Federal Register: March 12, 2007, Part 3. 40 CFR Part 122, 136, et al. Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; National Primary Drinking Water Regulations; and National Secondary Drinking Water Regulations; Analysis and Sampling procedures; Final Rule.


            81 5ZO7-OO1
Monday,

March 12, 2007
Part
Environmental

Protection  Agency

40 CFR Part 122, 136, et al.
Guidelines Establishing Test Procedures
for the Analysis of Pollutants Under the
Clean Water Act; National Primary
Drinking Water Regulations; and National
Secondary Drinking Water Regulations;
Analysis and Sampling Procedures; Final
Rule

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Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
ENVIRONMENTAL PROTECTION
AGENCY

40 CFR Parts 122,136,141,143, 430,
455, and 465
[EPA-HQ-OW-2003-0070; FRL-8203-8]
BIN 2040-AD71

Guidelines Establishing Test
Procedures for the Analysis of
Pollutants Under the Clean Water Act;
NationaJ Primary Drinking Water
Regulations; and National Secondary
Drinking Water Regulations; Analysis
and Sampling Procedures
AGENCY: Environmental Protection
Agency (EPA).
ACTION: Final rule.

SUMMARY: This rule modifies the testing
procedures approved for analysis and
sampling under the Clean Water Act
and Safe Drinking Water Act. EPA
proposed these changes for public
comment on August 18, 2003 and April
6, 2004. The Clean Water Act changes
adopted in this final rule fall into the
following categories: new vendor-
developed methods as well as EPA and
voluntary consensus standard bodies
(VCSB) methods, updated versions of
currently approved methods, revisions
to method modification and analytical
requirements, withdrawal of certain
outdated methods, and changes to
sample collection, preservation, and
holding time requirements. This rule
also changes regulations under the Safe
Drinking Water Act that establish
drinking water sampling and analysis
procedures. The changes include
approval of vendor-developed methods,
new EPA and VCSB methods, updated
VCSB methods, and approval of a
modification to the test kit used with
Syngenta Method AG—625 that restricts
its use in certain circumstances. The
addition of new and updated methods
to the wastewater and drinking water
regulations provides increased
flexibility to the regulated community
and laboratories in the selection of
analytical methods.
ADDRESSES: EPA has established a
docket for this action under Docket ID
No. EPA-OW-2003-0070. All
documents in the docket are listed on
the http://www.regulations.gov web site.
Although listed in the index, some
information is not publicly available,
e.g., CBI or other information whose
disclosure is restricted by statute.
Certain other material, such as
copyrighted material, is 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.regalations.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 (202) 566-1744,
and the telephone number is (202) 566-
2426 for the HQ Water Docket Center.
DATES: This regulation is effective April
11, 2007. The incorporation by reference
of these methods is approved by the
Director of the Federal Register on April
11, 2007. For judicial review purposes,
this final rule is promulgated as of 1:00
p.m. (Eastern time) on March 26, 2007
as provided at 40 CFR 23.2 and 23.7.
FOR FURTHER INFORMATION CONTACT: For
information regarding the changes to
wastewater regulations, contact Meghan
Hessenauer, Engineering and Analysis
Division (4303T), USEPA Office of
Science and Technology, 1200
Pennsylvania Ave., NW., Washington,
DC 20460, 202-566-1040 (e-mail:
hessenauer.meghan@epa.gov). For
information regarding the changes to
drinking water regulations, contact
Patricia Snyder Fair, Technical Support
Center (MS 140), USEPA, Office of
Ground Water and Drinking Water, 26
West Martin Luther King Drive,
Cincinnati, OH 45268, 513-569-7937 (e-
mail: fair.pat@epa.gov).

SUPPLEMENTARY INFORMATION:

A. Potentially Regulated Entities

1. Clean Water Act

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 test
procedures for analysis of a specific
pollutant, the NPDES permittee must
use an approved test procedure (or an
approved alternate test procedure) for
the specific pollutant when measuring
the required waste constituent.
Similarly, if EPA has established
sampling requirements, measurements
taken under an NPDES permit must
comply with these requirements.
Therefore, entities with NPDES permits
will potentially be regulated by the
actions in this rulemaking. Categories
and entities that may potentially be
subject to the requirements of today's
rule include:
Category
State, Territorial, and Indian Tribal
Governments.
Industry
Municipalities

Examples of potentially regulated entities
States, Territories, and Tribes authorized to administer the NPDES permitting program; States,
and Tribes providing certification under Clean Water Act section 401 .
Facilities that must conduct monitoring to comply with NPDES permits
POTWs that must conduct monitoring to comply with NPDES permits

Territories,

This table is not intended to be
exhaustive, but rather provides a guide
for readers regarding entities likely to be
regulated by this action. This table lists
types of entities that EPA is now aware
could potentially be regulated by this
action. Other types of entities not listed
in the table could also be regulated. To
determine whether your facility is
regulated by this action, you should
carefully examine the applicability
language at 40 CFR 122.1, (NPDES
purpose and scope), 40 CFR 136.1
(NPDES permits and CWA), 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.
2. Safe Drinking Water Act

Public water systems are the regulated
entities required to measure
contaminants in drinking water
samples. In addition, EPA Regions, as
well as States, and Tribal governments
with authority to administer the
regulatory program for public water
systems under the Safe Drinking Water
Act, may also measure contaminants in
water samples. When EPA establishes a
maximum contaminant level (MCL) for
a given drinking water contaminant, the
Agency also approves standardized test
procedures for analysis of the
contaminant. Public water systems
required to test water samples must use

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11201
one of the approved test procedures.
Categories and entities that may
ultimately be subject to the
requirements of today's rule include:
Category
Examples of potentially regulated entities
NAICS1
State, Local, & Tribal Governments .

Industry

Municipalities
States, local and tribal governments that analyze water samples on behalf of public
water systems required to conduct such analysis; States, local and tribal govern-
ments that themselves operate community and non-transient non-community water
systems required to monitor.
Private operators of community and non-transient non-community water systems re-
quired to monitor.
Municipal operators of community and non-transient non-community water systems
required to monitor.
924110

221310

924110
1 North American Industry Classification System.
This table is not intended to be
exhaustive, but rather provides a guide
for readers regarding entities likely to be
regulated by this action. The table lists
types of entities that EPA is now aware
could potentially be regulated by this
action. Other types of entities not listed
in the table could also be regulated. To
determine whether your facility is
regulated by this action, you should
carefully examine the applicability
language at 40 CFR 141.2 (definition of
public water system). 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)(l) of the Clean
Water Act (CWA), judicial review of
today's CWA rule may be obtained by
filing a petition for review in the 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 March 26,
2007 as provided at 40 CFR 23.2. Under
section 1448 (a) of the Safe Drinking
Water Act (SOWA), judicial review of
today's SDWA rule may be obtained by
filing a petition for review only in the
United States Court of Appeal for the
District of Columbia Circuit within 45
days from the date of promulgation of
this rule. For SDWA judicial review
purposes, this final rule is promulgated
as of 1 p.m. (Eastern time) on March 26,
2007 as provide at 40 CFR 23.7. 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-Intemational
ASTM: ASTM International
ATP: Alternate Test Procedure
CWA: Clean Water Act
EPA: Environmental Protection Agency
FLAA: Flame Atomic Absorption
Spectroscopy
ICP-AES: Inductively Coupled Plasma-
Atomic Emission Spectroscopy
ICP-MS: Inductively Coupled Plasma-Mass
Spectroscopy
NPDES: National Pollutant Discharge
Elimination System
NPDWR: National Primary Drinking Water
Regulations
NSDWR: National Secondary Drinking ,
Water Regulations
QC: Quality Control
SDWA: Safe Drinking Water Act
STGFAA: Stabilized Temperature Graphite
Furnace Atomic Absorption Spectroscopy
USGS: United States Geological Survey
VCSB: Voluntary Consensus Standard Body

D. Table of Contents

I. Statutory Authority
A. Clean Water Act
B. Safe Drinking Water Act
II. Summary of Final Rule
A. 40 CFR Part 122
B. 40 CFR Part 136
C. 40 CFR Parts 141 and 143
D. 40 CFR Part 430
E. 40 CFR Part 455
F. 40 CFR Part 465
III. Changes Between the Proposed Rule and
the Final Rule
A. Silver Determinations
B. ASTM Method D5673-02 "Standard
Test Method for Elements in Water by
Inductively Coupled Plasma—Mass
Spectrometry"
C. Ammonia Determinations
D. Available Cyanide Determinations
E. Kelada-01 Method for Determination of
Available Cyanide and Total Cyanide
F. Mandatory Replacement of Mercuric
Sulfate with Copper Sulfate in Methods
for Determination of Total Kjeldahl
Nitrogen
G. Approval of Additional Standards for
Turbidity Determinations
H. Allowed Use of Capillary Columns in
EPA Methods 601-613, 624, 625, and
1624B
I. Changes to Sampling Requirements at 40
CFR Parts 122, 136, and 403
J. Approval Status of Total Elements
Digestion
K. EPA Method 245.7 for Determination of
Mercury
L. Clarification of Reporting Requirements
M. Corrections to 40 CFR Part 136, Tables
IA, IB, 1C, ID, IE and Footnotes
N. Revisions to 40 CFR Part 136, Table II
O. Corrections to Tables 40 CFR 141.23,
141.24, 141.25, and 141.74 and
Footnotes
P. Retention of Syngenta Method AG-625
for Determination of Atrazine
Q. EPA Method 327.0 for Determination of
Chlorine Dioxide
R. Deferral of Action on Microtox® 1010
IV. Response to Comments
A. Use of Syngeuta Method AG-625 for
Determination of Atrazine
B. Results From Use of Revised Methods,
"The Determination of Radium-226 and
Radium-228 in Drinking Water by
Gamma-ray Spectrometry Using HPGE or
Ge(Li) Detectors." (Revision 1.2,
December 2004)
V. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory
Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order 13132: Federalism
F. Executive Order 13175: Consultation
and Coordination with Indian Tribal
Governments
G. Executive Order 13045: Protection of
Children From Environmental Health
Risks and Safety Risks
H. Executive Order 13211: Actions that
Significantly Affect Energy Supply,
Distribution, or Use
I. National Technology Transfer and
Advancement Act
J. Congressional Review Act

I, Statutory Authority

A. Clean Water Act
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

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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).
B. Safe Drinking Water Act
  The Safe Drinking Water Act (SDWA),
as amended in 1996, requires EPA to
promulgate national primary drinking
water regulations (NPDWRs) that
specify maximum contaminant levels
(MCLs) or treatment techniques for
drinking water contaminants (SDWA
section 1412 (42 U.S.C. 300g-l)).
NPDWRs apply to public water systems
pursuant to SDWA sections 1401(1)(A)
(42 U.S.C.  300f(l)(A)). According to
SDWA section 1401(1)(D), NPDWRs
include "*  * * criteria and procedures
to assure a supply of drinking water
which dependably complies with such
maximum contaminant levels; including
accepted methods for quality control
and testing procedures *  * *" (42
U.S.C. 300f(lMD)). In addition, SDWA
section 1445 (a) authorizes the
Administrator to establish regulations
for monitoring to help determine
whether persons are acting in
compliance with the requirements of the
SDWA (42 U.S.C. 300J-4). EPA's
promulgation of analytical methods for
NPDWRs is authorized under these
sections of the SDWA as well as the
general rulemaking authority in SDWA
section 1450(a) (42 U.S.C. 300j-9(a)).
   The SDWA also authorizes EPA to
promulgate national secondary drinking
water regulations (NSDWRs) for
contaminants in drinking water that
primarily affect the aesthetic qualities
relating to the public acceptance of
drinking water (SDWA section 1412 (42
U.S.C. 300g-l)). These regulations are
not Federally enforceable but are
guidelines for the States (40 CFR 143.1).
The NSDWRs also include analytical
techniques for determining compliance
with the regulations (40 CFR 143.4).
EPA's promulgation of analytical
methods for NSDWRs is authorized
under general rulemaking authority in
SDWA section 1450(a) (42 U.S.C. 300j-
9(a)).
II. Summary of Final Rule
   The following sections describe the
changes EPA is making in today's final
rule.
                        A. 40 CFR Part 122
                          1. Some EPA Effluent Guideline
                        regulations, as well as EPA's Sewage
                        Sludge Use and Disposal Regulations,
                        require the use of analytical methods
                        specifically prescribed by the Guideline
                        (see e.g. 40 CFR Part 420.21(c)). This
                        rule amends the National Pollutant
                        Discharge Elimination System (NPDES)
                        regulations at 40 CFR Part 122 to clarify
                        when an NPDES permittee must use for
                        its monitoring and reporting the
                        analytical methods specifically required
                        in Title 40 of the CFR, Chapter I,
                        Subchapters N and O (effluent
                        guidelines and sewage sludge,
                        respectively) rather than the methods in
                        40 CFR Part 136. The regulatory
                        language has been amended  to explicitly
                        require either use of methods at 40 CFR
                        Part 136, or other methods that are
                        specifically prescribed for the particular
                        wastestream or for sewage sludge
                        monitoring requirements.
                          2. The rule also corrects
                        inconsistencies in sampling
                        requirements by referencing back to 40
                        CFR Part 136 to explicitly require use of
                        procedures at 40 CFR Part 136.
                          3. Sections 122.21(g)(7),
                        122.21(h)(4)(i), and 122.21(j)(4)(viii)
                        require an NPDES permit applicant to
                        report quantitative data for certain
                        pollutants. The rule adds E. coli and
                        Enterococci to the list of parameters at
                        40 CFR 122.21(g)(7) and 122.21(h)(4)(i),
                        and adds E. coli\.o the list of parameters
                        at40CFRl22.21(j)(4)(viii).

                        B. 40 CFE Part 136
                          This rule approves new and revised
                        methods for inclusion in 40 CFR Part
                        136. Many of those methods are from
                        the voluntary consensus standards body
                        (VCSB) that publishes Standard
                        Methods for the Examination of Water
                        and Wastewater. Those "Standard
                        Methods" are now available in both
                        hard copy and electronic formats. The
                        publisher identifies Standard Methods
                        in two ways, depending on the medium
                        of publication. Hard copy methods are
                        identified by the method number (e.g.,
                        SM 4500-C1 E) and the edition of the
                        manual in which they appear (e.g., 18th,
                        19th, 20th Editions), while the
                        electronic versions available on-line are
                        identified by the same method number
                        and the year the method was approved
                        for release (e.g., 4500-C1 E-00).
                           The following discussion briefly
                        describes the changes to Part 136
                        methods approved today,
                           1. This rule amends the regulations at
                        40 CFR Part 136 to approve three new
                        methods submitted as alternate test
                        procedures for monitoring chemical
                        pollutants. These methods are "Test
Method for Determination of Dissolved
Inorganic Anions in Aqueous Matrices
Using Capillary Ion Electrophoresis and
Chromate Electrolyte" (D6508, Rev. 2)
by Waters Corporation, "Digestion and
Distillation of Total Cyanide in Drinking
and Wastewaters using MICRO DIST
and Determination of Cyanide by Flow
Injection Analysis" (QuikChem Method
10-204-00-1-X) by Lachat Instruments,
and "Kelada Automated Test Methods
for Total Cyanide, Acid Dissociable
Cyanide, and Thiocyanate" (Kelada-01)
by Dr. Nabih Kelada.
  2. The rule approves a broad purpose
digestion procedure for total recoverable
elements digestion. EPA is approving
EPA Method 200.2 (Revision 2.8,1994)
for use with Inductively Coupled
Plasma-Atomic Emission Spectroscopy
(ICP-AES), Inductively Coupled
Plasma-Mass Spectroscopy (ICP-MS),
Stabilized Temperature Graphite
Furnace Atomic Absorption (STGFAA),
and Flame Atomic Absorption
Spectroscopy (FLAA) methods.
  3. The rule approves three new multi-
element test  procedures. The approved
methods are  EPA Method 200.8 .
(Revision 5.4,1994), AOAC Method
993.14 [16th Edition], and ASTM
D5673-03 for determination of elements
by ICP-MS.
  4. EPA is also approving a new multi-
element test  procedure, EPA Method
200.9 (Revision 2.2, 1994), for
determination of elements by STGFAA.
  5. The rule approves four new
methods for  determination of
hexavalent chromium by ion
chromatography. The methods are EPA
Method 218.6, AOAC Method 993.23
[16th Edition], and ASTM D5257-97—
SM 3500-Cr C [20th Edition] and  SM
3500-Cr E [18th, 19th Editions].
  6. The rule approves five new
methods for  determination of anions  by
ion chromatography. The methods are
EPA Method 300.0 (Revision 2.1,1993),
EPA Method 300.1 (Revision 1.0,1997),
AOAC Method 993.30 [16th Edition],
ASTM D4327, and SM 4110 B [18th,
19th, and 20th Editions],
   7. The rule approves the use of six
automated cadmium reduction methods
to determine nitrate and nitrite
individually, as well as in combination.
The methods are EPA Method 353.2
(Revision 2.0,1993), ASTM D3867-99
(A) and (B),  SM 4500-NO3-E and F
[18th, 19th,  20th Editions] and 4500-
NO3-E and F (2000), and USGS Method
1-4545-85.
   8. The rule approves a new method
for determination of chlorine by low
level amperometry—SM 4500-C1 E
[18th, 19th,  20th Editions] and SM
4500-C1 E (2000).

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9. The rule replaces EPA Method
180.1 (1978) for determination of
turbidity with EPA Method 180.1
(Revision 2.0,1993).
10. The rule replaces EPA Method
200.7 (1990) for determination of
elements by ICP-AES with EPA Method
200.7 (Revision 4.4, 1994).
11. The rule replaces EPA Method
245.1 (1974) for determination of
mercury with EPA Method 245.1
(Revision 3.0,1994).
12. The rule replaces EPA Method
335.3 (1978) for determination of total
cyanide with EPA Method 335.4
(Revision 1.0,1993) with a footnote to
clarify the proper procedure for
removing sulfide interferences.
13. The rule replaces EPA Method
350.1 (1978) for determination of
ammonia with EPA Method 350.1
(Revision 2.0,1993).
14. The rule replaces EPA Method
351.2 (1978) for determination of total
Kjeldahl nitrogen (TKN) with EPA
Method 351.2 (Revision 2.0 1993).
15. The rule replaces EPA Method
353.2 (1978) for determination of
nitrate-nitrite with EPA Method 353.2
(Revision 2.0,1993).
16. The rule replaces EPA Method
365.1 (1978) for determination of
phosphorus (all forms) with EPA
Method 365.1 (Revision 2.0,1993).
17. The rule replaces EPA Method
375.2 (1978) for determination of sulfate
with EPA Method 375.2 (Revision 2.0,
1993).
18. The rule replaces EPA Method
410.4 (1978) for determination of
chemical oxygen demand (COD) with
EPA Method 410.4 (Revision 2.0,1993).
19. The rule replaces EPA Method
420.2 (1974) for determination of total
phenols with EPA Method 420.4
(Revision 1.0,1993).
20. The rule approves a new method
for the determination of mercury, EPA
Method 245.7 "Mercury in Water by
Cold Vapor Atomic Fluorescence
Spectrometry" [Revision 2.0, 2005]
(EPA-821-R-05-001).
21. The rule approves a new method
for determination of available cyanide
by ligand exchange followed by flow
injection analysis, ASTM D6888-04.
22. The rule approves a new method
for determination of cations by ion
chromatography, ASTM D6919-03.
23. The rule approves a new method
for determination of chloride by
potentiometry, SM 4500-C1-D [18th,
19th, 20th Editions] and SM 4500-C1~D
(2000).
24. The rule approves a new method
for determination of chloride by ion
selective electrode, ASTM D512-89
(1999).
25. The rule approves two new
methods for determination of total
cyanide by ion selective electrode, SM
4500-CN-F [18th, 19th, 20th Editions]
and SM 4500-CN-F (2000), and ASTM
D2036-98 A.
26. The rule approves two new
methods for determination of sulfide by
ion selective electrode, SM 4500-S2~G
[18th, 19th, 20th Editions] and ASTM
D4658-03 (1996).
27. The rule approves a new method
for determination of nitrate by ion
selective electrode, SM 4500-NO3-[18th,
19th, 20th Editions] and SM 4500-
NO3-(2000).
28. The rule approves an errata sheet
to correct typographical errors in the
following methods manuals, "Short-
term Methods for Estimating the
Chronic Toxicity of Effluents and
Receiving Waters to Freshwater
Organisms," Fourth Edition, U.S.
Environmental Protection Agency,
Office of Water, Washington DC, EPA/
821/R-02/013 (the "freshwater chronic
manual"), and "Methods for Measuring
the Acute Toxicity of Effluents and
Receiving Waters to Freshwater and
Marine Organisms," Fifth Edition, U.S.
Environmental Protection Agency,
Office of Water, Washington DC, EPA/
821/R-02/012 (the "freshwater acute
manual").
29. The rule approves the use of
newer versions of 74 methods published
by ASTM International. The new
versions are published in the 1994,
1996, and 1999 Annual Book of ASTM
Standards Vols. 11.01 and 11.02, in the
2000 Annual Book of ASTM Standards,
Vol. 11.02 and in individual standards
published after 2000.
30. The rule approves the use of
newer versions of 88 methods published
by the Standard Methods Committee
and adopts a new numbering system to
track the approved versions of Standard
Methods. The new versions are
published in Standard Methods Online
(APHA 2003).
31. The rule approves the use of
newer versions of 19 methods published
by AOAC—International. The new
versions of these methods are published
in Official Methods of Analysis of
AOAC-International, 16th Edition,
1995.
32. The rule approves the replacement
of the mercuric sulfate catalyst with
copper sulfate in methods approved for
the determination of total Kjeldahl
nitrogen (TKN).
33. The rule approves the use of
styrene divinyl benzene beads and
stabilized formazin as alternatives to the
presently approved formazin standard
for determination of turbidity.
34. As described in the preamble to
the April 2004 proposed rule (69 FR
18213), EPA is adopting a new § 136.6
to introduce greater flexibility in the use
of approved methods. The section
describes the circumstances in which
approved methods may be modified and
the requirements that analysts must
meet to use these modified methods in
required measurements without prior
EPA approval. The rule also includes
language at § 136.6(c) to clarify that
analysts need only meet method
performance requirements for target
analytes (those analytes being measured
for NPDES reporting) when using multi-
analyte methods for compliance
monitoring purposes. The rule also
includes the language at § 136.6(d) to
allow explicitly the use of capillary
(open tubular) GC columns with EPA
Methods 601-613, 624, 625, and 1624B
as alternatives to the packed GC
columns specified in those methods,
provided that analysts generate new
retention time tables with capillary
columns to be kept on file with other
information for review by auditors.
35. The rule withdraws 109 methods
contained in EPA's "Methods for the
Chemical Analysis of Water and
Wastes" for which approved
alternatives published by voluntary
consensus standards bodies (e.g., ASTM
and Standard Methods) are available.
36. The rule withdraws liquid-liquid
extraction (LLE) methods, including
EPA Methods 612 and 625, as approved
procedures for determination of 1,2-
dichlorobenzene, 1,3-dichlorobenzene,
and 1,4-dichlorobenzene.
37. The rule withdraws approval of all
oil and grease methods that use
chlorofluorocarbon-113 (CFC-113;
Freon-113) as an extraction solvent.
38. The rule revises Table II (Required
Containers, Preservation Techniques,
and Holding Times) and the footnotes to
the table at 40 CFR 136.3(e). The table
and footnotes specify approved
sampling, preservation, and holding
time requirements for the methods
approved for compliance monitoring to
reduce confusion, resolve any conflicts
with instructions in the underlying
compliance monitoring method, and
reflect current understanding of sample
preservation requirements. The most
significant of the changes are those
made to Footnote 6, which addresses
the preservation of samples to be
analyzed for cyanide. Based on
information gathered during the
development of new cyanide methods
approved in this rulemaking, and
information collated from various
commenters and experts in cyanide
analyses, EPA revised footnote 6 to
Table II by adding text that describes
procedures that are recommended for
removal or suppression of cyanide
interferences, including interferences

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from sulfur, sulfide, sulfite, thiocyanate,
and aldehydes. The recommended
procedures may differ from those
described in the older approved
methods.
  39. EPA is changing "Director of .the
Environmental Monitoring Systems
Laboratory" and "Director, Analytical
Methods Staff" to "Alternate Test
Procedure Program Coordinator,
Washington, DC" every place the
phrases appear in the regulations. This
reflects the current organizational
structure and title  for the head of EPA's
Alternate Test Procedure (ATP) Program
management. In addition, addresses for
submission of ATPs are being updated
to reflect the current location of the
Alternate Test Procedure Program
Coordinator.
  40. The rule makes other minor
editorial revisions to clarify existing
regulations.

C, 40 CFR Parts 141 and 143
  1. This rule amends the regulations at
40 CFR Part 141 and Part 143 to allow
the use of 66 methods in  "Standard
Methods Online" (APHA 2003) (40 CFR
141.21, 141.23, 141.74, and 143.4).
  2. This rule allows the use of 28
newer versions of  methods published by
ASTM International. The new versions
are published in the 1999 "Annual Book
of ASTM Standards,'" Vols.11.01 and
11.02, in the 2000  "Annual Book of
ASTM Standards," Vol. 11.02 and in
individual standards published after
2000 (40 CFR 141.23).
  3. This rule approves a new method
submitted as an alternate test procedure
for the determination of common
anions—chloride,  fluoride, nitrate,
nitrite, orthophosphate, and sulfate,
"Test Method for Determination of
Dissolved Inorganic Anions in Aqueous
Matrices Using Capillary Ion
Electrophoresis and Chromate
Electrolyte" (D6508, Rev. 2) by Waters
Corporation (40 CFR 141.23 and 143.4).
  4. This rule approves two new
methods for determination of available
cyanide, "Available Cyanide by Flow
Injection, Ligand Exchange, and
Amperometry," Method OIA-1677, DW
(January 2004), and ASTM D6888-04
(40 CFR 141.23).
  5. This rule approves the use of EPA
Method 300.1 (Revision 1.0,1997) for
compliance determinations of chloride,
fluoride, nitrate, nitrite, orthophosphate,
and sulfete (40 CFR 141.23 and § 143.4).
  6. This rule approves the use of EPA
Method 552.3 (Revision 1.0, 2003) for
compliance determinations of dalapon
(40 CFR 141.24).
   7. This rule amends 40 CFR 141.25 to
add a new method for determination of
radium-226 and radium-228. This
                        method, "The Determination of Radium-
                        226 and Radium-228 in Drinking Water
                        by Gamma-ray Spectrometry Using
                        HPGE or Ge(Li) Detectors" (Revision
                        1.2, December 2004), was developed by
                        the Environmental Resources Center at
                        the Georgia Institute of Technology, and
                        was originally submitted to EPA as an
                        alternate test procedure to the currently
                        approved methods for determination of
                        radium-226 and radium-228.
                          8. This rule allows States the option
                        of approving ITS Free chlorine test
                        strips as a test kit for the measurement
                        of free chlorine using "Free Chlorine
                        Species" (HOC1- and OC1-) by Test
                        Strip," ITS Method D99-003 (Revision
                        3.0, November 21, 2003) by Industrial
                        Test Systems, Inc. (40 CFR 141.74).
                          9. This rule approves EPA Method
                        327.0 (Revision  1.1, 2005) for
                        measurement of chlorine dioxide
                        residuals (40 CFR 141.74).
                          10. This rule approves the use of
                        styrene divinyl benzene beads and
                        stabilized formazin as alternatives to the
                        presently approved formazin standard
                        for determination of turbidity (40 CFR
                        141.74).
                          11. This rule revises footnote 17 to the
                        table at 40 CFR 141.23 to allow the use
                        of a 450-W UV lamp in the Kelada
                        Method-01 for determination of cyanide.
                          12. This rule allows the use of
                        Syngenta Method AG-625, with the
                        modified immunoassay testing product
                        manufactured by Beacon Analytical
                        Systems, for the measurement of
                        atrazine under certain conditions. It
                        may only be used by those systems that
                        do not use chlorine dioxide for drinking
                        water treatment. In addition, the results
                        of the analysis of samples with
                        concentrations of atrazine more than
                        one-half the atrazine MCL (i.e., more
                        than 1.5 |ig/L) must be confirmed using
                        another approved method (40 CFR
                        141.24).
                          13. This rules also revises footnote 8
                        to the table in paragraph (a)(l) to correct
                        a long-standing  discrepancy between
                        the footnote and the specifications in
                        Standard Method 9221 E. The table in
                        question lists Standard Method 9221 E
                        as one of two procedures that may be
                        used for monitoring fecal coliforms.
                        Footnote 8  simply notes the holding
                        time for the A-l broth used in this
                        procedure.  Today's action corrects the
                        holding time specified in the footnote 8
                        to match the 7-day holding time that is
                        specified in Standard Method 9221 E
                        (40 CFR 141.74)

                        D. 40 CFR Part 430
                           This rule amends the Effluent
                        Limitations Guidelines for the pulp,
                        paper, and paperboard point source
                        category at 40 CFR Part 430 to approve
a new method for determination of
chlorinated phenolics in wastewaters
generated by these industries. The rule
adds a new section, 430.02(g), to allow
the use of "Chlorinated Phenolics in
Water by In situ Acetylation and GC/MS
Determination" (Method CP-86.07)
developed by the National Council for
Air and Stream Improvement (NCASI)
as an alternative to otherwise required
Method 1653  in Part 430, Appendix A.

E. 40 CFR Part 455
  This rule amends the regulations at 40
CFR Part 455  by moving Table 7 from
40 CFR Part 455 to 40 CFR Part 136.3(a)
as new Table  IG.

F. 40 CFR Part 465
  This rule amends the Effluent
Limitations Guidelines for the  coil
coating point source category at 40 CFR
Part 465 to replace the method listed at
section 465.03(c) for determination of
oil and grease in wastewater samples
from all subcategories of coil coating
with EPA Method 16 64A for
determination of non-polar materials
(NPM), which is generally equivalent to
total petroleum hydrocarbons.

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. In some instances, EPA
revised for clarity the language of the
final rule from that in the proposed rule.

A. Silver Determinations
   EPA received comments on the
Agency's proposed withdrawal of EPA
Method 272.1 which included
information on how to keep silver in
solution in samples with known or
suspected high levels of silver by adding
a solution containing cyanogen
chloride. As a result, EPA has  added a
footnote to Table IB at § 136.3 to include
procedures for preparation and addition
of this reagent to digested samples of
this type to keep the silver in solution
for analysis by any of the approved
methods. The Agency is withdrawing
EPA Method  272.1, as proposed in April
2004 (69 FR 18183 April 6, 2004).

B. ASTM Method D5673-02 "Standard
Test Method for Elements in Water by
Inductively Coupled Plasma—Mass
Spectrometry"
   Based on comment received on the
Agency's proposed approval of ASTM
Method D5673-02, EPA is approving an
updated version of this method ASTM
D5673-03. EPA included the updated
version of this method in a notice of
data availability (70 FR 7909, February
16, 2005) and requested public

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11205
comment on whether it should be
approved. EPA received no adverse
comments.
C. Ammonia Determinations
EPA received comment on the
Agency's proposed approval of an
updated version of EPA Method 350.1.
The commenter stated that mandating
the use of ethylene-diamine-tetra-acetate
(EDTA) in the method could adversely
affect method performance when using
an automated analyzer and submitted
data to support this claim. Based on
EPA's review of the data, the Agency is
adding a footnote to Table IB at § 136.3
allowing analysts to omit EDTA from
EPA Method 350.1, provided that all of
the quality control (QC) acceptance
criteria in the method are met.

D. Available Cyanide Determinations
The Agency solicited comment
regarding problems encountered with
the use of ligand exchange-
amperometric detection methods for
determination of available cyanide in
samples that contain significant
amounts of solids and solicited
potential solutions to these problems.
Based on public comment, EPA is
adding a footnote to Table IB at § 136.3
that includes suggestions for sample
filtration and for limiting the time
between addition of ligand exchange
reagents and analysis to solve these
problems when necessary. The Agency
proposed ASTM Method D6888-03 for
determining available cyanide. Since
publication of the proposal, EPA has
received a revised version of this
method. EPA included this revised
version in a Notice of Data Availability
(NODA) and requested public comment
on the approval of this revised version
of the method (70 FR 7909, February 16,
2005). D6888-04 contains a new online
sulfide removal procedure and
represents a refinement to the proposed
version. EPA received no adverse
comments on this revised version of the
method and is approving ASTM Method
D6888-04 in today's rule.
E. Kelada-01 Method for Determination
of Available Cyanide and Total Cyanide
Based on a comment and data
received on the Agency's proposed
approval of the Kelada-01 method for
determination of available cyanide and
total cyanide for use in NPDES
compliance monitoring, a note has been
added at 40 CFR 136.3, Table IB,
Footnote 55 to allow the use of 450-W
UV lamp instead of the 550-W lamp
specified in the method if it provides
performance within the quality control
acceptance criteria of the method in a
given instrument. Similarly, modified
flow cell configurations and flow
conditions may be used in the method,
provided that the QC acceptance criteria
are met. The Agency also is adding the
note at 40 CFR 141.23, Footnote 17, as
this method was previously approved
for use in drinking water compliance
monitoring.

F. Mandatory Replacement of Mercuric.
Sulfate With Copper Sulfate in Methods
for Determination of Total Kjeldahl
Nitrogen
The Agency proposed the mandatory
replacement of mercury sulfate with
copper sulfate in total Kjeldahl nitrogen
(TKN) digestion. Comments expressed
concern that copper sulfate will provide
inferior performance in some samples,
and suggested that EPA allow the
continued use of mercury sulfate in
analyses, offering copper sulfate as an
option. Based on EPA's evaluation of
these comments, the Agency has
decided that it will continue to allow
the use of mercury sulfate in TKN
analyses.

G. Approval of Additional Standards for
Turbidity Determinations
Based on comments received on the
proposed approval of additional
standards for use in methods to
determine turbidity, the Agency is
replacing turbidity standard trade
names with more generic listings in the
footnote to Table IB at § 136.3. An
example formulation for each generic
listing is also included in order to
provide a reference to at least one
source of the generic standard material.
The Agency also is adding a similar
footnote to the table in 40 CFR 141.74
where the approved methods for the
determination of turbidity in drinking
water are listed.
H. Allowed Use of Capillary Columns in
EPA Methods 601-613, 624, 625, and
1624B
The Agency proposed new language
that explicitly allows the use of
capillary columns in place of packed
columns with EPA Methods 601-613,
624, 625, and 1624B, provided that all
QC tests in these methods are performed
and all QC acceptance criteria are met.
Based on comments received on this
proposal, EPA is clarifying the
regulations at § 136.6 to state that
retention times will change with the
switch from packed to capillary
columns, so analysts are not required to
meet the retention times specified in the
method when the switch is made.
Instead, analysts must generate new
retention time tables with capillary
columns to be kept on file with other
information for review by auditors.
I. Changes to Sampling Requirements at
40 CFR Parts 122, 136, and 403
The Agency proposed changes to the
sampling requirements specified at 40
CFR Parts 122,136 and 403. Based on
comments received on these proposed
updates, the sampling requirements
have been modified to include clarifying
language with respect to grab and
composite sampling requirements, and
to add E. coli and Enterococci to the
parameters listed at Part 122.21 for
which an NPDES applicant must
provide analytical information. In
addition, on October 14, 2005, EPA
published in the Federal Register final
changes to its General Pretreatment
Regulations (70 FR 60134). In these
regulations, EPA consolidated
monitoring requirements for indirect
dischargers into 40 CFR 403.12(g). In the
proposal for the current rule, EPA
proposed to modify 40 CFR 403.12 (b).
Based on changes made to 40 CFR Part
403 on October 14, 2005, however, the
proposed modifications to CFR 403.12
(b) are no longer required.

/. Approval Status of Total Elements
Digestion
The Agency proposed to approve a
"total recoverable" elements digestion
procedure, and also to retain "total"
elements digestion for graphite furnace
atomic absorption (GFAA) analyses.
Based on comments received on this
proposal, EPA is clarifying the language
in Table IB at § 136.3 to specify Section
4.1.3 of Methods for Chemical Analysis
of Water and Wastes (MCAWW) as the
approved digestion procedure for use
with non-platform graphite furnace
atomic absorption determinations.
K. EPA Method 245.7 for Determination
of Mercury
The Agency proposed approval of
EPA Method 245.7 (December 2003) as
an additional method for determination
of mercury. Based on comments
received on this proposal, EPA has
revised the method and is approving
EPA Method 245.7 (Revision 2.0, 2005)
in this rule. Specifically, EPA has
approved the method with the following
changes: includes a discussion of the
gas-liquid separator in Section 2.6,
reduces the amount of hydrochloric acid
used during sample digestion, includes
the addition of hydrochloric acid (HC1)
to standard solutions, clarifies that
additional procedures for handling
difficult matrices may be used provided
that laboratories meet the method
performance criteria, and revises
procedures for preparing reagent blanks
to remove the addition of stannous
chloride (SnCy and include addition of

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HC1. EPA also has corrected section
numbering and references throughout
Sections 4 and 7 of the method.
L. Clarification of Reporting
Requirements
  The Agency proposed to add a new
§ 136.7 that would clarify that a quality
control (QC) failure does not relieve a
permittee of the duty to report results
and that results are to be reported to the
level specified in the method or
required in the permit, whichever is
lower. EPA agrees with public comment
that the proposed revision was unclear.
In this rule, EPA is revising this action
to clarify our intent in text at § 136.3,
rather than take final action on the
proposed text at § 136.7.
  EPA proposed a new § 136.7
amendment to  resolve conflicts between
current reporting requirements at 40
CFR Parts  122 and 125 and preservation
requirements at 40 CFR 136.3(e) and
instructions  in compliance monitoring
methods specified in the tables at 40
CFR 136.3(a). For example, some
methods provide "reject tests" (e.g.
Method 5210 B 5-day BOD, section 6a,
Standard Methods, 20th edition) or state
that a "result may not be reported for
regulatory compliance purposes" (e.g.
Method OIA 1677: Available Cyanide,
section 9.3.4, OI Analytical) if an
analytical  quality control measure is
outside its control limit range
(acceptance criteria). However, it may
be necessary to report such results if
resampling; reanalysis or other
corrective  action is not possible. Not
reporting these results may cause a
permittee to be in violation of Part 122
or 125 reporting requirements.
Reporting  such available data is
recommended  as a good laboratory
practice (D3856-95 Standard Guide for
Good Laboratory Practices in
Laboratories Engaged in Sampling and
Analysis of Water, Annual Book of
ASTM Standards, Water and
Environmental Technology, Vol 11.01
Water (I), p.  353, 2003).
  For clarification, in this rule, EPA is
adding a statement to the text preceding
Tables IA  to IG at § 136.3(a), and Table
II at § 136.3(e)  to state that reporting
requirements of Parts 122 or 125 may
take precedence over the otherwise
applicable reporting or preservation
requirements of a particular analytical
method.

M. Corrections to 40 CFR Part 136,
Tables IA, IB, 1C, ID, IE and Footnotes
  The Agency is correcting errors that
were published in the proposed Table
IA (List of Approved Biological
Methods), Table IB (List of Approved
Inorganic Test Procedures), Table 1C
                         (List of Approved Test Procedures for
                         Non-Pesticide Organic Compounds),
                         Table ID (List of Approved Test
                         Procedures for Pesticides), and Table IE
                         (List of Approved Radiologic Test
                         Procedures) and the footnotes to those
                         tables.

                         N. Revisions to 40 CFR Part 136, Table
                         II
                          The rule revises Table II (Required
                         Containers, Preservation Techniques,
                         and Holding Times), and the  footnotes
                         to Table II at 40 CFR 136.3(e). The
                         action of updating Table II at § 136.3(e)
                         reflects EPA's evaluation of comments
                         received on the April 6, 2004 proposal.
                         EPA revised footnote 1 to more clearly
                         distinguish between polyethylene (P),
                         fluoropolymer (FP), glass (G), and low-
                         density polyethylene (LDPE)  and has
                         made it explicit that a sample to be used
                         to determine fluoride is to be collected
                         in a polyethylene bottle. EPA revised
                         footnotes 2 and 7 to add language to
                         make more clear that preservation must
                         be within 15 minutes after collection of
                         a grab sample, a composite sample, or
                         an aliquot split from a composite
                         sample collected automatically over
                         time.
                          EPA modified footnote 4 to clarify the
                         start of holding times for the  different
                         types of sample collection (grab
                         samples, composite samples  collected
                         automatically, and a set of grab samples
                         that is composited in the laboratory).
                         The revisions remove the requirement
                         for collection of samples to determine
                         cyanide in amber glass bottles with
                         PTFE-lined caps from footnote 6.
                         Footnotes 5 and 6 describe procedures
                         recommended for removal or
                         suppression of cyanide interferences,
                         including interferences from  oxidants,
                         sulfide, sulfite, thiocyanate, and
                         aldehydes. In addition, the footnote also
                         provides that other procedures for
                         removal  or suppression of cyanide
                         interferences may be employed,
                         provided the analyst demonstrates that
                         such other procedures more accurately
                         measure cyanide.
                           E]PA clarified requirements in
                         footnote 17 specific to sampling for
                         trace mercury, added EPA Method 245.7
                         to footnote 17, and removed footnote 17
                         from the "Preservation" and  "Maximum
                         Holding Time" headers. EPA has
                         clarified footnote 18 to indicate that the
                         number of significant figures is intended
                         to establish an absolute upper limit on
                         sample temperature and preclude
                         meeting the specification through
                         rounding of numbers and added an
                         exception to footnote 18 for a sample
                         analyzed immediately (in less than  15
                         minutes from collection). EPA deleted
                         footnote 19 because the information is
now in footnote 5. Deletion of this
footnote resulted in renumbering all of
the subsequent footnotes to Table II.
  EPA has also clarified that
preservation is not required for soil and
sediment samples. EPA also has  revised
preservation requirements for acrolein,
acrylonitrile, and purgeable aromatics to
remove inconsistences, revised
requirements for collection of samples
to be tested for Cryptosporidium and
Giardia, and established 0-8 °C as the
holding temperature for samples to be
tested for Cryptosporidium. In addition,
the Agency is correcting minor
formatting and typographical errors that
were published in the proposed Table II.
  EPA recognizes that the requirements
at § 136.3 may differ from those
described in some older approved
methods and today's action clarifies that
this section supersedes instructions in a
compliance method. Where there are
conflicts with existing methods
published by EPA, VCSBs, or other
entities, we expect that the next
revisions of these methods will conform
to the requirements at § 136.3(e).

O. Corrections to Tables 40 CFR  Parts
141.23, 141.24, 141.25, and 141.74 and
Footnotes
  The final rule corrects a number of
errors in the proposed tables at § 141.23
(Inorganic Chemical Sampling and
Analytical Requirements), 141.24
(Organic Chemicals, Sampling and
Analytical Requirements), 141.25
(Analytical Methods for Radioactivity)
and 141.74 (Analytical and Monitoring
Requirements) and the footnotes to
those tables. The Agency also revised
the wording of several entries for the
cyanide methods in the tables at 40 CFR
141.23 to more clearly distinguish
among the various methodologies listed
in those tables.
P. Retention of Syngenta Method AC—
625 for Determination ofAtrazine
  The Agency proposed to withdraw
approval of Syngenta Method AG—625
for the determination of atrazine in
drinking water. Based on comments
received regarding the April 6, 2004
proposal and comments received
regarding additional data submitted in
response to the Notice of Data
Availability (70 FR 7909, February 16,
2005), EPA has decided to retain
Syngenta Method AG-625 with  some
restrictions on its use. The revised
approval requires confirmation of any
compliance monitoring results for
atrazine that are greater than one half of
the MCL for atrazine, using an alternate
approved method. EPA based its
approval on the use of the modified
immunoassay testing product produced

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11207
by Beacon Analytical Systems, the only
version of the product that is currently
offered for sale. However, use is not
authorized for public water systems
which use chlorine dioxide for drinking
water treatment.

Q. EPA Method 327.0 for Determination
of Chlorine Dioxide
The Agency proposed to approve EPA
Method 327.0 (Revision 1.0, 2003) for
the determination of chlorine dioxide
(40 CFR 141.74). In the final rule, the
Agency has approved EPA Method
327.0 (Revision 1.1, 2005) and corrected
three typographical errors in the
proposed method.

R. Deferral of Action on Microtox® 1010
Because EPA is continuing to evaluate
public comment about use of the
Microtox® 1010 test procedure for
determinations of acute whole effluent
toxicity, and the data supporting use of
this test procedure, EPA is not taking
final action on the proposal to approve
Microtox® 1010 for compliance
monitoring.

IV. Response to Comments
EPA received two comments
regarding methods included in this final
rule from the August 18, 2003 proposal
(68 FR 49548), 115 comments on the
April 6, 2004 proposal (69 FR 18166),
and nine comments on the February 16,
2005 Notice of Data Availability
(NODA) (70 FR 7909). Commenters
represented a number of different
interests, including analytical
laboratories, water utilities, instrument
manufacturers, State and local
governments, trade associations,
scientists, and private citizens. A
summary of major public comments on
the proposed rules and the NODA and
the Agency's responses is presented in
this section, and section III of this
preamble. The public docket for this
rule includes the Agency's response to
all comments.
A. Use of Syngenta Method AG-625 for
Determination ofAtrazine
EPA proposed withdrawing approval
of Syngenta Method AG-625 (Syngenta
Crop Protection Inc.) for the
determination of atrazine. Based on
comments and additional data
submitted in response to the NODA,
EPA has decided to retain Syngenta
Method AG-625 as an approved method
for atrazine, subject to certain
conditions. Today's amended rule will
require the use of an alternate approved
method for atrazine to confirm any
results from the Syngenta method that
are greater than one half of the MCL for
atrazine. EPA's decision to retain the
approval of Method AG-625 is based on
using the modified immunoassay testing
product manufactured by Beacon
Analytical Systems (Atrazine Plate Kit—
Cat# CPP-004), the only version of the
product currently offered for sale.
However, based on data submitted in
response to the NODA, EPA is not
approving Method AG—625 for use
when chlorine dioxide is used for
drinking water treatment.
One commenter supported the
withdrawal of Syngenta Method AG-
625, citing EPA's Environmental
Technology Verification (ETV) study,
and suggested that the method had not
been validated adequately prior to
EPA's earlier approval. The commenter
also suggested that approval of a
modified version of AG—625 may be
preferable, but was concerned that the
method using the original testing
product could lead to reports of non-
compliance and/or increased treatment
cost based on erroneous atrazine
measurements in the interim.
Other comments questioned the
validity of data submitted by the
American Water Works Association
(AWWA) that demonstrated method
deficiencies and requested that the data
not be considered by EPA. The
commenters noted that data were not
accompanied by suitable quality control
checks and that some tests (i.e., testing
the effect of humic acid) were not
reproducible in later studies by the
same investigator. The commenters also
suggested that data generated by AWWA
was not generated according to Method
AG-625, but rather by simply using the
commercial testing product without
reference to the method.
As reported by Adams (Adams et al.,
JAWWA, 2004, pp. 126-139), the
original immunoassay test kit used with
Method AG-625 was subject to a
positive bias in the measurement of
atrazine in the presence of disinfectants
used in drinking water treatment, such
as chlorine, monochloroamine,
chloramine T, chlorine dioxide and
other substances. Additionally, data
reported by Adams using the modified
Beacon test kit, data from the
Environmental Technology Verification
(ETV) Program, and, in fact, data in the
December 2004 Syngenta study
(Atrazine: Final Report, Syngenta
Number T006141-04, 12/10/2004),
demonstrate that test kits marketed by
Beacon, Abraxis, and SDI show a
modest positive bias in raw and finished
drinking water for most samples (i.e.,
the measured concentrations in most
samples were higher than the expected
values). For a distinct minority of
samples in these two studies, no bias or
a negative bias was shown (i.e., the
measured concentrations were equal to
or lower than the expected
concentrations in a few samples). The
December 2004 Syngenta study
submitted to EPA demonstrated that the
modified Beacon immunoassay test kit
performed suitably in the presence of
chlorine, monochloroamine, chloramine
T, chloroform, and humic acid.
However the data show that an
interference occurred in the presence of
chlorine dioxide unless samples were
analyzed within one day of collection.
EPA agrees that data from both
Syngenta and AWWA (Adams) indicate
that, except for cases involving chlorine
dioxide, the modified testing product
performed substantially better with
regard to the positive bias and
interferences than did the original
product in the presence of disinfectants
and other interferences. EPA also agrees
that, in general, the immunoassay
products examined in these studies
exhibit some positive bias for atrazine.
Low results were only obtained from
analyses of a few samples.
EPA recognizes that a potential
positive bias is a concern for water
utilities, particularly those located in
areas such as the Midwest, where
atrazine is used extensively to control
weeds in corn and sorghum crops.
However, in many other areas, where it
is not used, atrazine is not likely to be
found in drinking water samples at all.
Because accurate information on the
occurrence of contaminants at
concentrations close to the MCL is
necessary for EPA to meet its obligation
to review MCLs every six years, EPA has
retained approval of Syngenta Method
AG— 625 for atrazine with the conditions
on its use described below. The
following conditions have been added
as Footnote 5 to the table at 40 CFR
"This method may not be used for the
analysis of atrazine in any system where
chlorine dioxide is used for drinking water
treatment. In samples from all other systems,
any result for atrazine generated by Method
AG-625 that is greater than one-half the
maximum contaminant level (MCL) (i.e.,
greater than 0.0015 mg/L or 1.5 (ig/L) must
be confirmed using another approved method
for this contaminant and should use
additional volume of the original sample
collected for compliance monitoring, hi
instances where a result from Method AG-
625 triggers such confirmatory testing, the
confirmatory result is to be used to determine
compliance."

The MCL for atrazine is 0.003 mg/L
(3 ng/L). Thus, any results from Method
AG-625 greater than 0.0015 mg/L (1.5
Hg/L) must be confirmed through the
use of another approved method for
atrazine. In such instances, the

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confirmatory result is used to determine
compliance, because the methods used
for confirmatory testing are considered
more accurate.
  EPA acknowledges that this
requirement for confirmation may cause
some utilities to choose not to employ
Method AG-625. However, the approval
of a method at 40 CFR Part 141 does not
constitute a requirement for its use
when other approved methods are
available. Furthermore, EPA has
concluded that, given the distribution of
atrazine use nationwide, the majority of
water utilities will not be negatively
affected by the confirmation
requirement and can take advantage of
the potential cost savings afforded by
Method AG-625 relative to other
approved methods for atrazine. EPA
notes that if utilities are monitoring for
a broad range of contaminants using
approved methods that cover multiple
analytes (e.g., Method 525.2), then the
use of a test kit may not offer a cost
advantage because of the ability to
include atrazine in a broad spectrum
method.
  Based on the data provided in
response to the proposed rule and
NODA, EPA agrees that the presence of
chlorine dioxide has substantial
potential to interfere with Method AG—
625. Therefore, EPA has not approved
the method for use in water systems
where chlorine dioxide is used for
drinking water treatment. While the
data from one study suggest that the
atrazine results are not affected if
samples are analyzed within 24 hours
after sample collection, the
circumstances surrounding this
observation in the study have not been
fully characterized. At a future date,
EPA may reconsider the use of Method
AG-625 by water systems using
chlorine dioxide, if more information is
available characterizing the performance
of the method.
B. Results From Use of Revised
Methods, "The Determination of
Radium-226 and. Radium-228 in
Drinking Water by Gamma-ray
Spectrometry Using HPGE or Ge(Li)
Detectors."(Revision 1.2, December
2004)
  The final rule establishing
radionuclide drinking water standards
published on December 7, 2000 (65 FR
76708) required drinking water systems
to sample and report on radionuclides
in their drinking water supplies during
the period from December 8, 2003 to
December 31, 2007, including the
combined result for radium-226 and
radium-228. Prior to today's rule,
separate methods were required for the
measurement of radium-226 and
                        radium-228. The separate results of the
                        two isotopes are summed to provide the
                        "combined" result that is compared to
                        the MCL. One commenter supported the
                        approval of the method from the Georgia
                        Institute of Technology because one
                        method can be used to measure both
                        radium isotopes and would make for a
                        faster result. The commenter also noted
                        that there are approximately 150,000
                        Public Water Supply source water taps
                        across the country that would have to be
                        sampled. Given these monitoring
                        requirements, the commenter was
                        concerned about sufficient laboratory
                        capacity to meet the monitoring
                        requirements of the December 2000 rule
                        because approval of the Georgia
                        Institute of Technology method would
                        not become effective until promulgation
                        of today's rule.
                          In response to this comment, EPA is
                        allowing community water systems to
                        use samples collected after January 1,
                        2005 and analyzed using the analytical
                        method approved in this rule to satisfy
                        the radium-226 and radium-228
                        monitoring requirements for the 2005-
                        2007 compliance period. (Minor
                        corrections to the method were made in
                        December 2004 and are reflected in the
                        version approved in this rule, so it was
                        not available for analyzing samples
                        collected prior to 2005.) Allowing this
                        early use of the method should alleviate
                        some of the laboratory capacity
                        concerns. EPA has included a footnote
                        in the revised table of analytical
                        methods for radioactivity at § 141.25 to
                        indicate that samples analyzed using the
                        newly approved method are acceptable.
                        Such "grandfathered" data must be
                        based on results from the analytical
                        method approved for use by this final
                        rule. The term "grandfathered data"
                        used in this rule does not apply to data
                        collected to  meet other grandfathering
                        provisions specified in the radionuclide
                        final rule that was published on
                        December 7, 2000 (65 FR 76708).
                        V. Statutory and Executive Order
                        Reviews

                        A. Executive Order 12866: Regulatory
                        Planning and .Review
                          Under Executive Order 12866 (58 FR
                        51735, October 4,1993), the Agency
                        must determine whether the regulatory
                        action is "significant" and therefore
                        subject to OMB review and the
                        requirements of the Executive Order.
                        The Executive Order defines
                        "significant regulatory action" as one
                        that is likely to result in a rule that may:
                           (1) Have an annual effect on the
                        economy of $100 million or more, or
                        adversely affect in a material way the
                        economy, a sector of the economy,
productivity, competition, jobs, the
environment, public health or safety, or
State, local, or Tribal governments or
communities;
  (2) Create a serious inconsistency or
otherwise interfere with an action taken
or planned by another agency;
  (3) Materially alter the budgetary
impact of entitlements, grants, user fees,
or loan programs or the rights and
obligations of recipients thereof; or
  (4) Raise novel legal or policy issues
arising out of legal mandates, the
President's priorities, or the principles
set forth in the Executive Order.
  It has been determined that this rule
is not a "significant regulatory action"  •
under the terms of Executive Order
12866 and is therefore not subject to
OMB  review.

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 etseq. This rule
does not impose any information
collection, reporting, or recordkeeping
requirements. This rule merely adds
new and updated versions of testing
procedures, withdraws some older
testing procedures, and establishes new
sample collection, preservation,  and
holding time requirements.
  Burden means the total time, effort, or
financial resources expended by persons
to generate, maintain, retain, or disclose
or provide information to or for a
Federal agency. This includes the time
needed to review instructions; develop,
acquire, install, and utilize technology
and systems for the purpose of
collecting, validating, and verifying
information, processing and
maintaining information,  arid disclosing
and providing information; adjust the
existing ways to comply with any
previously applicable instructions and
requirements; train personnel to be able
to respond to a collection of
information; search data sources;
complete and review the collection of
information; and transmit or otherwise
disclose the information.
  An Agency may not conduct or
sponsor, and a person is not required to
respond to a collection of information
unless it displays a currently valid OMB
control number. The OMB control
numbers for EPA's regulations in 40
CFR are listed in 40 CFR Part 9.

C. Regulatory Flexibility Act
  The 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

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11209
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 as
defined by the Small Business
Administration's (SBA) regulations at 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. The RFA provides
default definitions for each type of small
entity. It also authorizes an agency to
use alternative definitions for each
category of small entity, "which are
appropriate to the activities of the
agency" after proposing the alternative
definition(s) in the Federal Register and
taking comment (5 U.S.C. 60l(3)-(5)). In
addition to the above, to establish an
alternative small business definition,
agencies must consult with SBA's Chief
Counsel for Advocacy.
For purposes of assessing the impacts
of this rule on small entities for methods
under the Safe Drinking Water Act, EPA
considered small entities to be public
water systems serving 10,000 or fewer
persons. This is the cut-off level
specified by Congress in the 1996
Amendments to the Safe Drinking Water
Act for small system flexibility
provisions. In accordance with the RFA
requirements, EPA proposed using this
alternative definition in the Federal
Register (63 FR 7620, February 13,
1998), requested public comment,
consulted with the Small Business
Administration, and expressed its
intention to use the alternative
definition for all future drinking water
regulations in the Consumer Confidence
Reports regulation (63 FR 44511, August
19,1998). As stated in that final rule,
the alternative definition would be
applied to this regulation as well.
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 updated
versions of testing procedures,
withdraws some older testing
procedures, and approves new sample
collection, preservation, and holding
time requirements. Generally, these
changes will have a positive impact on
small entities by increasing method
flexibility, thereby allowing entities to
reduce costs by choosing more cost-
effective methods. In some cases,
analytical costs may increase slightly
due to the additional QC requirements
included in the methods that are being
approved to replace older EPA methods.
However, most laboratories that analyze
samples for EPA compliance monitoring
have already instituted QC requirements
as part of their laboratory practices. We
have determined that a small number of
small entities that are still using the
CFC-113 based oil and grease methods
may need to devote resources to analyst
training when they switch to hexane-
based methods. However, due to the
decreased availability of CFC-113 in the
marketplace, we anticipate that the cost
differential, if any, will soon favor the
use of the hexane-based methods. The
phaseout of CFC-113 based methods is
required to comply with the Montreal
Protocol which prohibits the use of
CFC-113 based methods after December
31,2005.
Although this final rule will not have
a significant economic impact on a
substantial number of small entities,
EPA nonetheless has tried to reduce the
impact of this rule on small entities.
Anticipating the prohibition of CFC-113
based methods, EPA promulgated
hexane-based methods in May 1999.
EPA has determined that most
laboratories have now switched to
hexane-based oil and grease methods,
making the analysis costs competitive
with the CFC-113 based methods.
D. Unfunded Mandates Reform Act
Title II of the Unfunded Mandates
Reform Act of 1995 (UMRA), Public
Law 104-4, establishes requirements for
Federal agencies to assess the effects of
their regulatory actions on State, Tribal,
and local governments and the private
sector. Under section 202 of the UMRA,
EPA generally must prepare a written
statement, including a cost-benefit
analysis, for proposed and final rules
with "Federal mandates" that may
result in expenditures to State, local,
and Tribal governments, in the
aggregate, or to the private sector, of
$100 million or more in any one year.
Before promulgating an EPA rule for
which a written statement is needed,
section 205 of the UMRA generally
requires EPA to identify and consider a
reasonable number of regulatory
alternatives and adopt the least costly,
most cost-effective or least burdensome
alternative that achieves the objectives
of the rule. The provisions of section
205 do not apply when they are
inconsistent with applicable law.
Moreover, section 205 allows EPA to
adopt an alternative other than the least
costly, most cost-effective or least
burdensome alternative if the
Administrator publishes with the final
rule an explanation of why that
alternative was not adopted.
Before EPA establishes any regulatory
requirements that may significantly or
uniquely affect small governments,
including Tribal governments, it must
have developed under section 203 of the
UMRA a small government agency plan.
The plan must provide for the
notification of potentially affected small
governments, enabling officials of
affected small governments to have
meaningful and timely input in the
development of EPA regulatory
proposals with significant Federal
intergovernmental mandates, and
informing, educating, and advising
small governments on compliance with
the regulatory requirements.
This rule contains no Federal
mandates (under the regulatory
provisions of Title II of UMRA) for
State, local, or Tribal governments or
the private sector. The rule imposes no
enforceable duty on any State, local, or
Tribal governments or the private sector.
In fact, this rule should (on the whole)
save money for governments and the
private sector by increasing method
flexibility, and allowing these entities to
reduce monitoring costs by taking
advantage of innovations. Thus, today's
rule is not subject to the requirements
of Sections 202 and 205 of the UMRA.
EPA has determined that this rule
contains no regulatory requirements that
might significantly or uniquely affect
small governments. Generally, this
action will have a positive impact by
increasing method flexibility, thereby
allowing method users to reduce costs
by choosing more cost effective
methods. In some cases, analytical costs
may increase slightly due to changes in
methods, but these increases are neither
significant nor unique to small
governments. This rule merely approves
new and updated versions of testing
procedures, withdraws some older
testing procedures, and approves 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
Executive Order 13132, entitled
"Federalism" (64 FR 43255, August 10,
1999), requires EPA to develop an
accountable process to ensure
"meaningful and timely input by State
and local officials in the development of
regulatory policies that have federalism
implications." "Policies that have
federalism implications" is defined in
the Executive Order to include

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regulations that 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."
  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. This rule merely
approves new and updated versions of
testing procedures, withdraws some
older testing procedures, and approves
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), 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

  Executive Order 13175, entitled
"Consultation and Coordination with
Indian Tribal Governments" (65 FR
67249, November 9, 2000), requires EPA
to develop an accountable process to
ensure "meaningful and timely input by
tribal officials in the development of
regulatory policies that have tribal
implications."
  This final rule does not have tribal
implications, as specified in Executive
Order 13175. It will not have substantial
direct effects on Tribal governments, on
the relationship between the Federal
government and Indian tribes, or on the
distribution of power and
responsibilities between the Federal
government and Indian tribes. This rule
merely approves new and updated
versions  of testing procedures,
withdraws some older testing
procedures, and approves new sample
collection, preservation, and holding
time requirements. The costs to Tribal
governments will be minimal (in fact,
governments may see a cost savings),
and the rule does not preempt State law.
Thus, Executive Order 13175 does not
apply to this rule.
                         G. Executive Order 13045: Protection of
                         Children From Environmental Health
                         Risks and Safety Risks
                          Executive Order 13045: "Protection of
                         Children from Environmental Health
                         Risks and Safety Risks" (62 FR 19885,
                         April 23,1997) applies to any rule that:
                         (1) Is determined to be "economically
                         significant" as defined under Executive
                         Order 12866, and (2) concerns an
                         environmental health or safety risk that
                         EPA has reason to believe may have a
                         disproportionate effect on children. If
                         the regulatory action meets both criteria,
                         the Agency must evaluate the
                         environmental health or safety effects of
                         the planned rule on children, and
                         explain why the  planned regulation is
                         preferable to other potentially effective
                         and reasonably feasible alternatives
                         considered by the Agency. This final
                         rule is not subject to the Executive
                         Order 13045 because it is not
                         economically significant as defined in
                         Executive Order  12866. Further it does
                         not concern an environmental health or
                         safety risk that EPA has reason to
                         believe may have a disproportionate
                         effect on children. This action approves
                         new and updated versions of testing
                         procedures, withdraws some older
                         testing procedures, and approves new
                         sample collection, preservation, and
                         holding time requirements.

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

                         /. National Technology Transfer and
                         Advancement Act
                          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 over 150
standards developed by Standard
Methods and ASTM International for
use in compliance monitoring.

/. Congressional Review Act

  The Congressional Review Act, 5
U.S.C. Section 801 etseq., 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. A major rule
cannot take effect until 60 days after it
is published in the Federal Register.
This action is not a "major rule" as
defined by 5 U.S. C Section 804(2). This
rule will be effective April 11, 2007.

List of Subjects

40 CFRPart 122
  Administrative practice and
procedure, Confidential business
information, Environmental protection,
Hazardous substances, Reporting and
recordkeeping requirements, Water
pollution control.

40 CFR Part 136
  Environmental protection,
Incorporation by reference, Reporting
and recordkeeping requirements, Water
pollution control.
40 CFR Part 141

  Chemicals, Environmental protection,
Incorporation by reference, Indians-
lands, Intergovernmental relations,
Radiation Protection, Reporting and
recordkeeping requirements, Water
supply.

40 CFR Part 143
  Chemicals, Environmental protection,
Incorporation by reference, Indians-
lands, Water supply.

40 CFR Part 430
  Environmental protection, Paper and
paper products industry, Reporting and
recordkeeping requirements, Waste
treatment and disposal, Water pollution
control.

40 CFR Part 455
  Chemicals, Environmental protection,
Packaging and containers, Pesticides
and pests, Waste treatment and
disposal, Water pollution control.

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              Federal  Register/Vol. 72, No.  47/Monday, March 12, 2007/Rules  and Regulations
                                                                     11211
40 CFR Part 465
  Coil coating industry, Environmental
protection, Reporting and recordkeeping
requirements, Waste treatment and
disposal, Water pollution control.
  Dated: July 21, 2006.
Stephen L. Johnson,
Administrator.
• For the reasons set out in the
preamble, title 40, chapter I of the Code
of Federal Regulations, is amended as
follows:

PART 122— EPA ADMINISTERED
PERMIT PROGRAMS: THE NATIONAL
POLLUTANT DISCHARGE
ELIMINATION SYSTEM

• 1. The authority citation for Part 122
continues to read as follows:
  Authority: The Clean Water Act, 33 U.S.C.
1251 etseq.
• 2. Section 122.1 is am ended by
revising paragraph (a)(4) to read as
follows:

§ 122.1 Purpose and Scope.
  (a)* * *
  (4) Regulatory provisions in Parts 125,
129, 133, 136 of this chapter and 40 CFR
subchapter N and subchapter O of this
chapter also implement the NPDES
permit program.
*****

• 3. Section 122. 21 is amended as
follows:
• a. By revising paragraph (g)(7)(i).
• b. By revising introductory text in
paragraph (h)(4)(i).
• c. By revising paragraph (j)(4)(viii).

§122.21  Application for a permit
(applicable to State programs, see § 123.25)
  (7) Effluent characteristics, (i)
Information on the discharge of
pollutants specified in this paragraph
(g)(7) (except information on storm
water discharges which is to be
provided as specified in § 122.26).
When "quantitative data" for a pollutant
are required, the applicant must collect
a sample of effluent and analyze it for
the pollutant in accordance with
analytical methods approved under Part
136 of this chapter unless use of another
method is required for the pollutant
under 40 CFR subchapters N or O.
When no analytical method is approved
under Part 136 or required under
subchapters N or O, the applicant may
use any suitable method but must
provide a description of the method.
When an applicant has two or more
outfalls with substantially identical
effluents, the Director may allow the
applicant to test only one outfall and
report that quantitative data as applying
to the substantially identical outfall.
The requirements in paragraphs
(g)(7)(vi) and (vii) of this section state
that an applicant must provide
quantitative data for certain pollutants
known or believed to be present do not
apply to pollutants present in a
discharge solely as the result of their
presence in intake water; however, an
applicant must report such pollutants as
present. When paragraph (g)(7) of this
section requires analysis of pH,
temperature, cyanide, total phenols,
residual chlorine, oil and grease, fecal
coliform (including E. coli), and
Enterococci  (previously known as fecal
streptococcus at § 122.26
(d)(2Xiii)(A)(3)), or volatile organics,
grab samples must be collected for those
pollutants. For all other pollutants, a 24-
hour composite sample, using a
minimum of four (4) grab samples, must
be used unless specified otherwise at 40
CFR Part 136. However, a minimum of
one grab sample may be taken for
effluents from holding ponds or  other
impoundments with a retention  period
greater than 24 hours. In addition, for
discharges other than storm water
discharges, the Director may waive
composite sampling for any outfall for
which the applicant demonstrates that
the use of an automatic sampler  is
infeasible and that the minimum of four
(4) grab samples will be a representative
sample of the effluent being discharged.
Results of analyses of individual grab
samples for any parameter may be
averaged to obtain the daily average.
Grab samples that are not required to be
analyzed immediately (see Table II at 40
CFR 136.3 (e)) may be composited in the
laboratory, provided that container,
preservation, and holding time
requirements are met (see Table  II at 40
CFR 136.3 (e)) and that sample integrity
is not compromised by compositing.
*    *    *    *    *
  (h) * * *
  (4) * * *
  (i) Quantitative data for the pollutants
or parameters listed below, unless
testing is waived by the Director. The
quantitative data may be data collected
over the past 365 days, if they remain
representative  of current operations, and
must include maximum daily value,
average daily value, and number of
measurements taken. The applicant
must collect and analyze samples in
accordance with 40 CFR Part 136. When
analysis of pH, temperature, residual
chlorine, oil and grease, or fecal
coliform (including E. coli), and
Enterococci (previously known as fecal
streptococcus) and volatile organics is
required in paragraphs (h)(4)(i)(A)
through (K) of this section, grab samples
must be collected for those pollutants.
For all other pollutants, a 24-hour
composite sample, using a minimum of
four (4) grab samples, must be used
unless specified otherwise at 40 CFR
Part 136. For a composite sample, only
one analysis of the composite of aliquots
is required. New dischargers must
include estimates for the pollutants or
parameters listed below instead of
actual sampling data, along with the
source of each estimate. All levels must
be reported or estimated as
concentration and as total mass, except
for flow, pH, and temperature.
  (4) * * *
  (viii) Applicants must collect samples
of effluent and analyze such samples for
pollutants in accordance with analytical
methods approved under 40 CFR Part
136 unless an alternative is specified in
the existing NPDES permit. When
analysis of pH, temperature, cyanide,
total phenols, residual chlorine,  oil and
grease, fecal coliform (including E. coli],
or volatile organics is required in
paragraphs (j)(4)(ii) through (iv) of this
section, grab samples must be collected
for those pollutants. For all other
pollutants, 24-hour composite samples
must be used. For a composite sample,
only one analysis of the composite of
aliquots is required.
*****

• 4. Section 122.41 is amended by
revising paragraphs  (j)(4) and (l)(4)(ii) to
read as follows:

§ 122.41  Conditions applicable to all
permits (applicable to State programs, see
§ 123.25).
  (})*  *  *
  (4) Monitoring must be conducted
according to test procedures approved
under 40 CFR Part 136 unless another
method is required under 40  CFR
subchapters N or O.
*****
  0)*  ,  *
  (4)* *  *
  (ii) If the permittee monitors any
pollutant more frequently than required
by the permit using test procedures
approved under 40 CFR Part  136, or
another method required for  an
industry-specific waste stream under 40
CFR subchapters N or O, the  results of
such monitoring shall be included in
the calculation and reporting of the data
submitted in the DMR or sludge
reporting form specified by the Director.

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• 5. Section 12 2.44 is amended by
revising paragraph (i)(l)(iv) to read as
follows:

§122.44  Establishing limitations,
standards, and other permit conditions
(applicable to State NPDES programs; see
§123.25).
*    *    *    *    *
  (i)*
  (0* * *
  (iv) According to test procedures
approved under 40 CFR Part 136 for the
analyses of pollutants or another
method is required under 40 CFR
subchapters N or O. In the case of
pollutants for which there are no
approved methods under 40 CFR Part
136 or otherwise required under 40 CFR
subchapters N or O, monitoring must be
conducted according to a test procedure
specified in the permit for such
pollutants.
PART 136—GUIDELINES
ESTABLISHING TEST PROCEDURES
FOR THE ANALYSIS OF POLLUTANTS

• 6. The authority citation for Part 136
continues to read as follows:
  Authority: Sees. 301, 304(h), 307, and
501(a) Pub. L. 95-217, 91 Stat. 1566, ef seq.
(33 U.S.C. 1251, ef seq.) (The Federal Water
Pollution Control Act Amendments of 1972
as amended by the Clean Water Act of 1977.)

• 7. Section 136.3 is amended as
follows:
                        • a. In paragraph (a) by revising the
                        introductory text and Tables IA, IB, 1C,
                        ID, and IE.
                        • b. In paragraph (a) by adding Table IG
                        after the notes of Table IF.
                        • c. In paragraph (b) by revising
                        references 6,10, and 17, and adding
                        references 63 through 69.
                        • d. By revising paragraphs (c), (d), and
                        (e).

                        § 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, 1C, ID, IE, IF, and IG. In the event
                        of a conflict between the reporting
                        requirements of 40 CFR Parts 122 and
                        1215 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, 1C, ID, IE, IF, and IG. The
                        incorporation by reference of these
                        documents, as specified in paragraph (b)
                        of this section, was approved by the
                        Director of the Federal Register in
                        accordance with 5 U.S.C. 552(a) and 1
                        CFR Part 51. Copies of the documents
                        may be obtained from the sources listed
                        in paragraph (b) of this section. You can
                        get information about obtaining these
                        documents from the EPA Office of
Water Engineering and Analysis
Division at 202-566-1000. Documents
may be inspected at EPA's Water
Docket, EPA West, 1301 Constitution
Avenue, NW., Washington, DC
(Telephone: 202-566-2426); or at the
National Archives and Records
Administration (NARA). For
information on the availability of this
material at NARA, call 202-741-6030,
or go to: http://www.archives.gov/
federal_register/code_ofJedeTal_
regulations/'ibrjocations.html
  These test procedures are
incorporated as they exist on the day of
approval and a notice of any change in
these test procedures will be published
in the Federal Register. The discharge
parameter values for which reports are
required must be determined by one of
the standard analytical test procedures
incorporated by reference and described
in Tables IA, IB, 1C, IE, IF, and IG or by
any alternate test procedure which has
been approved by the Administrator
under the  provisions of paragraph (d)  of
this section and §§ 136.4 and 136.5.
Under certain circumstances (paragraph
(b) or (c) of this section or 40 CFR
401.13) other test procedures may be
used if such other test procedures have
been previously approved by the
Regional Administrator of the Region  in
which the discharge will occur, and the
Director of the State in which such
discharge  will occur does not object to
the use of an additional or alternate test
procedure.
                               TABLE IA.—LIST OF APPROVED BIOLOGICAL METHODS
Parameter and units
Bacteria:
1 Coliform (fecal)
number per 100
ml.
2 Coliform (fecal) in
presence of chlo-
rine, number per
100 mL.
3 Coliform (total)
number per 100
mL.
4 Coliform (total),
in presence of
chlorine, number
per 100 mL.
5 E coli, number
per 100 mL28.
Method 1
Most Probable Number
(MPN), 5 tube 3 dilu-
tion, or
Membrane filter (MF) 2
single step.
MPN 5 tube 3 dilution
or
MF single step6
MPN 5 tube 3 dilution
or
MF2, single step or two
step.
MPN, 5 tube, 3 dilution,
or
MF2 with enrichment
MPN7'9'15, multiple
tube,
EPA
p 1323
p 1243 ... .
p. 1323 ....
p 1243 ....
p 1143
p. 1083 	
p. 1143 	
p 111 3


Standard
methods 18th,
1 9th, 20th Ed.
9221 C or E
9222D ...
9221 C or E
9222 D
9221 B
9222B ....
9221B 	
9222 (B+B 5c)
9221 B.1/
9221 F1214.
Standard
methods online
9221 C or E-99
9222 D-97
9221 C or E-99
9222 D-97
9221 B-99
9222B-97
9221 B-99
9222 (B+B 5c)-
97.
9221B.1-99/
9221 F121".
AOAC,
ASTM,
USGS

B-0050-
85s.


B-0025-
85s.



Other

-------
Federal Register/Vol. 72,  No. 47/Monday, March 12, 2007/Rules and Regulations
11213
          TABLE IA.— LIST OF APPROVED BIOLOGICAL METHODS—Continued
Parameter and units






6. Fecal
streptococci,
number per 100
mL



7. Enterococci,
number per 100
mL28.





Protozoa:
8. Crypto-
sporidiumZB.
9. Giardia28 	
Aquatic Toxicity:
10. Toxicity, acute,
fresh water orga-
nisms, LCso, per-
cent effluent.












1 1 . Toxicity, acute,
estuarine and
marine organisms
of the Atlantic
Ocean and Gulf
of Mexico, LCSO,
percent effluent.







12. Toxicity, chron-
ic, fresh water or-
ganisms, NOEC
or IC25, percent
effluent.






Method 1
multiple tube/multiple
well,

MF two step or

single step
MPN, 5 tube, 3 dilution,



MF2 or

Plate count
MPN7'9 multiple tube,


multiple tube/multiple
well.
MF 2. 6, 7, a, 9^ two step ...
single step or
plate count

Filtration/IMS/FA

Filtration/I MS/FA

Cehodaphnia dubia
acute.


Daphnia puplex and
Daphnia magna acute.
Fathead Minnow,
Pimephales promelas,
and Bannerfin shiner,
Cyprinella leedsi,
acute.
Rainbow Trout,
Oncorhynchus
mykiss, and brook
trout, Salvelinus
fontinalis, acute.
Mysid, Mysidopsis
bahia, acute.





Sheepshead Minnow,
Cyprinodon
variegatus, acute.
Silverside, Menidia
beryllina, Menidia
menidia, and Menidia
peninsulae, acute.
Fathead minnow.
Pimephales promelas.
larval survival and
growth.

Fathead minnow,
Pimephales promelas,
embryo-larval survival
and teratogenicity.
Daphnia, Ceriodaphnia
dubia, survival and re-
production.
EPA



1 1 03 1 20

160321, 160422
p 1393



p 1363
r' ' wu 	
p 1433
rm ' *^




1106 1 2"
160025.
p. 1433.

162226, 162327.

162327.

2002.0 2£>.



2021 .0 29.

2000.0 29.




201 9.0 29.




2007.0 29.






2004.0 29.


2006.0 29.



1 000.0 30.




1001.0 3°.



1 002.0 3°.

Standard
methods 1 8th,
19th, 20th Ed.
9223B13 	


9222B/9222G 19,
9213D.

9230B 	



9230C


9230B 	




9230C
















































Standard
methods online
9223B-9713 	


9222B-97/
9222G19.

9230B-93.



9230C-93


9230B-93.




9230C-93
















































AOAC,
ASTM,
USGS
991. 1511 ....


D5392-
93 10.





B-0055-
855.




D6503-
99 10.
D5259-
92io















































Other
Colilert® 13> 17,
Colilert-
igi»13, 16. 17


mColiBlue-24®1s










Entero-lert*13'23

-------
11214
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
TABLE IA— LIST OF APPROVED BIOLOGICAL METHODS—Continued
Parameter and units

13. Toxicity, chron-
ic, estuarine and
marine organisms
of the Atlantic
Ocean and Gulf
of Mexico, NOEC
or IC25, percent
effluent

<•

Method 1
Green alga,
Selenastrum
capricomutum, growth.
Sheepshead minnow,
Cyprinodon
variegatus, larval sur-
vival and growth.

Sheepshead minnow,
- Cyprinodon
variegatus, embryo-
larval survival and
teratogenicity.
Inland silverside,
Menidia beryllina, lar-
val survival and
growth.
Mysid, Mysidopsis
bahia, survival,
growth, and fecundity.
Sea urchin, Arbacia
punctulata, fertilization.
EPA
1003.0 3°.

1 004.0 31.

1 005.0 31.

1006.031.

1007.031.

1008.03i.

Standard
methods 18th,
19th, 20th Ed.

Standard
methods online

AOAC,
ASTM,
USGS

Other

1 The method must be specified when results are reported.
2 A 0.45-n membrane filter (MF) or other pore siz:e certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
3USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Labora-
tory, U.S. Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.
4 [Reserved]
5USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for
Collection and Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of Interior, Reston, VA.
6 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.
7Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/vol-
umes to account for the quality, character, consistency, and anticipated organism density of the water sample.
8When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncoliform bacteria, or sam-
ples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applica-
bility and comparability of results.
9 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.
i°ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. ASTM International. 100
Barr Harbor Drive, West Conshohocken, PA 19428.
"AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical
Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.
12 The multiple-tube fermentation test is used in 9221 B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-posi-
tive 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.
13These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme p-glucu-
ronidase produced by E. coli.
14After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of
gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supple-
mented in the laboratory with 50 ng/mL of MUG may be used.
15 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® may be enumer-
ated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray® 2000, and the MPN calculated from the table provided by the manufacturer.
i6Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of
incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
17 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray^OOO may be obtained from IDEXX Laboratories, Inc., 1 IDEXX
Drive, Westbrook, ME 04092.
ISA description of the mColiBlue24® test, Total Coliforms and £ coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
19 Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NAMUG media.
20USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli
Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-020.
21USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Esch-
erichia coli Agar ( modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-023.
22 Preparation and use of Ml agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. "New Medium for
the Simultaneous Detection of Total Coliform and Escherichia coli in Water." Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Meth-
od 1604: Total Coliforms and Escherichia coli (E. coll) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (Ml Me-
dium). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA 821-R-02-024.
23A description of the Enterolert® test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.

-------
Federal Register/Vol. 72, No. 47/Monday, March .12, 2007/Rules and Regulations 11215

24 USEPA. 2002. Method 1106.1: Enterooocci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA).
U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-021.
25USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus lndoxyl-|3-D-Glucoside Agar
(mEI). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-022.
26 Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to de-
termine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of
Cryptosporidium. USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of
Water, Washington, DC, EPAr821-R-01-026.
27 Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence
assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simulta-
neous detection of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtra-
tion/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-01-025.
23 Recommended for enumeration of target organism in ambient water only.
29 USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms.
Fifth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/012.
30 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms.
Fourth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/013.
31 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine
Organisms. Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R-02/014.

-------
TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES
Parameter





6. Arsenic— Total, " mg/L 	

Methodology68
Electrometric endpoint or phenol-
phthalein endpoint.
Electrometric or Colorimetric titration
to pH 4.5, manual, or
automatic
Digestion 4 followed by:
AA furnace 	
STGFAA .. . .
ICP/AES36
ICP/MS
Direct Current Plasma (DCP) 36
Cuiorimeific; (Etiuchrome cyanine R)
Manual, distillation (at pH 9.5) e fol-
lowed by:

Electrode 	
Automated phenate or
Automated electrode

Digestion'1 followed by:

STGFAA 	
ICP/AES36
ICP/MS
Digestion4 followed by 	


STGFAA 	
ICP/AES36 	
ICP/MS
Colorimetric (SDDC)
Digestion4 followed by:
AA furnace 	
Reference (method number or page)
EPA 35. 52


310.2 (Rev. '
1974) '.
200.9, Rev. 2.2
(1994).
200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).
350.1, Rev. 2.0
(1993).


350.1 60, Rev. 2.0
(1993).



200.9, Rev. 2.2
(1994).
200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).
206.5 (Issued
1978)'.

200.9, Rev. 2.2
(1994).
200.7, Rev. 4.4
(1994).
200 8 Rev 5 4
(1994).


Standard methods
(18th, 19th)
2310 B(4a) 	
2320 B 	
3111 D
3113 B 	
3120 B


3500-Ai D 	
4500-NH B3 	
4500-NH3C(18th
only).
4500-NH3 C
(19th) and
4500-NH3 E
(18th).
4500-NH3 D or E
(19th) and
4500-NH3 F or
G (18th).
4500-NH3 G
(19th) and
4500-NH3 H
(18th).

3111 B
3113 B 	
3120 B

3114 B 4d
3113 B
3120 B

3500-AsC 	
3111 D
3113 B 	 	
Standard methods
(20th)
2310 B(4a) 	
2320 B .


3120 B


3500-Ai B 	
4500-NH3 B 	
4500-NH3 C
4500-NH3 D or E
4500-NH3 G 	



3120 B



3120 B 	

3500-AsB 	


Standard methods
online
2310 B(4a)-97 	
2320 B-97

3111 D-99
3113 B-99.
3120 B-99


3500-Ai B-01.
4500-NHs B-97 	

4500-NH3 C-97.
4500-NH 3 D or E-
97.
4500-NH3 G-97

3111 B-99.
31 13 B-99.
3120 B-99.
3114 B 4.d-97 	
3113 B-99 	
3120 B-99.
3500-ASB-97 	
3111 D-99 	
3113 B-99 	
ASTM
D1067-92, 02 	
D1067-92, 02 	


D5673-03 	
D4190-94, 99 	
D 1426-98, 03 (A)
D 1426-98, 03 (B).

06919-03.
D5673-03 	
D2972-97, 03 (B)
D2972-97, 03 (C)
D5673-03 	
D2972-97, 03 (A)
D4382-95, 02.
USGS/AOAC/other
I-1020-852
97S.433, 1-1030-
852
I-2030-85 2
1-3051 -85 2
1-4471-9750
993.143
See footnote34
973.493
973. 49 3, I-3520-
852
I-4523-85 2
See footnote 7
993. 143
I-3062-852
I-4063-9840
993. 143
I-3060-85
I-3084-852
                                                                                              to
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                                                                                              a>
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                                                                                              era
                                                                                              o

-------
Federal Register/Vol. 72, No. 47/Monday,  March 12, 2007/Rules and Regulations
              11217


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"k 1
CO CD
q> CD
3> CO




1-309 5-85 2

0 0


M471-9750




993. 143
See footnote3'


i
o
973.44 ,3 p. 17
1 578-78 B
1-311 2-85 2
W471-9750



.
See footnote 3




p. S44.10
1-1 125-85 2
993.303

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1-21 87-85 2

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Digestion4 followed by:
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ICP/AES 	
nr.p nr

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11218
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Federal Register/Vol. 72,  No. 47/Monday, March  12, 2007/Rules and Regulations
11219
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-------
TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter


45 Osmium — Total4 mg/L 	




47. Palladium — Total,4 mg/L 	










51 Platinum — Total 4 mg/L













57 Residue — Volatile mg/L



59. Ruthenium— Total,4 mg/L 	

60. Selenium — Total,4 mg/L 	


Methodology68
Ion Chromatography 	
CIE/UV . . .
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EPA 35. 52
300 0 Rev 2 1
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252.2 (Issued
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253 2 ' (Issued
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420 1 1 (Rev
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365.3 ' (Issued
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d number or page)
Standard methods
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-------
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TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued
Parameter
72 Titanium — Total 4 mg/L 	
73 Turbidity NTU63

75. Zinc -Total", mg/L 	
Methodology58
ICP/AES
Digestion " followed by:
AA direct aspiration 	

DCP 	
Nephelometric 	
Digestion 4 followed by:
AA furnace 	
ICP/AES . . .
ICP/MS 	
DCP or 	
Colorimetric (Gallic Acid) 	
Digestion4 followed by:
AA furnace 	
ICP/AES36 	
ICP/MS 	
DCP 3e or



Reference (method number or page)
EPA 35. 52
200.7, Rev. 4.4
(1994).
283.2 1 (Issued
1978).
180.1, Rev. 2.0
(1993).

200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).


289.2 ' (Issued
1978).
200.7, Rev. 4.4
(1994).
200.8, Rev. 5.4
(1994).


Standard methods
(18th, 19th)
3111 D 	

2130 B 	
3111 D

3120 B 	

3500-V D 	
3111 B or C
3120 B 	

3500-Zn E.
3500-Zn F 	
Standard methods
(20th)


2130 B 	


3120 B 	

3500-V B 	
3120 B 	

3500-Zn B 	
Standard methods
online
3111 D-99.
2130 B-01 	
3111 D-99.
3120 B-99 	

3500-V B-97.
3111 BorC-99 	
3120 B-9958 	

3500-Zn B-97 	
ASTM

D1889-94, 00 	
D3373-93, 03.
05673-03
D4190-94, 99 	
D1691-95, 02 (A
or B).
D5673-03 	
D4190-94, 99 	

USGS/AOAC/other
See footnote34
1-3860-85?
1-4471-9750
993. 143
See footnote34
974. 27 3, p. 37 9, I-
3900-85 2
(-4471-9750
993. 143
See footnote34
See footnote33
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  Table 1B Notes:
  1 "Methods for Chemical Analysis of Water and Wastes," Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI), EPA-600/4-79-020 (NTIS PB 84-128677), Revised
March 1983 and 1979 where applicable.
  2Fishman, M. J., et al. "Methods for Analysis of  Inorganic Substances in Water and Fluvial Sediments," U.S. Department of the Interior, Techniques of Water-Resource Investigations of the U.S. Geological Survey,
Denver, CO, Revised 1989, unless otherwise stated.
  3"Official Methods of Analysis of the Association of Official Analytical Chemists," Methods Manual, Sixteenth Edition, 4th Revision, 1998.
  4 For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material
and to break down organic-metal complexes (to  convert the analyte to a detectable form for colorimetric analysis).  For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as
specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the
sample be taken to dryness. For direct  aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and  hydrochloric acids) digestion is preferred prior to analysis.  The approved total recover-
able  digestion is described as Method 200.2 in Supplement I of  "Methods for the Determination of Metals in Environmental Samples"  EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8,
and 200.9 from  the same Supplement.  However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA  graphite fur-
nace atomic  absorption methods, mercury by cold vapor atomic  absorption,  the noble metals and titanium  by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced
method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or the
EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (e.g.,  CEM microwave digestion, which may be used with certain analytes
as indicated in Table IB); the total recoverable  digestion procedures in EPA  Methods 200.7, 200.8, and 200.9 may be used for those respective methods.  Regardless of the digestion procedure,  the results of the anal-
ysis after digestion procedure are reported as "total" metals.
  5 Copper sulfate may be used in place of mercuric sulfate.
  6 Manual distillation is not required if comparability data on representative  effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to re-
solve any controversies.
  7Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY
10523.
  8The approved method is that cited in "Methods for Determination of  Inorganic Substances in Water and Fluvial Sediments", USGS TWRI, Book 5, Chapter A1 (1979).
  9American National Standard on Photographic Processing Effluents, April  2, 1975. Available from ANSI, 25 West 43rd St., New York, NY 10036.
  '""Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency," Supplement to the Fifteenth Edition of Standard Methods tor the Examination of Water and Wastewater
(1981).
  "The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
  12Carbonaceous biochemical oxygen demand  (CBOD5) must not be confused with the traditional BOD5 test method which  measures "total BOD." The addition of the nitrification inhibitor is not a procedural option,
but must be included to report  the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a dis-
charger's permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
  I3OIC Chemical Oxygen Demand Method, Oceanography International Corporation,  1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.
  l4Chemical Oxygen Demand, Method 8000,  Hach Handbook of Water Analysis, 1979, Hach Chemical Company,  P.O. Box 389, Loveland, CO 80537.
-------

   15The back titration method will be used to resolve controversy.
   16Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph for the Orion residual chlorine
method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
   17The approvad method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
   18National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971.
   '"Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis,  1979, Hach Chemical Company,  P.O. Box 389, Loveland, CO 80537.
   20When using a method with block digestion, this treatment is not required.
   21 Hydrogen-ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976,  Bran &  Luebbe (Technicon) Autoanalyzer II.  Bran & Luebbe Analyzing Technologies, Inc., Elmsford,  NY
10523.
   22lron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
   "Manganese, Periodate Oxidation Method,  Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.
   24Wershaw, R.  L.,ef a/., "Methods for Analysis of Organic Substances in Water," Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised  1987) p 14            %
   25Nitrogen, Nitrite,  Method  8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.                                                                                                             • •
   2eJust prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
   27The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted at a pH of 10.0±0.2. The approved methods are given on pp
576-81  of the 14th Edition: Method 510A for distillation,  Method 510B for the manual colorimetric procedure, or Method 510C for the manual spectrometric procedure.
   28R.F. Addison  and R.  G. Ackman,  "Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography," Journal of Chromatography, Vol. 47, No.3, pp. 421-426, 1970.
   29Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chlo-
ride are relatively  insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of
sample should be diluted  to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner.  For levels of silver below 1 mg/L the approved method is satisfactory.
   30The approved method is  that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition.
   31 For samples known or suspected to contain high levels of silver (e.g.,  in excess  of 4 mg/L), cyanogen iodide should be  used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by add-
ing 4.0 mL of concentrated NH^OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution  of I2 to  50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH  of the
digestate to >7 to  prevent the formation ofHCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen
Book 1, Chapter D1, 1975.                                                                                                                                                                            2
  33Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.                                                          -
  34"Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes,  Method AES0029," 1986—Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge
Parkway, Franklin,  MA 02038
  36Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC method for arsenic are provided in Appendix D of this part titled,
"Precision and Recovery Statements for Methods for Measuring Metals."
  36 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. "Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals",  CEM Corporation      S
P.O. Box 200, Matthews, NC 28106-0200, April  16, 1992. Available from the CEM Corporation.                                                                                                                O
  37When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.                                                                           "
  38Only use n-hexane extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664A). Use of other extraction
solvents (e.g., those in the 18th and 19th  editions) is prohibited.
  39Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.
  40Nitrogen, Total Kieldahl, Method PA1-DK02  (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.                         ^
  41 Nitrogen, Total Kjejdanl, Method PAI-DK03  (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, Ol Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.                                   £•
  42Method  1664,  Revision A  "n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated fT-Hexane Extractable Material (SGT-HEM;  Non-polar Material) by Extraction and Gravimetry" EPA-821-
R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161.
  43USEPA. 2001. Method 1631, Revision E, "Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic  Fluorescence Spectrometry" September 2002, Office of Water,  U.S. Environmental Protection
Agency (EPA-821-R-02-024). The application of clean techniques described in EPA's draft Method  1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels (EPA-821-R-96-011) are
recommended to preclude contamination at low-level, trace metal determinations.
  "Available Cyanide, Method OIA-1677, "Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry," ALPKEM,  A Division of Ol Analytical, P.O. Box 9010, College Station, TX 77842-9010.
  45"Methods of Analysis by the U.S.  Geological Survey National Water Quality Laboratory—Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method," Open File Report (OFR) 00-170.           Q
  46"Methods of Analysis by the U.S.  Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry," Open  File  Report (OFR)     o
93-449.
  47"Methods of Analysis by the U.S. Geological Survey  National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry," Open File  Report (OFR) 97-
198.
  48"Methods of Analysis by the U.S.  Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Di-     _
alysis" Open File Report (OFR) 92-146.                                                                                                                                                                CD
  ""Methods of Analysis  by the U.S. Geological Survey  National Water Quality Laboratory—Determination  of Arsenic and Selenium in Water and Sediment  by Graphite Furnace-Atomic Absorption  Spectrometry"     "
Open File Report (OFR) 98-639.                                                                                                                                                                       g
  50"Methods of Analysis by the U.S.  Geological Survey  National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission  Spectrometry and     "
Inductively Coupled Plasma-Mass Spectrometry," Open File Report (OFR) 98-165.
  51 "Methods of Analysis by the U.S.  Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment,"  Open File Report (OFR) 93-125.
  52AII EPA methods, excluding EPA Method 300.1, are published in  "Methods for the Determination of Metals in Environmental Samples," Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL-CI),    _cp
EPA/600/R-94/111, May 1994; and "Methods for the Determination of Inorganic Substances in Environmental Samples," NERL-CI, EPA/600/R-93/100, August,  1993. EPA Method  300.1 is available  from http://
www.epa.gov/safewater/methods/pdfs/met300.pdf.
  53Styrene  divinyl benzene beads (e.g. AMCO-AEPA-1  or equivalent) and stabilized formazin (e.g., Hach StablCal™ or equivalent) are acceptable substitutes for formazin.                                           £2.
  54Method  D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and  Chromate Electrolyte," available from Waters Corp 34 Maple
St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
  55 Kelada-01, "Kelada Automated Test Methods for Total Cyanide, Acid  Dissociable Cyanide, and Thiocyanate," EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information Service (NTIS), 5285
Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. The toll free telephone number is: 800-553-6847. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified
if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method,  provided
that the QC acceptance criteria are met.
  56QuikChem Method 10-204-00-1-X, "Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis" is available from Lachat
Instruments 6645 W. Mill Road, Milwaukee, Wl 53218, Telephone: 414-358-4200.
  57 When using  sulfide removal test procedures described in Method 335.4, reconstitute paniculate that is filtered with the sample prior to distillation.
  6sUnless otherwise stated, if the language  of this table specifies a sample digestion and/or distillation "followed by" analysis with a method, approved digestion and/or distillation are required prior to analysis.            ..^
  59Method 245.7, Rev. 2.0, "Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry," February 2005, EPA-821-R-05-001, available  from the U.S. EPA Sample Control Center (operated by CSC), 6101     N5
Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100,  Fax: 703-461-8056.
-------
  60The use of EDTA may decrease method sensitivity in some samples. Analysts may omit EDTA provided that all method specified quality control acceptance criteria are met.

  61 Samples analyzed for available cyanide using Methods OIA-1677 or D6888-04 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because

the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand ex-
change reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples.
bo
to
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-------
 Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and  Regulations
11227
TABLE 1C.—-LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS
Parameter '
1 . Acenaphthene 	
2. Acenaphthylene 	
3. Acrolein 	
4. Acrylonitrile 	
5 Anthracene
6. Benzene
7 Bsnzidine
8. Benzo(a)anthracene 	
9. Benzo(a)pyrene 	
10. Benzo(b)fluoranthene ..
1 1. Benzo(g,h,i) perylene ..
12. Benzo(k) fluoranthene
13. Benzyl chloride ...
14. Benzyl butyl phthalate
15. Bis(2-chloroethoxy)
methane.
16. Bis(2-chloroethyl) ether
17. Bis(2-ethylhexyl)
phthalate.
18. Bromodichloro-meth-
ane.
19. Bromoform 	
20. Bromomethane 	
21. 4-Bromophenyl phenyl
ether.
22. Carbon tetrachloride ...
23. 4-Chloro-3-methyl phe-
nol.
24. Chlorobenzene ..
25. Chloroethane ....
26. 2-Chloroethylvinyl
ether.
EPA method number2-7
GC
610
610
603
603
610
602
610
610
610
610
610
606
611
611
606
601
601
601
611
601
604
601, 602
601
601
GC/MS
625, 1625B 	
625, 1625B 	
624", 1624B.
624", 1624B.
625, 1625B 	
624 1624B
6255, 1625B ..
625, 1625B 	
625, 1625B 	
625, 1625B 	
625, 1625B 	
625, 1625B 	
625 1625B
625 1625B
625 1625B
625, 1625B
624, 1624B 	
624, 1624B
624, 1624B 	
625, 1625B 	
624 1624B
625, 1625B
624, 1624B
624 1624B
624 1624B

HPLC
610
610
610
605
610
" 610
610
610
610














Other approved methods
Standard Methods
[Edition(s)]
6440 B[18th, 19th,
20th],
6410 B, 6440 B,
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6200 B [20th] and
6210 B
[18th, 19th], 6200
C [20th] and
6220 B
[18th,19th],
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
(18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B[18th, 19th,
20th].
6410 B [18th, 19th,
20th],
6410 B [18th, 19th,
20th].
6410 B[18th, 19th,
20th].
6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210
B [18th, 19th).
6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210
B [18th, 19th].
6200 C [20th] and
6230 B [18th,
19th], 6200 B
[20th] and 6210
B [18th, 19th].
6410 B[18th, 19th,
20th],
6200 C [20th] and
6230 B [18th,
19th].
6410 B, 6420 B
[18th, 19th, 20th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220
B [18th, 19th],
6200 C [20th]
and 6230 B
[18th, 19th].
6200 B [20th] and '
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
Standard Methods
Online

6410 B-00 	
6410 B-00 	
6200 B and C-97.
6410 B-00 	
6410 B-00 	
6410 B-00 	
6410 B-00
6410 B-00

6410 B-00 	
6410 B-00
6410 B-00
6410 B-00 	
6200 B and C-97.
6200 B and C-97.
6200 B and C-97.
6410 B-00 	
6200 C-97
64 10 B-00, 6420
B-00.
6200 B and C-97
6200 B and C-97.
6200 B and C-97.
ASTM
D4657-92 (99) 	
D4657-92 (99) 	
D4657-92 (99) 	
D4657-92 (99) 	
04657-92 (99) 	
D4657-92 (99) 	
D4657-92 (99) 	
D4657-92 (99) 	









Other
See footnote9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote 3, p.1
See footnote9, p.
27
See footnote9, p.
27
See footnote8, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130: See foot-
note6, p. S102
See footnote9, p.
27
See footnote6, p.
27
See footnote 9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130
See footnote 6, p.
27
See footnote3, p.
130
-------
11228
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
     TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
27 Chloroform
28 Chloromethane
29. 2-Chloronaph-thalene
30 2-Chlorophenol
31. 4-Chlorophenyl phenyl
ether.
32 Chrysene
33. Dibenzo(a,h)an-
thraoene.
34. Dibromochloro-meth-
ane.
35. 1,2-Dichloro-benzene ..
36. 1,3-Dichloro-benzene ..
37. 1,4-Dichloro-benzene ..
38. 3,3-Dichloro-benzidine
39. Dichlorodifluoro-meth-
ane.
40. 1,1-Dichloroethane 	
41. 1,2-Dichloroethane 	
42. 1,1-Dichloroethene 	
43. trans-1,2-Dichloro-
ethene.
44. 2,4-Dichlorophenol 	
45. 1 ,2-Dichloro-propan8 ..
46. cis-1,3-Dichloro-
propene.
EPA method number2'7
GC
601
601
612
604
611
610
610
601
601, 602
601, 602
601, 602
601
601
601
601
601
604
601
601
GC/MS
624 1624B 	
624 1624B ...
625 1625B
625, 1625B ....
625, 1625B ....
625, 1625B ....
625, 1625B 	
624 1624B
624 1625B
624 1625B
624 1625B
625, 1625B 	
624, 1624B 	
624 1624B
624, 1624B 	
624, 1624B 	
625, 1625B 	
624 1624B
624 1624B

HPLC





610
610



605








Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th],
6200 B [20th] and
6210 B [18th,
19th] 6200 C
[20th] and 6230
B[18th, 19th].
6410 B[18th, 19th,
20th].
6410 B, 6420 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6200 B [20th] and
6210 B [18th,
19th] 6200 C
[20th] and 6230
B [18th, 19th],
6200 C [20th] and
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 C [20th] and
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 C [20th] and
6220 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6410 B [18th, 19th,
20th].
6200 C [20th] and
6230 B [18th,
19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th],
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th).
6410 B, 6420 B
[18th, 19th, 20th]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
Standard Methods
Online
6200 B and C-97
6200 B and C-97.
6410 B-00
64106(00, 6420
B-00.
6410 B-00
6410 B-00 	
6410 B-00
6200 B and C-97.
6200 C-97 	
6200 C-97
6200 C-97
64 10 B-00.
6200 C-97.
6200 B and C-97
6200 B and C-97
6200 B and C-97
6200 B and C-97
6410 B-00, 6420
B-00.
6200 B and C-97
6200 B and C-97
ASTM




D4657-92 (99) 	
D4657-92 (99) 	



Other
See footnote3, p.
130
See footnote9, p.
27
See footnote 9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote 9, p.
27
See footnote9, p.
.27
See footnote 9, p.
27
See footnote 9, p.
27
-------
       Federal Register/Vol.  72, No. 47/Monday, March  12, 2007/Rules and Regulations
11229
TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
47. trans-1,3-Dichloro-
propene.
48. Diethyl phthalate
49. 2,4-Dimethylphenol 	
50. Dimethyl phthalate 	
51. Di-n-butyl phthalate 	
52. Di-n-octyl phthalate 	
53. 2,3-Dinitrophenol 	
54. 2,4-Dinitrotoluene 	
55. 2,6-Dinitrotoluene 	
56 Epichlorohydrin
57. Ethylbenzene 	
58. Ruoranthene 	
59. Fluorene 	
60. 1,2,3,4,6,7,8-
Heptachloro-
dibenzofuran.
61. 1,2,3,4,7,8,9-
Heptachloro-
dibenzofuran.
62. 1,2,3,4,6,7,8-
Heptachlorodibenzo-p-
dioxin.
63. Hexachlorobenzene ....
64. Hexachloro-butadiene
65. Hexachlorocyclo-
pentadiene.
66. 1,2,3,4,7,8-
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8-
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9-
Hexachlorodibenzofuran.
69. 2,3,4,6,7,8-
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-
Hexachlorodibenzo-p-
dioxin.
71. 1,2,3,6,7,8-
Hexachlorodibenzo-p-
dioxin.
72. 1,2,3,7,8,9-
Hexachlorodibenzo-p-
dioxin 1613B10.
73. Hexachloroethane 	
74. ldeno(1,2,3-cd) pyrene
75. IsophoronG
76. Methylene chloride 	
77. 2-Methyl-4,6-
dinitrophenol.
78. Naphthalene 	

EPA method number2'7
GC
601
606
604
606
606
606
604
609
609
602
610
610

612
612
612





612
610
609
601
604
610
GC/MS
624, 1624B ....
625 1625B
625 1625B
625 1625B
625, 1625B 	
625, 1625B
625 1625B
625, 1625B 	
625 1625B

624, 1624B .. .
625, 1625B 	
625, 1625B 	
1613B10.
1613B10.
1613B'0.
625 1625B
625, 1625B 	
6256, 1625B ..
1613B10.
16138'°.
1613B1".
1613B10.
1613B10.
1613B10.
1613B'0.
625 1625B
625, 1625B 	
625 1625B
624, 1624B 	
625, 1625B
625, 1625B 	
HPLC










610
610


610

610
Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6410 B [18th, 19th,
20th].
6410 B, 6420 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th],
6410 B [18th, 19th,
20th],
6410 B[18th, 19th,
20th],
6410 B, 6420 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th).
6410 B [18th, 19th,
20th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220
B [18th, 19th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th].
6410 B[18th, 19th,
20th],
6410 B [18th, 19th,
20th],
6410 B[18th, 19th,
20th],
6410 B, 6440 B
[18th, 19th, 20th].
6410 B [18th, 19th,
20th].
6200 C [20th] and
6230 B [18th,
19th],
6410 B, 6420 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th].
Standard Methods
Online
6200 B and C-97.
6410 B-00
6410 B-00, 6420
B-00.
64' 10 B-00
6410 B-00
6410 B-00
64106-00,6420
B-00.
6410 B-00 	
6410 B-00

6200 B and C-97
6410 B-00 	
6410 B-00
6410 B-00
6410 B-00 	
6410 B-00 	
6410 B-00 	
6410 B-00 	
6410 B-00
6200 C— 97
6410 B-00, 6420
B-00.
6410 B-00

ASTM










D4657-92 (99) 	
D4657-92 (99) 	



D4657-92 (99) 	




Other
See footnote8, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 3, p.
130; See foot-
note 6, p. S102
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote8, p.
27
See footnote9, p.
27
See footnote9, p.
27
See footnote3, p.
130
See footnote9, p.
27
See footnote °, p.
27
-------
11230
Federal Register/Vol.  72, No. 47/Monday, March 12, 2007/Rules and Regulations
     TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
79 Nitrobenzene 	 	
80. 2-Nitrophenol 	
81 4-Nitrophenol 	 	 	
82. N-
Nitrosodimethylamine.
83. N-Nitrosodi-n-propyl-
amine.
84. N-
Nitrosodiphenylamine.
85.
Octachlorodibenzofuran.
86. Octachlorodibenzo-p-
dioxin.
87. 2,2'-Oxybis(2-
chloropropane) [also
known as bis(2-
ohloroisopropyl) ether].
88 PCB-1016
89. PCB-1221 	
90. PCB-1232 	
91. PCB-1242 	
92 PCB-1248 	
93 PCB-1254
94 PCB-1260
95. 1 ,2,3,7 ,8-Pentachloro-
dibenzofuran .
96. 2,3,4,7,8-Pentachloro-
dibenzofuran .
97. 1,2,3,7,8,-
Pentachlorodibenzo-p-
dioxin.
98. Pentachlorophenol 	
99. Phenanthrene 	
1 00 Phenol
101. Pyrene 	
102. 2,3,7,8-Tetra-
chlorodibenzofuran.
103. 2,3,7,8-Tetra-
chlorodibenzo-p-dioxin.
104. 1 , 1 ,2,2-Tetra-chloro
ethane .
105. Tetrachloroethene 	
106 Toluene
107. 1,2,4-Trichloro-ben-
zene.
EPA method number2.7
GC
609
604
604
607
607
607

611
608
608
608
608
608
608
608
604
610
604
610

601
601
602
612
GC/MS
625, 1625B 	
625 1625B
625, 1625B 	
6255, 1625E ...
6255, 1625B ...
6255, 1625B ...
1613B10'.
1613B10.
625, 1625B ....
625 .
625
625
625
625.
625 	
625
1613B<°.
1613B'0.
1613B'0.
625, 1625B 	
625, 1625B 	
625 1625B
625, 1625B 	
1613B10.
613, 625 5a,
161 3B10.
624 1624B
624 1624B .
624, 1624B ...
625, 1625B 	
HPLC










610
610



Other approved methods
Standard Methods
[Edition(s)]
6410 B [18th, 19th,
20th],
6410 B, 6420 B
[18th, 19th, 20th].
6410 B, 6420 B
[18th, 19th, 20th].
6410 B[18th, 19th,
20th],
6410 B [18th, 19th,
20th].
6410 B[18th, 19th,
20th].
6410 B[18th, 19th,
20th].
6410 B[18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th],
6410 B [18th, 19th,
20th].
6410 B [18th, 19th,
20th].
6410 B, 6630 B
[18th, 19th, 20th].
6410 B, 6630 B
[18th, 19th, 20th].
6410 B, 6440 B
[18th, 19th, 20th],
6410 B, 6420 B
[18th, 19th, 20th],
6410 B, 6440 B
[18th, 19th, 20th],
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6220
B [18th, 19th].
6410 B[18th, 19th,
20th],
Standard Methods
Online
6410 B-00 	
6410 B-00, 6420
B-00.
6410 B-00, 6420
B-00.
6410 B-00
6410 B-00 	
6410 B-00 	
6410 B-00.
6410 B-00 	
6410 B-00
6410 B-00
6410 B-00 .
6410 B-00 	
6410 B-00 	
6410 B-00 	
6410 B-00
6410 B-00, 6420
B-00.
6410 B-00
6200 B and C-97
6200 B and C-97
6200 B and C-97.
6410 B-00 	

ASTM
D4657-92 (99) 	











D4657-92 (99) 	
D4657-92 (99) 	



Other
See footnote 9, p.
27
See footnote9, p.
27
See footnote8, p.
27
See footnote 9, p.
27
See footnote0, p.
27
See footnote 9, p.
27
See footnote 3, p.
43; See foot-
note a
See footnote 3, p.
43; See foot-
note8
See footnote3, p.
43; See foot-
note8
See footnote3, p.
43; See footnote
8
See footnote 3, p.
43; See footnote
8
See footnote 3, p.
43; See footnote
8
See footnote 3, p.
140; See foot-
note 9, p. 27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 9, p.
27
See footnote 3, p.
130
See footnote 3, p.
130
See footnote 3, p.
130; See foot-
note 9, p. 27
-------
                 Federal  Register/Vol.  72,  No.  47/Monday,  March  12,  2007/Rules and Regulations
11231
        TABLE 1C.—LIST OF APPROVED TEST PROCEDURES FOR  NON-PESTICIDE ORGANIC COMPOUNDS—Continued
Parameter '
108. 1,1,1-Triohloro-ethane
1 09. 1,1 ,2-Trichloro-ethane
1 10. Trichloroethene 	
111. Trichlorofluoro-meth-
ana.
112. 2,4,6-Triohlorophenol
1 13. Vinyl chloride 	

EPA method number2-7
GC
601
601
601
601
604
601
GC/MS
624, 1624B 	
624, 1624B 	
624, 1624B
624 	
625 1625B
624, 1624B

HPLC

6200 B [20th]
and 6210 B
[18th, 19th],
6200 C [20th]
and 6230 B
[18th, 19th]




Other approved methods
Standard Methods
[Edition(s)]
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B[18th, 19th].
6200 B and C-97
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B [18th, 19th].
6200 B [20th] and
6210 B [18th,
19th], 6200 C
[20th] and 6230
B[18th, 19th].
6410 B, 6420 B
[18th, 19th, 20th].
6200 B [20th] and
6210 B [18th,
19th], £6200 C
[20th] and 6230
B[18th, 19th].
Standard Methods
Online
6200 B and C-97.
6200 B and C-97.
6200 B and C-97.
6410 B-00, 6420
B-00.
6200 B and C-97.
ASTM
See footnote3, p.
130.

Other
See footnote9, p.
27
  'All parameters are expressed in micrograms per liter (ng/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/L).
  2The full text of Methods 601-613, 624, 625, 1624B, and  1625B, are given at Appendix A, "Test Procedures for Analysis of Organic Pollutants," of this Part 136.
The full text of Method 1613B is incorporated by reference into this Part 136  and is available from the National Technical Information  Services as stock  number
PB95-104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, "Defini-
tion and Procedure for the Determination of the Method Detection Limit," of this Part 136.
  3"Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater," U.S. Environmental Protection Agency,
September, 1978.
  •* Method 624 may be extended to screen samples for Acrolein and Acrylonitrile. However, when they are known to be present, the preferred method for these two
compounds is Method 603 or Method 1624B.
  5Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they are
known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.
  5a625, screening only.
  6 "Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency," Supplement to the Fifteenth Edition of Standard Meth-
ods for the Examination of Water and Wastewater (1981).
  'Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624B,
and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-
going basis must spike and analyze 10% (5% for methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory
data quality in accordance with Sections 8.3 and 8.4 of these methods.  When the recovery of any parameter falls outside the warning limits, the analytical results for
that parameter in the unspiked sample are suspect. The results should  be reported, but cannot be used to demonstrate regulatory compliance. These quality control
requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
  8"Organochlorine Pesticides and PCBs in Wastewater Using  Empore™ Disk"  3M Corporation Revised 10/28/94.
  9USGS Method 0-3116-87 from "Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Con-
stituents in Water and Fluvial Sediments," U.S. Geological Survey, Open File Report 93-125.
  '"Analysts may use Fluid Management Systems, Inc. PowerPrep system in place of manual cleanup provided that the analysis meet the requirements of  Method
1613B (as specified in Section 9 of the method) and permitting authorities.


                             TABLE  ID.—LIST OF APPROVED TEST PROCEDURES FOR  PESTICIDES 1
Parameter
1 . Aldrin

2 Ametryn
3. Aminocarb 	
4. Atraton 	
5 Atrazine
6. Azinphos methyl 	
7. Barban
8. a-BHC . . ..

9. p-BHC

Method
GC
GC/MS
GC
TLC ...
GC .
GC
GC 	
TLC
GC
GC/MS
GC
GC/MS 	
EPAs.'
608
625






608
625 5
608
625 6
Standard Methods
18th, 19th, 20th Ed.
6630 B & C
6410 B ..






6630 B & C
6410 B
6630 C
6410 B 	
Standard Methods
Online

6410 B-00







6410 B-00

64 10 B-00.
ASTM
D3086-90
D5812-96 (2002) '..






D3086-90
05812-96(02) 	
D3086-90
05812-96(02) 	
Other

27; See footnote 8

pS68
See footnote3 p 94' See footnote6
p. S16
See footnote3 p 831 See footnote6
p. S68
See footnote3 p 83' See footnote6
p. S68; See footnote6
See footnote3 p 25' See footnote6,
p. S51
See footnote 3 p 1 04' See footnote 6
p. S64
See footnote3 p 7' See footnote8

See footnote 8

-------
11232
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
                TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued
Parameter
10 5-BHC

1 1 y-BHC (Lindane)


1 3 Carbaryl

1 5 Chlordane

17 2 4-D
18 4 4'-DDD

19 4 4'-DDE
20 4 4'-DDT
21 DemQton-O
22 Demeton-S
23 Oi37innn 	
24 Dicamba 	


27 Dioofol
28 Dieldrin


30 Disulfoton



33 Endosulfan II


35 Endrin


37 Ethion
38 Fenuron 	






43 Linuron 	


Method
GC 	
GC/MS 	
GC
GC/MS
GC
TLC
GC
GC
GC/MS 	
TLC
GC
GC
GC/MS
GC
GC/MS 	
GC
GC/MS 	
GC
GC .
GC 	
GC 	
GC
GC
GC 	
GC
GC/MS
GC
GC 	
TLC
GC
GC/MS 	
GC
GC/MS
GC
GC/MS 	
GC
GC/MS 	
GC
GC/MS 	
GC
TLC 	
TLC
GC
GC/MS
GC
GC/MS
GC
GC 	
GC

EPA"
608
625 5
608
625



608
625

608
625
608
625
608
625






603
625



603
625 5
603
625 5
603
625
603
625 5
603
625



603
625
603
625




Standard Methods
18th, 19th, 20th Ed.
6630 C 	
6410 B 	
6630 B & C
6410 B 	
6630 B


6630 B& C
6410 B 	
6640 B
6630 B & C
6410 B ... .
6630 B & C
6410 B 	
6630 B & C
6410 B 	




6630 B & C

6630 B & C
6410 B



6630 B & C
6410 B 	
6630 B & C
6410 B
6630 C
6410 B 	
6630 B & C
6410 B 	




6630 B& C 	
6410 B
6630 B&C
6410 B 	


6630 C ... .

Standard Methods
Online

6410 B-00,

6410 B-00




64 10 B-00.


6410 B-00

6410 B-00.
6410 B-00.







6410 B-00



"
6410 B-00.

6410 B-00

6410 B-00.
6410 B-OO.





6410 B-00

6410 B-00




ASTM
D3086-90 	
05812-96(02) 	
D3086-90
05812-96(02) 	
D3086-90
05812-96(02) 	

03086-90 .. .
05812-96(02) 	

D3086-90
05812-96(02) 	
03086-90
05812-96(02) 	
03086-90
05812-96(02) 	





03086-90, 	
05812-96(02).




03086-90
05812-96(02) 	
03086-90
05812-96(02) 	

D3086-90
05812-96(02) 	




D3086-90 	
05812-96(02) .. .
03086-90 .
05812- 96(02) 	




Other
See footnote 8

See footnote3 p 7' See footnote4 p
27; See footnote8
See footnote 3 p 7
See footnote 3 p 94 See footnote 6
p. S60
See footnote4 p 271 See footnote6
p. S73
See footnote3 p 7' See footnote4 p
27; See footnote8
See footnote 3 p 1 04' See footnote 6
p. S64.
See footnote 3 p 115' See footnote 4
p. 40
See footnote3 p 7' See footnote4 p
27; See footnote 8
See footnote3 p 7' See footnote4 p
27; See footnote a
See footnote3 p 7~ See footnote4 p
27; See footnote8
See footnote3 p 25- See footnote6
p. S51
See footnote3 p 25' See footnote6
p. S51
See footnote3, p. 25; See footnote4,
p. 27; See footnote6, p. S51
See footnote3, p. 115
See footnote4 p 27' See footnote6
p. S73
See footnote3 p 7

See footnote3 p 7- See footnote4 p
27; See footnote8
See footnote4 p 27- See footnote6
p. S73
See footnote3, p. 25; See footnote6
p. S51
See footnote3, p. 1041 See footnote6
p. S64
See footnote 3 p 7' See footnote 4 p
27; See footnote8
See footnote3 p 7' See footnote8

See footnote8
See footnote3 p 71 See footnote4 p
27; See footnote8
See footnote8

See footnote4, p 27' See footnote6
p. S73
See footnote3, p. 104; See footnote6,
p. S64
See footnote 3 p 1 04J See footnote 6
p. S64
See footnote3, p. 7; See footnote4, p.
27; See footnote 8
See footnote3 p 71 See footnote4 p
27; See footnote6, p S73; See
footnote8
See footnote4, p. 27; See footnote6,
p. S73
See footnote3, p. 104; See footnote6,
p. S64
See footnote3, p. 25; See footnote4,
p. 27; See footnote6, p. S51
-------
                   Federal  Register/Vol.  72,  No.  47/Monday,  March  12,  2007/Rules  and Regulations
11233
                         TABLE ID.—LIST OF  APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued
Parameter
45 Methiocarb
46 Methoxy-chlor
47 Mexacar-batG
48 Mirex
49 Monuron
50 Monuron-TCA
51 Nuburon
52. Parathion methyl
53, Parathion ethyl .. . .
54. PCNB 	
55 Perthane
56 Prometon
57 Prometryn
F,R Prnpa7Jr|A
59 Propham
60 Propoxur
61 Secbumeton
62 Siduron
63. Simazine 	
64 Strobane
65. Swep 	
66 245-T
67 2 4 5-TP (Silvex)
68. Terbuthylazine
69 Toxaphene
70 Trifluratin

Method
TLC
GC
TLC
GC
TLC
TLC
TLC
GC .
GC
GC . ..
GC
GC
GC
GC
TLC
TLC
TLC
TLC
GC
GC
TLC 	
GC
GC
GC
GC
GC/MS 	
GC

EPA 2.'
























608
625

Standard Methods
18th, 19th, 20th Ed.

6630 B & C

6630 B & C



6630 C 	
6630 C 	
6630 B & C 	









6630 B & C

6640 B
6640 B

6630 B & C
6410 B 	
6630 B

Standard Methods
Online

























6410 B-00.

ASTM

D3086-90
05812-96(02).







D3086-90
05812-96(02).












03086-90
05812-96(02).

Other
See footnote3, p. 94; See footnote6,
p. S60
See footnote3 p 7' See footnote4, p.
27; See footnote 8
See footnote3 p 941 See footnote6
p.S60
See footnote3 p 7' See footnote4 p.
27
See footnote3 p 104' See footnote6
p. S64
See footnote 3 p 1 04" See footnote 6
p. S64
See footnote 3 p 1 04" See footnote 6,
p. S64
See footnote3, p. 25; See footnote4,
p. 27
See footnote3, p. 25; See footnote4,
p. 27
See footnote3, p. 7
See footnote 4 p 27
See footnote3 p 83' See footnote6
p. S68; See footnote9
See footnote 3 p 83' See footnote 6
p. S68; See footnote9
See footnote3 p 83' See footnote6
p. S68; See footnote9
See footnote 3 p 1 04' See footnote e,
p. S64
See footnote3 p 94' See footnote6
p. S60
See footnote3 p 83' See footnote6
p. S68
See footnote 3 p 1 04' See footnote 6
p. S64
See footnote3, p. 83; See footnote6,
p. S68; See footnote9
See footnote 3 p 7
See footnote3, p. 104; See footnote6,
p. S64
See footnote3 p 1 15' See footnote4
p. 40
See footnote3 p 1 15' See footnote4
p. 40
See footnote3 p 83' See footnote6
p. S68
See footnote 3 p 7' See footnote 4 p
27; See footnote8
See footnote3 p 7' See footnote9

  1 Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, where entries are listed by chemical name.
  2The full text of Methods 608 and 625 are given at Appendix A, 'Test Procedures for Analysis of Organic Pollutants," of this Part 136. The standardized test procedure to be used to de-
termine the method detection  limit (MDL) for these test procedures is given at Appendix B, "Definition and Procedure for the Determination of the Method Detection Limit," of this Part 136.
  3"Methods tor  Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesti
EPA publication includes thin-layer chromatography (TLC) methods.
                                                                          sticides in Water and Wastewater," U.S. Environmental Protection Agency, September 1978. This
  ""Methods for Analysis of Organic Substances in Water and Fluvial Sediments," Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3 (1987).
  5The method may be extended to include cc-BHC. y-BHC. endosulfan I, endosutfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.
  6 "Selected Analytical Methods Approved and Cited by the United states Environmental Protection Agency." Supplement to the Fifteenth Edition of Standard Methods for the Examination of
Water and Wastewater (1981).
  'Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 (See Appendix  A of this Part 136) in
accordance with procedures given in Section 8.2  of each of these methods. Additionally, each laboratory, on an on-going basis,  must spike and analyze 10% of all samples analyzed with
Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods.  When the recovery of
any parameter falls outside the warning limits, the analytical  results for  that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to dem-
onstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
  8"Organochlorine Pesticides and PCBs in Wastewater Using Empore™ Disk", 3M Corporation. Revised 10/28/94.
  9USGS Method 0-3106-93 from "Methods of Analysis by the U.S.  Geological Survey National Water Quality Laboratory—Determination of Triazine and Other Nitrogen-containing Com-
pounds by Gas Chromatography wrth Nitrogen Phosphorus Detectors" U.S. Geological  Survey Open File Report 94-37.


                                 TABLE IE.—LIST OF APPROVED RADIOLOGIC  TEST TEST  PROCEDURES
Parameter and units
1 . Alpha-Total, pCi per
liter.
2. Alpha-Counting
error, pCi per liter.
3. Beta-Total, pCi per
liter.
Method
Proportional or scin-
tillation counter.
Proportional or scin-
tillation counter.
Proportional counter

Reference (method number or page)
EPA1
900 0
Appendix B ..
900.0 	

Standard Meth-
ods 18th, 19th,
20th Ed.
7110 B
7110 B
7110 B 	

Standard Meth-
ods Online
7110 B-00 	
7110 B-00
71 1 0 B-00

ASTM
D1943-90, 96 ....
D1 943-90, 96 ....
D1890-90, 96 ....
USGS2
pp. 75 and 78 3
p. 79
pp. 75 and 78 3
-------
11234
Federal Register/Vol.  72,  No. 47/Monday, March  12,  2007/Rules  and Regulations
                  TABLE IE.—LIST OF APPROVED RADIOLOGIC TEST TEST PROCEDURES—Continued
Parameter and units
4. Beta-Counting error,
pCi.
5. (a) Radium Total
pCi per liter.
(b) Ra, pCi per liter ....
Method
Proportional counter ...
Proportional counter
Scintillation counter ....
Reference (method number or page)
EPA1
Appendix B ..
9030
903.1 	 ;
Standard Meth-
ods 18th, 19th,
20th Ed.
7110 B
7500-Ra B
7500-Ra C 	
Standard Meth-
ods Online
7110 B-00
7500-Ra B-01 ....
7500-Ra C-01 ....
ASTM
D1 890-90, 96 	
D2460-90, 97 	
D3454-91. 97 	
USGS2
p. 79
D. 81
  1 Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agen-
cy, August 1980.
  2Fishman, M. J. and Brown, Eugene, "Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters," U.S. Geological Survey,
Open-File Report 76-177 (1976).
  3The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore,
the two results must be added to obtain the "total."
                           TABLE  IG.—TEST METHODS FOR  PESTICIDE ACTIVE INGREDIENTS
EPA Survey
Code
8
12
16
17
22
25
26
27
30
31 	
35
39
41
45
52
53
54
55
58
60
62
68
69
69
70
73
75
76
80
82
84
86
90
103
107
1 10
1 12
1 13
1 18
1 19
123
124
125
126
127
132
133
138
140
144
148
150
154
156 	
Pesticide name
Triadimefon 	 	

2 4-D1 2 4— D Salts and Esters [2 4— Dichloro-phenoxyacetic acid]
2 4— DB1 2 4— DB Salts and EstGrs [2 4— Dichlorophenoxybutyric acid] 	
Mevinphos . 	 	


MCPA- MCPA Salts and Esters [2-Methyl-4-chlorophenoxyacetic acid]
Dichlorprop; Dichlorprop Salts and Esters [2-(2,4-Dichlorophenoxy) propionic acid] 	
MCPP; MCPP Salts and Esters [2-(2-Methyl-4-chlorophenoxy) propionic acid] 	
TCMTB [2-(Thiocyanomethylthio) benzo-thiazole] 	 	


Metribuzin 	 	
Acephate 	



Ametryn 	






Captafol 	 	



Chlorothalonil 	 . 	 . 	





DCPA [Dimethyl 2 3 5 6-tetrachloro-terephthalate] 	 	
Dinoseb ... . 	
Dioxathion 	
Nabonate [Disodium cyanodithio-imidocarbonate] 	 . . 	

Endothall .. . . 	

Ethalfluralin 	 	




Glyphosate [N(Phosphonomethyl) glycine] 	 	
Heptachlor 	




Methomvl 	
CAS No.
43121-43-3
62-73-7
94-75-7
94-82-6
7786-34-7
21725-46-2
1918-16-7
94-74-6
120-36-5
93-65-2
21564-17-O
23950-58-5
709-98-8
21087-64-9
30560-19-1
50594-66-6
15972-60-8
116-06-3
834-12-8
1912-24-9
17804-35-2
314-40-9
1 689-84-5
1689-99-2
23184-66-9
2425-06-1
63-25-2
1 563-66-2
2675-77-6
1 897-45-6
961-11-5
2921-88-2
51630-58-1
333-41-5
298-00-0
1861-32-1
88-85-7
78-34-2
138-93-2
330-54-1
145-73-3
72-20-8
55283-68-6
563-12-2
13194-48-4
60168-88-9
55-38-9
1071-83-6
76-44-8
33820-53-0
330-55-2
121-75-5
10265-92-6
16752-77-5
EPA Analytical Method No.(s)
507/633/525 'l/1 656
1657/507/622/525 1
1658/515 1/615/5152/555
1658/515 1/615/5152/555
1657/507/622/525 1
629/507
1656/508/608 1/525 1
1658/615/555
1658/515.1/615/515 2/555
1658/615/555
637
525 1/507/633 1
632 1/1656
507/633/5251/1656
1656/1657
515 1/515 2/555
505/507/645/525 1/1656
531 1
507/619/525.1
505/507/619/525 1/1656
631
507/633/525 1/1656
1625/1661
1656
507/645/525 1/1656
1656
531 1/632/553
531.1/632
1656/508/608 1/525 1
508/6082/525 1/1656
1657/507/622/525 1
1657/508/622
1660
1657/507/614/622/525 1
1657/614/622
508/6082/525 1/515.1/515.2/1656
1658/515.1/615/5152/555
1657/614.1
630.1
632/553
548/548.1
1656/505/508/608/617/525 1
1 1656/627 See footnote 1
1657/614/614 1
1657/507/622/525 1
507/633 1/525 1/1656
1657/622
547
1 656/505/508/608/6 1 7/525. 1
1 656/627
553/632
1657/614
1657
531.1/632
-------
              Federal Register/Vol. 72, No.  47/Monday, March 12, 2007/Rules and Regulations
                                                                   11235
                    TABLE IG.—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS—Continued
EPA Survey
Coda
158 	
172 	
1 73 ...
175 	
178 	
182 	
183 	
185
186 	
192
197 	
203 	
204 	
205
206
208 	
212 	
218 	
219
220 	
223 	
224 	
226
230 ...
232 	
236 	
239 	
241 	
243 	
252
254
255
256 . .
257
259 	
262 	
263 	
264 	
268 	
Pesticide name
Methoxychlor 	 • 	 	
Nabam 	 	
Naled 	 . .
Nortlurazon 	 .. 	
Benfluralin 	
FGhsulfothion 	 . 	
Disulfoton 	 	 	 	
Phosmet
Azinphos Methyl 	
Organo-tin pesticides
Bolstar 	 	
Parathion 	 ....
Pendimethalin 	
Pentachloronitrobenzene
Pentachlorophenol
Permethrin 	 	
Phorate 	
Busan 85 [Potassium dimethyldithiocarbamate] .... 	
Busan 40 [Potassium N-hydroxymethyl-N-methyldithiocarbamate]
KN Methyl [Potassium N-methyl-dithiocarbamate] 	
Prometon 	 , , . .... ...
Prometryn 	 	 	 	
Propazins . , .
Pyrethrin 1 ... 	 . ., 	 	
Pyrethrin II 	 	 	
DEF [S S S-Tributyl phosphorotrithioate] ... 	
Simazine 	
Carbam-S [Sodium dimethyldithiocarbanate] 	
Vapam [Sodium methyldithiocarbamate] 	
Tebuthiuron
Terbacil 	
Terbufos . ...
Terbuthylazine 	 	 	 	

Dazomet 	 	 	
Toxaphene 	
Merphos [Tributyl phosphorotrithioate] 	
Trifluralin 	
Ziram [Zinc dimethvldithiocarbarnatel 	
CAS No.
72-43-5
142-59-6
300-76-5
27314-13-2
1861-40-1
115-90-2
298-04-4
732-11-6
86-50-0
12379-54-3
35400-43-2
56-38-2
40487-42-1
82-68-8
87_86-5
52645-53-1
298-02-2
128-03-0
51026-28-9
137-41-7
1610-18-0
7287-19-6
1 39-4Q-2
121-21-1
121-29-9
78-48-8
122-34-9
128-04-1
137-42-8
34014-18-1
5902-51-2
13071-79-9
5915-41-3
886-50-0
533-74-4
8001-35-2
150-50-5
1 582-09-8
137-30-4
EPA Analytical Method No.(s)
1656/505/508/608.2/617/525 1
630/630. 1
1657/622
507/645/525.1/1656
11656/1627
1657/622
1657/507/614/622/525 1
1657/622 1
1657/614/622
lnd-01/200 7/200 9
1657/622
1657/614
1656
1656/608 1/617
625/1625/515 2/555/515 1/ 525 1
6082/508/525 1/1656/1660
1657/622
630/630 1
630/630 1
630/630 1
507/619/525 1
507/619/525 1
507/619/525 1/1656
1660
1660
1657
505/507/6 1 9/525. 1 / 1 656
630/630. 1
630/630 1
507/525 1
507/633/525 1/1656
1657/507/614 1/525 1
619/1656
507/619/525 1
630/630 1/1659
1656/505/508/608/617/525 1
1657/507/525.1/622
1656/508/617/627/525 1
630/630.1
 1 Monitor and report as total Trifluralin.
  (b)***

References, Sources, Costs, and Table
Citations
*****
  (6) American Public Health
Association. 1992,1995, and 1998.
Standard Methods for the Examination
of Water and Wastewater. 18th, 19th,
and 20th Edition (respectively).
Available from: American Public Health
Association, 1015 15th Street, NW.,
Washington, DC 20005. Standard
Methods Online are available through
the Standard Methods Web site (http://
www.standardmethods.org). Tables IA,
IB, 1C, ID, IE.
*    *    *    *    *
  (10) ASTM International. Annual
Book of ASTM Standards, Water, and
Environmental Technology, Section 11,
Volumes 11.01 and 11.02, 1994, 1996,
1999, Volume 11.02, 2000, and
individual standards published after
2000. Available from: ASTM
International, 100 Barr Harbor Drive,
P.O. Box C700, West Conshohocken, PA
19428-2959, or http://www.astm.org.
Tables IA, IB, 1C, ID, and IE.
  (17) AOAC-International. Official
Methods of Analysis of AOAC-
International, 16th Edition, (1995).
Available from: AOAC-International,
481 North Frederick Avenue, Suite 500,
Gaithersburg, MD 20877. Table IB, See
footnote 3.
*****
  (63) Waters Corporation. Method
D6508, Rev. 2, "Test Method for
Determination of Dissolved Inorganic
Anions in Aqueous Matrices Using
Capillary Ion Electrophoresis and
Chromate Electrolyte," available from
Waters Corp, 34 Maple Street, Milford,
MA 01757, Telephone: 508/482-2131,
Fax: 508/482-3625, Table IB, See
footnote 54.
  (64) Kelada-01, "Kelada Automated
Test Methods for Total Cyanide, Acid
Dissociable Cyanide, and Thiocyanate,"
EPA 821-B-01-009 Revision 1.2,
August 2001 is available from National
Technical Information Service (NTIS),
5285 Port Royal Road, Springfield, VA
22161 [Order Number PB 2001-108275].
Telephone: 800-553-6847. Table IB, See
footnote 55.
  (65) QuikChem Method 10-204-00-
1—X, "Digestion and Distillation of Total
Cyanide in Drinking and Wastewaters
using MICRO DIST and Determination
of Cyanide by Flow Injection Analysis"
Revision 2.2, March 2005 is available
from Lachat Instruments 6645 W. Mill
Road, Milwaukee, WI 53218, Telephone:
414-358-4200. Table IB, See footnote
56.
  (66) "Methods for the Determination
of Metals in Environmental Samples,"
Supplement I, National Exposure Risk
Laboratory-Cincinnati (NERL-CI), EPA/
600/R-94/111, May 1994; and "Methods
for the Determination of Inorganic
Substances in Environmental Samples,"
NERL-CI, EPA/600/R-93/100, August,
1993 are available from National
Technical Information Service (NTIS),
5285 Port Royal Road, Springfield, VA
22161. Telephone: 800-553-6847. Table
IB.
  (67) "Determination of Inorganic Ions
in Drinking Water by Ion
Chromatography," Rev. 1.0,1997 is
available from from http://www.epa.gov/
safetwater/methods/metSOO.pdf. Table
IB.
  (68) Table IG Methods are available in
"Methods For The Determination of
Nonconventional Pesticides In
-------
11236
Federal Register/Vol.  72,  No. 47/Monday, March  12, 2007/Rules and  Regulations
Municipal and Industrial Wastewater,
Volume I," EPA 821-R-93-010A,
August 1993 Revision I, and "Methods
For The Determination of
Nonconventional Pesticides In
Municipal and Industrial Wastewater,
Volume II," EPA 821-R-93-010B
(August 1993) are available from
National Technical Information Service
(NTIS), 5285 Port Royal Road,
Springfield, VA 22161. Telephone: 800-
553-6847.
  (69) Method 245.7, Rev. 2.0, "Mercury
in Water by Cold Vapor Atomic
Fluorescence Spectrometry," February
2005, EPA-821-R-05-001, available
from the U.S. EPA Sample Control
Center (operated by CSC), 6101
Stevenson Avenue, Alexandria, VA
22304, Telephone: 703-461-8056. Table
IB, See footnote 59.
  (c) Under certain circumstances, the
Regional Administrator or the Director
in the Region or State where the
discharge will occur may determine for
                        a particular discharge that additional
                        parameters or pollutants must be
                        reported. Under such circumstances,
                        additional test procedures for analysis
                        of pollutants may be specified by the
                        Regional Administrator, or the Director
                        upon recommendation of the Alternate
                        Test Procedure Program Coordinator,
                        Washington, DC.
                          (d) Under certain circumstances, the
                        Administrator may approve additional
                        alternate test procedures for nationwide
                        use, upon recommendation by the
                        Alternate Test Procedure Program
                        Coordinator, Washington, DC.
                          (e) Sample preservation procedures,
                        container materials, and maximum
                        allowable holding times for parameters
                        are  cited in Tables I A, IB, 1C, ID, IE, IF,
                        and IG are prescribed in Table II.
                        Information in the table takes
                        precedence over information in specific
                        methods or elsewhere.  Any person may
                        apply for a variance from the prescribed
                        preservation techniques, container
materials, and maximum holding times
applicable to samples taken from a
specific discharge. Applications for
variances may be made by letters to the
Regional Administrator in the Region in
which the discharge will occur.
Sufficient data should be provided to
assure such variance does not adversely
affect the integrity of the sample. Such
data will be forwarded by the Regional
Administrator, to the Alternate Test
Procedure Program Coordinator,
Washington, DC, for technical review
and recommendations for action on the
variance application. Upon receipt of
the recommendations from the Alternate
Test Procedure Program Coordinator,
the Regional Administrator may grant a
variance applicable to the specific
discharge to the applicant. A decision to
approve or deny a variance will be made
within 90 days of receipt of the
application by the Regional
Administrator.
                TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES
Parameter number/name
Table IA— Bacterial Tests:
1-5. Coliform, total, fecal, and E. coli 	
6 Fecal streptococci 	
7 Enterococci 	
Table lA — Protozoan Tests:
9 Giardia 	
Table IA — Aquatic Toxicity Tests:
Table IB — Inorganic Tests:
1 . Acidity 	

4. Ammonia 	
9 Biochemical oxygen demand 	


14 Biochemical oxygen demand carbonaceous 	


17 Chlorine total residual 	
21. Color 	
23-24 Cyanide total or available (or CATC) 	
25 Fluoride 	 : 	

28 Hydrogen ion (pH) .... 	
31 43 Kjeldah! and organic N 	
Table IB—Metals: 7
35. Mercurv (CVAA1 	
Container1
PA, G 	
PA, G 	
PA, G 	
LDPE' field filtration
LDPE; field filtration ...
P FP G
P, FP, G 	
P, FP, G 	
P, FP, G 	 	
P, FP, G 	
P FP or Quartz
p FP G 	
P FP G 	
P FP G 	
P FP G
P, G 	
P, FP, G 	
P FP G 	
P 	
p FP G 	
P, FP, G 	
P, FP, G 	
P FP G
P, FP, G 	
Preservation2-3
Cool, <10°C,
0.0008%
Na2S2035.
Cool, <10°C
0.0008%
Na:.S203<>.
Cool, <10 °C,
0.0008%
Na2S2O35.
0-8 °C
0-8 °C 	
Cool £6 °C 1e
Cool, 56 °C18 ..
Cool, S6 °C18 .
Cool, 56 °C18,
H2SO4 to
pH<2.
Cool S6 °C 18
HNOi to pH<2

Cool S6 °C 1S
Cool £6 °C18
H2SO4 to
pH<2.
None required
Cool, 56 °C18 ..
Cool, £6 °C'8
NaOH to
pH>126, re-
ducing
agent5.
None required
HNOi or
H2SO4 to
pH<2.
None required
Cool, £6°C18,
H2SO4 to
pH<2.
Cool <6 °C 18
pH = 9.3-
9.7 ».
HNOri to pH<2
Maximum holding time4
6 hours
6 hours
6 hours
96 hours21
96 hours21
36 hours
14 days
1 4 days
28 days
48 hours
6 months
28 days
48 hours
28 days
28 days
Analyze within 15 minutes
48 hours
14 days
28 days
6 months
Analyze within 15 minutes.
28 days
28 days
28 days
-------
   Federal Register/Vol. 72, No. 47/Monday, March 12,  2007/Rules and Regulations
11237
TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued
Parameter number/name
35 Mercury (CVAFS)

3, 5-8, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51, 52, 58-60, 62, 63,
70-72, 74, 75. Metals, except boron, chromium VI, and mercury.
38. Nitrate 	
39. Nitrate-nitrite 	
40. Nitrite 	
41 Oi! and grease
42. Organic Carbon 	
44. Orthophosphate 	
46. Oxygen, Dissolved Probe 	
47. Winkler 	
48. Phenols 	
49 Phosphorous (elemental)
50 Phosphorous total . .
53 Residue, total 	
54, Residue, Filterable 	 	
55 Residue Nonfilterable (TSS)
56 Residue Settleable
57. Residue, Volatile 	
61. Silica 	
64 Specific conductance . ..
65. Sulfate 	
66. Sulfide 	



















67. Sulfite 	
68. Surfactants 	
69. Temperature 	
73. Turbidity 	
Table 1C — Organic Tests8
13, 18-20, 22, 24-28, 34-37, 39-43
Purgeable Halocarbons.
6, 57, 106. Purgeable aromatic hydroca
3 4. Acrolein and acrylonitrile
23, 30, 44, 49, 53, 77, 80, 81, 98, 100,
7 38 Benzidines" 12 . ..
14, 17, 48, 50-52. Phthalate esters"
82-84. Nitrosamines" 14 ....
88-94 PCBs" 	
54, 55, 75, 79. Nitroaromatics and isop



45-47, 56, 76, 104, 105, 108-111, 113.
rbons 	

112. Phenols" 	




"torone "

Container1
FP, G; and FP-lined
cap 17.
P FP G .
P, FP, G 	
P, FP, G ....
P, FP, G 	
G
P, FP, G 	
P, FP, G 	
G, Bottle and top 	
G, Bottle and top 	
G
G
P FP G
P FP G
P, FP, G ....
P, FP, G 	
P FP G
P, FP, G ....
P or Quartz 	
P FP G
P, FP, G 	
P, FP, G 	
P, FP, G 	
P, FP, G 	
P FP G
P, FP, G ....
G, FP-lined septum ...
G, FP-lined septum ...
G, FP-lined septum ...
G, FP-lined cap 	
G, FP-lined cap 	
G, FP-lined cap 	
G, FP-lined cap 	
G, FP-lined cap 	
G, FP-lined cap 	
Preservation2.3
5 mLA 12N
HCI or 5 mL7
L BrCI '7.
HNO3 to pH<2,
or at least 24
hours prior to
analysis 19.
Cool, 56 °C18 ..
Cool, 56°C18,
H2SO4 to
pH<2.
Cool, £6°C'8 ..
Cool to  ..
Cool, 56 °C18,
add zinc ace-
tate plus so-
dium hydrox-
ide to pH>9.
None required
Cool, 56 °C18 ..
None required
Cool, 56 °C18
Cool, 56°C'e,
0.008%
Na2S2O35.
Cool, 56 °C 18,
0.008%
Na2S2035,
HCI to pH 29.
Cool, 56 °C'»,
0.008%
Na2S2O35,
pH to 4-5 '°.
Cool, 56 °C<8,
0.008%
Na2S2O3s.
Cool, 56 °C18,
0.008%
Na2S2O35.
Cool, 56 °C'8 ..
Cool, 56 °C 18,
store in dark,
0.008%
Cool, 56 "C18 ..
Cool, 56 °C'S,
store in dark,
0.008%
Na2S2O35.
Maximum holding time4
90 days '7
6 months
48 hours
28 days
48 hours
28 days
28 days
Filter within 15 minutes; Ana-
lyze within 48 hours
Analyze within 15 minutes
8 hours
28 days
48 hours
28 days
7 days
7 days
7 days
48 hours
7 days
28 days
28 days
28 days
7 days
Analyze within 15 minutes
48 hours
Analyze
48 hours
14 days
14 days9
14 days10
7 days until extraction, 40 days
after extraction
7 days until extraction 13
7 days until extraction, 40 days
after extraction
7 days until extraction, 40 days
after extraction
1 year until extraction, 1 year
after extraction
7 days until extraction, 40 days
after extraction
-------
11238
Federal  Register/Vol.  72,  No.  47/Monday,  March  12,  2007/Rules  and  Regulations
                TABLE  II—REQUIRED CONTAINERS,  PRESERVATION TECHNIQUES,  AND  HOLDING TIMES—Continued
Parameter number/name
1, 2, 5, 8-12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons11
15 16 21 31 87 Haloethers11
29 35-37 63-65 107. Chlorinated hydrocarbons11 	
60-62, 66-72, 85, 86, 95-97, 102, 103. CDDs/CDFs".
Aqueous Samples' Field and Lab Preservation .
Solids and Mixed-Phase Samples' Field Preservation
Tissue Samples: Field Preservation .. . 	 	
Solids Mixed-Phase and Tissue Samples1 Lab Preservation
Table ID— Pesticides Tests:
1 70 Pesticides ' 1
Table IE— Radiological Tests:
1—5 Alpha beta and radium 	 	

Container1
G, FP-lined cap 	
G FP-lined cap
G, FP-lined cap 	
G
G
G 	
G
G, FP-lined cap 	
P FP, G

Preservation2'3
Cool, S6 °C 12 with sodium hydroxide solution (e.g.. 5 % w/v), refrigerate as specified, and analyze within 48 hours. Otherwise, to  extend the holding time to
14 days and mitigate interferences, treat the sample immediately using any or all of the  following techniques, as necessary, followed by adjustment of the sample pH to >12 and refrigeration
as specified. There may be  interferences that are not mitigated by approved procedures.  Any procedure for removal or suppression of an interference may be employed, provided the labora-
tory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g., ferric ferrocyanide)  or a strong cyanide complex (e.g., cobalt cyanide) are more  accurately measured if
the laboratory holds the sample at room temperature and pH >12 for a minimum of  4 hours  prior to analysis, and performs UV  digestion or dissolution under alkaline (pH-12) conditions, if
necessary.
  (1)  Sulfur: To remove  elemental sulfur (S8), fitter the sample  immediately. If the filtration time will exceed 15 minutes, use a larger filter or a method that  requires a  smaller sample volume
(e.g.  EPA Method  335.4 or Lachat Method 01). Adjust the pH  of the filtrate to >12 with NaOH, refrigerate the  filter and filtrate, and ship or transport to the laboratory. In the laboratory,  ex-
tract the filter with  100 mL of 5% NaOH solution for a minimum of Z hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the  initial filtrate, lower trra
pH to approximately 12  with concentrated hydrochloric or sulfuric acid, and analyze  the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate
from the solids, test the  sample with and without the solids procedure if a tow detection limit for cyanide is necessary. Do not use the solids  procedure if a higher cyanide concentration is ob-
tained w|thout it. Alternatively, analyze the filtrates from the sample  and the solids separately, add  the amounts  determined (in ug or mg), and divide by the original sample volume to obtain
the cyanide concentration.
   (2) Sulfide: If the sample contains sulfide as  determined by lead acetate paper, or  if sulfide is known or suspected to be present, immediately conduct one of the volatilization treatments or
the precipitation treatment  as  follows:  Volatilization—Headspace expelling.  In  a fume  hood or well-ventilated area, transfer 075 Itter of'sample to  a 4.4-L  collapsible  container (e.g.,
Cubitainer™). Acidify with concentrated hydrochloric acid to pH <2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel the headspace into the fume hood or
open area by collapsing the container without  expelling the  sample.  Refill the headspace by expanding the container.  Repeat expelling a total of five  headspace volumes. Adjust the pH to
>12,  refrigerate, and ship or transport to the laboratory.  Scaling to a smaller or larger sample volume must  maintain the air to sample volume  ratio. A larger volume of air  will  result in  too
great a loss of cyanide (> 10%).  Dynamic stripping:  In a fume  hood  or well-ventilated area, transfer 0.75  liter of sample to a container of the material specified and acidify wrth concentrated
hydrochloric acid to pH <2.  Using a  calibrated air sampling pump or flowmeter. purge the acidified sample into the fume  hood or  open area through a fritted glass aerator at a flow rate of
2.25 L/min for 4 minutes. Adjust the pH to >12. refrigerate, and ship  or transport to the laboratory. Scaling to a  smaller or larger sample volume  must maintain the air to sample volume ratio.
A larger volume of air will result in too great a toss  of cyanide (>10%). Precipitation: If  the sample contains paniculate matter that would be removed by filtration, filter the  sample prior to
treatment to assure that cyanide associated with the paniculate matter is included in  the measurement. Ship or transport the filter to the laboratory. In the  laboratory, extract the filter with  100
mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12
with concentrated hydrochloric  or sulfuric acid, and analyze the combined filtrate. Because the detection  limit for cyanide  will be increased  by dilution  by the filtrate from  the solids, test the
sample with and without the solids procedure if a tow detection limit for cyanide  is necessary. Do not  use the  solids procedure if a higher cyanide concentration is obtained without it. Alter-
natively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in ug or mg), and divide by the original sample volume to obtain the cyanide concentra-
tion.  For removal of sulfide  by precipitation, raise the pH of the sample to >12 with NaOH solution, then add approximately 1 mg of  powdered cadmium  chloride for each mL of sample.  For
example, add approximately  500 mg to a 500-mL sample. Cap and shake the container to mix. Allow  the precipitate to settle and test the  sample with lead acetate paper. If necessary,  add
cadmium chloride but avoid adding  an excess. Finally, filter through 0.45 micron filter. Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the labora-
tory,  extract the filter with  100 mL of 5% NaOH solution tor a minimum  of 2 hours. Filter the extract  and discard the solids. Combine the  5%  NaOH-extracted filtrate with the  initial filtrate,
lower the  pH to approximately 12 with concentrated  hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate form the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids  procedure If a higher  cyanide concentra-
tion is obtained without it. Alternatively,  analyze the filtrates from the  sample and the solids separately, add the  amounts determined (in (g or mg), and divide by the original sample volume to
obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM  D6888),  it may be necessary to increase the  ligand-exchange reagent to offset any excess of cadmium
chloride.
   (3) Sulfite,  thiosulfate, or  thiocyanate: If sulfite, thiosulfate,  or thiocyanate is known or suspected to  be  present, use  UV digestion with a glass coil (Method  Kelada-01) or ligand exchange
(Method OIA-1677) to preclude cyanide loss or positive interference.
-------
                 Federal  Register/Vol.  72,  No. 47/Monday, March 12,  2007/Rules  and Regulations
                                                                                    11239
  (4) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be present, treat the sample with 20 ml of 3.5% ethylenediamine solution per liter
of sample.
  (5) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the distillation flask, a reduction in the pH of the absorber solution, and incomplete cya-
nide spike recovery. When significant carbonate is present, adjust the pH to > 12 using calcium hydroxide instead of sodium hydroxide. Allow the precipitate to settle and decant or filter the
sample prior to analysis (also see Standard Method 4500-CN B 3 d)
  (6) Chlorine, hypochlonte, or other oxidant: Treat a sample  known or suspected to contain chlorine, hypochlorite, or other oxidant as directed  in footnote 5.
  'For dissolved metals, filter grab samples within 15 minutes of collection and  before adding preservatives. For a composite sample collected with an automated sampler (e.g., using a 24-
hour composite sampler; see 40 CFR 122.21 (g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of collection and before adding preservatives. If it
is known or suspected that dissolved sample integrity will be  compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between
dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically.
  'Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
  * If the sample is not adjusted to pH 2. then the sample must be analyzed within seven days of sampling.
  10The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.
  11 When the extractable analytes of concern fall within a single chemical  category, the specified preservative and maximum holding times should be observed tor optimum safeguard of
sample integrity (i.e., use all necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two or more chemical categories, the sample may be pre-
served by cooling to <6 °C, reducing residual chlorine with 0.008% sodium  thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for
seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
thiosulfate reduction), and footnotes 12.  13 (regarding the analysis of benzidine).
  12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine.
  13 Extracts may be stored up to 30 days at <0 °C.
  "For the analysis of diphenylnitrosamine. add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours of sampling.
  15The pH adjustment may be performed upon receipt at the laboratory and  may  be omitted if the samples  are  extracted within 72 hours of collection. For the analysis of aldrin, add
0.008%  Na2S2p3.
  16Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still present when the samples arrive at the laboratory. However, even if ice is present
when the samples arrive, it is necessary to  immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the iso-
lated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a
variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature.
  "Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved with
BrCI or HCI solution within 48 hours of sample collection.  The time to preservation may be extended to 28 days '
-------
11240
Federal Register/Vol. 72, No. 47/Monday,  March 12, 2007/Rules and Regulations
criteria of the approved method at this
part.
  (5) Method-defined Analyte means an
analyte defined solely by the method
used to determine the analyte. Such an
analyte may be a physical parameter, a
parameter that is not a specific
chemical, or a parameter that may be
comprised of a number of substances.
Examples of such analytes include
temperature, oil and grease, total
suspended solids, total phenolics,
turbidity, chemical oxygen demand, and
biochemical oxygen demand.
  (6) QC means "quality control."
  (b) Method Modifications.
  (1) Allowable Changes. Except as set
forth in paragraph (b)(3) of this section,
an analyst may modify an approved test
procedure (analytical method) provided
that the chemistry of the method or the
determinative technique is not changed,
and provided that the requirements of
paragraph (b)(2) of this section are met.
  (i) Potentially acceptable
modifications regardless of current
method performance include changes
between automated and manual discrete
instrumentation; changes in the
calibration range (provided that the
modified range covers any relevant
regulatory limit); changes in equipment
such as using similar equipment from a
vendor other than that mentioned in the
method (e.g., a purge-and-trap device
from OIA rather than Tekmar), changes
in equipment operating parameters such
as changing the monitoring wavelength
of a colorimeter or modifying the
temperature program for a specific GC
column; changes to chromatographic
columns (treated in greater detail in
paragraph (d) of this section); and
increases in purge-and-trap sample
volumes (provided specifications in
paragraph (e) of this section are met).
The changes are only allowed provided
that all the requirements of paragraph
(b)(2) of this section are met.
  (ii) If the characteristics of a
wastewater matrix prevent efficient
recovery of organic pollutants and
prevent the method from meeting QC
requirements, the analyst may attempt
to resolve the issue by using salts as
specified in Guidance on Evaluation,
Resolution, and Documentation of
Analytical Problems Associated with
Compliance Monitoring (EPA 821-B-
93-001, June 1993), provided that such
salts do not react with or introduce the
target pollutant into the sample (as
evidenced by the analysis of method
blanks, laboratory control samples, and
spiked samples that also contain such
salts) and that all requirements  of
paragraph (b)(2) of this section are met.
Chlorinated samples must be
                        dechlorinated prior to the addition of
                        such salts.
                          (iii) If the characteristics of a
                        wastewater matrix result in poor sample
                        dispersion or reagent deposition on
                        equipment and prevents the analyst
                        from meeting QC requirements, the
                        analysts may attempt to resolve the
                        issue by adding an inert surfactant (i.e.
                        a surfactant that will not affect the
                        chemistry of the method), which may
                        include Brij-35 or sodium dodecyl
                        sulfate (SDS), provided that such
                        surfactant does not react with or
                        introduce the target pollutant into the
                        sample (as evidenced by the analysis of
                        method blanks, laboratory control
                        samples, and spiked samples that  also
                        contain such surfactant) and that all
                        requirements of paragraph fb)(2) of this
                        section are met. Chlorinated samples
                        must be dechlorinated prior to the
                        addition  of such surfactant.
                          (2) Requirements. A modified method
                        must produce equivalent performance to
                        the approved methods for the analyte(s)
                        of interest, and the equivalent
                        performance must be documented.
                          (i) Requirements for Establishing
                        Equivalent Performance
                          (A) If the approved method contains
                        QC tests and QC acceptance criteria, the
                        modified method must use these QC
                        tests and the modified method must
                        meet the QC acceptance criteria. The
                        Analyst may only rely on QC tests and
                        QC acceptance criteria in a method if it
                        includes wastewater matrix QC tests
                        and QC acceptance criteria (e.g., as
                        matrix spikes) and both initial (start-up)
                        and ongoing QC tests and QC
                        acceptance criteria.
                          (B) If the approved method does not
                        contain QC tests and QC acceptance
                        criteria, or if the QC tests and QC
                        acceptance criteria in the method  do not
                        meet the requirements of paragraph
                        (b)(2)(i)(A) of this section, the analyst
                        must employ QC tests specified in
                        Protocol for EPA Approval of Alternate
                        Test Procedures for Organic and
                        Inorganic Analytes in Wastewater and
                        Drinking Water (EPA-821-B-98-002,
                        March 1999) and meet the QC
                        provisions specified therein. In
                        addition, the Analyst must perform on-
                        going QC tests, including assessment of
                        performance of the modified method on
                        the sample matrix (e.g., analysis of a
                        matrix spike/matrix spike duplicate pair
                        for every twenty samples of a discharge
                        analyzed), and analysis of an ongoing
                        precision and recovery sample and a
                        blank with each batch of 20 or fewer
                        samples.
                          (C) Calibration must be performed
                        using the modified method and the
                        modified method must be tested with
                        every wastewater matrix to which it will
be applied (up to nine distinct matrices;
as described in the ATP Protocol, after
validation in nine distinct matrices, the
method may be applied to all
wastewater matrices), in addition to any
and all reagent water tests. If the
performance in the wastewater matrix or
reagent water does not meet the QC
acceptance  criteria the method
modification may not be used.
  (D) Analysts must  test representative
effluents with the modified method, and
demonstrate that the results are
equivalent or superior to results with
the unmodified method.
  (ii) Requirements for Documentation.
The modified method must be
documented in a method write-up or an
addendum that describes the
modification(s) to the approved method.
The write-up or addendum must
include a reference number (e.g.,
method number), revision number, and
revision date so that it may be
referenced accurately. In addition, the
organization that uses the modified
method must document the results of
QC tests and keep these records, along
with a  copy of the method write-up or
addendum, for review by an auditor.
  (3) Restrictions. An analyst may not
modify an approved analytical method
for a method-defined analyte. In
addition, an analyst may not modify an
approved method if the modification
would  result in measurement of a
different form or species of an analyte
(e.g., a  change to a metals digestion or
total cyanide distillation). An analyst
may also may not modify any sample
preservation and/or holding time
requirements of an approved method.
  (c) Analytical Requirements for Multi-
analyte Methods (Target Analytes). For
the purpose of NPDES reporting, the
discharger or permittee must meet QC
requirements only for the analyte(s)
being measured and reported under the
NPDES permit.
  (d) The following modifications to
approved methods are authorized in the
circumstances described below:
  (1) Capillary Column. Use of a
capillary (open tubular) GC column
rather  than a packed column is allowed
with EPA Methods 601-613, 624, 625,
and 1624B  in Appendix A to this part,
provided that all QC tests for the
approved method are performed and all
QC acceptance criteria are met. When
changing from a packed column to a
capillary column, retention times will
change. Analysts are not required to
meet retention time  specified in the
approved method when this change is
made.  Instead, analysts must generate
new retention time tables with capillary
columns to be kept on file along with
-------
               Federal  Register/Vol.  72, No.  47/Monday,  March 12, 2007/Rules  and Regulations
                                                                                       11241
other startup test and ongoing QC data,
for review by auditors.
   (2) Increased sample volume in purge
and trap methodology. Use of increased
sample volumes, up to a maximum of 25
mL,  is allowed for an approved method,
provided that the height of the water
column in the purge vessel is at least 5
cm. The analyst should also use one or
more surrogate analytes that are
chemically similar to the analytes of
interest in order to demonstrate that the
increased sample volume does not
adversely affect the analytical results.

PART 141—NATIONAL PRIMARY
DRINKING WATER REGULATIONS
• 11. The authority citation for part 141
continues to read as follows:
                  Authority: 42 U.S.C. 300f, 300g-l, 300g-2,
                300g-3, 300g-4, 300g-5, 300g-6, 300J-4,
                300J-9, and300j-ll.

                • 12. Section 141.21 is amended by
                adding four sentences to the end of
                footnote 1 to the Table in paragraph
                (f)(3) to read as follows:

                §141.21  Coliform sampling.
                *****
                  ffl*  *  «
                  (3)*  *  *
                  i* *  * in addition, the following
                online versions may also be used: 9221
                A, B, D-99, 9222 A, B, C-97, and 9223
                B-97. Standard Methods Online are
                available at http://
                www.standardmethods.org. The year in
                which each method was approved by
                the Standard Methods Committee is
                  designated by the last two digits in the
                  method number. The methods listed are
                  the only Online versions that may be
                  used.
                  *****

                  • 13. Section 141.23 is amended as
                  follows:
                  • a. In paragraph (a)(4)(i) by revising the
                  table entries for "Cyanide," "Nitrate,"
                  and "Nitrite".
                  • b. In paragraph (k)(l) by revising the
                  table.

                  § 141.23   Inorganic chemical sampling and
                  analytical requirements.
                                                                                  (a)
                                   DETECTION LIMITS FOR  INORGANIC CONTAMINANTS
    Contaminant
MCL (mg/L)
Methodology
Detection Limit (mg/L)
Cyanide 	  0.2
               Distillation, Spectrophotometric3	
               Distillation, Automated, Spectrophotometric3 	
               Distillation, Amenable, Spectrophotometric4 	
               Distillation, Selective Electrode3.4	
               UV, Distillation, Spectrophotometric9	
               Micro Distillation, Flow Injection, Spectrophotometric3
               Ligand Exchange with Amperometry* 	
                                                  0.02
                                                  0.005
                                                  0.02
                                                  0.05
                                                  0.0005
                                                  0.0006
                                                  0.0005
Nitrate 	  10 (as N)
Nitrite 	  1 (as N)
               Manual Cadmium Reduction 	
               Automated Hydrazine Reduction
               Automated Cadmium Reduction .
               Ion Selective Electrode	
               Ion Chromatography	
               Capillary Ion Electrophoresis	
               Spectrophotometric	
               Automated Cadmium Reduction .
               Manual Cadmium Reduction 	
               Ion Chromatography	
               Capillary Ion Electrophoresis	
                                                  0.01
                                                  0.01
                                                  0.05
                                                  1
                                                  0.01
                                                  0.076
                                                  0.01
                                                  0.05
                                                  0.01
                                                  0.004
                                                  0.103
  3 Screening method for total cyanides.
  « Measures "free" cyanides when distillation, digestion, or ligand exchange is omitted.

  9 Measures total cyanides when UV-digestor is used, and "free" cyanides when UV-digestor is bypassed.
  00'
Contaminant
1 Alkalinity

2. Antimony 	

3. Arsenic'4 	

Methodology 13

Electrometric titration
Inductively Coupled Plas-
ma (ICP)— Mass Spec-
trometry.
Hydride-Atomic Absorp-
tion.
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Inductively Coupled Plas-
ma15.
ICP-Mass Spectrometry
EPA


200.82
200.9 2
200.72 	
200.8 2
ASTM3
01067-92 02 B

D3697-92 02



SM4(18th, 19th
ed.)
2320 B


3113B
3120 B

SM4(20thed.)
2320 B



3120 B

SM Online22
2320 B-97
1-1030-85 5.

3113 B-99 	
3120 B-99

Other






-------
11242
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
Contaminant


4 Asbestos 	



6. Beryllium 	












12 Cyanide












1 4 Lead

Methodology '3
Atomic Absorption; Plat-
form.
Atomic Absorption* Fur-
nace.
lion.
Transmission Electron
Microscopy.
Transmission Electron
Microscopy.
ma.
CP-Mass Spectrometry

nace.
nductively Coupled Plas-
ma.
CP-Mass Spectrometry
Atomic Absorption; Plat-
form.
nace.
Inductively Coupled Plas-
ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption' Fur-
nace.
EDTA titrimetric

Aspiration.
ma.

ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
nace.
nace.
Aspiration.
ma.
ICP-Mass Spectrometry ..
Atomic Absorption; Plat-
form.
Manual Distillation fol-
lowed by
Spectrophotometric
Amenable.
Manual.
Spectra-photometric
Semi-automated.
UV Distillation
Spectrophotometric.
Micro Distillation Flow
Injection,
Spectrophotometric.
Amperometry21.

SPADNS.



phoresis.
nace.
ICP-Mass Spectrometry
EPA
200.9 2

100. 19
100.2 10
200 7 2
200.8 2

200.72 	
200.8 2
200.9 2
200.72
200.82
200.9 2


200 7 2

200 7 2
200.8 2
200.92


200 7 2
200.82
200.9 2



335.4 6



300 O6
300.1 19





200.8 2
ASTM3
D2972-97 03 C 	
D2972-97 03 B




D3645-97 03 B


D511-93 03 A 	
D51 1-93 03 B

D69 19-03


D1688-95 02 C
D 1688-95 02 A

D1 125-95 (Reapproved
1999) A.
D2036-98A 	
D2036-98 B 	
D2036-98A 	



D6888-04 	
D4327-97 03

D1179-93 99 B 	



D3559-96 03 D 	

SM»(18th, 19th
ed.)
3113 B ..
3114 B

3120 B
3111D
3113 B
3120 B 	
3113 B

3113 B 	
3500-Ca D ..
3111 B
3120 B .. .

3120 B 	
3113 B
3113 B
3111 B
3120 B
2510 B 	
4500-CN- C ..
4500-CN- G ..
4500-CN- E ..
4500-CN- F



4110 B
4500-F- B D
4500-F- C 	

4500-F- E ... .

3113 B 	

SM« (20th ed.)



3120 B


3120 B 	


3500-Ca B 	

3120 B 	

3120 B 	



3120 B
2510 B 	
4500-CN- C.
4500-CN- G ..
4500-CN- E ...
4500-CN- F ...



4110 B
4500-F " B D
4500-F- C 	

4500-F- E 	



SM Online22
3113 B-99
3114 B 97

3120 B 99
3111 D 99
3113 B-99
31208-99.
3113 B-99

3113 B-99
3500-Ca B-97.
3111 B-99
3120 B-99

3120 B-99
3113 B-99
3113 B-99
3111 B-99
3120 B-99
2510 B-97.

4500-CN- G-
99.
4500-CN- E-
99.
4500-CN- F-
99.


4110 B-00
4500-F- B D-
97.
4500-F- C-97.

4500-F- E-97

31 13 B-99.

Other





















I-3300-85 5

Kelada-01 17
QuikChem 10-
204-00-1-
X18
OIA-1677
DW20


380-75WE11
129-71W"
D6508, Rev.
223

-------
Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules  and Regulations
11243
Contaminant

15. MagnGsium . .



16. Mercury 	
17. Nickel


18. Nitrate 	




19. Nitrite



20. Ortho-phos-
phate12.





21. pH 	
22 Selenium

23. Silica






24. Sodium 	

25. Temperature 	
26. Thallium 	
Methodology "
Atomic Absorption; Plat-
form.
Differential Pulse Anodic
Stripping Voltametry.
Atomic Absorption 	
ICP
Complexation Titrimetric
Methods.
Manual, Cold Vapor 	
Automated, Cold Vapor ..
ICP-Mass Spectrometry
Inductively Coupled Plas-
ma.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Ion Chromatography 	
Automated Cadmium Re-
duction.
Manual Cadmium Reduc-
tion.
Capillary Ion Electro-
phoresis.
Ion Chromatography
Automated Cadmium Re-
duction.
Manual Cadmium Reduc-
tion.
Spectrophotometric 	
Capillary Ion Electro-
phoresis.
Colorimetric Automated
Ascorbic Acid.
Colorimetric ascorbic
acid, single reagent.
Colorimetric
Phosphomolybdate;
Automated-seg-
mented flow;
Ion Chromatography 	
Capillary Ion Electro-
phoresis.
Electrometric 	

tion.
ICP-Mass Spectrometry
Atomic Absorption; Plat-
form.
Atomic Absorption; Fur-
nace.
Colorimetric Molybdate
Blue.
mented Flow.
Colorimetric 	
Molybdosilicate
Heteropoly blue 	
Automated for Molyb-
date-reactive Silica.
Inductively Coupled Plas-
ma.
Inductively Coupled Plas-
ma.
Atomic Absorption' Direct
Aspiration.
Thermometric 	
ICP-Mass Soectrometrv
EPA
200.9 2

200 7 2


245.1 2 	
245.2 1
200.82
200.72 ..
200.82
200.92

300.0 6
300.1 '»
353.2 6 ..



300 Oe
300.1 «
3S3.26 	


365 1 6 .




300.0 e ..
300.1 "> 	
150.1,
150.2'
200.82
200.9 2






200.7 2 ..
200.72


200.8 2
ASTM3

0511-93 03 B 	

0511-93, 03 A 	
069 1 9-03
D3223-97 02 	



04327-97 03
03867-90 A

D3867-90 B

04327-97 03
03867-90 A 	
03867-90 B 	



0515-88 A



04327-97 03 	

01293-95 99
03859-98 03 A
D3859-98 03 B


0859-94 00





D69 19-03


SM"(18th, 19th
ad.)

3111 B 	
3120 B
3500-Mg E 	

3112B 	
3120 B 	
3111 B
3113 B 	
4110 B 	
4500-NO3- F
4500-NO3~ 0
4500-NO3- E

4110 B
4500-NO3- F
4500-NO3- E
4500-NO2~ B

4500-P F
4500-P E



4110 B 	

4500-H+ B 	
3114 B
3113 B 	



4500-Si D
4500-Si E .. .
4500-Si F 	
3120 B
3111 B

2550

SM4(20thed.)


3120 B
3500-Mg B 	


3120 B


4110 B 	
4500-NO3- F
4500-NO3~ D
4500-NO3- E

4110 B
4500-NO3^ F
4500-NO3- E
4500-NO2~ B

4500-P F
4500-P E



4110B

4500-H + B





4500-SiC>2 C
4500-SiO2 D
4500-Si02 E
3120 B


2550

SM Online22

3111 B-99.
3120 B-99.
3500-Mg B-97.

3112 B-99.
3120 B-99.
3111 B-99
3113 B-99.
4110 B-00 	
4500-NO3~ F-
00.
4500-NO3- D-
00.
4500-NO3- E-
00.
4110 B-00
4500-NO3- F-
00.
4500-NO3- E-
00.
4500-NO2- B-
00.





4110 B-00.

4500-H* B-00.
3114 B-97
3113 B-99



4500-SiO2 C-
97.
4500-SiO2 D-
97.
4500-SiO2 E-
97.
3120 B-99
3111 B 99

2550-00

Other
Method 1001 ie








B-1011 8

601 7

D6508, Rev.
223
B-10118


D6508, Rev.
2 23

I-1601-856
1-2601 -90 5
I-2598-85 5

D6508, Rev.
223


1-1 700-85 6
I-2700-85 5





•



-------
11244
Federal  Register/Vol.  72,  No. 47/Monday, March 12, 2007/Rules and Regulations

Contaminant

Methodology <3
Atomic Absorption; Plat-
form.
EPA
200.9 2.
ASTM3

SM4(18th, 19th
ed.)

SM'(20thed.)

SM Online22

Other

  The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents listed in footnotes 1-11, 16-20, and 22-23 was
approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1  CFR Part 51. Copies of the documents may be obtained from the sources listed below. Informa-
tion regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket, EPA West,
1301 Constitution Avenue, NW., Room 3334, Washington, DC 20460 (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information on the
availability of this material at NARA, call 202-741-6030, or go to: http:ffwww.archives.gov/federal_'Bgister/code ot_federal_regulations/ibr_locations.html.
  ' "Methods for Chemical Analysis of Water and Wastes." ipA/600<4-79/020. March 1983.  Available at NTIS,~PB84-128677.
  2 "Methods for the Determination of Metals in  Environmental Samples—Supplement I." EPA/600/R-94/111, May 1994. Available at NTIS, PB95-125472.
  sAnnual Book of ASTM Standards, 1994, 1996, 1999, or 2003, vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. The previous
versions of D1688-95A. D1688-95C (copper), D3559-95D (lead). D1293-95 (pH), D1125-91A (conductivity) and D859-94 (silica) are also approved. These previous versions D1688-90A. C;
D3559-90D, D1293-84. D1125-91A and D859-88. respectively are located in the Annual Book of ASTM Standards. 1994, Vol. 11.01. Copies may be obtained from ASTM International, 100
Barr Harbor Drive, West Conshohocken, PA 19428.
  'Standard Methods for the Examination ot Water and  Wastewater, 18th edition (1992),  19th edition (1995). or 20th edition (1998). American Public Health Association. 1015 Fifteenth
Street,  NW., Washington,  DC 20005. The cited  methods published in any of  these three editions may be used, except that the versions of 3111  B. 3111 D, 3113 B and 3114 B in the 20th
edition may not be used. •
  5Method 1-2601-90, Methods for Analysis by the U.S.  Geological Survey National Water Quality  Laboratory—Determination of Inorganic and Organic Constituents  in Water and Fluvial
Sediment, Open File Report 93-125, 1993; For Methods 1-1030-85, 1-1601-85;  1-1700-85; I-2598-85; I-2700-85;  and I-3300-85 See Techniques of Water Resources Investigation of the
U.S. Geological Survey, Book 5, Chapter A-1. 3rd edition.. 1989; Available from Information  Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225-0425.
  ""Methods for the Determination of Inorganic  Substances in Environmental  Samples," EPA/600/R-93/100, August 1993. Available at NTIS, PB94-120821.
  7The procedure shall be done in accordance with the Technical Bulletin 601 " Standard Method of Test for Nitrate in Drinking Water," July 1994, PN 221890-001, Analytical Technology,
Inc. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129.
  "Method B-1011. "Waters Test Method for Determination  of Nitrite/Nitrate in Water Using Single Column Ion Chromatography," August 1987. Copies may be obtained from Waters Cor-
poration Technical Services Division, 34 Maple  Street, Milford, MA 01757. Telephone: 508/482-2f31,  Fax:  508/482-3625.
  "Method 100 1, "Analytical Method For Determination of Asbestos Fibers in Water," EPA/600/4-83/043, EPA, September 1983. Available at NTIS, PB83-260471.
  '"Method 100.2, "Determination of Asbestos Structure Over 10-um In Length In Drinking Water," EPA/600/R-94/134, June 1994.  Available at NTIS, PB94-201902.
  11 Industrial Method No. 129-71W. "Fluoride in Water and  Wastevvater," December 1972, and Method No. 380-75WE, "Fluoride in Water and  Wastewater," February 1976, Technicon In-
dustrial Systems. Copies may be obtained from  Bran & Luebbe, 1025 Busch Parkway,  Buffalo Grove,  IL 60089.
  12 Unfittered, no digestion or hydrolysis.
  w Because  MDLs reported In EPA Methods 200.7 and 200.9 were determined using a 2x preconcentration step during sample digestion, MDLs determined when samples are analyzed by
direct analysis (i.e.. no sample digestion) will be higher. For  direct analysis of cadmium and arsenic  by Method 200.7, and arsenic by Method 3120 B. sample preconcentration using pneu-
matic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and
lead by Method 3113 B; and lead by Method D3559-90D,  unless multple in-furnace depositions are made.
  14lf ultrasonic nebulization is used in the determination of arsenic by Methods 200.7, 200.8, or SM  3120 B, the arsenic must be in the pentavalent state to provide uniform signal response.
For Methods 200.7 and 3120 B, both  samples and standards must be diluted in the same mixed acid matrix concentration of nitric and hydrochloric acid with the addition of 100 yl of 30%
hydrogen peroxide per 100 ml of solution. For direct analysis of arsenic with Method 200.8  using ultrasonic nebulization, samples and standards must contain 1 mg/L of  sodium hypochlorite.
  15Starting January 23, 2006, analytical methods using the  ICP-AES technology may not be used because the detection limits for these methods are 0.008 mg/L or higher. This restriction
means that the two ICP-AES methods (EPA Method 200.7 and SM 3120 B)  approved for use for the MCL of 0.05 mg/L may not be used for compliance determinations Tor the revised MCL
of 0 010 mg/L However, prior to January 23, 2006, systems  may have compliance samples  analyzed  with these less sensitive methods.
  '«The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erianger, KY 41018. Or from the Hach Company, P.O. Box
389, Loveland, CO 80539.
  17The description for the Kelada-01 Method,  "Kelada Automated "est Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate," Revision 1.2, August 2001, EPA # 821-B-
  	..i a given instrument. Similarly	_. .........                     ,                  .,                 .            .  ..  	
  1»The description for the QuikChem Method 10-204-00-1-X, "Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST and determination of cyanide by
flow injection analysis," Revision 2.1, November 30, 2000, for cyanide is available from Lachat Instruments, 6645 W. Mill Hd., Milwaukee, Wl 53218. Telephone: 414-358-4200.
  ""Methods for the  Determination of Organic and Inorganic Compounds in Drinking Water," Vol. 1, EPA 815-R-00-014, August 2000. Available at NTIS, PB2000-106981.
  20Method OIA-1677, DW "Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry," January 2004.  EPA-821-R-04-001, Available from ALPKEM, A Division of Ol Ana-
lytical, P.O.  Box 9010, College Station, TX 77842-9010.
  21 Sulfide  levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide method to determine if a sulfide in-
terference is present,  and treat samples accordingly.
  ^Standard Methods Online are available at http^/www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last
two digits in the method number. The methods listed are the only online versions that may be used.
  23Method D6508 Rev  2, 'Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte," available from
Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
• 14. Section 141.24 is amended as
follows:
• a. By revising the introductory text of
paragraph (e)(l).
• b. By revising entries 23, 24, 26, 30,
49, and 50 in the table to paragraph
   c. By adding a new footnote 5 to the
 table to paragraph (e)(l).

 §141.24  Organic chemicals, sampling and
 analytical requirements.
 *****
   (e)*  *  *
   (1) The following documents are
 incorporated by reference. This
 incorporation by reference was
 approved by the Director of the Federal
 Register in accordance with 5 U.S.C.
 552(a) and 1 CFR Part 51. Copies may
 be inspected at EPA's Drinking Water
 Docket, 1301 Constitution Avenue, NW.,
 EPA West, Room 3334, Washington, DC
 20460 (Telephone: 202-566-2426); or at
 the National Archives and Records
 Administration (NARA). For
 information on the availability of this
 material at NARA, call 202-741-6030,
 or go to: http://www.archives.gov/
                               federal_register/
                               code_of_federal_regulations/
                               ibr_locations.html. Method 508A and
                               515.1 are in Methods for the
                               Determination of Organic Compounds
                               in Drinking Water, EPA/600/4-88-039,
                               December 1988, Revised, July 1991.
                               Methods 547, 550 and 550.1 are in
                               Methods for the Determination of
                               Organic Compounds in Drinking
                               Water—Supplement I, EPA/600-4-90-
                               020, July 1990. Methods  548.1, 549.1,
                               552.1 and 555  are in Methods for the
                               Determination of Organic Compounds
                               in Drinking Water—Supplement II,
                               EPA/600/R-92-129, August 1992.
                               Methods 502.2, 504.1, 505, 506, 507,
                               508, 508.1, 515.2, 524.2 525.2, 531.1,
                               551.1 and 552.2 are  in Methods for the
                               Determination of Organic Compounds
                               in Drinking Water—Supplement III,
                               EPA/600/R-95-131, August 1995.
                               Method 1613 is titled "Tetra-through
                               Octa-Chlorinated Dioxins and Furans
                               by Isotope-Dilution HRGC/HRMS,"
                               EPA/821-B-94-005, October 1994.
                               These documents are available from the
                               National Technical  Information Service,
                               NTIS PB91-231480, PB91-146027,
PB92-207703, PB95-261616 and PB95-
104774, U.S. Department of Commerce,
5285 Port Royal Road, Springfield,
Virginia 22161. The toll free number is:
800-553-6847. Method 6651 shall be
followed in accordance with Standard
Methods for the Examination of Water
and Wastewater,  18th edition (1992),
19th edition (1995), or 20th edition
(1998), American Public Health
Association (APHA); any of these three
editions may be used. Method 6610
shall be followed in accordance  with
Standard Methods for the Examination
of Water and  Wastewater, (18th  Edition
Supplement)  (1994), or with the 19th
edition (1995) or 20th edition (1998) of
Standard Methods for the Examination
of Water and  Wastewater; any  of these
publications may be used. The APHA
documents are available from APHA,
1015 Fifteenth Street NW., Washington,
DC 20005.  Other required analytical test
procedures germane to the conduct of
these analyses are contained in
Technical Notes  on Drinking Water
Methods, EPA/600/R-94-173, October
1994, NTIS PB95-104766. EPA Methods
515.3 and 549.2 are available from U.S.
-------
               Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations
                                                                        11245
Environmental Protection Agency,
National Exposure Research Laboratory
(NERL)-Cincinnati, 26 West Martin
Luther King Drive, Cincinnati, OH
45268. ASTM Method D 5317-93, 98
(Reapproved 2003) is available in the
Annual Book of ASTM Standards,
(1999), Vol. 11.02, ASTM International,
100 Barr Harbor Drive, West
Conshohocken, PA 19428, any edition
containing the cited version of the
method may be used. EPA Method
515.4, "Determination of Chlorinated
Acids in Drinking Water by Liquid-
Liquid Microextraction, Derivatization
and Fast Gas Chromatography with
Electron Capture Detection," Revision
1.0, April 2000, EPA/815/B-00/001 and
EPA Method 552.3, "Determination of
Haloacetic Acids and Dalapon in
Drinking Water by Liquid-Liquid
Microextraction, Derivatization, and Gas
Chromatography with Electron Capture
Detection," Revision 1.0, July 2003, EPA
815-B-03-002, can be accessed and
downloaded directly online at http://
www.epa.gov/safewater/methods/
sourcalt.html. Syngenta Method AG-
625, "Atrazine in Drinking Water by
Immunoassay," February 2001, is
available from Syngenta Crop
Protection, Inc., 410 Swing Road, P.O.
Box 18300, Greensboro, NC 27419.
Telephone: 336-632-6000. Method
531.2 "Measurement of N-
methylcarbamoyloximes and N-
methylcarbamates in Water by Direct
Aqueous Injection HPLC with
Postcolumn Derivatization," Revision
1.0, September 2001, EPA 815-B-01-
002, can be accessed and downloaded
directly online at http://www.epa.gov/
safewater/methods/sourcalt.html.
                       Contaminant
                                                            EPA Method'
                                   Standard
                                   Methods
                                                                                           ASTM
                                                                                                            Other
23. 2,4-D4 (as acids, salts, and esters)
24. 2,4,5-TP< (Silvex)
                 515.2, 555,
                   515.1, 515.3,
                   515.4.
                 515.2, 555,
                   515.1, 515.3,
                   515.4.
      D5317-93, 98
       (Reapproved
       2003).
      D5317-93, 98
       (Reapproved
       2003).
26. Atrazine 2 .
                                                          507, 525.2,
                                                           508.1,505,
                                                           551.1.
                                                              Syngenta5 AG-625
30. Dalapon
                 552.1 515.1,
                   552.2, 515.3,
                   515.4, 552.3.
49. Pentachlorophenol ...


50. Picloram4	
                 515.2,525.2,
                   555, 515.1,
                   515.3, 515.4.
                 515.2, 555,
                   515.1, 515.3,
                   515.4.
      05317-93,98
       (Reapproved
       2003).
      05317-93,98
       (Reapproved
       2003).
  1 For previously approved EPA methods which remain available for compliance monitoring until June 1, 2001, see paragraph (e)(2) of this sec-
tion.
  Substitution of the detector specified in Method 505, 507, 508, or 508.1 for the purpose of achieving lower detection limits is allowed as fol-
lows: Either an electron capture or nitrogen phosphorus detector may be used provided all regulatory requirements and quality control criteria are
met.

  4Accurate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA Methods 515.1, 515.2, 515.3, 515.4,
and 555 and ASTM Method D 5317-93, 98 (Reapproved 2003).
  6 This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for drinking water treatment. In sam-
ples from all other systems, any result for atrazine generated by  Method AG-625 that is greater than one-half the maximum contaminant level
(MCL) (in other words, greater than 0.0015mg/L or 1.5 ug/L) must be confirmed using another approved method for this contaminant and should
use additional volume of the original sample collected for compliance monitoring. In instances where a result from Method AG-625 triggers such
confirmatory testing, the confirmatory result is to be used to determine compliance.
                                        • 15. Section 141.25 is amended by
                                        revising the table in paragraph (a) to
                                        read as follows:
                                        §141.25  Analytical methods for
                                        radioactivity.
                                          (a)*  *  *
Contaminant
Naturally Occurring:
Gross alpha" and beta 	
Gross alpha11 	

Methodology
Evaporation 	
Coprecipitation

Reference (Method of Page Number)
EPA1
900.0

EPA2
p. 1 ...

EPA3
00-01
00-02
EPA"
p. 1 	
SM5
302,71108,
7110B-00.
7110 C, 7110
C-00.
ASTM6


USGS7
R-1 120-76.
DOE»

Other

-------
11246
Federal  Register/Vol.  72,  No. 47/Monday,  March  12,  2007/Rules and Regulations
Contaminant

Radium 228 	

Man-Made:
Radioactive Iodine 	
Radioactive Strontium 89,
90.


Methodology
Radon emanation ...
Radiochemical 	
Radiochemical 	
Radiochemical 	
Fluorometric 	
ICP-MS 	
Alpha Spectrometry
Laser
Phosphorimetry.
Radiochemical 	
Gamma Ray Spec-
trometry.
Radiochemical 	
Gamma Ray Spec-
trometry.
Radiochemical 	
Liquid Scintillation ..
Gamma Ray Spec-
trometry.
Reference (Method of Page Number)
EPA'
903.1
903.0
904.0
908.0
908.1
200.8"

901.0
901.1
902.0
901.1
905.0
906.0
901.1
902.0
901.0
EPA* EPA3
p. 16
p. 13
p. 24




p. 4 ...
p 6
p. 9 ...
p. 29
p. 34


Ra-04
Ra-03
Ra-05


00-07




Sr-04
H-02 ..


EPA4
p. 19 	
P. 19 	


p. 33 	

p. 92 	

p. 92 	
p. 65 	
p. 87 	
p. 92 	


SMS
305, 7500-Ra
C, 7500-
Ra C-01.
304, 7500-Ra
B, 7500-Ra
B-01.
7500-Ra D,
7500-Ra
D-01.
7500-U B,
7500-U B-
00.
7500-U C
(17th Ed.).
3125 	
7500-U C
(18th, 19th-,
or 20th
Ed.), 7500-
U C-00.
7500-Cs B,
7500-Cs
B-00.
7120, 7120-
97.
7500-I B,
7500-I B-
00.
7500-I C,
7500-I C-
00.
7500-I D,
7500-I D-
00.
7120, 7120-
97.
303, 7500-Sr
B, 7500-Sr
B-01.
306, 7500-
3H B,
7500-3H
B-00.
7120, 7120-
97.
7500-Cs B,
7500-Cs
B-00.
7500-I B,
7500-I B-
00.
ASTM «
D34 54-97
D2460-97
D2907-97
D5673-03.
D3972-
97, 02.
D5174-
97, 02.
D2459-72
D3649-
91,98a.
D3649-
91, 98a.
D4785-
93, OOa.
D4107-
91, 98
(Re-
ap-
proved
2002).
D3649-
91, 98a.
D4785-
93, OOa.
USGS?
R-1 141-76
R-1 140-76
R-1 142-76
R-1 180-76,
R-1 181-
76.
R-1 182-76
R-1 11 1-76.
R-1 11 0-76
R-1 160-76
R-1 171-76.
R-1 110-76
DOE8
Ra-04 	

U-04.
U-02.
4.5.2.3.
4.5.2.3.
Sr-01,
Sr-02.
Ga-01-R.
Other
NY9,
GA«
NY 8;
NJ10,
GA">
  The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 and 13 through 14 was approved by the Director
of the  Federal Register in accordance with 5 U.S.C. 552{a) and 1  CFR Part 51. Copies of the documents may be obtained from the sources listed below.  Information regarding obtaining
these documents can be obtained  from the Safe Drinking Water Hotline at 800-426-4791. Documents may be  inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Ave-
nue, NW., Room 3334 . Washington, DC 20460 (Telephone: 202-566-2426); or at the National Archives and Records Administration (NARA). For information  on the availability of this mate-
rial at NARA.  call 202-741-6030. or go to: http://www.archives.gov/federal_registar/code_otjgderal_regulations/!tirjocations.html.
  ' "Prescribed Procedures for the Measurement of Radioactivity In Drinking water," EPA 600/4-80-032, August 1980. Available at the U.S. Department of Commerce, National Technical In-
formation Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800-553-6847), PB 80-224744.
  2 "Interim Radiochemical Methodology for Drinking Water,"  EPA 600/4-75-008 (revised), March 1976. Available NTIS, ibid.
  3 "Radiochemistry Procedures Manual," EPA 520/5-84-006, December 1987. Available NTIS, bid.
  4 "Radiochemical Analytical Procedures for Analysis of Environmental Samples," March 1979. Available at NTIS, Ibid. EMSL LV 053917.
  5 "Standard Methods for the Examination of Water and Wastewator," 13th,  17th, 18th,  19th or 20th edition, 1971, 1989, 1992, 1995, 1998. Available at American Public Health Association,
1015 Fifteenth Street,  NW., Washington, DC 20005. Methods 302, 303, 304, 305 and 306 are only in the 13th edition. Methods 7110B  7500-Ra B,  7500-Ra C, 7500-Ra D, 7500-U B,
7500-Cs B, 7500-I B, 7500-1 C,  7500-1  D, 7500-Sr B, and 7500-:'H B are in the 17th,'18th, 19th and 20th editions. Method 7110 C is in the 18th, 19th and 20th editions. Method 7500-U
C Fluorometric Uranium is only in  the 17th Edition, and 7500-U C Alpha Spectrometry is only in the 18th,  19th and 20th editions. Method 7120 is only in the  19th and 20th editions. Method
3125 is only in the 20th edition. Methods 7110 B-00, 7110 C-00, 7500-Ra  B-01, 7500-Ra C-01, 7500-Ra D-01, 7500-U B-00,  7500-U C-00,  7500-I B-00, 7500-I C-00, 7500-I D-00,
7120-97, 7500-Sr B-01, and TSOO-^H B-00 are available online at http://www.stantts.filmettKxis.org. The  year In which each method was approved by the Standard Methods Committee is
designated by the last two digits in the method number. The methods listed are the only online versions that may be used.
  "Annual Book of ASTM Standards, Vol. 11.01 and 11.02, 2002; ASTM International; any year containing the cited version of the method may be used. Copies of these two volumes and
the 2003 version of D 5673-03 may be obtained from ASTM International,  100 Barr Harbor  Drive, P.O.  Box C700. West Conshohocken, PA 19428-2959.
  7 "Methods  for Determination of Radioactive Substances in Water and Fluvial Sediments,"  Chapter A5 in  Book 5 of Techniques of Water-Resources Investigations of the United States Geo-
logical Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal Center,  Denver, CO 80225-0425.
  »"EML Procedures Manual," 28th (1997) or 27th (1990)  Editions. Volumes 1 and 2; either edition may be used. In the 27th Edition Method Ra-04 is listed as Ra-05 and Method Qa-01-R
is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S.  Department ot Energy  (DOE), 376 Hudson Street, New York, NY 10014-3621.
  9"Determination of Ra-226 and Ra-228 (Ra-02)," January 1980,  Revised June 1982. Available at Radiological Sciences Institute for Laboratories and Research, New York State Depart-
ment ot Health, Empire State  Plaza, Albany. NY 12201.
   10"Determination of Radium 228 in Drinking Water," August 1980. Available at State of New Jersey. Department of Environmental Protection, Division of Environmental Quality, Bureau of
Radiation and Inorganic Analytical  Services, 9 Swing Street, Trenton, NJ 08625.
   11 Natural uranium and thorium-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods; americium-241 is approved with co-
precipitation methods.
   12 It uranium (U) is determined by mass, a 0.67 pCi/u.g  of uranium conversron factor must  be used. This conversion factor  is based on the 1:1  activity ratio of U-234 and U-238 that is
characteristic of naturally occurring uranium.
   13 "Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry," Revision 5.4, which is published  in "Methods for the Determination of  Met-
als in  Environmental Samples—Supplement I,1" EPA 600-R-94-111, May 1994. Available at NTIS, PB 95-125472.
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               Federal Register/Vol. 72,  No. 47/Monday, March  12, 2007/Rules and Regulations
                                                                           11247
  14"Tha Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors," Revision 1.2, December 2004. Available from the
Environmental Resources Center, Georgia Institute of Technology, 620 Cherry Street, Atlanta, GA 30332-0335, USA, Telephone: 404-894-3776. This method may be used to analyze for ra-
dium-226 and radium-228 in samples collected after January 1. 2005 to satisfy the radium-226 and radium-228 monitoring requirements specified at 40 CFR 141.26.
• 16. Section 141.74 is amended as
follows:
• a. By revising the entry for turbidity
in the table in paragraph (a)(l).
• b. By revising footnotes 1,8,10,11,
and 12 to the table in paragraph (a)(l).
• c. By adding footnote 13 to the table
in paragraph (a)(l).
• d. By revising paragraph (a)(2).
§ 141.74  Analytical and monitoring
requirements.

  (a)*  * *
  (1)*  * *
       Organism
                  Methodology
                                                                                                                 Citation1
Turbidity13	  Nephelometric Method 	  2130 B
                       Nephelometric Method 	  180.1 9
                       Great Lakes Instruments	  Method 210
                       Hach FilterTrak  	  1013312
  *****
  1 Except where noted, all methods refer to Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition
(1995), or 20th edition (1998), American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods pub-
lished in any of these three editions may be used. In addition, the following online versions may also be used: 2130 B-01, 9215 B-00, 9221 A,
B, C, E-99, 9222 A, B, C, D-97, and 9223 B-97. Standard Methods Online are available at httpMvww.standardmethods.org. The year in which
each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed
are the only Online versions that may be used.

  SA-1 broth may be held up to 7 days in a tightly closed screw cap tube at 4 °C.
  9"Methods for the Determination  of Inorganic Substances  in Environmental Samples,"  EPA/600/R-93/100, August 1993. Available at NTIS,
PB94-121811.
  10GLI Method 2, "Turbidity," November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, Wl 53223.
  11A description of the SimPlate method,  "IDEXX SimPlate TM HPC Test Method for Heterotrophs in Water," November 2000, can be obtained
from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092, telephone (800) 321-0207.
  12 A description of the Hach FilterTrak Method 10133, "Determination of Turbidity by Laser Nephelometry," January 2000, Revision 2.0, can be
obtained from; Hach Co.,  P.O. Box 389, Loveland, CO 80539-0389,  telephone: 800-227-4224.
  13Styrene divinyl  benzene  beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g. Hach  StablCal™ or equivalent) are accept-
able substitutes for formazin.
  (2) Public water systems must
measure residual disinfectant
concentrations with one of the
analytical methods in the following
table. If approved by the State, residual
disinfectant concentrations for free
chlorine and combined chlorine also
may be measured by using DPD
colorimetric test kits. In addition States
may approve the use of the ITS free
chlorine test strip for the determination
of free chlorine. Use of the test strips is
described in Method D99-003, "Free
Chlorine Species (HOC1- and OC1-) by
Test Strip," Revision 3.0, November 21,
2003, available from Industrial Test
Systems, Inc., 1875 Langston St., Rock
Hill, SC 29730. Free and total chlorine
residuals may be measured
continuously by adapting a specified
chlorine residual method for use with a
continuous monitoring instrument
provided the chemistry, accuracy, and
precision remain the same. Instruments
used for continuous monitoring must be
calibrated with a grab sample
measurement at least every five days, or
with a protocol approved by the State:
Residual
Free Chlorine 	



Total Chlorine



Chlorine Dioxide 	



Ozone 	
Methodology
Amperometric Titration 	
DPD Ferrous Titrimetric 	
DPD Colorimetric 	
Syringaldazine (FACTS)
Amperometric Titration
Amperometric Titration (low level measure-
ment).
DPD Ferrous Titrimetric
DPD Colorimetric
lodometric Electrode
Amperometric Titration 	
DPD Method
Amperometric Titration 	
Spectrophotometric
Indiao Method 	
SM1
4500-CI D 	
4500-CI F 	
4500-CI G 	
4500-CI H
4500-CI D
4500-CI E 	
4500-CI F
4500-CI G
4500-CI I
4500-CIO2 C 	
4500-CIO2 D
4500-CIO2 E 	

4500-O, B 	
SM Online2
4500-CI D-00 	
4500-CI F-00.
4500-CI G-00.
4500-CI H-00
4500-CI D-00
4500-CI E-00.
4500-CI F-00.
4500-CI G-00
4500-CI I-OO
4500-CIO2 C-00.

4500-CIO2 E-00

4500-O, B-97.
Other
D 1253-03 3



D1 253-03 3






327 0 Revision 1 1 4

  1 All the listed methods are contained in the 18th, 19th, and 20th editions of Standard Methods for the Examination of Water and Wastewater,
1992, 1995, and 1998; the cited methods published in any of these three editions may be used.
  2Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard
Methods Committee is designated by the last two digits in the method  number. The methods listed are the only Online versions that may be
used.
  3Annual Book of ASTM Standards, Vol. 11.01,  2004 ; ASTM International; any year containing the cited version of the method  may be used.
Copies of this method may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700 West Conshohocken, PA 19428-2959.
  "EPA Method 327.0, Revision 1.1, "Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using Lissamine Green B and Horse-
radish  Peroxidase  with  Detection  by  Visible Spectrophotometry,"  USEPA, May  2005,   EPA 815-R-05-008. Available  online at http://
www.epa.gov/safewater/methods/sourcalt.html.
-------
11248
Federal Register/Vol. 72,  No.  47/Monday,  March 12,  2007/Rules  and Regulations
PART 143—NATIONAL SECONDARY
DRINKING WATER REGULATIONS

• 17. The authority citation for part 143
continues to read as follows:
                               Authority: 42 U.S.C. 300f et seq.

                             m 18. Section § 143.4 is amended by
                             revising the table in paragraph (b) to
                             read as follows:
§143.4   Monitoring.
*     *     *     *

  (b)*   *  *
Contaminant



2 Chloride


3 Color







7 Odor
8 Silver


9 Sulfate

10 Total Dissolved Solids
1 1 Zinc

EPA
200 7 2
200 8 2
200 9 2
300 O1
300. 1e



200 72
200 9 2

200 7 2
200 8 2
200 9 2

200 7 2
200 8 2
200 9 2
3000'
300. 16
375 2 '

200 7 2
200. 8 2
ASTM3



D4327-97 03

D512-89 (Re-
approved
1999) B.











D4327-97 03

D516-90, 02 ...


SM" 18th and 19th ed.
3120 B
31 13 B
31 11 D 	
4110B 	
4500-CI- D 	 '. 	
4500-Ch B
2120 B . . 	
5540 C
3120 B 	
3111 B
3113 B 	
3120 B .. . . 	
3111 B
3113 B 	
2150 B 	
3120 B 	
3111 B
31 13 B
4110 B
4500-SO42- F 	
4500-SO42-C, D 	
4500-SO42~ E 	
2540 C . 	
3120 B
3111 B 	
SM420thed.
3120 B


4110 B
4500-CI- D 	
4500-CI- B
2120 B 	
5540 C
3120 B


3120 B 	


2150 B 	
3120 B 	


4110 B
4500-SOi2- F.
4500-SO42-C, D.
4500-SO42- E.
2540 C 	
3120 B

SM7 Online
3120 B-99
3113 B-99
31 1 1 D-99
4110 B-00
4500-CI- D-97.
4500-CI- B-97
2120 B-01.
5540 C-00
3120 B-99
311 1 B-99
3113 B-99.
3120 B-99.
3111 B-99
3113 B-99.
2150 B-97.
3120 B-99.
3111 B-99
3113 B-99
4110 B-00

2540 C-97.
3120 B-99
3111 B-99.
Other






D6508, Rev. 2s








I-3720-85 5




D6508, Rev. 2s


  The procedures shall be done in accordance wrth the documents listed below. The incorporation by reference ot the following documents was approved by the Director of the Federal Reg-
ister in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these documents can
be obtained from the Safe Drinking Water Hotline at 800-426-4791. Documents may be inspected at EPA's Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW.. Room 3334,
Washington, DC (Telephone: 202-566-2426); or at the National Arcnwes and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030,
or go to: hftp://mm.archives.gov/feaeral_register/code_otJederaLregulations/ibr_locations.html.
  ' "Methods for the Determination of Inorganic Substances in Environmental Samples," EPA/600/R-93-100, August 1993. Available at NTIS, PB94-120821.
  2"Methods for the Determination of Metals in Environmental Samples—Supplement I," EPA/600/R-94-111, May 1994. Available at NTIS, PB 95-125472.
  3 Annual Book ot ASTM Standards, 1994, 1996, 1999, or 2004. Vols. 11.01 and 11.02, ASTM International; any year containing the  cited version of the method may be used. Copies may
be obtained from the ASTM International, 100 Barr Hartor Drive, West Conshohocken, PA 19428.
  'Standard Methods tor the Examination ot Water and Wastewaler, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American  Public Health Association,  1015 Fifteenth
Street, NW., Washington, DC 20005. The cited methods published n any of these three editions may be used, except that the versions of 3111 B, 3111 D, and 3113 B in the 20th edition
may not be used.
  5Method I-3720-85, Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd ed., 1989. Available from Information Services, U.S. Geological
Survey, Federal Center, Box 25286, Denver, CO 80225-0425.
  •"Methods for the Determination of Organic and Inorganic Compojnds in Drinking Water," Vol. 1, EPA 815-R-00-014, August 2000. Available at  NTIS, PB2000-106981.
  'Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last
two digits in the method  number. The methods listed are the only online versions that may be used.
  8Method D6508, Rev.  2,  "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrtees Using Capillary Ion  Electrophoresis and Chromate Electrolyte," available from
Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
PART 430—THE PULP, PAPER, AND
PAPERBOARD POINT SOURCE
CATEGORY

• 19. The authority citation for part 430
continues to read as follows:
   Authority: Sections 301, 304, 306, 307,
308, 402, and 501 of the Clean Water Act, as
amended, (33 U.S.C. 1311,1314, 1316, 1317,
1318,1342, and 1361), and Section  112 of the
Clean Air Act, as amended (42 U.S.C. 7412).

• 20. Section 430.02 is amended by
adding paragraph (g) to read as follows:

§430.02  Monitoring requirements.
*****
   (g) Analyst may use NCASI Method
CP-86.07, "Chlorinated Phenolics in
Water by In situ Acetylation and GC/MS
Determination"  (January 2002) for
determination of certain chlorinated
                             phenols, chlorinated guaiacols,
                             chlorinated catechols, chlorinated
                             benzaldehydes (i.e., vanillins and
                             syringaldehydes), and trichlorsyringol
                             (analytes specified in the method) in
                             bleach plant filtrate as an alternative to
                             EPA Method 1653. NCASI Method CP-
                             86.07 is available from the Publications
                             Coordinator, NCASI, P.O. Box 13318,
                             Research Triangle Park, NC 27709-3318.
                             Telephone: 919-588-1987.

                             PART 455—PESTICIDE  CHEMICALS

                             • 21. The authority citation for Part 455
                             continues to read as follows:
                               Authority: Sees. 301, 304, 306, 307, and
                             501, Pub. L. 92-500, 86 Stat. 816, Pub. L. 95-
                             217, 91 Stat. 156, and Pub.  L.  100-4 (33
                             U.S.C. 1311, 1314, 1316, 1317, 1361).
• 22. Section 455.50 is revised to read
as follows:

§ 455.50  Identification of test procedures.
  The pesticide active ingredients to
which this section applies and for
which effluent limitations guidelines
and standards are specified in this Part
are named, together with the Chemical
Abstracts Service (CAS) number
(provided to assist in identifying the
pesticide active ingredient only) and
analytical method(s) designation(s) in
Table IG at 40 CFR 136.3(a). Except as
provided in 40  CFR 136.5, the discharge
parameter values required under the
Clean Water Act  must be determined by
one of the analytical methods cited and
described in Table IG at 40 CFR
136.3(a). Pesticide  manufacturers may
not use the analytical method cited in
-------
              Federal  Register/Vol.  72,  No. 47/Monday,  March 12, 2007/Rules and Regulations
                                                                    11249
Table IB, Table 1C, or Table ID of 40 CFR
136.3(a) to make these determinations
(except where the method cited in those
tables is identical to the method
specified in Table IG at 40 CFR
13 6.3 (a)). The full texts of the analytical
methods cited in Table IG at 40 CFR
136.3(a) are contained in the Methods
For The Determination of
Nonconventional Pesticides In
Municipal and Industrial Wastewater,
Volume I,  EPA 821-R-93-010A (August
1993 Revision I) and Volume II, EPA
821-R-93-010B (August 1993) (the
"Compendium"). Each pesticide
chemical manufacturer that is required
to determine discharge parameter values
under this Part using one of the
analytical methods cited in Table IG at
40 CFR 136.3(a) must request in writing
a copy of the Compendium from the
permit authority or local control
authority (as applicable) prior to
determining such discharge parameter
values, unless the manufacturer already
has a copy.
• 23. Part 455 is amended by removing
and reserving Table 7 to Part 455.

PART 465—COIL COATING POINT
SOURCE CATEGORY

• 24. The authority citation for Part 465
continues to read as follows:
  Authority: Sees. 301,304 (b), (c), (e), and
(g), 306 (b) and (c), 307 (b) and (c), and 501
of the Clean Water Act (the Federal Water
Pollution Control Act of 1972, as amended by
the Clean Water Act of 1977)(the "Act"); 33
U.S.C. 1311, 1314 (b), (c), (e), and (g), 1316
(b) and (c), 1317 (b) and (c}, and 1361; 86
Stat. 816, Pub. L. 92-500; 91 Stat. 1567, Pub.
L. 95-217.

• 25. Section 465.03 is amended by
revising paragraph (c) to read as follows:

§465.03  Monitoring and reporting
requirements.
*    *    *    *     *

  (c) The analytical method required for
determination of petroleum
hydrocarbons (non-polar material) is
given under the listing for "oil and
grease" at 40 CFR  I36.3(a), Table IB and
must be used after December 31, 2005.
*    A    *    *     *

[FRDoc. 07-1073 Filed 3-9-07; 8:45 am]
BILLING CODE 6560-50-P
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