executive Order Reviews

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

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 revised 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 final rule on
small entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. This action
approves new and revised 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. Although EPA expects
that in some cases the analytical costs could increase slightly due to
additional QC requirements for a few old EPA-approved methods that lack
QA/QC, EPA has determined that most laboratories that analyze samples
for EPA compliance monitoring have already instituted QC requirements
as part of their laboratory practices and this rule will not have a
significant economic impact on a substantial number of small entities.

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 final 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 revised versions of
testing procedures, and new sample collection, preservation, and
holding time requirements.
    Thus, today's rule is not subject to the requirements of Section
203 of UMRA.

E. Executive Order 13132: Federalism

    This final 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 rule merely approves new and revised versions of testing
procedures, and new sample collection, preservation, and holding time
requirements. The costs to State and local governments will be minimal.
In fact, governments may see a cost savings because the rule adds
flexibility for laboratories and permittees to choose between
additional approved test methods and it also provides additional
flexibility to modify existing test methods. Thus, laboratories and
permittees will not make as many requests for approval of alternative
test methods or method modifications, 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 solicited comment on the proposed rule
from State and local officials.

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

    This final 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 revised
versions of testing procedures, and new sample collection,
preservation, and holding time requirements. The costs to tribal
governments will be minimal. In fact, tribal governments may see a cost
savings because the rule adds flexibility for laboratories and
permittees to choose between additional approved test methods and it
also provides additional flexibility to modify existing test methods.
Thus, laboratories and permittees will not make as many requests for
approval of alternative test methods or method modifications. 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 solicited comment on the proposed rule from tribal
officials. EPA did not receive any comments from Indian tribes.

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 rule approves new and revised
versions of testing procedures, and new sample collection,
preservation, and holding time requirements.

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 final rule approves the use of technical standards developed
by the Standard Methods Committee, and ASTM International for use in
compliance monitoring where the Agency has determined that those
standards meet the needs of Clean Water Act programs. EPA is not adding
two of the proposed ASTM methods to this final rule because these
methods have not undergone full inter-laboratory validation as
recommended in current Agency guidance (see Section III.C of this
preamble). All other proposed voluntary consensus standards are
approved in today's rule.

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 final 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 approves new and revised
versions of testing procedures to measure pollutants in water.

K. Congressional Review Act

    The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the
Small Business Regulatory Enforcement Fairness Act of 1996, generally
provides that before a rule may take effect, the agency promulgating
the rule must submit a rule report, which includes a copy of the rule,
to each House of the Congress and to the Comptroller General of the
United States. EPA will submit a report containing this rule and other
required information to the U.S. Senate, the U.S. House of
Representatives, and the Comptroller General of the United States prior
to publication of the rule in the Federal Register. This action is not
a ``major rule'' as defined by 5 U.S.C. 804(2). This rule will be
effective June 18, 2012.

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: April 17, 2012.
Lisa P. Jackson,
Administrator.
    For the reasons set out in the preamble, title 40, chapter I of the
Code of Federal Regulations, is amended as follows:

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

0
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.)

0
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.
* * * * *

0
3. Section 136.3 is amended:
0
a. By revising paragraph (a) introductory text and Tables IA, IB, IC,
ID, IG, and IH;
0
b. By revising paragraph (b);
0
c. By revising paragraph (e) introductory text;
0
d. By revising Table II to paragraph (e).
    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. The methods listed in Tables
IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see
paragraph (b) of this section, with the exception of EPA Methods 200.7,
601-613, 624, 625, 1613, 1624, and 1625. The full texts of Methods 601-
613, 624, 625, 1613, 1624, and 1625 are printed in appendix A of this
part 136, and the full text of Method 200.7 is printed in appendix C of
this part 136. The full text for determining the method detection limit
when using the test procedures is given in appendix B of this part 136.
The full text of Method 200.7 is printed in appendix C of this part
136. 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 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. Sec.  136.4 and 136.5. Under certain
circumstances paragraph (c) of this section, Sec.  136.5(a) through (d)
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 11,15...........
     dry weight.                     dilution, or          1681 11,20...........
                                    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.                                      ....................
                                     \5\.
    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\.
5. E. coli, number per 100 mL \21\  MPN \6,8,16\ multiple  .....................  9221B.1-2006/9221F-                               ....................
                                     tube, or.                                     2006 12,14.
                                    multiple tube/         .....................  9223 B-200 4\13\.....  991.15 \10\..............  Colilert[supreg]13,1
                                     multiple well, or                                                                               8
                                                                                Colilert-
                                                                                18[supreg]13,17,18
                                    MF 2,6,7,8 single      1603 \22\............  .....................  .........................  mColiBlue-
                                     step.                                                                                24[supreg]19
    6. Fecal streptococci, number   MPN, 5 tube 3          p. 139 \3\...........  9230 B-2007.                                      ....................
     per 100 mL.                     dilution, or
                                    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]13
     mL \22\.                        tube/multiple well,                                                                             ,24
                                     or
                                    MF 2,6,7,8 single      1600 \25\............  9230 C-2007                                       ....................
                                     step or.
                                    Plate count..........  p. 143 \3\.                                                              ....................
    8. Salmonella, number per gram  MPN multiple tube      1682 \23\.                                                               ....................
     dry weight \11\.
Aquatic Toxicity:
    9. Toxicity, acute, fresh       Ceriodaphnia dubia     2002.0.\26\                                                              ....................
     water organisms, LC50,          acute.
     percent effluent.
                                    Daphnia puplex and     2021.0.\26\                                                              ....................
                                     Daphnia magna acute.
                                    Fathead Minnow,        2000.0.\26\                                                              ....................
                                     Pimephales promelas,
                                     and Bannerfin
                                     shiner, Cyprinella
                                     leedsi, acute.
                                    Rainbow Trout,         2019.0.\26\                                                              ....................
                                     Oncorhynchus mykiss,
                                     and brook trout,
                                     Salvelinus
                                     fontinalis, acute.
    10. Toxicity, acute, estuarine  Mysid, Mysidopsis      2007.0.\26\                                                              ....................
     and marine organisms of the     bahia, acute.
     Atlantic Ocean and Gulf of
     Mexico, LC50, percent
     effluent.

                                    Sheepshead Minnow,     2004.0 \26\                                                              ....................
                                     Cyprinodon
                                     variegatus, acute.
                                    Silverside, Menidia    2006.0 \26\                                                              ....................
                                     beryllina, Menidia
                                     menidia, and Menidia
                                     peninsulae, acute.
    11. Toxicity, chronic, fresh    Fathead minnow,        1000.0.\27\
     water organisms, NOEC or        Pimephales promelas,
     IC25, percent effluent.         larval survival and
                                     growth.
                                    Fathead minnow,        1001.0.\27\
                                     Pimephales promelas,
                                     embryo-larval
                                     survival and
                                     teratogenicity.
                                    Daphnia, Ceriodaphnia  1002.0.\27\
                                     dubia, survival and
                                     reproduction.
                                    Green alga,            1003.0.\27\
                                     Selenastrum
                                     capricornutum,
                                     growth.
    12. Toxicity, chronic,          Sheepshead minnow,     1004.0.\28\
     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.\28\
                                     Cyprinodon
                                     variegatus, embryo-
                                     larval survival and
                                     teratogenicity.
                                    Inland silverside,     1006.0.\28\
                                     Menidia beryllina,
                                     larval survival and
                                     growth.
                                    Mysid, Mysidopsis      1007.0.\28\
                                     bahia, survival,
                                     growth, and
                                     fecundity.
                                    Sea urchin, Arbacia    1008.0.\28\
                                     punctulata,
                                     fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:
\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\ Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. US EPA.
\4\ 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. 1989. USGS.
\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\ Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
\11\ Recommended for enumeration of target organism in sewage sludge.
\12\ The multiple-tube fermentation test is used in 9221B.1-2006. 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.

\13\ 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.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.1-2006, 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-2006. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [mu]g/mL of MUG may be used.
\15\ Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-
  10-003. April 2010. U.S. EPA.
\16\ 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.
\17\ 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.
\18\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories, Inc.
\19\ A description of the mColiBlue24[supreg] test, is available from Hach Company.
\20\ Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
\21\ Recommended for enumeration of target organism in wastewater effluent.
\22\ Method 1603: Escherichia coli (E. coli ) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (modified
  mTEC), EPA-821-R-09-007. December 2009. U.S. EPA.
\23\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-06-014. July 2006. U.S.
  EPA.
\24\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\25\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-09-016.
  December 2009. U.S. EPA.
\26\ Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA-821-R-02-012. Fifth Edition,
  October 2002. U.S. EPA.
\27\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. EPA-821-R-02-013. Fourth Edition,
  October 2002. U.S. EPA.
\28\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. EPA-821-R-02-014. Third
  Edition, October 2002. U.S. EPA.

                                                  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 aspiration    ......................  3111 D-1999 or 3111 E- .....................  I-3051-85.\2\
                                      \36\                                            1999.
                                        AA furnace.........  ......................  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-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        .....................  I-4523-85.\2\
                                         salicylate, or       (1993).                4500-NH3 H-1997......
                                         other substituted
                                         phenols in
                                         Berthelot reaction
                                         based methods.

                                        Automated electrode  Ion Chromatography....  .....................  D6919-09.............  See footnote.\7\
5. Antimony--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration \36\.
                                        AA furnace.........  ......................  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                97.\50\
6. Arsenic-Total,\4\ mg/L..........  Digestion,\4\ followed  206.5 (Issued 1978)
                                      by any of the           \1\.
                                      following:
                                        AA gaseous hydride.  ......................  3114 B-2009 or.......  D2972-08 (B).........  I-3062-85.\2\
                                                                                3114 C-2009..........
                                        AA furnace.........  ......................  3113 B-2004..........  D2972-08 (C).........  I-4063-98.\49\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                05.\70\
                                        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 B-2004..........  D4382-02(07).........
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  .....................  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-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.......  D3645-08 (A).........  I-3095-85.\2\
                                         aspiration.                                 3111 E-1999..........
                                        AA furnace.........  ......................  3113 B-2004..........  D3645-08 (B).........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES............  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-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..........  .....................  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 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-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 300.1-1, Rev 1.0    D-2000.
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-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..........  D3557-02(07) (A or B)  974.27,\3\ p. 37.\9\,