[Federal Register Volume 72, Number 47 (Monday, March 12, 2007)]
[Rules and Regulations]
[Pages 11200-11249]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 07-1073]
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Part III
Environmental Protection Agency
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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
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules
and Regulations
[[Page 11200]]
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ENVIRONMENTAL PROTECTION AGENCY
40 CFR Parts 122, 136, 141, 143, 430, 455, and 465
[EPA-HQ-OW-2003-0070; FRL-8203-8]
RIN 2040-AD71
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
AGENCY: Environmental Protection Agency (EPA).
ACTION: Final rule.
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SUMMARY: This rule modifies the testing procedures approved for
analysis and sampling under the Clean Water Act 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outdated methods, and changes to sample collection, preservation, and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.regulations.gov or in hard copy at the HQ Water Docket Center, EPA/
DC, EPA West, Room 3334, 1301 Constitution Ave., NW., Washington, DC.
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal holidays. The telephone number for the
Public Reading Room is (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:
[email protected]). 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: [email protected]).
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:
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Examples of potentially regulated
Category entities
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State, Territorial, and Indian States, Territories, and Tribes
Tribal Governments. authorized to administer the NPDES
permitting program; States,
Territories, and Tribes providing
certification under Clean Water Act
section 401.
Industry.......................... Facilities that must conduct
monitoring to comply with NPDES
permits.
Municipalities.................... POTWs that must conduct monitoring
to comply with NPDES permits.
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This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be regulated by this
action. This table lists types of entities that EPA is now aware 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
[[Page 11201]]
one of the approved test procedures. Categories and entities that may
ultimately be subject to the requirements of today's rule include:
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Examples of potentially
Category regulated entities NAICS \1\
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State, Local, & Tribal States, local and tribal 924110
Governments. governments that
analyze water samples
on behalf of public
water systems required
to conduct such
analysis; States, local
and tribal governments
that themselves operate
community and non-
transient non-community
water systems required
to monitor.
Industry......................... Private operators of 221310
community and non-
transient non-community
water systems required
to monitor.
Municipalities................... Municipal operators of 924110
community and non-
transient non-community
water systems required
to monitor.
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\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)(1) 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 (SDWA), 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-International
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, IC, 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[supreg] 1010
IV. Response to Comments
A. Use of Syngenta 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
[[Page 11202]]
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-1)).
NPDWRs apply to public water systems pursuant to SDWA sections
1401(1)(A) (42 U.S.C. 300f(1)(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(1)(D)). 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-1)).
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 to the list of parameters at 40 CFR 122.21(j)(4)(viii).
B. 40 CFR 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-Cl 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-Cl 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 I-4545-85.
8. The rule approves a new method for determination of chlorine by
low level amperometry--SM 4500-Cl E [18th, 19th, 20th Editions] and SM
4500-Cl 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-Cl-D [18th, 19th, 20th Editions] and
SM 4500-Cl-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 Sec. 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 Sec. 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 Sec. 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
[[Page 11204]]
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 sulfate (40 CFR 141.23 and Sec. 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'' (HOCl- and OCl-) 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 [mu]g/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)(1) 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-1 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 1664A 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 Sec. 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
[[Page 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 Sec. 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 Sec.
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 Sec. 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 Sec.
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.
J. 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 Sec. 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 (HCl) 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 (SnCl2) and include addition of
[[Page 11206]]
HCl. 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 Sec. 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 Sec. 136.3, rather than take final action on the proposed text at
Sec. 136.7.
EPA proposed a new Sec. 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 Sec. 136.3(a), and Table II at Sec.
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, IC, 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 IC (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 Sec. 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.
EPA 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 [deg]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 Sec. 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 Sec. 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 Sec. 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 AG-625 for Determination of Atrazine
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
[[Page 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[reg] 1010
Because EPA is continuing to evaluate public comment about use of
the Microtox[reg] 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[reg]
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 of Atrazine
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 141.24(e)(1).
``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 [mu]g/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.''
The MCL for atrazine is 0.003 mg/L (3 [mu]g/L). Thus, any results
from Method AG-625 greater than 0.0015 mg/L (1.5 [mu]g/L) must be
confirmed through the use of another approved method for atrazine. In
such instances, the
[[Page 11208]]
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 Sec. 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 et seq.
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, and
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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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.
601(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
[[Page 11210]]
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.
I. 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.
J. Congressional Review Act
The Congressional Review Act, 5 U.S.C. Section 801 et seq., as
added by the Small Business Regulatory Enforcement Fairness Act of
1996, generally provides that before a rule may take effect, the agency
promulgating the rule must submit a rule report, which includes a copy
of the rule, to each House of the Congress and to the Comptroller
General of the United States. EPA will submit a report containing this
rule and other required information to the U.S. Senate, the U.S. House
of Representatives, and the Comptroller General of the United States
prior to publication of the rule in the Federal Register. 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 CFR Part 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.
[[Page 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.
0
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
0
1. The authority citation for Part 122 continues to read as follows:
Authority: The Clean Water Act, 33 U.S.C. 1251 et seq.
0
2. Section 122.1 is amended by revising paragraph (a)(4) to read as
follows:
Sec. 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.
* * * * *
0
3. Section 122.21 is amended as follows:
0
a. By revising paragraph (g)(7)(i).
0
b. By revising introductory text in paragraph (h)(4)(i).
0
c. By revising paragraph (j)(4)(viii).
Sec. 122.21 Application for a permit (applicable to State programs,
see Sec. 123.25)
* * * * *
(g) * * *
(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 Sec.
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 Sec.
122.26 (d)(2)(iii)(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.
* * * * *
(j) * * *
(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.
* * * * *
0
4. Section 122.41 is amended by revising paragraphs (j)(4) and
(l)(4)(ii) to read as follows:
Sec. 122.41 Conditions applicable to all permits (applicable to State
programs, see Sec. 123.25).
* * * * *
(j) * * *
(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.
* * * * *
(l) * * *
(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.
* * * * *
[[Page 11212]]
0
5. Section 122.44 is amended by revising paragraph (i)(1)(iv) to read
as follows:
Sec. 122.44 Establishing limitations, standards, and other permit
conditions (applicable to State NPDES programs; see Sec. 123.25).
* * * * *
(i) * * *
(1) * * *
(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
0
6. The authority citation for Part 136 continues to read as follows:
Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91
Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977.)
0
7. Section 136.3 is amended as follows:
0
a. In paragraph (a) by revising the introductory text and Tables IA,
IB, IC, ID, and IE.
0
b. In paragraph (a) by adding Table IG after the notes of Table IF.
0
c. In paragraph (b) by revising references 6, 10, and 17, and adding
references 63 through 69.
0
d. By revising paragraphs (c), (d), and (e).
Sec. 136.3 Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are
listed together with test procedure descriptions and references in
Tables IA, IB, IC, ID, IE, IF, and IG. In the event of a conflict
between the reporting requirements of 40 CFR Parts 122 and 125 and any
reporting requirements associated with the methods listed in these
tables, the provisions of 40 CFR Parts 122 and 125 are controlling and
will determine a permittee's reporting requirements. The full text of
the referenced test procedures are incorporated by reference into
Tables IA, IB, IC, ID, IE, IF, 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_of_federal_regulations/ibr_locations.html
These test procedures are incorporated as they exist on the day of
approval and a notice of any change in these test procedures will be
published in the Federal Register. The discharge parameter values for
which reports are required must be determined by one of the standard
analytical test procedures incorporated by reference and described in
Tables IA, IB, IC, 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 Sec. Sec. 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
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods Standard methods AOAC, ASTM,
Parameter and units Method \1\ EPA 18th, 19th, 20th Ed. online USGS Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), Most Probable p. 132 \3\.......... 9221C or E.......... 9221C or E-99........
number per 100 mL. Number (MPN),
5 tube 3
dilution, or
Membrane filter p. 124 \3\.......... 9222D............... 9222D-97............. B-0050-85 \5\.
(MF) \2\,
single step.
2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 \3\.......... 9221C or E.......... 9221C or E-99........
presence of chlorine, dilution, or
number per 100 mL.
MF, single step p. 124 \3\.......... 9222D............... 9222D-97.............
\6\.
3. Coliform (total), MPN, 5 tube, 3 p. 114 \3\.......... 9221B............... 9221B-99.............
number per 100 mL. dilution, or
MF \2\, single p. 108 \3\.......... 9222B............... 9222B-97............. B-0025-85 \5\.
step or two
step.
4. Coliform (total), in MPN, 5 tube, 3 p. 114 \3\.......... 9221B............... 9221B-99.............
presence of chlorine, dilution, or
number per 100 mL.
MF \2\ with p. 111 \3\.......... 9222 (B+B.5c)....... 9222 (B+B.5c)-97.....
enrichment.
5. E. coli, number per MPN \7,\ \9,\ .................... 9221B.1/9221F\12\ 9221B.1-99/9221F\12\
100 mL \28\. \15\, multiple \14\. \14\.
tube,
[[Page 11213]]
multiple tube/ .................... 9223B \13\.......... 9223B-97 \13\........ 991.15 \11\... Colilert[supreg]
multiple well, \13,\ \17\,
Colilert-18[supreg]
\13,\ \16,\ \17\
MF two step, or 1103.1 \20\......... 9222B/9222G \19\, 9222B-97/9222G \19\.. D5392-93 \10\.
9213D.
single step.... 1603 \21\, 1604 \22\ .................... ..................... .............. mColiBlue-24[supreg]
\18\
6. Fecal streptococci, MPN, 5 tube, 3 p. 139 \3\.......... 9230B............... 9230B-93.............
number per 100 mL. dilution,.
MF \2\, or..... p. 136 \3\.......... 9230C............... 9230C-93............. B-0055-85 \5\.
Plate count.... p. 143 \3\..........
7. Enterococci, number MPN \7,\ \9\ .................... 9230B............... 9230B-93.............
per 100 mL \28\. multiple tube,.
multiple tube/ .................... .................... ..................... D6503-99 \10\. Entero-lert[supreg]
multiple well. \13,\ \23\
MF \2,\ \6,\ 1106.1 \24\......... 9230C............... 9230C-93............. D5259-92 \10\.
\7,\ \8,\ \9\, 1600 \25\...........
two step. p. 143 \3\..........
single step, or
Plate count....
Protozoa:
8. Crypto-sporidium \28\. Filtration/IMS/ 1622 \26\, 1623 \27\
FA.
9. Giardia \28\.......... Filtration/IMS/ 1623 \27\...........
FA.
Aquatic Toxicity:
10. Toxicity, acute, Ceriodaphnia 2002.0 \29\.........
fresh water organisms, dubia acute.
LC50, percent effluent.
Daphnia puplex 2021.0 \29\.........
and Daphnia
magna acute.
Fathead Minnow, 2000.0 \29\.........
Pimephales
promelas, and
Bannerfin
shiner,
Cyprinella
leedsi, acute.
Rainbow Trout, 2019.0 \29\.........
Oncorhynchus
mykiss, and
brook trout,
Salvelinus
fontinalis,
acute.
11. Toxicity, acute, Mysid, 2007.0 \29\.........
estuarine and marine Mysidopsis
organisms of the bahia, acute.
Atlantic Ocean and Gulf
of Mexico, LC50, percent
effluent.
Sheepshead 2004.0 \29\.........
Minnow,
Cyprinodon
variegatus,
acute.
Silverside, 2006.0 \29\.........
Menidia
beryllina,
Menidia
menidia, and
Menidia
peninsulae,
acute.
12. Toxicity, chronic, Fathead minnow, 1000.0 \30\.........
fresh water organisms, Pimephales
NOEC or IC25, percent promelas,
effluent. larval
survival and
growth.
Fathead minnow, 1001.0 \30\.........
Pimephales
promelas,
embryo-larval
survival and
teratogenicity.
Daphnia, 1002.0 \30\.........
Ceriodaphnia
dubia,
survival and
reproduction.
[[Page 11214]]
Green alga, 1003.0 \30\.........
Selenastrum
capricornutum,
growth.
13. Toxicity, chronic, Sheepshead 1004.0 \31\.........
estuarine and marine minnow,
organisms of the Cyprinodon
Atlantic Ocean and Gulf variegatus,
of Mexico, NOEC or IC25, larval
percent effluent. survival and
growth.
Sheepshead 1005.0 \31\.........
minnow,
Cyprinodon
variegatus,
embryo-larval
survival and
teratogenicity.
Inland 1006.0 \31\.........
silverside,
Menidia
beryllina,
larval
survival and
growth.
Mysid, 1007.0 \31\.........
Mysidopsis
bahia,
survival,
growth, and
fecundity.
Sea urchin, 1008.0 \31\.........
Arbacia
punctulata,
fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45-[mu] membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.
\4\ [Reserved]
\5\ USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and
Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of 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.
\7\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
\8\ When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncoliform bacteria, or samples that
may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
comparability of results.
\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.
\10\ 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.
\11\ 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 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate
and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent
of all total coliform-positive tubes on a seasonal basis.
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth
or acidity within 48 h 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supplemented in the
laboratory with 50 [mu]g/mL of MUG may be used.
\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[supreg] may be enumerated with
the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg] 2000, and the MPN calculated from the table provided by the manufacturer.
\16\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\17\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\18\ A description of the mColiBlue24[supreg] test, Total Coliforms and E. 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 NA MUG media.
\20\ USEPA. 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.
\21\ USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (
modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-023.
\22\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. 2002. Method 1604:
Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.
Environmental Protection Agency, Office of Water, Washington, DC, EPA 821-R-02-024.
\23\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
[[Page 11215]]
\24\ USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental
Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-021.
\25\ USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). U.S.
Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-02-022.
\26\ Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA-
821-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 simultaneous detection
of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.
Environmental Protection Agency, Office of Water, Washington, DC, EPA-821-R-01-025.
\28\ 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.
[[Page 11216]]
Table IB.--List of Approved Inorganic Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
----------------------------------------------------------------------------------------------------------------------------------------------
Parameter Methodology \58\ Standard methods Standard methods Standard methods
EPA \35,\ \52\ (18th, 19th) (20th) online ASTM USGS/AOAC/other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L.... Electrometric ...................... 2310 B(4a)............ 2310 B(4a)............ 2310 B(4a)-97.......... D1067-92, 02......... I-1020-85 \2\
endpoint or
phenolphthalein
endpoint.
2. Alkalinity, as CaCO3, mg/L. Electrometric or ...................... 2320 B................ 2320 B................ 2320 B-97.............. D1067-92, 02......... 973.43 \3\, I-1030-85
Colorimetric \2\
titration to pH
4.5, manual, or
automatic........ 310.2 (Rev. 1974) \1\. ...................... ...................... ....................... ..................... I-2030-85 \2\
3. Aluminum--Total,\4\ mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99.............. ..................... I-3051-85 \2\
aspiration \36\.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99..............
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-9750
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14\3\
Direct Current ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Plasma (DCP)
\36\.
Colorimetric ...................... 3500-Al D............. 3500-Al B............. 3500-Al B-01...........
(Eriochrome
cyanine R).
4. Ammonia (as N), mg/L....... Manual, 350.1, Rev. 2.0 (1993) 4500-NH B3............ 4500-NH3 B............ 4500-NH3 B-97.......... ..................... 973.49 \3\
distillation (at
pH 9.5) \6\
followed by:
Nesslerization... ...................... 4500-NH3 C (18th only) ...................... ....................... D1426-98, 03 (A)..... 973.49 \3\, I-3520-85
\2\
Titration........ ...................... 4500-NH3 C (19th) and 4500-NH3 C............ 4500-NH3 C-97..........
4500-NH3 E (18th).
Electrode........ ...................... 4500-NH3 D or E (19th) 4500-NH3 D or E....... 4500-NH3 D or E-97..... D1426-98, 03 (B).....
and 4500-NH3 F or G
(18th).
Automated 350.1 \60\, Rev. 2.0 4500-NH3 G (19th) and 4500-NH3 G............ 4500-NH3 G-97.......... ..................... I-4523-85 \2\
phenate, or. (1993). 4500-NH3 H (18th).
Automated ...................... ...................... ...................... ....................... ..................... See footnote 7
electrode.
Ion ...................... ...................... ...................... ....................... D6919-03.............
Chromatography.
5. Antimony--Total, \4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration \36\.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99..............
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
6. Arsenic--Total, \4\ mg/L... Digestion \4\ 206.5 (Issued 1978)
followed by. \1\.
AA gaseous ...................... 3114 B 4.d............ ...................... 3114 B 4.d-97.......... D2972-97, 03 (B)..... I-3062-85 \2\
hydride.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D2972-97, 03 (C)..... I-4063-98 \49\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
Colorimetric ...................... 3500-As C............. 3500-As B............. 3500-As B-97........... D2972-97, 03 (A)..... I-3060-85
(SDDC).
7. Barium--Total,\4\ mg/L..... Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99.............. ..................... I-3084-85 \2\
aspiration \36\.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D4382-95, 02.........
[[Page 11217]]
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP \36\......... ...................... ...................... ...................... ....................... ..................... See footnote \34\
8. Beryllium--Total,\4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99.............. D3645-93 (88), 03 (A) I-3095-85 \2\
aspiration.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D3645-93 (88), 03 (B)
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP, or.......... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Be D.............
(aluminon).
9. Biochemical oxygen demand Dissolved Oxygen ...................... 5210 B................ 5210 B................ 5210 B-01.............. ..................... 973.44,\3\ p. 17.\9\,
(BOD5), mg/L. Depletion. I-1578-78 \8\
10. Boron--Total,\37\ mg/L.... Colorimetric ...................... 4500-B B.............. 4500-B B.............. 4500-B B-00............ ..................... I-3112-85 \2\
(curcumin).
ICP/AES, or...... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B 99.............. ..................... I-4471-97 \50\
DCP.............. ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote 34
11. Bromide, mg/L............. Titrimetric...... ...................... ...................... ...................... ....................... D1246-95, 99 (C)..... p. S44.\10\
................. ...................... ...................... ...................... ....................... ..................... I-1125-85 \2\
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
12. Cadmium--Total,\4\ mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D3557-95, 02 (A or B) 974.27,\3\ p. 37.\9\,
aspiration \36\. I-3135-85 \2\ or I-
3136-85 \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D3557-95, 02 (D)..... I-4138-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-1472-85\2\ or I-
4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP \36\......... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Voltametry \11\, ...................... ...................... ...................... ....................... D3557-95, 02 (C).....
or.
Colorimetric ...................... 3500-Cd D.............
(Dithizone).
13. Calcium--Total,\4\ mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. D511-93, 03(B)....... I-3152-85 \2\
aspiration.
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
DCP, or.......... ...................... ...................... ...................... ....................... ..................... See footnote \34\
Titrimetric ...................... 3500-Ca D............. 3500-Ca B............. 3500-Ca B-97........... D511-93, 03(A).......
(EDTA).
Ion ...................... ...................... ...................... ....................... D6919-03.............
Chromatography.
14. Carbonaceous biochemical Dissolved Oxygen ...................... 5210 B................ 5210 B................ 5210 B-01..............
oxygen demand (CBOD5), mg/L Depletion with
\12\. nitrification
inhibitor.
15. Chemical oxygen demand Titrimetric...... 410.3 (Rev. 1978) \1\. 5220 C................ 5220 C................ 5220 C-97.............. D1252-95, 00 (A)..... 973.46 \3\, p. 17 \9\
(COD), mg/L. I-3560-85 \2\
Spectrophotometri 410.4, Rev. 2.0 (1993) 5220 D................ 5220 D................ 5220 D-97.............. D1252-95, 00 (B)..... See footnotes \13,
c, manual or 14\. I-3561-85 \2\
automatic.
16. Chloride, mg/L............ Titrimetric: ...................... 4500-Cl-B............. 4500-Cl-B............. 4500-Cl-B-97........... D512-89(99) (B)...... I-1183-85 \2\
(silver nitrate)
or.
(Mercuric ...................... 4500-Cl-C............. 4500-Cl-C............. 4500-Cl-C-97........... D512-89 (99) (A)..... 973.51 \3\, I-1184-85
nitrate). \2\
Colorimetric: ...................... ...................... ...................... ....................... ..................... I-1187-85 \2\
manual or.
Automated ...................... 4500-Cl-E............. 4500-Cl-E............. 4500-Cl-E-97........... ..................... I-2187-85 \2\
(Ferricyanide).
Potentiometric ...................... 4500-Cl-D............. 4500-Cl-D............. 4500-Cl-D-97...........
Titration.
Ion Selective ...................... ...................... ...................... ....................... D512-89(99)(C).......
Electrode.
[[Page 11218]]
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
17. Chlorine--Total residual, Amperometric ...................... 4500-Cl D............. 4500-Cl D............. 4500-Cl D-00........... D1253-86 (96), 03....
mg/L; Titrimetric. direct, or.
Amperometric ...................... 4500-Cl E............. 4500-Cl E............. 4500-Cl E-00...........
direct (low
level).
Iodometric direct ...................... 4500-Cl B............. 4500-Cl B............. 4500-Cl B-00...........
Back titration ...................... 4500-Cl C............. 4500-Cl C............. 4500-Cl C-00...........
ether end-point
\15\ or.
DPD-FAS.......... ...................... 4500-Cl F............. 4500-Cl F............. 4500-Cl F-00...........
Spectrophotometri ...................... 4500-Cl G............. 4500-Cl G............. 4500-Cl G-00...........
c, DPD or.
Electrode........ ...................... ...................... ...................... ....................... ..................... See footnote \16\
18. Chromium VI dissolved, mg/ 0.45-micron
L. Filtration
followed by:
AA chelation- ...................... 3111 C................ ...................... 3111 C-99.............. ..................... I-1232-85
extraction or.
Ion 218.6, Rev. 3.3 (1994) 3500-Cr E............. 3500-Cr C............. 3500-Cr C-01........... D5257-97............. 993.23
Chromatography.
Colorimetric ...................... 3500-Cr D............. 3500-Cr B............. 3500-Cr B-01........... D1687-92, 02 (A)..... I-1230-85
(Diphenyl-carbaz
ide).
19. Chromium--Total,\4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. D1687-92, 02 (B)..... 974.27 \3\, I-3236-85
aspiration \36\. \2\
AA chelation- ...................... 3111 C................ ...................... 3111 C-99..............
extraction.
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D1687-92, 02 (C)..... I-3233-93 \46\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP,\36\ or...... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Cr D............. 3500-Cr B............. 3500-Cr B-01...........
(Diphenyl-carbaz
ide).
20. Cobalt--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D3558-94, 03 (A or B) p. 37 \9\, I-3239-85
aspiration. \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D3558-94, 03 (C)..... I-4243-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP.............. ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
21. Color, platinum cobalt Colorimetric ...................... 2120 E................ 2120 E................ ....................... ..................... See footnote \18\
units or dominant wavelength, (ADMI), or.
hue, luminance purity.
(Platinum ...................... 2120 B................ 2120 B................ 2120 B-01.............. ..................... I-1250-85 \2\
cobalt), or.
Spectrophotometri ...................... 2120 C................ 2120 C................
c.
22. Copper--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D1688-95, 02 (A or B) 974.27 \3\ p. 37 \9\
aspiration \36\. I-3270-85 \2\ or I-
3271-85 \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D1688-95, 02 (C)..... I-4274-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP \36\ or...... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Cu D............. 3500-Cu B............. 3500-Cu B-99...........
(Neocuproine) or.
(Bicinchoninate). ...................... 3500-Cu E............. 3500-Cu C............. 3500-Cu C-99........... ..................... See footnote \19\
[[Page 11219]]
23. Cyanide--Total, mg/L...... Automated ...................... ...................... ...................... ....................... ..................... Kelada-01 \55\
Distillation and
Colorimetry, or.
Manual 335.4, Rev. 1.0 (1993) 4500-CN C............. 4500-CN C............. ....................... D2036-98(A).......... 10-204-00-1-X \56\
distillation \57\.
with MgCl2
followed by:
Titrimetric or... ...................... 4500-CN D............. 4500-CN D............. 4500-CN D-99........... ..................... p. 22 \9\
Spectrophotometri ...................... 4500-CN E............. 4500-CN E............. 4500-CN E-99........... D2036-98(A).......... I-3300-85
c, manual or.
Automated \20\ or 335.4, Rev. 1.0 (1993) ...................... ...................... ....................... ..................... 10-204-00-1-X \56\, I-
\57\. 4302-85 \2\
Ion Selective ...................... 4500-CN F............. 4500-CN F............. 4500-CN F-99........... D2036-98(A)..........
Electrode.
24. Available Cyanide, mg/L... Cyanide Amenable ...................... 4500-CN G............. 4500-CN G............. 4500-CN G-99........... D2036-98(B)..........
to Chlorination
(CATC); Manual
distillation
with MgCl2
followed by
Titrimetric or
Spectrophotometr
ic.
Flow injection ...................... ...................... ...................... ....................... D6888-04............. OIA-1677 \44\
and ligand
exchange,
followed by
amperometry \61\.
Automated ...................... ...................... ...................... ....................... ..................... Kelada-01 \55\
Distillation and
Colorimetry.
25. Fluoride--Total, mg/L..... Manual ...................... 4500-F B.............. 4500-F B.............. 4500-F B-97............
distillation\6\
followed by:
Electrode, manual ...................... 4500-F B.............. 4500-F B.............. 4500-F C-97............ D1179-93, 99 (B).....
or.
Automated........ ...................... ...................... ...................... ....................... ..................... I-4327-85 \2\
Colorimetric, ...................... 4500-F D.............. 4500-F D.............. 4500-F D-97............ D1179-93, 99 (A).....
(SPADNS) or.
Automated ...................... 4500-F E.............. 4500-F E.............. 4500-F E-97............
complexone.
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97,03.......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
26. Gold--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration, or.
AA furnace, or... 231.2 (Rev. 1978) \1\.
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
27. Hardness--Total, as CaCO3, Automated 130.1 (Issued 1971)
mg/L. colorimetric,. \1\.
Titrimetric ...................... 2340 B or C........... 2340 B or C........... 2340 B or C-97......... D1126-86(92), 02..... 973.5 2B \3\, I-1338-
(EDTA) or. 85\2\
Ca plus Mg as
their
carbonates, by
inductively
coupled plasma
or AA direct
aspiration. (See
Parameters 13
and 33)..
28. Hydrogen ion (pH), pH Electrometric ...................... 4500-H+ B............. 4500-H+ B............. 4500-H+ B-00........... D1293-84 (90), 99 (A 973.41.\3\, I-1586-85
units. measurement or. or B). \2\
Automated 150.2 (Dec. 1982) \1\. ...................... ...................... ....................... ..................... See footnote\21\, I-
electrode. 2587-85\2\
29. Iridium--Total,\4\ mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration or.
AA furnace....... 235.2 (Issued 1978)
\1\.
30. Iron--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D1068-96, 03 (A or B) 974.27 \3\, I-3381-85
aspiration \36\. \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D1068-96, 03 (C).....
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
DCP \36\ or...... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Fe D............. 3500-Fe B............. 3500-Fe B-97........... D1068-96, 03 (D)..... See footnote \22\
(Phenanthroline).
31. Kjeldahl Nitrogen \5\-- Digestion and ...................... 4500-Norg B or C and 4500-Norg B or C and 4500-Norg B or C-97 and D3590-89, 02 (A).....
Total, (as N), mg/L. distillation 4500-NH3 B. 4500-NH3 B. 4500-NH3 B-97.
followed by:
\20\
Titration or..... ...................... 4500-NH3 C (19th) and 4500-NH3 C............ 4500-NH3 C-97.......... D3590-89, 02 (A)..... 973.48 \3\
4500-NH 3 E (18th).
[[Page 11220]]
Nesslerization or ...................... 4500-NH3 C (18th Only) ...................... ....................... D3590-89, 02 (A).....
Electrode........ ...................... 4500-NH3 F or G (18th) 4500-NH3 D or E....... 4500-NH3 D or E-97.....
and 4500-NH3 D or E
(19th).
Automated phenate 351.1 (Rev. 1978) \1\. ...................... ...................... ....................... ..................... I-4551-78 \8\
colorimetric.
Semi-automated 351.2, Rev. 2.0 (1993) ...................... ...................... ....................... D3590-89, 02 (B)..... I-4515-91 \45\
block digestor
colorimetric.
Manual or block ...................... ...................... ...................... ....................... D3590-89, 02 (A).....
digestor
potentiometric.
Block digester, ...................... ...................... ...................... ....................... ..................... See footnote \39\
followed by Auto
distillation and
Titration, or.
Nesslerization, ...................... ...................... ...................... ....................... ..................... See footnote \40\
or.
Flow injection ...................... ...................... ...................... ....................... ..................... See footnote \41\
gas diffusion.
32. Lead--Total,\4\ mg/L...... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D3559-96, 03 (A or B) 974.27 \3\, I-3399-85
aspiration \36\. \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D3559-96, 03 (D)..... I-4403-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP \36\......... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Voltametry \11\ ...................... ...................... ...................... ....................... D3559-96, 03 (C).....
or.
Colorimetric ...................... 3500-Pb D............. 3500-Pb B............. 3500-Pb B-97...........
(Dithizone).
33. Magnesium--Total,\4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. D511-93, 03(B)....... 974.27 \3\, I-3447-85
aspiration. \2\
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
DCP or........... ...................... ...................... ...................... ....................... ..................... See footnote \34\
Gravimetric...... ...................... 3500-Mg D.............
Ion ...................... ...................... ...................... ....................... D6919-03.............
Chromatography.
34. Manganese--Total,\4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. D858-95, 02 (A or B). 974.27 \3\, I-3454-85
aspiration \36\. \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D858-95, 02 (C)......
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP36, or........ ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500--Mn D............ 3500-Mn B............. 3500-Mn B-99........... ..................... 920.203 \3\
(Persulfate), or.
(Periodate)...... ...................... ...................... ...................... ....................... ..................... See footnote \23\
35. Mercury--Total \4\, mg/L.. Cold vapor, 245.1, Rev. 3.0 (1994) 3112 B................ ...................... 3112 B-99.............. D3223-97, 02......... 977.22 \3\, I-3462-
manual or. 85\2\
Automated........ 245.2 (Issued 1974)...
Cold vapor atomic 245.7 Rev. 2.0 (2005)
fluorescence \59\.
spectrometry
(CVAFS).
Purge and Trap 1631E \43\............
CVAFS.
36. Molybdenum--Total \4\, mg/ Digestion \4\
L. followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99.............. ..................... I-3490-85 \2\
aspiration.
[[Page 11221]]
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. ..................... I-3492-96 \47\
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
37. Nickel--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D1886-90, 94 (98) (A I-3499-85 \2\
aspiration \36\. or B).
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D1886-90, 94 (98) (C) I-4503-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP \36\, or..... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Ni D (17th
(heptoxime). Edition).
38. Nitrate (as N), mg/L...... Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
Ion Selective ...................... 4500-NO3 D........... 4500-NO3 D........... 4500-NO3 D-00.........
Electrode.
Colorimetric 352.1 \1\............. ...................... ...................... ....................... ..................... 973.50 \3\, 419D \1,\
(Brucine \7\, p. 28 \9\
sulfate), or.
Nitrate-nitrite N
minus Nitrite N
(See parameters
39 and 40)..
39. Nitrate-nitrite (as N), mg/ Cadmium ...................... 4500-NO3 E............ 4500-NO3 E............ 4500-NO3 E-00.......... D3867-99(B)..........
L. reduction,
manual or.
Automated, or.... 353.2, Rev. 2.0 (1993) 4500-NO3 F............ 4500-NO3 F............ 4500-NO3 F-00.......... D3867-99(A).......... I-4545-85 \2\
Automated ...................... 4500-NO3 H............ 4500-NO3 H............ 4500-NO3 H-00..........
hydrazine.
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97............. 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
40. Nitrite (as N), mg/L...... Spectrophotometri ...................... 4500-NO2 B............ 4500-NO2 B............ 4500-NO2 B-00.......... ..................... See footnote \25\
c: Manual or.
Automated ...................... ...................... ...................... ....................... ..................... I-4540-85 \2\
(Diazotization).
Automated 353.2, Rev. 2.0 (1993) 4500-NO3 F............ 4500-NO3 F............ 4500-NO3 F-00.......... D3867-99(A).......... I-4545-85 \2\
(*bypass cadmium
reduction).
Manual (*bypass ...................... 4500-NO3 E............ 4500-NO3 E............ 4500-NO3 E-00.......... D3867-99(B)..........
cadmium
reduction).
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev.2 \54\
41. Oil and grease--Total Hexane 1664A \42\............ ...................... 5520 B \38\........... 5520 B-01 \38\.........
recoverable, mg/L. extractable
material (HEM):
n-Hexane
extraction and
gravimetry.
Silica gel 1664A \42\............
treated HEM (SGT-
HEM): Silica gel
treatment and
gravimetry..
42. Organic carbon--Total Combustion or ...................... 5310 B, C, or D....... 5310 B, C, or D....... 5310 B, C, or D-00..... D2579-93 (A or B).... 973.47,\3\ p. 14 \24\
(TOC), mg/L. oxidation.
43. Organic nitrogen (as N), Total Kjeldahl N
mg/L. (Parameter 31)
minus ammonia N
(Parameter 4).
44. Orthophosphate (as P), mg/ Ascorbic acid
L. method:.
Automated, or.... 365.1, Rev. 2.0 (1993) 4500-P F.............. 4500-P F.............. ....................... ..................... 973.56 \3\, I-4601-85
\2\
Manual single ...................... 4500-P E.............. 4500-P E.............. ....................... D515-88(A)........... 973.55 \3\
reagent.
Manual two 365.3 (Issued 1978)\1\
reagent.
[[Page 11222]]
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
45. Osmium--Total \4\, mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99..............
aspiration, or.
AA furnace....... 252.2 (Issued 1978)
\1\.
46. Oxygen, dissolved, mg/L... Winkler (Azide ...................... 4500-O C.............. 4500-O C.............. 4500-O C-01............ D888-92, 03 (A)...... 973.4 5B \3\, I-1575-
modification), 78 \8\
or.
Electrode........ ...................... 4500-O G.............. 4500-O G.............. 4500-O G-01............ D888-92, 03 (B)...... I-1576-78 \8\
47. Palladium--Total,\4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. ..................... p. S27 \10\
aspiration, or.
AA furnace....... 253.2 \1\ (Issued ...................... ...................... ....................... ..................... p. S28 \10\
1978).
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
48. Phenols, mg/L............. Manual 420.1 \1\ (Rev. 1978). ...................... ...................... ....................... ..................... See footnote \27\
distillation
\26\ Followed
by:
Colorimetric 420.1 \1\ (Rev. 1978). ...................... ...................... ....................... ..................... See footnote \27\
(4AAP) manual,
or.
Automated........ 420.4 Rev. 1.0 (1993).
49. Phosphorus (elemental), mg/ Gas-liquid ...................... ...................... ...................... ....................... ..................... See footnote \28\
L. chromatography.
50. Phosphorus--Total, mg/L... Persulfate ...................... 4500-P B.5............ 4500-P B.5............ ....................... ..................... 973.55 \3\
digestion
followed by:
\20\
Manual or........ 365.3 \1\ (Issued 4500-P E.............. 4500-P E.............. ....................... D515-88(A)...........
1978).
Automated 365.1 Rev. 2.0 (1993). 4500-P F.............. 4500-P F.............. ....................... ..................... 973.56 \3\, I-4600-85
ascorbic acid \2\
reduction.
Semi-automated 365.4 \1\ (Issued ...................... ...................... ....................... D515-88(B)........... I-4610-91 \48\
block digestor. 1974).
51. Platinum--Total,\4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration.
AA furnace....... 255.2 \1\.............
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
52. Potassium--Total,\4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. ..................... 973.53 \3\, I-3630-85
aspiration. \2\
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
Flame ...................... 3500-K D.............. 3500-K B.............. 3500-K B-97............
photometric, or.
Colorimetric..... ...................... ...................... ...................... ....................... ..................... 317 B \17\
Ion ...................... ...................... ...................... ....................... D6919-03.............
Chromatography.
53. Residue--Total, mg/L...... Gravimetric, 103- ...................... 2540 B................ 2540 B................ 2540 B-97.............. ..................... I-3750-85 \2\
105[deg].
54. Residue--filterable, mg/L. Gravimetric, ...................... 2540 C................ 2540 C................ 2540 C-97.............. ..................... I-1750-85 \2\
180[deg].
55. Residue--non-filterable Gravimetric, 103- ...................... 2540 D................ 2540 D................ 2540 D-97.............. ..................... I-3765-85 \2\
(TSS), mg/L. 105 [deg]C post
washing of
residue.
56. Residue--settleable, mg/L. Volumetric, ...................... 2540 F................ 2540 F................ 2540 F-97..............
(Imhoff cone),
or gravimetric.
57. Residue--Volatile, mg/L... Gravimetric, 550 160.4 \1\............. ...................... ...................... ....................... ..................... I-3753-85 \2\
[deg]C.
58. Rhodium--Total,\4\ mg/L... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration, or.
AA furnace....... 265.2 \1\.............
59. Ruthenium--Total,\4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration, or.
AA furnace....... 267.2 \1\.............
60. Selenium--Total,\4\ mg/L.. Digestion \4\
followed by:
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. D3859-98, 03 (B)..... I-4668-98 \49\
[[Page 11223]]
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
AA gaseous ...................... 3114 B................ ...................... 3114 B-97.............. D3859-98, 03 (A)..... I-3667-85 \2\
hydride.
61. Silica--Dissolved,\37\ mg/ 0.45 micron
L. filtration
followed by:
Colorimetric, ...................... 4500-Si D............. 4500-SiO2 C........... 4500-SiO2C-97.......... D859-94, 00.......... I-1700-85 \2\
Manual or.
Automated ...................... ...................... ...................... ....................... ..................... I-2700-85 \2\
(Molybdosilicate
), or.
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
62. Silver--Total,4, 31 mg/L.. Digestion 4, 29
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... ..................... 974.27 \3\, p. 37
aspiration. \9\, I-3720-85 \2\
AA furnace....... ...................... 3113 B................ ...................... 3113 B-99.............. ..................... I-4724-89 \51\
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
63. Sodium--Total,\4\ mg/L.... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. ..................... 973.54 \3\, I-3735-85
aspiration. \2\
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
DCP, or.......... ...................... ...................... ...................... ....................... ..................... See footnote \34\
Flame photometric ...................... 3500-Na D............. 3500-Na B............. 3500-Na B-97...........
Ion ...................... ...................... ...................... ....................... D 6919-03............
Chromatography.
64. Specific conductance, Wheatstone bridge 120.1 \1\ (Rev. 1982). 2510 B................ 2510 B................ 2510 B-97.............. D1125-95 (99) (A).... 973.40 \3\, I-2781-85
micromhos/cm at 25[deg]C. \2\
65. Sulfate (as SO4), mg/L.... Automated 375.2, Rev. 2.0 (1993)
colorimetric.
Gravimetric...... ...................... 4500-SO4 \2\ C or D... 4500-SO4 \2\ C or D... ....................... ..................... 925.54 \3\
Turbidimetric.... ...................... ...................... ...................... ....................... D516-90, 02.......... 426C \3\0
Ion 300.0, Rev 2.1 (1993) 4110 B................ 4110 B................ 4110 B-00.............. D4327-97, 03......... 993.30 \3\
Chromatography. and 300.1, Rev 1.0
(1997).
CIE/UV........... ...................... ...................... ...................... ....................... ..................... D6508, Rev. 2 \54\
66. Sulfide (as S), mg/L...... Titrimetric ...................... 4500-S \2\ F (19th) 4500-S \2\ F.......... 4500-S \2\ F-00........ ..................... I-3840-85 \2\
(iodine), or. 4500-S \2\ E (18th).
Colorimetric ...................... 4500-S \2\ D.......... 4500-S \2\ D.......... 4500-S \2\ D-00........
(methylene blue).
Ion Selective ...................... 4500-S \2\ G.......... 4500-S \2\ G.......... 4500-S \2\ G-00........ D4658-03.............
Electrode.
67. Sulfite (as SO3), mg/L.... Titrimetric ...................... 4500-SO3 \2\ B........ 4500-SO3 \2\ B........ 4500-SO3 \2\ B-00......
(iodine-iodate).
68. Surfactants, mg/L......... Colorimetric ...................... 5540 C................ 5540 C................ 5540 C-00.............. D2330-88, 02.........
(methylene blue).
69. Temperature, [deg]C....... Thermometric..... ...................... 2550 B................ 2550 B................ 2550 B-00.............. ..................... See footnote \32\
70. Thallium--Total, \4\ mg/L. Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99..............
aspiration.
AA furnace....... 279.2 \1\ (Issued
1978).
STGFAA........... 200.9, Rev. 2.2 (1994)
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99..............
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
71. Tin--Total,\4\ mg/L....... Digestion \4\
followed by:
AA direct ...................... 3111 B................ ...................... 3111 B-99.............. ..................... I-3850-78 \8\
aspiration.
AA furnace, or... ...................... 3113 B................ ...................... 3113 B-99..............
STGFAA........... 200.9, Rev. 2.2 (1994)
[[Page 11224]]
ICP/AES.......... 200.7, Rev. 4.4 (1994)
72. Titanium--Total,\4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99..............
aspiration.
AA furnace....... 283.2 \1\ (Issued
1978).
DCP.............. ...................... ...................... ...................... ....................... ..................... See footnote \34\
73. Turbidity, NTU \53\....... Nephelometric.... 180.1, Rev. 2.0 (1993) 2130 B................ 2130 B................ 2130 B-01.............. D1889-94, 00......... I-3860-85 \2\
74. Vanadium--Total,\4\ mg/L.. Digestion \4\
followed by:
AA direct ...................... 3111 D................ ...................... 3111 D-99..............
aspiration.
AA furnace....... ...................... ...................... ...................... ....................... D3373-93, 03.........
ICP/AES.......... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99.............. ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP, or.......... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-V D.............. 3500-V B.............. 3500-V B-97............
(Gallic Acid).
75. Zinc -Total \4\, mg/L..... Digestion \4\
followed by:
AA direct ...................... 3111 B or C........... ...................... 3111 B or C-99......... D1691-95, 02 (A or B) 974.27 \3\, p. 37
aspiration \36\. \9\, I-3900-85 \2\
AA furnace....... 289.2 \1\ (Issued
1978).
ICP/AES \36\..... 200.7, Rev. 4.4 (1994) 3120 B................ 3120 B................ 3120 B-99 \59\......... ..................... I-4471-97 \50\
ICP/MS........... 200.8, Rev. 5.4 (1994) ...................... ...................... ....................... D5673-03............. 993.14 \3\
DCP,\36\ or...... ...................... ...................... ...................... ....................... D4190-94, 99......... See footnote \34\
Colorimetric ...................... 3500-Zn E.............
(Dithizone) or.
(Zincon)......... ...................... 3500-Zn F............. 3500-Zn B............. 3500-Zn B-97........... ..................... See footnote \33\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI), EPA-600/4-79-020 (NTIS PB 84-
128677), Revised March 1983 and 1979 where applicable.
\2\ Fishman, M. J., et al. ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques of Water-Resource Investigations of the
U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.
\3\ ``Official Methods of Analysis of the Association of Official Analytical Chemists,'' Methods Manual, Sixteenth Edition, 4th Revision, 1998.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize
analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic
absorption determinations a digestion using nitric acid (as specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure
used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a
combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of ``Methods
for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using
the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury
by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up
should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique
or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used
with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the
digestion procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate may be used in place of mercuric sulfate.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual
distillation will be required to resolve any controversies.
\7\ Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
\8\ The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5, Chapter A1 (1979).
\9\ American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd st., New York, NY 10036.
\10\ ``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).
\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\ Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ``total BOD.'' The addition of the nitrification inhibitor is not
a procedural option, but must be included to report the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the
procedure for reporting the results. Only when a discharger's permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.
\14\ Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
[[Page 11225]]
\15\ The back titration method will be used to resolve controversy.
\16\ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph for the Orion
residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
\17\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
\18\ National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971.
\19\ Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\20\ When using a method with block digestion, this treatment is not required.
\21\ Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc.,
Elmsford, NY 10523.
\22\ Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\23\ Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.
\24\ Wershaw, R. L.,et al., ``Methods for Analysis of Organic Substances in Water,'' Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972
Revised 1987) p. 14.
\25\ Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The 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 10.00.2. 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.
\28\ R.F. Addison and R. G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,'' Journal of Chromatography, Vol. 47, No.3, pp. 421-426, 1970.
\29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such
as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12.
Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For
levels of silver below 1 mg/L the approved method is satisfactory.
\30\ The 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 adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After
digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and
adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well.
Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour.
Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ Stevens, H.H., Ficke, J. F., and Smoot, G. F., ``Water Temperature--Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the
U.S. Geological Survey, Book 1, Chapter D1, 1975.
\33\ Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\ ``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--Revised 1991, Thermo Jarrell Ash Corporation,
27 Forge Parkway, Franklin, MA 02038
\35\ Precision 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, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992. Available from the CEM Corporation.
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use n-hexane 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.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.
\40\ Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.
\41\ Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842.
\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and
Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161.
\43\ USEPA. 2001. Method 1631, Revision E, ``Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry'' September 2002, Office of Water, U.S.
Environmental Protection Agency (EPA-821-R-02-024). The application of clean techniques described in EPA's draft Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality
Criteria Levels (EPA-821-R-96-011) are recommended to preclude contamination at low-level, trace metal determinations.
\44\ Available Cyanide, Method OIA-1677, ``Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,'' ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX
77842-9010.
\45\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method,'' Open File Report
(OFR) 00-170.
\46\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry,'' Open
File Report (OFR) 93-449.
\47\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry,'' Open File
Report (OFR) 97-198.
\48\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish
That Includes Dialysis'' Open File Report (OFR) 92-146.
\49\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption
Spectrometry'' Open File Report (OFR) 98-639.
\50\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission
Spectrometry and Inductively Coupled Plasma-Mass Spectrometry,'' Open File Report (OFR) 98-165.
\51\ ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment,'' Open File
Report (OFR) 93-125.
\52\ All EPA methods, excluding EPA Method 300.1, are published in ``Methods for the Determination of Metals in Environmental Samples,'' Supplement I, National Exposure Risk Laboratory-
Cincinnati (NERL-CI), EPA/600/R-94/111, May 1994; and ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' NERL-CI, EPA/600/R-93/100, August, 1993. EPA Method
300.1 is available from http://www.epa.gov/safewater/methods/pdfs/met300.pdf.
\53\ Styrene divinyl benzene beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin.
\54\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,'' available from
Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
\55\ Kelada-01, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,'' EPA 821-B-01-009, Revision 1.2, August 2001, National Technical Information
Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001-108275]. 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.
\56\ QuikChem Method 10-204-00-1-X, ``Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis'' is
available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414-358-4200.
\57\ When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method, approved digestion and/or distillation are
required prior to analysis.
\59\ Method 245.7, Rev. 2.0, ``Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,'' February 2005, EPA-821-R-05-001, available from the U.S. EPA Sample Control Center (operated
by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304, Telephone: 703-461-2100, Fax: 703-461-8056.
[[Page 11226]]
\60\ The 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 exchange reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples.
[[Page 11227]]
Table IC.--List of Approved Test Procedures for Non-Pesticide Organic Compounds
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA method number \2,\ \7\ Other approved methods
--------------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter \1\ Standard Methods
GC GC/MS HPLC [Edition(s)] Standard Methods Online ASTM Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................. 610 625, 1625B........... 610 6440 B [18th, 19th, ........................ D4657-92 (99)........... See footnote \9\, p. 27
20th].
2. Acenaphthylene................ 610 625, 1625B........... 610 6410 B, 6440 B, [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
3. Acrolein...................... 603 624 \4\, 1624B.......
4. Acrylonitrile................. 603 624 \4\, 1624B.......
5. Anthracene.................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
6. Benzene....................... 602 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th,19th], 6200 C
[20th] and 6220 B
[18th,19th].
7. Benzidine..................... .............. 625 \5\, 1625B....... 605 ........................ ........................ ........................ See footnote \3\, p.1
8. Benzo(a)anthracene............ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
9. Benzo(a)pyrene................ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
10. Benzo(b)fluoranthene......... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
11. Benzo(g,h,i) perylene........ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
12. Benzo(k) fluoranthene........ 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
13. Benzyl chloride.............. .............. ..................... .............. ........................ ........................ ........................ See footnote \3\, p.
130: See footnote \6\,
p. S102
14. Benzyl butyl phthalate....... 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
15. Bis(2-chloroethoxy) methane.. 611 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
16. Bis(2-chloroethyl) ether..... 611 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
17. Bis(2-ethylhexyl) phthalate.. 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
18. Bromodichloro-methane........ 601 624, 1624B........... .............. 6200 C [20th] and 6230 B 6200 B and C-97.........
[18th, 19th], 6200 B
[20th] and 6210 B
[18th, 19th].
19. Bromoform.................... 601 624, 1624B........... .............. 6200 C [20th] and 6230 B 6200 B and C-97.........
[18th, 19th], 6200 B
[20th] and 6210 B
[18th, 19th].
20. Bromomethane................. 601 624, 1624B........... .............. 6200 C [20th] and 6230 B 6200 B and C-97.........
[18th, 19th], 6200 B
[20th] and 6210 B
[18th, 19th].
21. 4-Bromophenyl phenyl ether... 611 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
22. Carbon tetrachloride......... 601 624, 1624B........... .............. 6200 C [20th] and 6230 B 6200 C-97............... ........................ See footnote \3\, p. 130
[18th, 19th].
23. 4-Chloro-3-methyl phenol..... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
24. Chlorobenzene................ 601, 602 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97......... ........................ See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6220 B
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
25. Chloroethane................. 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
26. 2-Chloroethylvinyl ether..... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
[[Page 11228]]
27. Chloroform................... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97......... ........................ See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
28. Chloromethane................ 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th] 6200 C
[20th] and 6230 B
[18th, 19th].
29. 2-Chloronaph-thalene......... 612 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
30. 2-Chlorophenol............... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B(00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
31. 4-Chlorophenyl phenyl ether.. 611 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
32. Chrysene..................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
33. Dibenzo(a,h)an-thracene...... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
34. Dibromochloro-methane........ 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th] 6200 C
[20th] and 6230 B
[18th, 19th].
35. 1,2-Dichloro-benzene......... 601, 602 624, 1625B........... .............. 6200 C [20th] and 6220 B 6200 C-97............... ........................ See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
36. 1,3-Dichloro-benzene......... 601, 602 624, 1625B........... .............. 6200 C [20th] and 6220 B 6200 C-97............... ........................ See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
37. 1,4-Dichloro-benzene......... 601, 602 624, 1625B........... .............. 6200 C [20th] and 6220 B 6200 C-97............... ........................ See footnote \9\, p. 27
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
38. 3,3-Dichloro-benzidine....... .............. 625, 1625B........... 605 6410 B [18th, 19th, 6410 B-00...............
20th].
39. Dichlorodifluoro-methane..... 601 ..................... .............. 6200 C [20th] and 6230 B 6200 C-97...............
[18th, 19th].
40. 1,1-Dichloroethane........... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
41. 1,2-Dichloroethane........... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
42. 1,1-Dichloroethene........... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
43. trans-1,2-Dichloro-ethene.... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
44. 2,4-Dichlorophenol........... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
45. 1,2-Dichloro-propane......... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
46. cis-1,3-Dichloro-propene..... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
[[Page 11229]]
47. trans-1,3-Dichloro-propene... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
48. Diethyl phthalate............ 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
49. 2,4-Dimethylphenol........... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
50. Dimethyl phthalate........... 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
51. Di-n-butyl phthalate......... 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
52. Di-n-octyl phthalate......... 606 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
53. 2,3-Dinitrophenol............ 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ ........................
19th, 20th].
54. 2,4-Dinitrotoluene........... 609 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
55. 2,6-Dinitrotoluene........... 609 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
56. Epichlorohydrin.............. .............. ..................... .............. ........................ ........................ ........................ See footnote \3\, p.
130; See footnote \6\,
p. S102
57. Ethylbenzene................. 602 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97......... ........................ ........................
[18th, 19th], 6200 C
[20th] and 6220 B
[18th, 19th].
58. Fluoranthene................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
59. Fluorene..................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
60. 1,2,3,4,6,7,8-Heptachloro- .............. 1613B \10\...........
dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro- .............. 1613B \10\...........
dibenzofuran.
62. 1,2,3,4,6,7,8- .............. 1613B \10\...........
Heptachlorodibenzo-p-dioxin.
63. Hexachlorobenzene............ 612 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
64. Hexachloro-butadiene......... 612 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
65. Hexachlorocyclo-pentadiene... 612 625 \5\, 1625B....... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
66. 1,2,3,4,7,8- .............. 1613B \10\...........
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8- .............. 1613B \10\...........
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9- .............. 1613B \10\...........
Hexachlorodibenzofuran.
69. 2,3,4,6,7,8- .............. 1613B \10\...........
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-Hexachlorodibenzo- .............. 1613B \10\...........
p-dioxin.
71. 1,2,3,6,7,8-Hexachlorodibenzo- .............. 1613B \10\...........
p-dioxin.
72. 1,2,3,7,8,9-Hexachlorodibenzo- .............. 1613B \10\...........
p-dioxin 1613B \10\.
73. Hexachloroethane............. 612 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
74. Ideno(1,2,3-cd) pyrene....... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
75. Isophorone................... 609 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
76. Methylene chloride........... 601 624, 1624B........... .............. 6200 C [20th] and 6230 B 6200 C-97............... ........................ See footnote \3\, p. 130
[18th, 19th].
77. 2-Methyl-4,6-dinitrophenol... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
78. Naphthalene.................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... ........................ See footnote \9\, p. 27
19th, 20th].
[[Page 11230]]
79. Nitrobenzene................. 609 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
20th].
80. 2-Nitrophenol................ 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
81. 4-Nitrophenol................ 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
82. N-Nitrosodimethylamine....... 607 6255, 1625B.......... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
83. N-Nitrosodi-n-propylamine.... 607 6255, 1625B.......... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
84. N-Nitrosodiphenylamine....... 607 6255, 1625B.......... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \9\, p. 27
20th].
85. Octachlorodibenzofuran....... .............. 1613B \10\*..........
86. Octachlorodibenzo-p-dioxin... .............. 1613B \10\...........
87. 2,2'-Oxybis(2-chloropropane) 611 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00...............
[also known as bis(2- 20th].
chloroisopropyl) ether].
88. PCB-1016..................... 608 625.................. .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p. 43;
20th]. See footnote \8\
89. PCB-1221..................... 608 625.................. .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p. 43;
20th]. See footnote \8\
90. PCB-1232..................... 608 625.................. .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p. 43;
20th]. See footnote \8\
91. PCB-1242..................... 608 625.................. .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p. 43;
20th]. See footnote \8\
92. PCB-1248..................... 608 625..................
93. PCB-1254..................... 608 625.................. .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p. 43;
20th]. See footnote \8\
94. PCB-1260..................... 608 625.................. .............. 6410 B, 6630 B [18th, 6410 B-00............... ........................ See footnote 3, p. 43;
19th, 20th]. See footnote 8
95. 1,2,3,7,8-Pentachloro- .............. 1613B\10\............
dibenzofuran.
96. 2,3,4,7,8-Pentachloro- .............. 1613B\10\............
dibenzofuran.
97. 1,2,3,7,8,-Pentachlorodibenzo- .............. 1613B\10\............
p-dioxin.
98. Pentachlorophenol............ 604 625, 1625B........... .............. 6410 B, 6630 B [18th, 6410 B-00............... ........................ See footnote \3\, p.
19th, 20th]. 140; See footnote \9\,
p. 27
99. Phenanthrene................. 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
100. Phenol...................... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
101. Pyrene...................... 610 625, 1625B........... 610 6410 B, 6440 B [18th, 6410 B-00............... D4657-92 (99)........... See footnote \9\, p. 27
19th, 20th].
102. 2,3,7,8-Tetra- .............. 1613B10..............
chlorodibenzofuran.
103. 2,3,7,8-Tetra-chlorodibenzo- .............. 613, 625 \5a\, 1613B
p-dioxin. \10\.
104. 1,1,2,2-Tetra-chloro ethane. 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97......... ........................ See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
105. Tetrachloroethene........... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97......... ........................ See footnote \3\, p. 130
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
106. Toluene..................... 602 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6220 B
[18th, 19th].
107. 1,2,4-Trichloro-benzene..... 612 625, 1625B........... .............. 6410 B [18th, 19th, 6410 B-00............... ........................ See footnote \3\, p.
20th]. 130; See footnote \9\,
p. 27
[[Page 11231]]
108. 1,1,1-Trichloro-ethane...... 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
109. 1,1,2-Trichloro-ethane...... 601 624, 1624B........... 6200 B [20th] 6200 B and C-97......... ........................ See footnote \3\, p. 130
and 6210 B
[18th, 19th],
6200 C [20th]
and 6230 B
[18th, 19th]
110. Trichloroethene............. 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
111. Trichlorofluoro-methane..... 601 624.................. .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], 6200 C
[20th] and 6230 B
[18th, 19th].
112. 2,4,6-Trichlorophenol....... 604 625, 1625B........... .............. 6410 B, 6420 B [18th, 6410 B-00, 6420 B-00.... ........................ See footnote \9\, p. 27
19th, 20th].
113. Vinyl chloride.............. 601 624, 1624B........... .............. 6200 B [20th] and 6210 B 6200 B and C-97.........
[18th, 19th], >6200 C
[20th] and 6230 B
[18th, 19th].
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ All parameters are expressed in micrograms per liter ([mu]g/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/L).
\2\ The full text of Methods 601-613, 624, 625, 1624B, and 1625B, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The full text of Method
1613B is incorporated by reference into this Part 136 and is available from the National Technical Information Services as stock number PB95-104774. The standardized test procedure to be
used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection Limit,'' of this
Part 136.
\3\ ``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection Agency, September, 1978.
\4\ Method 624 may be 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.
\5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they are known to be present, Methods 605,
607, and 612, or Method 1625B, are preferred methods for these compounds.
\5a\ 625, screening only.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,'' Supplement to the Fifteenth Edition of Standard Methods for the Examination of
Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624B, and 1625B (See Appendix A of
this Part 136) in accordance with procedures each in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for methods 624
and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of
any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to
demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'' 3M Corporation Revised 10/28/94.
\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial
Sediments,'' U.S. Geological Survey, Open File Report 93-125.
\10\ Analysts may use Fluid Management Systems, Inc. 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\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
EPA \2,\ Standard Methods 18th,
Parameter Method \7\ 19th, 20th Ed. Standard Methods Online ASTM Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin........................ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96 (2002)......... 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
2. Ametryn....................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\, p
S68
3. Aminocarb..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S16
4. Atraton....................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
5. Atrazine...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
6. Azinphos methyl............... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
7. Barban........................ TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
8. [alpha]-BHC................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
9. [beta]-BHC.................... GC.................. 608 6630 C.................. ........................ D3086-90,............... See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
[[Page 11232]]
10. [delta]-BHC.................. GC.................. 608 6630 C.................. ........................ D3086-90,............... See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
11. [gamma]-BHC (Lindane)........ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
....................
12. Captan....................... GC.................. ........... 6630 B.................. ........................ D3086-90,............... See footnote \3\, p. 7
D5812-96(02)............
13. Carbaryl..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94, See footnote \6\,
p. S60
14. Carbo-phenothion............. GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
15. Chlordane.................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
16. Chloro-propham............... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64.
17. 2,4-D........................ GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
18. 4,4'-DDD..................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
19. 4,4'-DDE..................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
20. 4,4'-DDT..................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
21. Demeton-O.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
22. Demeton-S.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
23. Diazinon..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27; See footnote \6\, p. S51
24. Dicamba...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 115
25. Dichlofen-thion.............. GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
26. Dichloran.................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
27. Dicofol...................... GC.................. ........... ........................ ........................ D3086-90,...............
D5812-96(02)............
28. Dieldrin..................... GC.................. 608 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
29. Dioxathion................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
30. Disulfoton................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 25; See footnote \6\,
p. S51
31. Diuron....................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
32. Endosulfan I................. GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
33. Endosulfan II................ GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \8\
D5812-96(02)............
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
34. Endosulfan Sulfate........... GC.................. 608 6630 C.................. ........................ ........................ See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
35. Endrin....................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
D5812-96(02)............ 27; See footnote \8\
GC/MS............... 625 \5\ 6410 B.................. 6410 B-00...............
36. Endrin aldehyde.............. GC.................. 608 ........................ ........................ ........................ See footnote \8\
GC/MS............... 625
37. Ethion....................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
38. Fenuron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
39. Fenuron-TCA.................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
40. Heptachlor................... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
GC/MS............... 625 6410 B.................. 6410 B-00............... D5812-96(02)............ 27; See footnote \8\
41. Heptachlor epoxide........... GC.................. 608 6630 B & C.............. ........................ D3086-90,............... See footnote \3\, p. 7; See footnote \4\, p.
GC/MS............... 625 6410 B.................. 6410 B-00............... D5812- 96(02)........... 27; See footnote \6\, p. S73; See footnote
\8\
42. Isodrin...................... GC.................. ........... ........................ ........................ ........................ See footnote \4\, p. 27; See footnote \6\,
p. S73
43. Linuron...................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
44. Malathion.................... GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27; See footnote \6\, p. S51
[[Page 11233]]
45. Methiocarb................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S60
46. Methoxy-chlor................ GC.................. ........... 6630 B & C.............. ........................ D3086-90, D5812-96(02).. See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
47. Mexacar-bate................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p.S60
48. Mirex........................ GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7; See footnote \4\, p.
27
49. Monuron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
50. Monuron-TCA.................. TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
51. Nuburon...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
52. Parathion methyl............. GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27
53. Parathion ethyl.............. GC.................. ........... 6630 C.................. ........................ ........................ See footnote \3\, p. 25; See footnote \4\,
p. 27
54. PCNB......................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
55. Perthane..................... GC.................. ........... ........................ ........................ D3086-90, D5812-96(02).. See footnote \4\, p. 27
56. Prometon..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
57. Prometryn.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
58. Propazine.................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
59. Propham...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
60. Propoxur..................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 94; See footnote \6\,
p. S60
61. Secbumeton................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
62. Siduron...................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
63. Simazine..................... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68; See footnote \9\
64. Strobane..................... GC.................. ........... 6630 B & C.............. ........................ ........................ See footnote \3\, p. 7
65. Swep......................... TLC................. ........... ........................ ........................ ........................ See footnote \3\, p. 104; See footnote \6\,
p. S64
66. 2,4,5-T...................... GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
67. 2,4,5-TP (Silvex)............ GC.................. ........... 6640 B.................. ........................ ........................ See footnote \3\, p. 115; See footnote \4\,
p. 40
68. Terbuthylazine............... GC.................. ........... ........................ ........................ ........................ See footnote \3\, p. 83; See footnote \6\,
p. S68
69. Toxaphene.................... GC.................. 608 6630 B & C.............. ........................ D3086-90, D5812-96(02).. See footnote \3\, p. 7; See footnote \4\, p.
27; See footnote \8\
GC/MS............... 625 6410 B.................. 6410 B-00...............
70. Trifluralin.................. GC.................. ........... 6630 B.................. ........................ ........................ See footnote \3\, p. 7; See footnote \9\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where entries are listed by chemical name.
\2\ The full text of Methods 608 and 625 are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The standardized test procedure to be used to
determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection Limit,'' of this Part
136.
\3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection Agency, September 1978. This EPA
publication includes thin-layer chromatography (TLC) methods.
\4\``Methods for Analysis of Organic Substances in Water and Fluvial Sediments,'' Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3 (1987).
\5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of Standard Methods for the Examination of
Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 (See Appendix A of this Part 136) in
accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 10% of all samples analyzed with Method
608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter
falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory
compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk'', 3M Corporation, Revised 10/28/94.
\9\ USGS Method 0-3106-93 from ``Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Triazine and Other Nitrogen-containing Compounds by Gas
Chromatography with Nitrogen Phosphorus Detectors'' U.S. Geological Survey Open File Report 94-37.
Table IE.--List of Approved Radiologic Test Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
--------------------------------------------------------------------------------------------------------------------------------------
Parameter and units Method Standard Methods 18th,
EPA \1\ 19th, 20th Ed. Standard Methods Online ASTM USGS \2\
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter..... Proportional or 900.0................ 7110 B.................... 7110 B-00................. D1943-90, 96.............. pp. 75 and 78 \3\
scintillation
counter.
2. Alpha-Counting error, pCi per Proportional or Appendix B........... 7110 B.................... 7110 B-00................. D1943-90, 96.............. p. 79
liter. scintillation
counter.
3. Beta-Total, pCi per liter...... Proportional counter. 900.0................ 7110 B.................... 7110 B-00................. D1890-90, 96.............. pp. 75 and 78 \3\
[[Page 11234]]
4. Beta-Counting error, pCi....... Proportional counter. Appendix B........... 7110 B.................... 7110 B-00................. D1890-90, 96.............. p. 79
5. (a) Radium Total pCi per liter. Proportional counter. 903.0................ 7500-Ra B................. 7500-Ra B-01.............. D2460-90, 97.............. ..........................
(b) Ra, pCi per liter.............
Scintillation counter 903.1................ 7500-Ra C................. 7500-Ra C-01.............. D3454-91, 97.............. p. 81
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA-600/4-80-032 (1980), U.S. Environmental Protection Agency, August 1980.
\2\ Fishman, 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).
\3\ The 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 Pesticide name CAS No. EPA Analytical Method No.(s)
----------------------------------------------------------------------------------------------------------------
8.................. Triadimefon.............. 43121-43-3 507/633/525.1/1656
12................. Dichlorvos............... 62-73-7 1657/507/622/525.1
16................. 2,4-D; 2,4-D Salts and 94-75-7 1658/515.1/615/515.2/555
Esters [2,4-Dichloro-
phenoxyacetic acid].
17................. 2,4-DB; 2,4-DB Salts and 94-82-6 1658/515.1/615/515.2/555
Esters [2,4-
Dichlorophenoxybutyric
acid].
22................. Mevinphos................ 7786-34-7 1657/507/622/525.1
25................. Cyanazine................ 21725-46-2 629/507
26................. Propachlor............... 1918-16-7 1656/508/608.1/525.1
27................. MCPA; MCPA Salts and 94-74-6 1658/615/555
Esters [2-Methyl-4-
chlorophenoxyacetic
acid].
30................. Dichlorprop; Dichlorprop 120-36-5 1658/515.1/615/515.2/555
Salts and Esters [2-(2,4-
Dichlorophenoxy)
propionic acid].
31................. MCPP; MCPP Salts and 93-65-2 1658/615/555
Esters [2-(2-Methyl-4-
chlorophenoxy) propionic
acid].
35................. TCMTB [2- 21564-17-0 637
(Thiocyanomethylthio)
benzo-thiazole].
39................. Pronamide................ 23950-58-5 525.1/507/633.1
41................. Propanil................. 709-98-8 632.1/1656
45................. Metribuzin............... 21087-64-9 507/633/525.1/1656
52................. Acephate................. 30560-19-1 1656/1657
53................. Acifluorfen.............. 50594-66-6 515.1/515.2/555
54................. Alachlor................. 15972-60-8 505/507/645/525.1/1656
55................. Aldicarb................. 116-06-3 531.1
58................. Ametryn.................. 834-12-8 507/619/525.1
60................. Atrazine................. 1912-24-9 505/507/619/525.1/1656
62................. Benomyl.................. 17804-35-2 631
68................. Bromacil; Bromacil Salts 314-40-9 507/633/525.1/1656
and Esters.
69................. Bromoxynil............... 1689-84-5 1625/1661
69................. Bromoxynil octanoate..... 1689-99-2 1656
70................. Butachlor................ 23184-66-9 507/645/525.1/1656
73................. Captafol................. 2425-06-1 1656
75................. Carbaryl [Sevin]......... 63-25-2 531.1/632/553
76................. Carbofuran............... 1563-66-2 531.1/632
80................. Chloroneb................ 2675-77-6 1656/508/608.1/525.1
82................. Chlorothalonil........... 1897-45-6 508/608.2/525.1/1656
84................. Stirofos................. 961-11-5 1657/507/622/525.1
86................. Chlorpyrifos............. 2921-88-2 1657/508/622
90................. Fenvalerate.............. 51630-58-1 1660
103................ Diazinon................. 333-41-5 1657/507/614/622/525.1
107................ Parathion methyl......... 298-00-0 1657/614/622
110................ DCPA [Dimethyl 2,3,5,6- 1861-32-1 508/608.2/525.1/515.1/515.2/1656
tetrachloro-
terephthalate].
112................ Dinoseb.................. 88-85-7 1658/515.1/615/515.2/555
113................ Dioxathion............... 78-34-2 1657/614.1
118................ Nabonate [Disodium 138-93-2 630.1
cyanodithio-
imidocarbonate].
119................ Diuron................... 330-54-1 632/553
123................ Endothall................ 145-73-3 548/548.1
124................ Endrin................... 72-20-8 1656/505/508/608/617/525.1
125................ Ethalfluralin............ 55283-68-6 1656/627 See footnote 1
126................ Ethion................... 563-12-2 1657/614/614.1
127................ Ethoprop................. 13194-48-4 1657/507/622/525.1
132................ Fenarimol................ 60168-88-9 507/633.1/525.1/1656
133................ Fenthion................. 55-38-9 1657/622
138................ Glyphosate 1071-83-6 547
[N(Phosphonomethyl)
glycine].
140................ Heptachlor............... 76-44-8 1656/505/508/608/617/525.1
144................ Isopropalin.............. 33820-53-0 1656/627
148................ Linuron.................. 330-55-2 553/632
150................ Malathion................ 121-75-5 1657/614
154................ Methamidophos............ 10265-92-6 1657
156................ Methomyl................. 16752-77-5 531.1/632
[[Page 11235]]
158................ Methoxychlor............. 72-43-5 1656/505/508/608.2/617/525.1
172................ Nabam.................... 142-59-6 630/630.1
173................ Naled.................... 300-76-5 1657/622
175................ Norflurazon.............. 27314-13-2 507/645/525.1/1656
178................ Benfluralin.............. 1861-40-1 11656/1627
182................ Fensulfothion............ 115-90-2 1657/622
183................ Disulfoton............... 298-04-4 1657/507/614/622/525.1
185................ Phosmet.................. 732-11-6 1657/622.1
186................ Azinphos Methyl.......... 86-50-0 1657/614/622
192................ Organo-tin pesticides.... 12379-54-3 Ind-01/200.7/200.9
197................ Bolstar.................. 35400-43-2 1657/622
203................ Parathion................ 56-38-2 1657/614
204................ Pendimethalin............ 40487-42-1 1656
205................ Pentachloronitrobenzene.. 82-68-8 1656/608.1/617
206................ Pentachlorophenol........ 87-86-5 625/1625/515.2/555/515.1/ 525.1
208................ Permethrin............... 52645-53-1 608.2/508/525.1/1656/1660
212................ Phorate.................. 298-02-2 1657/622
218................ Busan 85 [Potassium 128-03-0 630/630.1
dimethyldithiocarbamate].
219................ Busan 40 [Potassium N- 51026-28-9 630/630.1
hydroxymethyl-N-
methyldithiocarbamate].
220................ KN Methyl [Potassium N- 137-41-7 630/630.1
methyl-dithiocarbamate].
223................ Prometon................. 1610-18-0 507/619/525.1
224................ Prometryn................ 7287-19-6 507/619/525.1
226................ Propazine................ 139-40-2 507/619/525.1/1656
230................ Pyrethrin I.............. 121-21-1 1660
232................ Pyrethrin II............. 121-29-9 1660
236................ DEF [S,S,S-Tributyl 78-48-8 1657
phosphorotrithioate].
239................ Simazine................. 122-34-9 505/507/619/525.1/1656
241................ Carbam-S [Sodium 128-04-1 630/630.1
dimethyldithiocarbanate].
243................ Vapam [Sodium 137-42-8 630/630.1
methyldithiocarbamate].
252................ Tebuthiuron.............. 34014-18-1 507/525.1
254................ Terbacil................. 5902-51-2 507/633/525.1/1656
255................ Terbufos................. 13071-79-9 1657/507/614.1/525.1
256................ Terbuthylazine........... 5915-41-3 619/1656
257................ Terbutryn................ 886-50-0 507/619/525.1
259................ Dazomet.................. 533-74-4 630/630.1/1659
262................ Toxaphene................ 8001-35-2 1656/505/508/608/617/525.1
263................ Merphos [Tributyl 150-50-5 1657/507/525.1/622
phosphorotrithioate].
264................ Trifluralin.............. 1582-09-8 1656/508/617/627/525.1
268................ Ziram [Zinc 137-30-4 630/630.1
dimethyldithiocarbamate].
----------------------------------------------------------------------------------------------------------------
\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, IC, 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, IC, 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/met300.pdf. Table IB.
(68) Table IG Methods are available in ``Methods For The
Determination of Nonconventional Pesticides In
[[Page 11236]]
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 IA,
IB, IC, 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
----------------------------------------------------------------------------------------------------------------
Preservation
Parameter number/name Container \1\ \2,3\ Maximum holding time \4\
----------------------------------------------------------------------------------------------------------------
Table lA--Bacterial Tests:
1-5. Coliform, total, PA, G.................... Cool, <10 [deg]C, 6 hours
fecal, and E. coli. 0.0008% Na2S2O3
\5\.
6. Fecal streptococci..... PA, G.................... Cool, <10 [deg]C, 6 hours
0.0008% Na2S2O3
\5\.
7. Enterococci............ PA, G.................... Cool, <10 [deg]C, 6 hours
0.0008% Na2S2O3
\5\.
Table lA--Protozoan Tests:
8. Cryptosporidium........ LDPE; field filtration... 0-8 [deg]C....... 96 hours \21\
9. Giardia................ LDPE; field filtration... 0-8 [deg]C....... 96 hours \21\
Table lA--Aquatic Toxicity
Tests:
10-13. Toxicity, acute and P, FP, G................. Cool, <=6 [deg]C 36 hours
chronic. \16\.
Table lB--Inorganic Tests:
1. Acidity................ P, FP, G................. Cool, <=6 [deg]C 14 days
\18\.
2. Alkalinity............. P, FP, G................. Cool, <=6 [deg]C 14 days
\18\.
4. Ammonia................ P, FP, G................. Cool, <=6 [deg]C 28 days
\18\, H2SO4 to
pH<2.
9. Biochemical oxygen P, FP, G................. Cool, <=6 [deg]C 48 hours
demand. \18\.
10. Boron................. P, FP, or Quartz......... HNO3 to pH<2..... 6 months
11. Bromide............... P, FP, G................. None required.... 28 days
14. Biochemical oxygen P, FP G.................. Cool, <=6 [deg]C 48 hours
demand, carbonaceous. \18\.
15. Chemical oxygen demand P, FP, G................. Cool, <=6 [deg]C 28 days
\18\, H2SO4 to
pH<2.
16. Chloride.............. P, FP, G................. None required.... 28 days
17. Chlorine, total P, G..................... None required.... Analyze within 15 minutes
residual.
21. Color................. P, FP, G................. Cool, <=6 [deg]C 48 hours
\18\.
23-24. Cyanide, total or P, FP, G................. Cool, <=6 [deg]C 14 days
available (or CATC). \18\, NaOH to
pH>12 \6\,
reducing agent
\5\.
25. Fluoride.............. P........................ None required.... 28 days
27. Hardness.............. P, FP, G................. HNO3 or H2SO4 to 6 months
pH<2.
28. Hydrogen ion (pH)..... P, FP, G................. None required.... Analyze within 15 minutes
31, 43. Kjeldahl and P, FP, G................. Cool, <=6 [deg]C 28 days
organic N. \18\, H2SO4 to
pH<2.
Table IB--Metals: \7\
18. Chromium VI........... P, FP, G................. Cool, <=6 [deg]C 28 days
\18\, pH = 9.3-
9.7 \20\.
35. Mercury (CVAA)........ P, FP, G................. HNO3 to pH<2..... 28 days
[[Page 11237]]
35. Mercury (CVAFS)....... FP, G; and FP-lined cap 5 mL/L 12N HCl or 90 days \17\
\17\. 5 mL/L BrCl \17\.
3, 5-8, 12, 13, 19, 20, P, FP, G................. HNO3 to pH<2, or 6 months
22, 26, 29, 30, 32-34, at least 24
36, 37, 45, 47, 51, 52, hours prior to
58-60, 62, 63, 70-72, 74, analysis \19\.
75. Metals, except boron,
chromium VI, and mercury.
38. Nitrate............... P, FP, G................. Cool, <=6 [deg]C 48 hours
\18\.
39. Nitrate-nitrite....... P, FP, G................. Cool, <=6 [deg]C 28 days
18, H2SO4 to
pH<2.
40. Nitrite............... P, FP, G................. Cool, <=6 [deg]C 48 hours
\18\.
41. Oil and grease........ G........................ Cool to <=6 28 days
[deg]C \18\, HCl
or H2SO4 to pH<2.
42. Organic Carbon........ P, FP, G................. Cool to <=6 28 days
[deg]C \18\,
HCl, H2SO4, or
H3PO4 to pH<2.
44. Orthophosphate........ P, FP, G................. Cool, <=6 [deg]C Filter within 15 minutes; Analyze
\18\. within 48 hours
46. Oxygen, Dissolved G, Bottle and top........ None required.... Analyze within 15 minutes
Probe.
47. Winkler............... G, Bottle and top........ Fix on site and 8 hours
store in dark.
48. Phenols............... G........................ Cool, <=6 [deg]C 28 days
\18\, H2SO4 to
pH<2.
49. Phosphorous G........................ Cool, <=6 [deg]C 48 hours
(elemental). \18\.
50. Phosphorous, total.... P, FP, G................. Cool, <=6 [deg]C 28 days
\18\, H2SO4 to
pH<2.
53. Residue, total........ P, FP, G................. Cool, <=6 [deg]C 7 days
\18\.
54. Residue, Filterable... P, FP, G................. Cool, <=6 [deg]C 7 days
\18\.
55. Residue, Nonfilterable P, FP, G................. Cool, <=6 [deg]C 7 days
(TSS). \18\.
56. Residue, Settleable... P, FP, G................. Cool, <=6 [deg]C 48 hours
\18\.
57. Residue, Volatile..... P, FP, G................. Cool, <=6 [deg]C 7 days
\18\.
61. Silica................ P or Quartz.............. Cool, <=6 [deg]C 28 days
\18\.
64. Specific conductance.. P, FP, G................. Cool, <=6 [deg]C 28 days
\18\.
65. Sulfate............... P, FP, G................. Cool, <=6 [deg]C 28 days
\18\.
66. Sulfide............... P, FP, G................. Cool, <=6 [deg]C 7 days
\18\, add zinc
acetate plus
sodium hydroxide
to pH>9.
67. Sulfite............... P, FP, G................. None required.... Analyze within 15 minutes
68. Surfactants........... P, FP, G................. Cool, <=6 [deg]C 48 hours
\18\.
69. Temperature........... P, FP, G................. None required.... Analyze
73. Turbidity............. P, FP, G................. Cool, <=6 [deg]C 48 hours
18.
Table lC--Organic Tests \8\
13, 18-20, 22, 24-28, 34- G, FP-lined septum....... Cool, <=6 [deg]C 14 days
37, 39-43, 45-47, 56, 76, \18\, 0.008%
104, 105, 108-111, 113. Na2S2O3 \5\.
Purgeable Halocarbons.
6, 57, 106. Purgeable G, FP-lined septum....... Cool, <=6 [deg]C 14 days \9\
aromatic hydrocarbons. \18\, 0.008%
Na2S2O3 \5\, HCl
to pH 2 \9\.
3, 4. Acrolein and G, FP-lined septum....... Cool, <=6 [deg]C 14 days \10\
acrylonitrile. \18\, 0.008%
Na2S2O3 \5\, pH
to 4-5 \10\.
23, 30, 44, 49, 53, 77, G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
80, 81, 98, 100, 112. \18\, 0.008% after extraction
Phenols \11\. Na2S2O3 \5\.
7, 38. Benzidines \11\, G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction \13\
\12\. \18\, 0.008%
Na2S2O3 \5\.
14, 17, 48, 50-52. G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
Phthalate esters \11\. \18\. after extraction
82-84. Nitrosamines\11\ G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
\14\. 18, store in after extraction
dark, 0.008%
Na2S2O3\5\.
88-94. PCBs \11\.......... G, FP-lined cap.......... Cool, <=6 [deg]C 1 year until extraction, 1 year
\18\. after extraction
54, 55, 75, 79. G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
Nitroaromatics and \18\, store in after extraction
isophorone \11\. dark, 0.008%
Na2S2O3\5\.
[[Page 11238]]
1, 2, 5, 8-12, 32, 33, 58, G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
59, 74, 78, 99, 101. \18\, store in after extraction
Polynuclear aromatic dark, 0.008%
hydrocarbons \11\. Na2S2O3\5\.
15, 16, 21, 31, 87. G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
Haloethers \11\. \18\, 0.008% after extraction
Na2S2O3\5\.
29, 35-37, 63-65, 107. G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
Chlorinated hydrocarbons \18\. after extraction
\11\.
60-62, 66-72, 85, 86, 95-
97, 102, 103. CDDs/CDFs
\11\.
Aqueous Samples: Field G........................ Cool, <=6 [deg]C 1 year
and Lab Preservation. \18\, 0.008%
Na2S2O3\5\, pH<9.
Solids and Mixed-Phase G........................ Cool, <=6 [deg]C 7 days
Samples: Field \18\.
Preservation.
Tissue Samples: Field G........................ Cool, <=6 [deg]C 24 hours
Preservation. 18.
Solids, Mixed-Phase, G........................ Freeze, <=-10 1 year
and Tissue Samples: [deg]C.
Lab Preservation.
Table lD--Pesticides Tests:
1-70. Pesticides \11\..... G, FP-lined cap.......... Cool, <=6 [deg]C 7 days until extraction, 40 days
18, pH 5-9 \15\. after extraction
Table lE--Radiological Tests:
1-5. Alpha, beta, and P, FP, G................. HNO3 to pH<2..... 6 months
radium.
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE; Teflon[supreg]), or other
fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is made of
a sterlizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density polyethylene.
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
minutes of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour
composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at <=6
[deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <=6 [deg]C,
unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
is completed. Add the preservative to the sample container prior to sample collection when the preservative
will not compromise the integrity of a grab sample, a composite sample, or an aliquot split from a composite
sample ; otherwise, preserve the grab sample, composite sample, or aliquot split from a composite sample with
in 15 minutes of collection. If a composite measurement is required but a composite sample would compromise
sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over
the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations
averaged. Alternatively, grab samples may be collected in the field and composited in the laboratory if the
compositing procedure produces results equivalent to results produced by arithmetic averaging of the results
of analysis of individual grab samples. For examples of laboratory compositing procedures, see EPA Method
1664A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and (v) (volatile organics).
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such
material for transportation is responsible for ensuring such compliance. For the preservation requirements of
Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
(HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid
(HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before the start of analysis and still be considered valid (e.g., samples analyzed for
fecal coliforms may be held up to 6 hours prior to commencing analysis). Samples may be held for longer
periods only if the permittee or monitoring laboratory has data on file to show that, for the specific types
of samples under study, the analytes are stable for the longer time, and has received a variance from the
Regional Administrator under Sec. 136.3(e). For a grab sample, the holding time begins at the time of
collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), the holding time begins at the time of
the end of collection of the composite sample. For a set of grab samples composited in the field or
laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
sample stability. See Sec. 136.3(e) for details. The date and time of collection of an individual grab
sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and
that are all collected on the same calendar date, the date of collection is the date on which the samples are
collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
automatically on a given date, the date of collection is the date on which the sample is collected. For a
composite sample collected automatically, and that is collected across two calendar dates, the date of
collection is the dates of the two days; e.g., November 14-15.
\5\ Add a reducing agent only if an oxidant (e.g., chlorine) is present. Reducing agents shown to be effective
are sodium thiosulfate (Na2S2O3), ascorbic acid, sodium arsenite (NaAsO2), or sodium borohydride (NaBH4).
However, some of these agents have been shown to produce a positive or negative cyanide bias, depending on
other substances in the sample and the analytical method used. Therefore, do not add an excess of reducing
agent. Methods recommending ascorbic acid (e.g., EPA Method 335.4) specify adding ascorbic acid crystals, 0.1--
0.6 g, until a drop of sample produces no color on potassium iodide (KI) starch paper, then adding 0.06 g (60
mg) for each liter of sample volume. If NaBH4 or NaAsO2 is used, 25 mg/L NaBH4 or 100 mg/L NaAsO2 will reduce
more than 50 mg/L of chlorine (see method (Kelada-01'' and/or Standard Method 4500-CN- for more information).
After adding reducing agent, test the sample using KI paper, a test strip (e.g. for chlorine, SenSafeTM Total
Chlorine Water Check 480010) moistened with acetate buffer solution (see Standard Method 4500-Cl.C.3e), or a
chlorine/oxidant test method (e.g., EPA Method 330.4 or 330.5), to make sure all oxidant is removed. If
oxidant remains, add more reducing agent. Whatever agent is used, it should be tested to assure that cyanide
results are not affected adversely.
\6\ Sample collection and preservation: Collect a volume of sample appropriate to the analytical method in a
bottle of the material specified. If the sample can be analyzed within 48 hours and sulfide is not present,
adjust the pH to >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
laboratory 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), filter 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, 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 low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g 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
0.75 liter of sample to a 4.4-L collapsible container (e.g., CubitainerTM). 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 with 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 loss of cyanide (>10%). Precipitation: If the sample
contains particulate matter that would be removed by filtration, filter the sample prior to treatment to
assure that cyanide associated with the particulate 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 low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g or mg), and divide by the original sample volume to obtain the cyanide concentration. 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
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 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 concentration 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.
[[Page 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 cyanide 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, hypochlorite, or other oxidant: Treat a sample known or suspected to contain chlorine,
hypochlorite, or other oxidant as directed in footnote 5.
\7\ 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.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
\10\ The 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 for 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 preserved by cooling to <=6 [deg]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 [deg]C.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
of sampling.
\15\ The 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% Na2S2O3.
\16\ Sufficient 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 isolated cases where it can be documented that this holding
temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance.
The request for a variance should include supportive data which show that the toxicity of the effluent samples
is not reduced because of the increased holding temperature.
\17\ 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 BrCl or HCl solution within 48
hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory
within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample
should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669.
If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be
filtered in a designated clean area in the field within the time period necessary to maintain sample
integrity. A sample that has been collected for determination of total or dissolved trace level mercury must
be analyzed within 90 days of sample collection.
\18\ Aqueous samples must be preserved at <=6 [deg]C, and should not be frozen unless data demonstrating that
sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
regulatory authority. Also, for purposes of NPDES monitoring, the specification of ``<= [deg]C'' is used in
place of the ``4 [deg]C'' and ``<4 [deg]C'' sample temperature requirements listed in some methods. It is not
necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three
significant figures are specified so that rounding down to 6 [deg]C may not be used to meet the <=6 [deg]C
requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than
15 minutes).
\19\ An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at
least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must
be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment
samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and
holding time requirements in the approved metals methods.
\20\ To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6.
The allowance in this footnote supersedes preservation and holding time requirements in the approved
hexavalent chromium methods, unless this supersession would compromise the measurement, in which case
requirements in the method must be followed.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
0
8. Section 136.4 is amended by revising the first sentence of paragraph
(d) introductory text to read as follows:
Sec. 136.4 Application for alternate test procedures.
* * * * *
(d) An application for approval of an alternate test procedure for
nationwide use may be made by letter in triplicate to the Alternate
Test Procedure Program Coordinator, Office of Science and Technology
(4303), Office of Water, U.S. Environmental Protection Agency, 1200
Pennsylvania Ave., NW., Washington, DC 20460. * * *
* * * * *
0
9. Section 136.5 is amended as follows:
0
a. In paragraph (b) by revising the last sentence.
0
b. By revising paragraph (c).
0
c. In paragraph (d) by revising the second and third sentences.
0
d. By revising paragraphs (e)(1) and (e)(2).
Sec. 136.5 Approval of alternate test procedures.
* * * * *
(b) * * * Where the Director recommends rejection of the
application for scientific and technical reasons which he provides, the
Regional Administrator shall deny the application and shall forward
this decision to the Director of the State Permit Program and to the
Alternate Test Procedure Program Coordinator, Office of Science and
Technology (4303), Office of Water, U.S. Environmental Protection
Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
(c) Before approving any application for an alternate test
procedure proposed by the responsible person or firm making the
discharge, the Regional Administrator shall forward a copy of the
application to the Alternate Test Procedure Program Coordinator, Office
of Science and Technology (4303), Office of Water, U.S. Environmental
Protection Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460.
(d) * * * Prior to the expiration of such ninety day period, a
recommendation providing the scientific and other technical basis for
acceptance or rejection will be forwarded to the Regional Administrator
by the Alternate Test Procedure Program Coordinator, Washington, DC. A
copy of all approval and rejection notifications will be forwarded to
the Alternate Test Procedure Program Coordinator, Office of Science and
Technology (4303), Office of Water, U.S. Environmental Protection
Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460, for the
purposes of national coordination.
(e) Approval for nationwide use. (1) As expeditiously as is
practicable after receipt by the Alternate Test Procedure Program
Coordinator, Washington, DC, of an application for an alternate test
procedure for nationwide use, the Alternate Test Procedure Program
Coordinator, Washington, DC, shall notify the applicant in writing
whether the application is complete. If the application is incomplete,
the applicant shall be informed of the information necessary to make
the application complete.
(2) As expeditiously as is practicable after receipt of a complete
package, the Alternate Test Procedure Program Coordinator shall perform
any analysis necessary to determine whether the alternate test
procedure satisfies the applicable requirements of this part, and the
Alternate Test Procedure Program Coordinator shall recommend to the
Administrator that he/she approve or reject the application and shall
also notify the application of the recommendation.
* * * * *
0
10. Section 136.6 is added to Part 136 to read as follows:
Sec. 136.6 Method Modifications and Analytical Requirements.
(a) Definitions of terms used in this Section.
(1) Analyst means the person or laboratory using a test procedure
(analytical method) in this Part.
(2) Chemistry of the Method means the reagents and reactions used
in a test procedure that allow determination of the analyte(s) of
interest in an environmental sample.
(3) Determinative Technique means the way in which an analyte is
identified and quantified (e.g., colorimetry, mass spectrometry).
(4) Equivalent Performance means that the modified method produces
results that meet the QC acceptance
[[Page 11240]]
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 (b)(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
[[Page 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
0
11. The authority citation for part 141 continues to read as follows:
Authority: 42 U.S.C. 300f, 300g-1, 300g-2, 300g-3, 300g-4, 300g-
5, 300g-6, 300j-4, 300j-9, and 300j-11.
0
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:
Sec. 141.21 Coliform sampling.
* * * * *
(f) * * *
(3) * * *
1* * * 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.
* * * * *
0
13. Section 141.23 is amended as follows:
0
a. In paragraph (a)(4)(i) by revising the table entries for
``Cyanide,'' ``Nitrate,'' and ``Nitrite''.
0
b. In paragraph (k)(1) by revising the table.
Sec. 141.23 Inorganic chemical sampling and analytical requirements.
* * * * *
(a) * * *
(4) * * *
(i) * * *
Detection Limits for Inorganic Contaminants
--------------------------------------------------------------------------------------------------------------------------------------------------------
Contaminant MCL (mg/L) Methodology Detection Limit (mg/L)
--------------------------------------------------------------------------------------------------------------------------------------------------------
* * * * * * *
Cyanide................................. 0.2 Distillation, Spectrophotometric3.................. 0.02
................................ Distillation, Automated, Spectrophotometric3....... 0.005
................................ Distillation, Amenable, Spectrophotometric4........ 0.02
................................ Distillation, Selective Electrode3, 4.............. 0.05
................................ UV, Distillation, Spectrophotometric9.............. 0.0005
................................ Micro Distillation, Flow Injection, 0.0006
Spectrophotometric3.
................................ Ligand Exchange with Amperometry4.................. 0.0005
* * * * * * *
Nitrate................................. 10 (as N) Manual Cadmium Reduction........................... 0.01
................................ Automated Hydrazine Reduction...................... 0.01
................................ Automated Cadmium Reduction........................ 0.05
................................ Ion Selective Electrode............................ 1
................................ Ion Chromatography................................. 0.01
................................ Capillary Ion Electrophoresis...................... 0.076
Nitrite................................. 1 (as N) Spectrophotometric................................. 0.01
................................ Automated Cadmium Reduction........................ 0.05
................................ Manual Cadmium Reduction........................... 0.01
................................ Ion Chromatography................................. 0.004
................................ Capillary Ion Electrophoresis...................... 0.103
* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
* * * * *
\3\ Screening method for total cyanides.
\4\ 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.
* * * * *
(k) * * *
(1) * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
SM \4\ (18th, SM \4\ (20th
Contaminant Methodology \13\ EPA ASTM \3\ 19th ed.) ed.) SM Online \22\ Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alkalinity................ Titrimetric...... ................ D1067-92, 02 B.. 2320 B......... 2320 B......... 2320 B-97...... ...............
Electrometric ................ ................ ............... ............... I-1030-85 \5\..
titration.
2. Antimony.................. Inductively 200.8 \2\
Coupled Plasma
(ICP)--Mass
Spectrometry.
Hydride-Atomic ................ D3697-92, 02....
Absorption.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ ................ 3113 B......... ............... 3113 B-99...... ...............
Absorption;
Furnace.
3. Arsenic \14\.............. Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma
\15\.
ICP-Mass 200.8 \2\
Spectrometry.
[[Page 11242]]
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ D2972-97, 03 C.. 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
Hydride Atomic ................ D2972-97, 03 B.. 3114 B......... ............... 3114 B-97......
Absorption.
4. Asbestos.................. Transmission 100.1 \9\
Electron
Microscopy.
Transmission 100.2 \10\
Electron
Microscopy.
5. Barium.................... Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic ................ ................ 3111D.......... ............... 3111 D-99......
Absorption;
Direct.
Atomic ................ ................ 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
6. Beryllium................. Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ D3645-97, 03 B.. 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
7. Cadmium................... Inductively 200.7 \2\
Coupled Plasma.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ ................ 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
8. Calcium................... EDTA titrimetric. ................ D511-93, 03 A... 3500-Ca D...... 3500-Ca B...... 3500-Ca B-97...
Atomic ................ D511-93, 03 B... 3111 B......... ............... 3111 B-99......
Absorption;
Direct
Aspiration.
Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
Ion ................ D6919-03........
Chromatography.
9. Chromium.................. Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ ................ 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
10. Copper................... Atomic ................ D1688-95, 02 C.. 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
Atomic ................ D1688-95, 02 A.. 3111 B......... ............... 3111 B-99......
Absorption;
Direct
Aspiration.
Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
ICP-Mass 200.8 \2\
spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
11. Conductivity............. Conductance...... ................ D1125-95 2510 B......... 2510 B......... 2510 B-97......
(Reapproved
1999) A.
12. Cyanide.................. Manual ................ D2036-98 A...... 4500-CN- C..... 4500-CN- C.....
Distillation
followed by
Spectrophotome ................ D2036-98 B...... 4500-CN- G..... 4500-CN- G..... 4500-CN- G-99..
tric,
Amenable.
Spectro- ................ D2036-98 A...... 4500-CN- E..... 4500-CN- E..... 4500-CN- E-99.. I-3300-85 \5\
photometric
Manual.
Spectro- 335.4 \6\
photometric
Semi-
automated.
Selective ................ ................ 4500-CN- F..... 4500-CN- F..... 4500-CN- F-99..
Electrode.
UV, Distillation, ................ ................ ............... ............... ............... Kelada-01 \17\
Spectrophotometr
ic.
Micro ................ ................ ............... ............... ............... QuikChem 10-204-
Distillation, 00-1-X \18\
Flow Injection,
Spectrophotometr
ic.
Ligand Exchange ................ D6888-04........ ............... ............... ............... OIA-1677, DW
and Amperometry \20\
\21\.
13. Fluoride................. Ion 300.0 \6\, 300.1 D4327-97, 03.... 4110 B......... 4110 B......... 4110 B-00......
Chromatography. \19\
Manual Distill.; ................ ................ 4500-F- B, D... 4500-F- B, D... 4500-F- B, D-97
Color. SPADNS.
Manual Electrode. ................ D1179-93, 99 B.. 4500-F- C...... 4500-F- C...... 4500-F- C-97...
Automated ................ ................ ............... ............... ............... 380-75WE \11\
Electrode.
Automated ................ ................ 4500-F- E...... 4500-F- E...... 4500-F- E-97... 129-71W \11\
Alizarin.
Capillary Ion ................ ................ ............... ............... ............... D6508, Rev. 2
Electrophoresis. \23\
14. Lead..................... Atomic ................ D3559-96, 03 D.. 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
ICP-Mass 200.8 \2\
spectrometry.
[[Page 11243]]
Atomic 200.9 \2\
Absorption;
Platform.
Differential ................ ................ ............... ............... ............... Method 1001
Pulse Anodic \16\
Stripping
Voltametry.
15. Magnesium................ Atomic Absorption ................ D511-93, 03 B... 3111 B......... ............... 3111 B-99......
ICP.............. 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Complexation ................ D511-93, 03 A... 3500-Mg E...... 3500-Mg B...... 3500-Mg B-97...
Titrimetric
Methods.
Ion ................ D6919-03........
Chromatography.
16. Mercury.................. Manual, Cold 245.1 \2\....... D3223-97, 02.... 3112 B......... ............... 3112 B-99......
Vapor.
Automated, Cold 245.2 \1\
Vapor.
ICP-Mass 200.8 \2\
Spectrometry.
17. Nickel................... Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ ................ 3111 B......... ............... 3111 B-99......
Absorption;
Direct.
Atomic ................ ................ 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
18. Nitrate.................. Ion 300.0 \6\ 300.1 D4327-97, 03.... 4110 B......... 4110 B......... 4110 B-00...... B-1011 \8\
Chromatography. \19\
Automated Cadmium 353.2 \6\....... D3867-90 A...... 4500-NO3- F.... 4500-NO3- F.... 4500-NO3- F-00.
Reduction.
Ion Selective ................ ................ 4500-NO3- D.... 4500-NO3- D.... 4500-NO3- D-00. 601 \7\
Electrode.
Manual Cadmium ................ D3867-90 B...... 4500-NO3- E.... 4500-NO3- E.... 4500-NO3- E-00.
Reduction.
Capillary Ion ................ ................ ............... ............... ............... D6508, Rev. 2
Electrophoresis. \23\
19. Nitrite.................. Ion 300.0 \6\ 300.1 D4327-97, 03.... 4110 B......... 4110 B......... 4110 B-00...... B-1011 \8\
Chromatography. \19\
Automated Cadmium 353.2 \6\....... D3867-90 A...... 4500-NO3- F.... 4500-NO3- F.... 4500-NO3- F-00.
Reduction.
Manual Cadmium ................ D3867-90 B...... 4500-NO3- E.... 4500-NO3- E.... 4500-NO3- E-00.
Reduction.
Spectrophotometri ................ ................ 4500-NO2- B.... 4500-NO2- B.... 4500-NO2- B-00.
c.
Capillary Ion ................ ................ ............... ............... ............... D6508, Rev. 2
Electrophoresis. \23\
20. Ortho-phosphate \12\..... Colorimetric, 365.1 \6\....... ................ 4500-P F....... 4500-P F.......
Automated,
Ascorbic Acid.
Colorimetric, ................ D515-88 A....... 4500-P E....... 4500-P E.......
ascorbic acid,
single reagent.
Colorimetric ................ ................ ............... ............... ............... I-1601-85 \5\
Phosphomolybdate
;
Automated- ................ ................ ............... ............... ............... I-2601-90 \5\
segmented flow;
Automated ................ ................ ............... ............... ............... I-2598-85 \5\
Discrete.
Ion 300.0 \6\....... D4327-97, 03.... 4110 B......... 4110 B......... 4110 B-00......
Chromatography. 300.1 \19\......
Capillary Ion ................ ................ ............... ............... ............... D6508, Rev. 2
Electrophoresis. \23\
21. pH....................... Electrometric.... 150.1, 150.2 \1\ D1293-95, 99.... 4500-H+ B...... 4500-H+ B...... 4500-H+ B-00...
22. Selenium................. Hydride-Atomic ................ D3859-98, 03 A.. 3114 B......... ............... 3114 B-97......
Absorption.
ICP-Mass 200.8 \2\
Spectrometry.
Atomic 200.9 \2\
Absorption;
Platform.
Atomic ................ D3859-98, 03 B.. 3113 B......... ............... 3113 B-99......
Absorption;
Furnace.
23. Silica................... Colorimetric, ................ ................ ............... ............... ............... I-1700-85 \5\
Molybdate Blue.
Automated- ................ ................ ............... ............... ............... I-2700-85 \5\
segmented
Flow.
Colorimetric..... ................ D859-94, 00.....
Molybdosilicate.. ................ ................ 4500-Si D...... 4500-SiO2 C.... 4500-SiO2 C-97.
Heteropoly blue.. ................ ................ 4500-Si E...... 4500-SiO2 D.... 4500-SiO2 D-97.
Automated for ................ ................ 4500-Si F...... 4500-SiO2 E.... 4500-SiO2 E-97.
Molybdate-
reactive Silica.
Inductively 200.7 \2\....... ................ 3120 B......... 3120 B......... 3120 B-99......
Coupled Plasma.
24. Sodium................... Inductively 200.7 \2\
Coupled Plasma.
Atomic ................ ................ 3111 B......... ............... 3111 B-99......
Absorption;
Direct
Aspiration.
Ion ................ D6919-03........
Chromatography.
25. Temperature.............. Thermometric..... ................ ................ 2550........... 2550........... 2550-00........
26. Thallium................. ICP-Mass 200.8 \2\
Spectrometry.
[[Page 11244]]
Atomic 200.9 \2\ ......
Absorption;
Platform.
--------------------------------------------------------------------------------------------------------------------------------------------------------
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. 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 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.
\1\ ``Methods for Chemical Analysis of Water and Wastes,'' EPA/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.
\3\ Annual 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.
\4\ 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 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.
\5\ Method I-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 I-1030-85; I-1601-85; I-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.
\6\ ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93/100, August 1993. Available at NTIS, PB94-120821.
\7\ The 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.
\8\ 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 Corporation, Technical Services Division, 34 Maple Street, Milford, MA 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
\9\ 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.
\10\ Method 100.2, ``Determination of Asbestos Structure Over 10-[mu]m 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 Wastewater,'' December 1972, and Method No. 380-75WE, ``Fluoride in Water and Wastewater,''
February 1976, Technicon Industrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089.
\12\ Unfiltered, no digestion or hydrolysis.
\13\ 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 pneumatic 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 multiple in-furnace depositions are made.
\14\ If 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 [mu]L 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.
\15\ Starting 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 for 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.
\16\ The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018. Or from
the Hach Company, P.O. Box 389, Loveland, CO 80539.
\17\ The description for the Kelada-01 Method, ``Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate,'' Revision
1.2, August 2001, EPA 821-B-01-009 for cyanide is available from the National Technical Information Service (NTIS), PB 2001-108275, 5285
Port Royal Road, Springfield, VA 22161. 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.
\18\ 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 Rd., Milwaukee, WI 53218. Telephone: 414-358-4200.
\19\ ``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.
\20\ Method 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 OI Analytical, 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 interference is present, and treat samples accordingly.
\22\ 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.
\23\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and
Chromate Electrolyte,'' available from Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
* * * * *
0
14. Section 141.24 is amended as follows:
0
a. By revising the introductory text of paragraph (e)(1).
0
b. By revising entries 23, 24, 26, 30, 49, and 50 in the table to
paragraph (e)(1).
0
c. By adding a new footnote 5 to the table to paragraph (e)(1).
Sec. 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.
[[Page 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.
----------------------------------------------------------------------------------------------------------------
Standard
Contaminant EPA Method1 Methods ASTM Other
----------------------------------------------------------------------------------------------------------------
* * * * * * *
23. 2,4-D 4 (as acids, salts, 515.2, 555, 515.1, ........... D5317-93, 98
and esters). 515.3, 515.4. (Reapproved 2003).
24. 2,4,5-TP \4\ (Silvex)..... 515.2, 555, 515.1, ........... D5317-93, 98
515.3, 515.4. (Reapproved 2003).
* * * * * * *
26. Atrazine 2................ 507, 525.2, 508.1, 505, ........... ...................... Syngenta 5 AG-625
551.1.
* * * * * * *
30. Dalapon................... 552.1 515.1, 552.2,
515.3, 515.4, 552.3.
* * * * * * *
49. Pentachlorophenol......... 515.2, 525.2, 555, ........... D5317-93, 98
515.1, 515.3, 515.4. (Reapproved 2003).
50. Picloram 4................ 515.2, 555, 515.1, ........... D5317-93, 98
515.3, 515.4. (Reapproved 2003).
* * * * * * *
----------------------------------------------------------------------------------------------------------------
\1\ For previously approved EPA methods which remain available for compliance monitoring until June 1, 2001, see
paragraph (e)(2) of this section.
\2\ Substitution of the detector specified in Method 505, 507, 508, or 508.1 for the purpose of achieving lower
detection limits is allowed as follows: Either an electron capture or nitrogen phosphorus detector may be used
provided all regulatory requirements and quality control criteria are met.
* * * * *
\4\ Accurate 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).
\5\ 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) (in other words, greater than 0.0015mg/L
or 1.5 [mu]g/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.
* * * * *
0
15. Section 141.25 is amended by revising the table in paragraph (a) to
read as follows:
Sec. 141.25 Analytical methods for radioactivity.
(a) * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (Method of Page Number)
---------------------------------------------------------------------------------------------------------
Contaminant Methodology EPA
EPA \1\ \2\ EPA \3\ EPA \4\ SM \5\ ASTM \6\ USGS \7\ DOE \8\ Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Naturally Occurring:
Gross alpha \11\ and beta Evaporation.... 900.0 p. 1.. 00-01... p. 1...... 302, 7110 B, .......... R-1120-76....
7110 B-00.
Gross alpha \11\......... Coprecipitation ......... ...... 00-02... .......... 7110 C, 7110 C-
00.
[[Page 11246]]
Radium 226............... Radon emanation 903.1 p. 16. Ra-04... p. 19..... 305, 7500-Ra D3454-97.. R-1141-76.... Ra-04..... NY \9\,
C, 7500-Ra C-
01.
Radiochemical.. 903.0 p. 13. Ra-03... .......... 304, 7500-Ra D2460-97.. R-1140-76.... .......... GA \14\
B, 7500-Ra B-
01.
Radium 228............... Radiochemical.. 904.0 p. 24. Ra-05... p. 19..... 7500-Ra D, .......... R-1142-76.... .......... NY \9\,
7500-Ra D-01. NJ \10\,
GA \14\
Uranium \12\............. Radiochemical.. 908.0 ...... ........ .......... 7500-U B, 7500-
U B-00.
Fluorometric... 908.1 ...... ........ .......... 7500-U C (17th D2907-97.. R-1180-76, R- U-04......
Ed.). 1181-76.
ICP-MS......... 200.8 ...... ........ .......... 3125.......... D5673-03..
\13\
Alpha ......... ...... 00-07... p. 33..... 7500-U C D3972-97, R-1182-76.... U-02......
Spectrometry. (18th, 19th, 02.
or 20th Ed.),
7500-U C-00.
Laser ......... ...... ........ .......... .............. D5174-97,
Phosphorimetry. 02.
Man-Made:
Radioactive Cesium....... Radiochemical.. 901.0 p. 4.. ........ .......... 7500-Cs B, D2459-72.. R-1111-76....
7500-Cs B-00.
Gamma Ray 901.1 ...... ........ p. 92..... 7120, 7120-97. D3649-91, R-1110-76.... 4.5.2.3...
Spectrometry. 98a.
Radioactive Iodine....... Radiochemical.. 902.0 p. 6.. ........ .......... 7500-I B, 7500-
I B-00.
p. 9.. ........ .......... 7500-I C, 7500-
I C-00.
7500-I D, 7500- D3649-91,
I D-00. 98a.
Gamma Ray 901.1 ...... ........ p. 92..... 7120, 7120-97. D4785-93, ............. 4.5.2.3...
Spectrometry. 00a.
Radioactive Strontium 89, Radiochemical.. 905.0 p. 29. Sr-04... p. 65..... 303, 7500-Sr .......... R-1160-76.... Sr-01, Sr-
90. B, 7500-Sr B- 02.
01.
Tritium.................. Liquid 906.0 p. 34. H-02.... p. 87..... 306, 7500-\3\ D4107-91, R-1171-76....
Scintillation. H B, 7500-\3\ 98
H B-00. (Reapprov
ed 2002).
Gamma Emitters........... Gamma Ray 901.1 ...... ........ p. 92..... 7120, 7120-97. D3649-91, R-1110-76.... Ga-01-R...
Spectrometry. 98a.
902.0 ...... ........ .......... 7500-Cs B, D4785-93,
7500-Cs B-00. 00a.
901.0 ...... ........ .......... 7500-I B, 7500-
I B-00.
--------------------------------------------------------------------------------------------------------------------------------------------------------
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 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://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
\1\ ``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 Information 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, ibid.
\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 Wastewater,'' 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-I C, 7500-I D, 7500-Sr B, and 7500-\3\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 7500-\3\H B-00 are available online 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.
\6\ 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 Geological Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal
Center, Denver, CO 80225-0425.
\8\ ``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 Ga-01-R is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S. Department of 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 Department of 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 Ewing 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\ If uranium (U) is determined by mass, a 0.67 pCi/[mu]g of uranium conversion 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 Metals in Environmental Samples--Supplement I,'' ' EPA 600-R-94-111, May 1994. Available at NTIS, PB 95-125472.
[[Page 11247]]
\14\ ``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. 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 radium-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.
* * * * *
0
16. Section 141.74 is amended as follows:
0
a. By revising the entry for turbidity in the table in paragraph
(a)(1).
0
b. By revising footnotes 1, 8, 10, 11, and 12 to the table in paragraph
(a)(1).
0
c. By adding footnote 13 to the table in paragraph (a)(1).
0
d. By revising paragraph (a)(2).
Sec. 141.74 Analytical and monitoring requirements.
(a) * * *
(1) * * *
----------------------------------------------------------------------------------------------------------------
Organism Methodology Citation \1\
----------------------------------------------------------------------------------------------------------------
* * * * * * *
Turbidity \13\........................... Nephelometric Method............. 2130 B
Nephelometric Method............. 180.1 \9\
Great Lakes Instruments.......... Method 2 \10\
Hach FilterTrak.................. 10133 \12\
----------------------------------------------------------------------------------------------------------------
* * * * *
\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 published 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 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.
* * * * *
\8\ A-1 broth may be held up to 7 days in a tightly closed screw cap tube at 4 [deg]C.
\9\ ``Methods for the Determination of Inorganic Substances in Environmental Samples,'' EPA/600/R-93/100, August
1993. Available at NTIS, PB94-121811.
\10\ GLI Method 2, ``Turbidity,'' November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street,
Milwaukee, WI 53223.
\11\ A 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.
\13\ Styrene divinyl benzene beads (e.g. AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g. Hach StablCal
TM or equivalent) are acceptable 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 (HOCl- and OCl-) 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 Methodology SM \1\ SM Online \2\ Other
----------------------------------------------------------------------------------------------------------------
Free Chlorine............... Amperometric 4500-Cl D...... 4500-Cl D-00... D1253-03 \3\
Titration.
DPD Ferrous 4500-Cl F...... 4500-Cl F-00...
Titrimetric.
DPD Colorimetric.... 4500-Cl G...... 4500-Cl G-00...
Syringaldazine 4500-Cl H...... 4500-Cl H-00...
(FACTS).
Total Chlorine.............. Amperometric 4500-Cl D...... 4500-Cl D-00... D1253-03 \3\
Titration.
Amperometric 4500-Cl E...... 4500-Cl E-00...
Titration (low
level measurement).
DPD Ferrous 4500-Cl F...... 4500-Cl F-00...
Titrimetric.
DPD Colorimetric.... 4500-Cl G...... 4500-Cl G-00...
Iodometric Electrode 4500-Cl I...... 4500-Cl I-00...
Chlorine Dioxide............ Amperometric 4500-ClO2 C.... 4500-ClO2 C-00.
Titration.
DPD Method.......... 4500-ClO2 D....
Amperometric 4500-ClO2 E.... 4500-ClO2 E-00.
Titration.
Spectrophotometric.. ............... ............... 327.0, Revision 1.1 \4\
Ozone....................... Indigo Method....... 4500-O3 B...... 4500-O3 B-97 ..
----------------------------------------------------------------------------------------------------------------
\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.
\2\ 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.
\3\ Annual 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.
\4\ EPA Method 327.0, Revision 1.1, ``Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using
Lissamine Green B and Horseradish 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.
[[Page 11248]]
* * * * *
PART 143--NATIONAL SECONDARY DRINKING WATER REGULATIONS
0
17. The authority citation for part 143 continues to read as follows:
Authority: 42 U.S.C. 300f et seq.
0
18. Section Sec. 143.4 is amended by revising the table in paragraph
(b) to read as follows:
Sec. 143.4 Monitoring.
* * * * *
(b) * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
SM \4\ 18th and
Contaminant EPA ASTM \3\ 19th ed. SM \4\ 20th ed. SM \7\ Online Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aluminum..................... 200.7 \2\ .................... 3120 B............. 3120 B............. 3120 B-99.........
200.8 \2\ .................... 3113 B............. ................... 3113 B-99.........
200.9 \2\ .................... 3111 D............. ................... 3111 D-99.........
2. Chloride..................... 300.0 D4327-97, 03........ 4110 B............. 4110 B............. 4110 B-00.........
\1\,
300.1 \6\
4500-Cl D......... 4500-Cl D......... 4500-Cl D-97.....
D512-89 (Reapproved 4500-Cl B......... 4500-Cl B......... 4500-Cl B-97.....
1999) B.
D6508, Rev. 2 \8\
3. Color........................ ......... .................... 2120 B............. 2120 B............. 2120 B-01.........
4. Foaming Agents............... ......... .................... 5540 C............. 5540 C............. 5540 C-00.........
5. Iron......................... 200.7 \2\ .................... 3120 B............. 3120 B............. 3120 B-99.........
200.9 \2\ .................... 3111 B............. ................... 3111 B-99.........
.................... 3113 B............. ................... 3113 B-99.........
6. Manganese.................... 200.7 \2\ .................... 3120 B............. 3120 B............. 3120 B-99.........
200.8 \2\ .................... 3111 B............. ................... 3111 B-99.........
200.9 \2\ .................... 3113 B............. ................... 3113 B-99.........
7. Odor......................... .................... 2150 B............. 2150 B............. 2150 B-97.........
8. Silver....................... 200.7 \2\ .................... 3120 B............. 3120 B............. 3120 B-99. I-3720-85 \5\
200.8 \2\ .................... 3111 B............. ................... 3111 B-99.........
200.9 \2\ .................... 3113 B............. ................... 3113 B-99.........
9. Sulfate...................... 300.0 D4327-97, 03........ 4110 B............. 4110 B............. 4110 B-00.........
\1\,
300.1 \6\
375.2 \1\ .................... 4500-SO4 \2\ F.... 4500-SO4 \2\ F....
4500-SO4 \2\ C, D. 4500-SO4 \2\ C, D.
D516-90, 02......... 4500-SO4 \2\ E.... 4500-SO4 \2\ E....
D6508, Rev. 2 \8\
10. Total Dissolved Solids...... .................... 2540 C............. 2540 C............. 2540 C-97.........
11. Zinc........................ 200.7 \2\ .................... 3120 B............. 3120 B............. 3120 B-99.........
200.8 \2\ .................... 3111 B............. ................... 3111 B-99.........
--------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents 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 Avenue, NW., Room 3334, Washington, DC (Telephone: 202-566-2426); or at the
National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
\1\ ``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 of 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 Harbor Drive, West Conshohocken, PA 19428.
\4\ 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 published in 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.
\5\ Method 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.
\6\ ``Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,'' Vol. 1, EPA 815[dash]R-00-014, August 2000. Available at
NTIS, PB2000-106981.
\7\ 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.
\8\ Method D6508, Rev. 2, ``Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and
Chromate Electrolyte,'' available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482-2131, Fax: 508/482-3625.
PART 430--THE PULP, PAPER, AND PAPERBOARD POINT SOURCE CATEGORY
0
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).
0
20. Section 430.02 is amended by adding paragraph (g) to read as
follows:
Sec. 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
0
21. The authority citation for Part 455 continues to read as follows:
Authority: Secs. 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).
0
22. Section 455.50 is revised to read as follows:
Sec. 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
[[Page 11249]]
Table IB, Table IC, 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 136.3(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.
0
23. Part 455 is amended by removing and reserving Table 7 to Part 455.
PART 465--COIL COATING POINT SOURCE CATEGORY
0
24. The authority citation for Part 465 continues to read as follows:
Authority: Secs. 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.
0
25. Section 465.03 is amended by revising paragraph (c) to read as
follows:
Sec. 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 136.3(a), Table IB and must be used after
December 31, 2005.
* * * * *
[FR Doc. 07-1073 Filed 3-9-07; 8:45 am]
BILLING CODE 6560-50-P